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FIELD OF THE INVENTION
[0001] The present invention generally relates to a foldable box. More particularly, the present invention relates to a box that is stored flat and folds into a three-dimensional box.
BACKGROUND OF THE INVENTION
[0002] Boxes are used everyday for many purposes. They are used for storage, shipping and even gift-giving. Because of the variety of uses, boxes come in a variety of sizes and shapes. From boxes that hold a small piece of jewelry to ones that hold refrigerators.
[0003] But when a box is manufactured by a manufacturing company the box is usually shipped in a three-dimensional form. The manufacturing company than must pay for additional shipping cost for empty space within the box. Additionally, the boxes are also more susceptible to damage when shipped in this fashion.
[0004] To overcome these shipping problems, box designers have made collapsible boxes. These boxes are shipped flat and need to be constructed by the ultimate user of the box.
[0005] To construct these boxes, the user must unfold the box and place certain folds into certain slots, or in the alternative use glue or tape. These actions are time consuming and labor intensive. Stores must pay for this extra time to construct these boxes. The consumer at the store also has a delay because the boxes will usually be constructed in front of the consumer. This delay results in loss time for all parties involved.
[0006] Some stores in order not to delay the customer may employ extra personnel to build boxes. This, however, does not alleviate all of the stores problems because now the store must find space to store the boxes in their three-dimensional form. This means there will be less space for the products in which they stock.
SUMMARY OF THE INVENTION
[0007] The present invention overcomes the problem of the conventional art by constructing a foldable box that is stored in a flat position. In order to fold the box into a three dimensional position, all a user must do is unfold one piece of the box which will in turn construct the whole box.
[0008] Foldable boxes of this sort comprise a bottom panel, a plurality of sides panels, and at least four connectors having a first portion and a second portion whereby the first portion of each connector is foldably connected to a side panel. The second portion of each connector is then adhered to a second side panel with the first and second side panels being adjacent to one another.
[0009] Furthermore, all of the side panels have a bottom edge. The bottom edge of the side panels are foldably connected to said bottom panel.
[0010] The box also has a holding means for holding the foldable box in a constructed form. The holding means can be placed on an inner corner of said side panels. The inner corner being between the adhered connector and the edge of said side panel. The holding means may be a peelable adhesive or Velcro strip or any other device which will serve the same purpose.
[0011] In another embodiment, the foldable box comprises a bottom panel, a cover, a retaining lip, a plurality of sides panels and at least four connectors with the connectors having a first portion and a second portion. The first portion of each connector is foldably connected to a first side panel. The second portion of said each connector is adhered to a second side panels. The first and second side panels being adjacent to one another.
[0012] The side panels have a bottom edge. The bottom edge of the side panels are foldably connected to said bottom panel. The cover is foldably connected to a top of one of said side panels. A lip is foldably connected to the cover opposite to the side panel foldably connected to the cover.
[0013] To place the box in a closed constructed position the cover is placed on a top portion of the sides. The lip then falls onto the entire side panel opposite to the side panel foldably connected to the cover and is locked into place.
[0014] A holding means is then placed on an inner corner of said side panels. The inner corner being between the adhered connector and the edge of said side panel. The holding means can be a peelable adhesive or Velcro strip.
[0015] The holding means may also be a foldable member located on one of said side panels.
[0016] In a third embodiment, the foldable box comprises a bottom panel, a plurality of side panels, a first connector, a second connector, a cover and a cover connector.
[0017] The plurality of side panels consist of a front panel, a back panel, a left panel and a right panel, and each side panel consists of a left portion, a right portion, a top portion and a bottom portion.
[0018] The connectors each have a first portion and a second portion. The first portion of the first connector foldably connects to the bottom portion of said left panel and is substantially adhered to the bottom panel. The second portion foldably connects to the bottom of the front panel and the bottom.
[0019] The first portion of the second connector foldably connects the bottom of the back panel and the bottom of the right panel. The sides are each connected to each other on the right and left portions, respectively.
[0020] To construct box from a flat position to a working position a user pulls the sides to an upright position and folds the cover on tops of the sides.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The following description of preferred embodiments of the present invention will be better understood when read in conjunction with the appended drawings. It should be understood, however, that the invention is not limited to the precise arrangements shown.
[0022] FIG. 1 is a perspective view of the first embodiment of the present invention in its constructed form;
[0023] FIG. 2 is a top view of the first embodiment of the present invention in its constructed form;
[0024] FIG. 3 is a perspective view of the first embodiment of the present invention in its transition from a flat unfolded box to its constructed form;
[0025] FIG. 4 is a top view of the first embodiment of the present invention in its flat, unfolded form;
[0026] FIG. 5 is a top view of the second embodiment of the present invention in its flat, unfolded form;
[0027] FIG. 6 is a perspective view of the second embodiment of the present invention in its transition from a flat unfolded box to its constructed form;
[0028] FIG. 7 is a perspective view of the second embodiment of the present invention in its constructed form;
[0029] FIG. 8 is a top view of the third embodiment of the present invention in its flat, unfolded form;
[0030] FIG. 9 is a perspective view of the third embodiment of the present invention in its transition from a flat unfolded box to its constructed form; and
[0031] FIG. 10 is a perspective view of the third embodiment of the present invention in its constructed form.
[0032] FIG. 11 is a top view of the third embodiment of the present invention in its folded state.
[0033] FIG. 12 is a bottom view of the third embodiment of the present invention in its folded state.
DETAILED DESCRIPTION
[0034] Manufactures of boxes often run in to difficulty when shipping boxes because of the way in which they are shipped. To cut down on shipping cost it is more cost efficient to ship boxes in a flat position. However, flat boxes must be assembles to the party it is shipped to. This takes time on the part of the ultimate user.
[0035] To cut down on this time, a box can be constructed in such a way as to make the assembly time to construct a box minimal. This is accomplished by having foldable connectors attached to certain parts of the box. When the box is flat the connectors are also flat. To construct a box a user must only lift one part of the box. This triggers a chain reaction and as the user pulls the part the connectors in turn pull other parts of the box. The box is then fully three dimensional with minimal work on the part of the user. The user will not have to add any additional glue or tape to the box.
[0036] The boxes may be constructed out of any material that may be foldably connected such as all types of cardboard and flexible plastics. The material may also be decorated so the box is aesthetically pleasing to the eye. This is accomplished by lining the material with certain types of laminate and cloth-like materials.
[0037] FIG. 1 is one embodiment of the present invention. In FIG. 1 , the box 10 is in its three-dimensional form. The box has a cover 11 that is foldably connected to an outside connector 12 at crease 13 . The outside connector is also foldable connected to the bottom of the box (not shown) at crease 22 .
[0038] The boxes have a right side 14 , a front side 15 , a left side 16 and a rear side 21 . Right side 14 is foldable connected to front side 15 at crease 23 . Front side 15 is foldable connected to left side 16 at crease 26 . Left side 16 is foldable connected to rear side 21 at crease 22 . Rear side 21 is foldably connected to right side 14 at crease 24 .
[0039] The box also has a front connector 26 having portions 17 and 18 and rear connector having portions 19 and 20 . Portion 18 of the front connector is adhered to the bottom of the box and is foldably connected to the bottom of the left side 16 . Portion 17 is foldable connected to portion 18 and the bottom side of the front side 17 .
[0040] The rear connector 27 is connected between the bottom of back side 21 and the bottom of right side 14 . The rear connector is folded in two parts at crease 25 .
[0041] FIG. 1 shows the box in its constructed form with the sides 14 , 15 16 and 21 in an upright position. The connectors 26 and 27 are on top of the bottom portion not allowing the bottom to visible.
[0042] FIG. 2 shows the foldable box 10 from a top view in its constructed position. From this view point, the bottom of the box is split into four sections. Sections 17 and 18 represent one connector 26 and sections 19 and 20 represent the second connector 27 . These connectors 26 and 27 when in their unfolded state cover the entire bottom layer of the box.
[0043] The cover is connected to connector 12 at crease 13 . If a user wanted to close the box 10 . The user will lift the cover 11 and fold the cover over the opening created by sides 14 , 15 , 16 and 21 . The connector 12 then rests on side 21 .
[0044] FIG. 3 shows the box in use as the box is folded from a flat state to a box shape. The sides 14 , 15 , 16 and 21 are shown. These sides are all interconnected as discussed above.
[0045] The connector 18 is adhered to the bottom of the box 30 and is connected to side 15 at crease 31 . The other portion of connector 26 is connected to the bottom of side 14 .
[0046] Connector 27 is connected to the bottom of side 16 and 21 . The connector 27 while opening forms a triangular shape.
[0047] The bottom 30 , cover 11 and connector 12 all remain flat while the sides of the box are formed.
[0048] FIG. 4 shows the box in its flat position. Sides 14 and 15 are visible from the top. While sides 16 and 21 are covered by sides 14 and 15 .
[0049] Connectors 26 and 27 are also folded so as to form two triangular areas.
[0050] FIG. 5 is another embodiment of the foldable box. This foldable box 50 has a cover which is separately assembled and is not foldably connected to the box.
[0051] In this embodiment the box 50 has a bottom 51 and four sides 52 , 53 , 54 and 55 . The sides 52 , 53 , 54 and 55 are foldably connected to the bottom by four connectors 56 , 57 , 58 , 59 located in the corners of the box.
[0052] FIG. 6 shows the box in a partially assembled state. Here, sides 52 and 54 are connected to the bottom at crease. Sides 52 and 54 are also connected to the bottom at crease 60 and 61 .
[0053] Also shown are the four connectors 56 - 59 . These connectors 56 - 59 are foldably attached to the edge of each side. That is, side 52 is attached to side 53 by connector 56 . Side 53 is attached to side 54 by connector 57 . Side 54 is attached to side 55 by connector 58 . Side 55 is attached to side 52 by connector 59 .
[0054] Also shown on sides 52 and 54 are additional means 64 for ensuring that the sides of the box are tightly in place. This makes sure that when a user folds the box 50 , the box 50 will not inadvertently collapse while in use.
[0055] The additional means 64 can be an adhesive, tape or Velcro strip. This additional means 64 is already in place when a user assembles the box. The user does not need any additional items to make the box.
[0056] A securing means (not shown) can also be attached to a side of the box as will be discussed in detail in FIGS. 8-10 . This securing means adds additional strength to the box when the box is constructed by a user. That is, when the sides are in their upright position the securing means ensures the box will not collapse when the box is in use.
[0057] FIG. 7 shows the box in its constructed state. The sides 52 - 55 are in their upright position with the bottom face down. The additional securing means 64 are not visible when the box 50 in its constructed state.
[0058] FIG. 8 shows a third embodiment of the present invention. In this embodiment the sides 81 - 84 and the bottom 92 are constructed as in the second embodiment. However, in this embodiment the cover 89 is integrated into the construction of the box 80 . During shipping, when the box 80 is in its flat state, the cover 89 , lip 90 and securing panel 92 may be turned and stored against the bottom portion of the box 80 , as shown below in FIGS. 11 and 12 .
[0059] In this embodiment, sides 81 - 84 are constructed with cover 89 being foldably attached to side 82 at crease 93 . Side 84 has a magnet 102 that is found beneath the surface of side 84 . The magnet 102 is attractive on both sides of side 84 . That is, the attractive side of the magnet 102 is used on the inside of the box and the outside of the box when the box is in its constructed state.
[0060] Additionally, cover 89 is attached to lip 90 . Lip 90 secures the cover 89 to the constructed box 80 at side 84 when the box is in a constructed state. Under the surface of the lip 90 is a magnet 100 . (Please note, all the magnets 100 , 102 , and 103 of this embodiment are about one inch in length and about ¼ to one inch in height.) Magnet 100 is secured to magnet 102 when the box is in a constructed state. Therefore, when the box is in a closed position magnet 100 will be attracted to magnet 102 , thereby locking the cover to the box.
[0061] A securing panel 91 is attached to side 84 at crease 94 . This securing panel 91 adds additional strength to the box when the box 80 is constructed by a user. That is when the sides 81 - 84 are in their upright position the securing panel 91 is placed between sides 81 and 83 and is pressed flush against side 84 . This ensures box 80 will not collapse when the box 80 is in use. The securing panel 91 also has a magnet 103 beneath its surface. The magnet has the same attractive pole as found in magnet 100 and magnet 103 is attracted to magnet 102 when the securing panel is placed in its constructed state.
[0062] The securing panel 91 also has a ribbon, string or any other material 104 used to pull the securing panel 91 from either its collapse state or constructed state. For example, to unfold the box, a user pulls ribbon 104 thereby lifting securing panel 91 away from side 84 . Once the securing panel is clear of sides 81 and 83 , sides 81 and 83 can be folded inwardly thereby collapsing the box.
[0063] In another embodiment, the box may also include additional means 95 for ensuring that the sides of the box are tightly in place. The additional means 95 can be an adhesive, tape or Velcro strip. This additional means 95 is already in place when a user assembles the box. The user does not need any additional items to make the box.
[0064] FIG. 9 shows the third embodiment in a transition state between folded and unfolded. The box 80 as it is being lifted from its unfolded state will raise the sides 81 - 84 of the box 80 .
[0065] FIG. 10 shows the box 80 with the sides 81 - 84 raised. To fully close the box 80 , the cover 89 is thrown over the open area created by sides 81 - 84 . The cover 80 is then secured by the use of locking means 94 such as the magnets explained above. However, other types of locking means such as snaps may be placed on the lip and the sides to lock the cover 89 in place.
[0066] FIG. 11 shows the top view of the collapsed box 80 . From this view it is shown that sides 84 and 82 are folded on top of bottom 92 , and sides 81 and 84 folded on top of sides 82 and 84 .
[0067] FIG. 12 shows the underside of the collapsed box 80 . From this view, the top 89 is folded and pressed against bottom 92 of the box 80 . The lip 90 projects straight out from the cover and also is pressed against bottom 92 .
[0068] The securing panel 91 is folded so that the securing panel is flush against side 84 . (Crease 94 allows the securing panel 360 degrees of rotation.) The top portion of the securing panel slightly touching the top position of lip 90 . Between the securing panel 91 and lip 90 is ribbon 104 . The ribbon 104 protrudes from the unconstructed box and allows a user to unfold the box by pulling on ribbon 104 . This action raises the securing panel from the collapsed position. Once the securing panel 91 is raised, a user can easily lift the lip 90 and cover 89 away from the bottom 92 thus making the construction the box a simple operation.
[0069] In this specification, the invention has been described with reference to specific exemplary embodiments thereof. However it is evident that various modifications and changes may be made thereto without departing from the broader spirit and scope of the invention as set forth in the claims that follow. The specification and drawings are accordingly to be regarded in an illustrative manner rather than a restrictive sense.
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A foldable box that includes a bottom panel, four sides panels and connectors with each connectors having a first portion and a second portion. The first portion of the connector is foldably connected to a side panel and the second connector is adhered to another side panel, these panels being adjacent to each other. The above connector placement allows a user to transform a box from an unfolded first position to a folded second position in one easy step. The box is then secured in this position by means of a holding member, such as, an adhesive, Velcro, magnets or a folding member.
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This application is a division of commonly-assigned U.S. patent application Ser. No. 10/846,731, filed May 13, 2004 now U.S. Pat. No. 7,135,904, which claims the benefit of U.S. Provisional Application No. 60/535,907, filed Jan. 12, 2004, each of which is hereby incorporated by reference herein in its entirety.
BACKGROUND OF THE INVENTION
This invention relates to circuitry and methods for causing a signal to jitter, e.g., to facilitate testing of the jitter-tolerance of circuitry receiving the signal.
An example of circuitry that may need to be tested for jitter-tolerance is serializer/deserializer (SERDES) circuitry. SERDES circuitry may be used in a transmitter for converting data supplied as a succession of parallel words to a continuous stream of serial bits. Circuitry that receives this serial data signal may use another SERDES to recover the successive bits from the received signal and reassemble those bits into successive parallel words for further processing. Clock data recovery (CDR) techniques may be used as part this data recovery operation. (The term “words” is used herein to mean any plural number of bits that may be treated as a significant unit of information. For example, a word may be eight bits; but a word can also be any other plural number of bits such as ten bits or 16 bits. There is no special significance to the use of the term word herein, and other terms such as nibble, byte, or group could have been used instead with no change in scope or coverage.)
In real-world applications the serial data signal received by a receiver is rarely, if ever, perfect. One of its imperfections may be jitter. Jitter is variation in the timing of transitions in the binary level of the received signal. Such transitions should occur only at boundaries between unit intervals (UIs) in the data signal. A UI is the time duration of any one bit in the data signal. It is not necessary for the data signal to transition after each UI; but when a transition does occur, it should be at the end of one UI and the start of the next UI. Because the UI is a fixed amount of time, transitions in the received serial data signal should occur only at certain times relative to one another (i.e., integer multiples of the UI). This fact may be used by a SERDES to help it synchronize its operations (e.g., its data recovery operations) to the incoming serial data signal. However, jitter can cause the timing of transitions in the received data signal to deviate from proper timing. For example, jitter can cause a transition in the received data signal to be delayed by some fraction of a UI, or to occur earlier than it should by some fraction of a UI. A SERDES should be able to tolerate some amount of jitter without losing its ability to correctly recover received serial data.
Known automatic test equipment (ATE) for production testing is not well adapted to producing serial data signals with jitter to facilitate production testing of the jitter tolerance of SERDES or other receiver circuitry. It would therefore be desirable to provide circuitry and methods for facilitating the use of automatic test equipment to test the jitter tolerance of circuitry such as SERDES circuitry.
SUMMARY OF THE INVENTION
In accordance with this invention, jitter can be added to a serial data signal by adding jitter to the clock signal that is used as the time base for the data signal. Jitter may be added to the clock signal by delaying that signal by a time-varying amount. In the presently preferred embodiments, the amount of this delay varies cyclically over time. The frequency of this cyclical variation may be controllable to allow variation of the frequency of the jitter. Alternatively or in addition, the maximum amount of the time delay variation may be controllable to allow variation of the magnitude or amplitude of the jitter. The data signal to which jitter has been added can be used to test the jitter-tolerance of circuitry that receives and must recover data from that signal. For example, circuitry for adding jitter to a data signal can be included in devices that are going to be tested (e.g., production-tested) using automatic test equipment (ATE). Such a device can then be tested using ATE and can itself generate a data signal having jitter for use in testing other components of the device (or other devices). Modification of the ATE is not required. The invention can be implemented in apparatus and/or method embodiments.
Further features of the invention, its nature and various advantages, will be more apparent from the accompanying drawings and the following detailed description of the preferred embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified block diagram of an illustrative embodiment of circuitry constructed in accordance with the invention.
FIG. 2 is an illustrative graph of circuit operation information that is useful in explaining certain aspects of the invention.
FIG. 3 is an illustrative graph of signal information that is useful in explaining certain aspects of the invention.
FIG. 4 is a graph showing illustrative modification of the FIG. 3 signal information in accordance with the invention.
FIG. 5 is similar to FIG. 2 , but is redrawn in relationship to FIG. 4 .
DETAILED DESCRIPTION
FIG. 1 shows an illustrative embodiment in which the invention is implemented largely as self-test circuitry that has been included in a device under test (DUT) 10 . DUT 10 may also include other conventional circuitry that is not shown in FIG. 1 ; and that other circuitry can be of many different types and/or forms. Later it will be explained that implementing the invention as self-test circuitry is only one of many possibilities, and that the invention can be alternatively implemented in other ways and in other contexts if desired. For example, circuitry of the type shown in FIG. 1 (or at least the transmitter portion of that circuitry) can become part of test equipment (e.g., ATE) for use in testing the jitter tolerance of other devices.
In the illustrative embodiment shown in FIG. 1 , DUT 10 includes four SERDES circuits 20 -A 1 , 20 -A 2 , 20 -B 1 , and 20 -B 2 , each of which can be conventional. Each SERDES circuit 20 receives a clock signal 22 -A or 22 -B, and may use the clock signal it receives to synchronize data output or transmitter operations of the SERDES. Such transmitter operations may include converting successive words of parallel data to a serial data output signal 24 . This may include multiplying the frequency of the received clock signal 22 within the SERDES for at least some of the clock requirements of the SERDES. The data that each SERDES 20 outputs via its serial data output lead 24 can come from elsewhere (e.g., other circuitry on or off DUT 10 ), or it can be test data generated by the SERDES itself.
Another typical capability of each SERDES 20 is to receive a serial data signal 26 and convert that signal to successive words of parallel data. Each SERDES 20 may output the parallel words of data that it recovers to other circuitry on or off DUT 10 , or (especially in a test mode of operation) the SERDES may use that data internally (e.g., comparing it to expected data to test whether it is correctly recovering data from incoming signal 26 ).
An overview of the remaining circuitry shown in FIG. 1 will now be provided. A master reference clock signal (REF_CLK) is supplied on lead 30 . This signal can come from any suitable source on or off DUT 10 . In the particular embodiment shown in FIG. 1 it is assumed that REF_CLK comes from test equipment (e.g., ATE) external to DUT 10 . Elements 40 , 50 , 60 , and 70 operate to produce (on lead 72 ) a version of REF_CLK having jitter. The frequency and/or amplitude of this jitter can be varied if desired. Multiplexer 80 -A allows either the signal on lead 30 (REF_CLK) or the signal on lead 72 (REF_CLK with jitter) to be selected as the reference clock signal 22 -A used by SERDES 20 -A 1 and 20 -A 2 . Multiplexer 80 -B allows a similar selection between signals 30 and 72 for the reference clock signal 22 -B used by SERDES 20 -B 1 and 20 -B 2 . The selection control signals (SEL_GRP_A and SEL_GRP_B) for multiplexers 80 can come from any suitable source on or off DUT 10 . In the particular embodiment shown in FIG. 1 it is assumed that SEL_GRP_A and SEL_GRP_B come from test equipment external to DUT 10 .
Continuing with the overview discussion, the FIG. 1 arrangement allows the reference clock signal 22 -A applied to the group A SERDES (i.e., 20 -A 1 and 20 -A 2 ) to be the REF_CLK-with-jitter signal 72 . At the same time, the reference clock signal 22 -B applied to the group B SERDES (i.e., 20 -B 1 and 20 -B 2 ) can be the REF_CLK signal 30 without jitter. SERDES 20 -A 1 and 20 -A 2 can then be operated to output serial test data signals 24 -A 1 and 24 -A 2 . Because SERDES 20 -A 1 and 20 -A 2 are operating with a reference clock signal 22 -A having jitter, the serial data signals 24 -A 1 and 24 -A 2 will have similar jitter.
Output signal 24 -A 1 is applied to SERDES 20 -B 1 input 26 -B 1 via one of leads 90 . (Leads 90 are shown as external to DUT- 10 and are assumed in this embodiment to be connections that are established temporarily for testing purposes. It will be understood, however, that other ways of providing connections like 90 are also possible, including providing them as selectively usable connections on DUT 10 .) If SERDES 20 -B 1 is able to correctly interpret the jittery data signal 26 -B 1 it receives, it is judged to be tolerant of that amount of jitter. SERDES 20 -B 1 may itself be able to determine whether it is correctly interpreting data, and may produce an output signal indicating when it is or is not achieving such correct interpretation. Alternatively, other circuitry (e.g., the test equipment testing DUT 10 ) may be used to receive the data SERDES 20 -B 1 recovers and to determine the correctness of that data. As mentioned above, the FIG. 1 circuitry may allow the jitter of signal 72 and therefore the jitter of signal 24 -A 1 / 26 -B 1 to be varied in frequency and/or amplitude. The ability of SERDES 20 -B 1 to tolerate jitter can thereby be tested over a range of jitter frequencies and/or amplitudes if desired.
At the same time that SERDES 20 -B 1 is being tested for tolerance to jitter in its incoming serial data signal 26 -B 1 , SERDES 20 -B 2 can be tested for its tolerance to jitter in the similarly jittery serial data signal 26 -B 2 it receives via another one of leads 90 from the serial data output 24 -A 2 of SERDES 20 -A 2 .
After SERDES 20 -B 1 and 20 -B 2 have been tested for jitter tolerance as described above, the process can be reversed to test the jitter tolerance of SERDES 20 -A 1 and 20 -A 2 . For example, the states of multiplexers 80 -A and 80 -B may be reversed so that SERDES 20 -B 1 and 20 -B 2 receive the jittery reference clock signal (from lead 72 ) and SERDES 20 -A 1 and 20 -A 2 receive the no-jitter reference clock signal (from lead 30 ). The jittery serial data output signal 24 -B 1 of SERDES 20 -B 1 is applied via one of leads 90 to the serial data input lead 26 -A 1 of SERDES 20 -A 1 to test the jitter tolerance of that SERDES. Similarly, the jittery serial data output signal 24 -B 2 of SERDES 20 -B 2 is applied via another of leads 90 to the serial data input lead 26 -A 2 of SERDES 20 -A 2 to test the jitter tolerance of that SERDES.
After all desired jitter-tolerance testing has been performed, all of SERDES 20 can be operated with a normal REF_CLK signal from lead 30 .
We turn now to a more detailed consideration of elements 40 , 50 , 60 , and 70 in FIG. 1 . Clock divider circuitry 40 receives REF_CLK signal 30 and a frequency division parameter value via leads DIV[9:0]. FIG. 1 shows the DIV[9:0] signals coming from an external source such as the test equipment being used to test DUT 10 . It will be understood, however, that these signals can come from any suitable source on or off DUT 10 . The value of parameter DIV[9:0] is preferably variable over time. Circuitry 40 produces a clock-type output signal 42 (divided clock or jitter control signal) having a frequency which is the REF_CLK signal frequency divided by the current value of parameter DIV. The frequency of divided clock signal 42 is at least partly determinative of the frequency of the jitter given the version of the reference clock signal on lead 72 . The frequency of this jitter can therefore be changed by changing the value of the DIV parameter (assuming no change in the MAX_COUNT parameter discussed below). Increasing the value of DIV decreases the jitter frequency, and vice versa (again assuming no change in the MAX_COUNT parameter). In the illustrative embodiment being described, DIV[9:0] can have any value from 1 to 1024. It will be understood, however, that this is only an example, and that any desired range of values can be used for this parameter.
When enabled by an up output signal from state machine circuitry 60 , up/down counter circuitry 50 responds to each cycle of the signal on lead 42 by incrementing a count it maintains and outputs via leads 52 (the signals DELAY_SET[6:0]). On the other hand, when state machine 60 is outputting a down signal, counter circuitry 50 decrements its count in response to each signal 42 cycle.
The operations of state machine 60 are controlled in part by the MAX_COUNT[6:0] signals it receives. If the value of the parameter represented by the MAX_COUNT signals is 0, state machine 60 enters or remains in a “no operation” state, in which it asserts neither up nor down. Accordingly, no jitter will be produced. On the other hand, if the value of the MAX_COUNT parameter is not 0, state machine 60 will assert up until DELAY_SET equals MAX_COUNT. Then state machine 60 will assert down until DELAY_SET equals 0. Then up will be asserted again, and so on, so that counter 50 repeatedly counts up and down between 0 and MAX_COUNT. It will soon become apparent how the value of parameter MAX_COUNT controls the amplitude of the jitter given to the signal on lead 72 . MAX_COUNT can be varied to vary jitter amplitude if desired. (MAX_COUNT also has an effect on jitter frequency, as will be made clearer below.) FIG. 1 shows the MAX_COUNT signals coming from the test equipment being used to test DUT 10 . But it will be understood that these signals can come from any suitable source on or off DUT 10 .
In addition to being applied to state machine 60 , the DELAY_SET[6:0] output signals 52 of up/down counter 50 are applied to glitch-free controlled delay line circuitry 70 . This circuitry can delay the REF_CLK signal it also receives by any of many different amounts of delay, the amount of that delay being controlled by the current value of the DELAY_SET parameter. Output 72 of circuitry 70 is this selectively delayed REF_CLK signal.
An illustrative construction of circuitry 70 includes a plurality of signal delay circuit elements connected in series. For example, each of these delay circuit elements may delay the signal applied to it by 20 pS. One hundred of these elements may be connected in series, thereby providing a maximum delay of 2 nS. Output signal 72 may be derived from the output of any of these 100 delay elements, the current value of DELAY_SET controlling that selection. Accordingly, in this example DELAY_SET may have any value from 0 to 100. Of course, if MAX_COUNT is less than 100, then the highest value DELAY_SET will reach will be MAX_COUNT, not 100. Also, in this example the maximum value that MAX_COUNT can have is 100. It will be understood, however, that these particular values are only illustrative, and that the circuitry can be constructed to support (1) any amount of incremental delay of REF_CLK, and (2) any number of such increments.
Circuitry constructed in accordance with the invention may be capable of a wider range of operation, but in any particular test it will generally be desirable to limit the amplitude of the jitter (i.e., the maximum amount of delay of REF_CLK by circuitry 70 ) to some fraction of UI. The frequency of the jitter is also logically limited to a fraction of the expected maximum serial bit rate of the circuitry being tested. Moreover, there may be a relationship between these two variables, because most systems to be tested will probably be able to tolerate higher amplitude jitter at lower jitter frequencies, but only lower amplitude jitter at higher jitter frequencies. In any event, the circuitry of this invention is able to provide any desired combination of jitter frequency and amplitude.
FIGS. 2-5 are provided to ensure that the concepts of frequency and amplitude of jitter are clear. FIG. 2 is a plot of the amount by which signal 72 is delayed relative to signal 30 as a test proceeds with particular values for jitter frequency and amplitude. ( FIG. 2 can also be thought of as a plot of the DELAY_SET parameter value over time.) The peak-to-peak “magnitude” of the jitter is the maximum amount of delay of signal 72 relative to signal 30 . This is computable as MAX_COUNT*TAP_DELAY, where TAP_DELAY is the delay increment characteristic of circuitry 70 . (Alternatively, jitter “amplitude” may be thought of as one-half the peak-to-peak excursion shown in FIG. 2 , in which case amplitude will be computed as MAX_COUNT*TAP_DELAY/2.) The period of the jitter is the time required for the delay of signal 72 relative to signal 30 to go from 0 to maximum and then back to 0 again. Jitter frequency is the reciprocal of jitter period, which is computable as FMOD=REF_CLK/(2*MAX_COUNT*DIV). It will thus be seen that jitter frequency is a function of both DIV and MAX_COUNT.
FIG. 3 shows the UIs in a serial data signal with no jitter. (The time scale of FIG. 3 is different from that of FIG. 2 , but the same as that of FIG. 4 ). FIG. 3 shows the locations of all possible transitions in the data signal, and therefore the measure of UI for the depicted signal.
FIG. 4 shows the addition of jitter to the FIG. 3 signal information in accordance with this invention. FIG. 4 shows that this jitter can cause each possible transition in the FIG. 3 signal to be somewhat delayed (typically by some fraction of a UI). The maximum amount of this delay is labelled as the “magnitude” of jitter in FIG. 4 .
FIG. 5 is plotted on a time axis that is perpendicular to the FIG. 4 time axis (and with magnitude of delay in FIG. 4 transferred to the magnitude axis in FIG. 5 ) to show that over time the amount of delay in the FIG. 4 jitter alternately increases and decreases. FIG. 5 is therefore identical to FIG. 2 , but rotated 90° and linked to one illustrative transition time in FIG. 4 .
It will be understood that the foregoing is only illustrative of the principles of the invention, and that various modifications can be made by those skilled in the art without departing from the scope and spirit of the invention. For example, the circuitry shown as DUT 10 in FIG. 1 (or at least part of that circuitry) can be made part of test equipment (e.g., ATE) for testing the jitter tolerance of other devices. One or more of the serial data outputs 24 of the FIG. 1 circuitry would then be connected to the serial data inputs (similar to 26 ) of the SERDES or other receiver circuitry of another device to be tested for jitter tolerance. That other device could also receive the REF_CLK signal without jitter. The FIG. 1 circuitry would be operated generally as described above to produce one or more serial data output signals 24 with jitter. The ability of the SERDES or other receiver circuitry in the other device to correctly interpret that jittery data would provide a measure of the jitter tolerance of the other device.
As used herein and in the appended claims, the word “successive” does not necessarily mean immediately following. It can just mean later in time.
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To facilitate measurement of the jitter tolerance of circuitry such as serializer/deserializer (SERDES) circuitry, test circuitry is provided that can add jitter to a data signal. The jitter added is preferably controllable and variable with respect to such parameters as jitter frequency (i.e., how rapid is the jitter) and/or amplitude (i.e., how large or great is the amount of the jitter).
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BACKGROUND OF THE INVENTION
This invention relates generally to the field of envelope handling apparatus, and more particularly to an apparatus for closing and sealing the flaps of envelopes traveling along a feed path after insert material has been inserted into the envelopes by an inserting machine.
Envelope inserting machines have long been well known and are utilized in a large variety of document processing applications which involve inserting one or more items into an envelope for further handling, such as mailing. One particular application where these machines are used involves high speed collating machines which store a plurality of different types of insert material which are added to a basic document that is traveling along an elongate feed, at the end of which the basic document and the insert materials are formed into collations which are inserted into envelopes. One typical example of such an application is the mailing of monthly statements to customers from bank credit card operations, telephone or other utility companies, book clubs, catalog mail order companies, and many other types of business operations in which various material is mailed to tens or perhaps hundreds of thousands of customers each month.
These examples involve a typical document handling process in which a basic document, such as the monthly invoice to customers, is computer printed on forms passed through a high speed computer printer in continuous web form, and are then fed through a suitable separating machine and entered into the feed path of a collating machine. The collating machine then adds any desired number of other documents, such as advertising material, services information brochures, announcements of forthcoming services, sweepstakes entries, etc., to the basic document as the latter travels along the feed path of the collation machine. All of the collated material may be passed through an accumulator or other device that arranges the material in a precisely aligned packet which is then fed to an inserting machine where the packet is inserted into an envelope which is suitably held at an inserting station. After the packet of documents is inserted into the envelope, it is typically fed through a machine which moistens the envelope flap, turns it 180° and presses it against the back of the envelope to seal it thereto. The now closed and sealed envelope is then typically fed either through a postage metering machine for printing a postage indicia on the envelope or may be fed directly to suitable stacking device for further processing.
The problem that arises is that occasionally a collation of insert material is inserted into an envelope out of proper alignment with the envelope, or the individual documents of the collation are not properly aligned so that the collation cannot fit properly within the envelope, or even a properly aligned collation is not fully inserted into the envelope. In any of these situations, the result is that a marginal portion of the insert material is disposed above the crease line which joins the sealing flap to the main body of the envelope, thereby preventing the flap from being turned through the approximately 180° angle to permit the flap to be sealed against the back surface of the envelope. The marginal portion of the insert material collation may be either just a corner portion if the collation is inserted at an angle, or a lengthy marginal portion if the collation is inserted in longitudinal alignment with the envelope, but but the collation is out of alignment or it is not inserted far enough for the trailing edge of the collation to be disposed beyond the crease line. In either event, when the envelope passes through the envelope flap closing and sealing apparatus, the flap cannot rotate evenly about the crease line. If the collation is inserted at an angle with just a corner portion protruding beyond the crease line, the flap is unevenly folded and the envelope then jams in the closing and sealing apparatus. The entire inserting machine then shuts down until an operator clears the jam, with the result that the overall output of the inserting apparatus is substantially reduced, since in a typical situation, about 300 envelopes could have been processed in the time required for an operator to clear the jam.
On the other hand, if the insert material is inserted in longitudinal alignment with the envelope but not fully inserted, the flap may fold over evenly but not along the crease line, with the result that the moistened adhesive on the edge of the flap will bond to the insert material, not to the rear surface of the envelope, thereby preventing the envelope from being opened without the likelihood of tearing the insert material. Since the envelope in this condition may not jam in the closing and sealing appaaratus, but rather continues on in the stream of envelopes, such improperly sealed envelopes reach their destination in this condition, which is generally an entirely unacceptable result.
Thus, there is a need for a machanism that will detect whether insert material has been properly inserted into envelopes moving through the flap closing and sealing mechanism of high speed inserting apparatus, and which will both prevent the flap of any envelope containg improperly inserted material from being turned to the sealing position and also eject such envelope from the main stream of envelopes and direct it into a collection bin from which it can be retrieved by an operator, all while maintaining continuity of operation of the inserting apparatus.
BRIEF SUMMARY OF THE INVENTION
The present invention substantially obviates, if not entirely eliminates, the above shortcomings and other disadvantages of current envelope flap closing and sealing devices by providing an envelope flap closing and sealing apparatus which prevents the flaps of envelopes which contain improperly inserted insert material from being turned and sealed, and which ejects such envelopes from the feed path thereof, thereby preventing jams which would shut down the inserting apparatus or causing flaps to seal to the insert material. It has been descovered that if the rigid flap engaging bar which normally forces the flap downwardly to commence the approximately 180° turning movement of the flap is replaced with an elongate strip of very thin, flexible material which has insufficient regidity to commence the turning movement of the flaps is there is any impediment to free turning movement of the flaps, the flaps that are obstructed from free turning movement can be maintained in a flat orientation, and this orientation can be sensed to cause operation of a diverting mechanism to thus divert that envelope from the normal feed.
Thus, the principles of the present invention are embodied in an apparatus for closing and sealing the flaps of envelopes that have passed through an inserting machine in which collations of insert material have been inserted into the envelopes, and for detecting whether or not certain envelopes cannot be properly closed and sealed, and for separating such envelopes from those that are properly closed and sealed. In that environment, and in its broader aspects, the apparatus comprises means defining a feed path along which envelopes are fed into the flap closing and sealing apparatus from an inserting machine, and means for feeding envelopes along the feed path with the flaps thereof lying in the plane of the envelopes in an extended positon beyond the crease line of the envelopes. There is means disposed in the feed path for normally turning the flaps through approximately 180° along the crease line to substantially close the flaps against the rear surface of the envelopes, and for maintaining the flaps in the extended position if the flaps encounter any resistance to being turned freely about the crease line. A detecting means is disposed in the feed path for detecting the presence of an envelope with the flap having been maintained in the extended position. Finally, there is means responsive to operation of the detecting means detecting an envelope with the flap lying in the extended position for ejecting such envelope from the feed path, with the result that envelopes with improperly closed flaps are diverted from the feed path and are accessible for manual retrieval without otherwise affecting the operation of the envelope closing and sealing apparatus.
In some of its more limited apects, the means for normally turning the flaps through the approximately 180° along the crease line and for maintaining the flaps which cannot be turned freely in the extended position comprises a first flap engagng member mounted in the feed path in overlying relationship to the flaps when they are lying in the extended position, for exerting a sufficiently light downward force on the flaps to commence the turning movement thereof if the turning movement is not obstructed so that said flap can turn freely, and a second flap engaging member mounted adjacent the first flap engaging member and in operative association therewith such that the second flap engaging member completes the turning movement of the flaps if the first flap engaging member has caused the flaps to turn through a portion of the 180° movement. The first flap engaging member is a strip of resilient material which as only sufficient rigidity to turn the flap if it is not obstructed by insert material projecting beyond the crease line of the flap.
The apparatus includes a detecting device which can detect whether or not the flap of an envelope has been turned, and if not, the detecting device actuates a pivotable gate in the feed path of the envelopes to divert any envelope on which the flap has not been properly turned and sealed from the normal feed path so that the envelope can be retrieved, adjusted as to the position of the insert material and reinserted into the feed path, all without interruption in the continuity of operation of the closing and sealing apparatus or any other machine or component in the overall process.
Having briefly described the general nature of the present invention, it is a principal object thereof to provide an envelope closing and sealing apparatus which can detect the presence of an unsealable envelope and eject that envelope from the mainstream of envelopes to prevent an envelope jam and machine shutdown.
It is another object of the present invention to provide an envelope closing and sealing apparatus which detects the presence of an unsealable envelope by maintaining the envelope flap in an open, extended position so that the envelope can be retrieved, the contents adjusted and the envelope reinserted into the mainstream of envelopes, again without an envelope jam or machine shutdown.
It is a further object of the present invention to provide an envelope closing and sealing apparatus which is relatively simple and inexpensive in construction, operates at a high rate of speed and is highly reliable.
These and other objects and features of the present invention will be more apparent from an understanding of the following detailed description of a presently preferred mode of carrying out the invention when considered in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the envelope flap closing and sealing apparatus of the present invention, showing an envelope entering the apparatus with the flap lying open in an extended postion.
FIG. 2 is a fragmentary side view of the apparatus shown in FIG. 1 illustrating the vertically spaced relationship of the envelope flap turning mechanism.
FIG. 3 is a fragmentary perspective view of the apparatus shown in FIG. 1 showing an envelope with insert material properly inserted therein and the flap in a partial stage of closure.
FIG. 4 is a view similar to FIG. 2 but showing an envelope in which the insert material is not fully inserted into the envelope so as to prevent the flap from closing, with the flap turning mechanism now maintaining the flap in the flat, extended position.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings, and particularly to FIG. 1 thereof, the reference numeral 10 indicates generally the flap closing and sealing apparatus of the present invention. The reference numeral 12 indicates generally the discharge end of a conventional envelope inserting machine which feeds one or more documents from individual feeders and either inserts a succession of single documents into envelopes, or forms a succession of collations of a plurality of documents and inserts the collations into envelopes. Since the details of the inserting machine form no part of the present invention, further description thereof is not deemed necessary for a full understanding of the present invention, other than to note that the envelope feeding device of the inserting machine delivers the envelopes with the insert material therein to the infeed end of the envelope closing and sealing apparatus 10 of the present invention.
Thus, the apparatus 10 includes a frame which supports in a suitable manner all of the parts of the apparatus, including an elongate plate 14 which provides a flat supporting surface for envelopes E which are fed through the apparatus 10 by a conveyor belt 16 which is suitably mounted on drive pulleys 18 which in turn are suitably mounted on the frame adjacent the infeed end 20 and the outfeed end 22 of the apparatus 10. A plurality of pressure rollers 24 are rotatably mounted on arms 26 which are pivotally Connected to rods 28 suitably mounted on the frame so that the rollers 24 are directly over the conveyor belt 16. A suitable spring 30 mounted on each rod 28 and bearing on the arms 26 causes the rollers 24 to apply sufficient pressure to the upper surface of the envelope E so that the conveyor belt 16 moves the envelope E through the apparatus 10 for closure or non-closure of the flap, as the case may be, as fully described below.
The reference numeral 32 indicates generally an envelope diverting mechanism which, when activated, diverts an envelope from the main feed path of envelopes which have been closed and sealed by the apparatus 10. Thus, the diverting mechanism has a supporting plate 34 which abuts the outfeed end 22 of the support plate 14 of the apparatus 10 and, in effect, forms an extension thereof. The plate 34 includes a movable gate 36 which is pivotally connected to the plate 34 as indicated by the reference numeral 38. A suitable actuator 40, such as a rotary solenoid, is connected to the gate 38 so that when the solenoid is energized, the gate 36 is rotated from the flat, solid line position shown in FIG. 1 to the raised dotted line position 36'. It will be apparent that when the gate 36 is in the flat position, an envelope E being fed out of the apparatus 10 by the conveyor belt 16 will pass over the gate 36 and be conveyed by another suitable conveyor means to the next processing machine or component in the overall envelope handling system, which may, for example, be a mailing machine which prints a postage indicia on the now sealed envelope. However, if the gate 36 is in the raised position 36', an envelope will be intercepted by the gate 36 and diverted downwardly out of the normal feed path of envelopes moving along the supporting plate 34. In practice, a suitable collection bin (not shown) would be mounted beneath the opening formed by the gate 36 when in the raised position 36' to collect and store any envelopes that are diverted from the main feed path.
Still referring to FIG. 1, the support plate 14 for the apparatus 10 includes a suitable registration member 42 which provides a registration guide 44 which the bottom edge of envelopes passing through the apparatus 10 engage to properly align the envelopes with the flap closing mechanism now to be described. The outer edge 46 of the support plate 14 is cut back over a major portion of the length of the apparatus 10, as indicated by the reference numeral 48, so that this edge 48 is disposed directly under the crease line 50 of the envelope E which separates the body of the envelope E from the flap F connected thereto. Although not shown, in practice the registration member 42 would be laterally adjustable to move the registration guide 44 to accommodate envelopes of different height.
With reference now to FIGS. 1 and 2, the reference numeral 52 indicates generally a flap turning mechanism which is disposed in the envelope feed path extending through the apparatus 10 for normally turning the flap F through approximately 180° along the crease line 50 to substantially close the flap against the rear surface of the envelope E, and for maintaining the flap F in an open or extended position if the flap encounters any resistance to being turned freely about the crease line 50. Thus, the flap turning mechanism 52 comprises a first flap engaging member 54 which is an elongate strip of flexible material having one end 56 thereof suitably mounted on one of the rods 28 so that the member 54 extends generally parallel to the edge 48 of the support plate 14 and in overlying relationship with the flap F as the envelope E passes through the apparatus 10. The other end 58 of the member 54 is normally disposed slightly below the plane of the support plate 14, as best seen in FIG. 2, so that it bears lightly on the upper surface of the flap F and exerts a light downward force on the flap F as the envelope E is moved along the support plate 14, the degree of regidity of the material from which the member is formed being insufficient to commence the turning movement of the flap F about the crease line 50 if the flap F encounters any resistance to turning by improperly inserted insert material projecting from the enveloope E byond the crease line 50. This is clearly shown in FIG. 2, and further explained below in the description of operation of the apparatus 10.
The flap turning mechanism 52 also includes a second flap engaging member 60 which is mounted in operative association with the first flap engaging member 54 such that the second flap engaging member 60 completes the turning movement of the flap F if the first flap engaging member 54 has been able to commence the turning movement of the flap F. The second flap engagement member 60 is in the form of an elongate rod, one end 62 of which is mounted adjacent to the end 56 of the first flap engaging member 54, the rod having a relatively straight portion 61 extending longitudinally and generally parallel to the first flap engaging member 54 for approximately the length thereof. The rod 60 further includes a curved portion 62 which curves laterally inwardly toward the envelope E and which lies in a plane just below the plane of the envelope E, so that the lead edge of the flap F adjacent the juncture thereof with the envelope E at the crease line 50 passes over the curved portion 62 of the bar 60 so as to urge the flap through the remaining portion of the 180° movement as the remainder of the flap passes over the curved portion 62 of the bar 60. This briefly described procedure would be the normal operation of the flap turning mechanism 52 if the insert material has been properly inserted into the envelope E by the inserting machine 12 and therefore offers no resistance to turning of the flap F abut the crease line 50. This will also be further described below in connection with the operation of the apparatus 10.
However, in the event that the insert material is not properly inserted into the envelope, and a portion of it projects slightly beyond the crease line 50, the flap F is not free to turn about the crease line 50 since the turning motion of the flap F is obstructed by the insert material. In this event, the first flap engaging member 54 cannot depress the flap F since, as stated above, it does not have sufficient rigidity to do so when improperly inserted insert material is projecting beyond the crease line 50, and the flap remains in the flat, extended position shown in FIG. 3, as mere fully explained below.
The apparatus 10 is provided with a detecting device 64 which is mounted on a suitable bracket 66 in the feed path of the envelopes in position to detect the presence of an envelope E in which the flap F has not been turned and remains in the flat extended position. The detecting device 64 may be any type of device, such as a photo detector, which can detect the present of an extended flap F since the line of sight of the detector 64 is slightly beyond the path of movement of the crease line 50 as it moves along the edge 48 of the support plate 14. The support plate 14 has a further inward depression 66 to permit the flap F to fold under and make contact with the reverse side of the envelope E. The detector 64 is appropriately connected to the actuator 40 so that when it detects the presence of a flap F, it actuates the actuator 40 to open the gate 36.
The operation of the apparatus 10 will now be described. With reference to FIGS. 1 and 3, assume that an envelope E is fed into the apparatus 10 from the inserting machine 12 which has insert material properly inserted therein, as indicated in FIG. 3 by the dash line rectangle indicated by the reference letter I within the outline of the envelope E. As the envelope E is fed through the apparatus 10 by the conveyor belt 16 and pressure rollers 24, the first flap engaging member 54 begins to bear on the upper surface of the flap F, as seen in FIG. 3, and thereby exerts a downward force of relatively small magnitude on the flap F to urge it downwardly in a rotating motion about the crease line 50. With the flap F thus partially depressed, when the lead edge corner 70 of the flap F and crease line 50 approach the curved portion 62 of the rod 60, the portion 72 of the outer edge of the flap F that is immediately adjacent to the lead edge corner 70 is slightly above the curved portion 62 of the rod 60, and the remaining portion 74 of the outer edge is slightly below the straight portion 61 of the rod 60. Upon further movement of the envelope E, the remaining portion 72 of the outer edge of the flap F rides over the curved portion 62 of the bar 60 which causes the entire flap F to progressively turn through the approximately 180° angle to bring the flap into juxtaposition with the rear surface of the envelope E. In this situation, as the envelope E continues to move, the detecting device 64 does not detect the presence of the flap F since it is out of range of the detecting device 64, with the result that the actuator 40 for the gate 36 is not activated and the gate 36 remains in the flat position to permit the envelope E to pass over it and on into the next processing machine. As the envelope E with the flap F in closed position moves past the detecting device 64, a sealing roller assembly 65 presses the moistened adhesive on the flap F into engagement with the rear surface of the envelope E to seal the flap F thereto in known manner.
With reference now to FIGS. 1 and 3, assume that an envelope E is fed into the apparatus 10 from the inserting machine 12 which has insert material improperly inserted therein, as indicated in FIG. 4 by the dash line rectangle indicated by the reference letter I', so that a portion of the insert material I' is projecting slightly out of the envelope E beyond the crease line 50, as indicated in FIG. 4 by the dash line I". In this situation, as the envelope E is fed through the apparatus 10 by the conveyor belt 16 and pressure rollers 24, the first flap engaging member 54 again begins to bear on the upper surface of the flap F, as seen in FIG. 4, and still exerts a downward force on the flap F to urge it downwardly about the crease line 50. However, since a portion of the insert material I" is extending beyind the crease line 50, the flap cannot turn freely about the crease line 50 and therefore remains substantially in the flat extended position shown in FIGS. 1 and 4, and the fexible strip 54 simply bends upwardly and rides over the flap F. As the envelope E moves forwardly, the portion 72 of the outer edge of the flap F is again slightly above the curved portion 62 of the rod 60, but the remaining portion 74 of the outer edge remains slightly above the straight portion 61 of the rod 60. Upon further movement of the envelope E, the portion 72 of the outer edge of the flap F still rides over the curved portion 62 of the bar 60, but since the flap F is still in the flat extended position, the entire flap now rides over the rod, as seen in FIG. 4. In this situation, the envelope E continues to move, the detecting device 64 detects the presence of the flap F since it is lying within the range of the detecting device 64, with the result that the actuator 40 for the gate 36 is activated and the gate 36 is pivoted upwardly so as to project into the path of movement of the envelope, and the envelope E is diverted downwardly from the normal feed path into a bin or other collection instrumentality. And this occurs without interruption in the operation of the closing and sealing apparatus 10 or any other machine or component in the processing system.
It is to be understood that the present invention is not to be considered as limited to the specific embodiment described above and shown in the accompanying drawings, which is merely illustrative of the best mode presently contemplated for carrying out the invention and which is susceptible to such changes as may be obvious to one skilled in the art, but rather that the invention is intended to cover all such variations, modifications and equivalents thereof as may be deemed to be within the scope of the claims appended hereto.
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An apparatus is disclosed for closing and sealing the flaps of envelopes that have passed through an inserting machine in which collations of insert material have been inserted into the envelopes, and for detecting whether or not certain envelopes cannot be properly closed and sealed and for separating such envelopes from those that are properly closed and sealed. The apparatus is constructed and arranged such that if insert material is improperly inserted into the envelope such that the flap cannot turn freely about the crease line that connectes the flap to the envelopem, the flap will remain substantially in the flat, extended position it occupies when the envelope enters the closing and sealing apparatus. That position of the flap is sensed and the envelope is then diverted from the normal path of properly closed and sealed envelopes into a collection bin for retreival by an operator.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. application Ser. No. 11/303,620, entitled “SOLID-STATE IMAGING DEVICE AND METHOD FOR DRIVING THE SAME,” filed on Dec. 16, 2005, the entirety of which is incorporated herein by reference to the extent permitted by law. The present invention claims priority to Japanese Patent Application No. P2004-367223, filed Dec. 20, 2004, the entirety of which is also incorporated herein by reference to the extent permitted by law.
FIELD OF THE INVENTION
The present invention relates to solid-state imaging devices for capturing images and producing image signals by means of a plurality of photoelectric conversion elements and also to driving methods for driving such imaging devices. More particularly the present invention relates to a solid-state imaging device which performs an addition operation on pixel data and then outputs the result, and to a driving method therefor.
DESCRIPTION OF THE RELATED ART
In general, driving modes for an image sensor includes an all-image readout mode in which all pixels are read out for normal applications and a low-resolution readout mode in which pixels are read out at a low resolution for high frame rate applications. In the mode for high frame rate applications, data rate is effectively reduced by skipping pixels, but aliasing noise is undesirably increased at the same time due to low sampling frequency. To reduce the aliasing noise, there is a known method of adding and averaging signals of adjacent pixels instead of skipping pixels in the course of readout (See, for example, Japanese Unexamined Patent Application Publication No. 2004-356791).
SUMMARY OF THE INVENTION
However, this known method has a disadvantage of low flexibility in operation, since it performs simple addition and averaging operations during reading. For example, when an addition operation is performed on even numbers of pixels out of a plurality of pixels arranged in rows and columns, an addition operation adjacent pixels on a color-by-color basis of the Bayer array produces unequal pitches between the virtual pixel centers which are output upon completion of the addition operation. This results in an image inconsistent with an expected low-resolution image in the Bayer array, which causes degradation of the quality in the processed image.
The present invention addresses the problem described above. More specifically, according to an embodiment of the present invention, a solid-state imaging device includes a pixel array in which a plurality of pixel cells, each of which includes a plurality of photoelectric conversion elements, is arranged, and an adder for performing an addition operation on a plurality of signals output from the photoelectric conversion elements of the pixel array in a predetermined combination of the photoelectric conversion elements, while setting between the signals to be added a ratio determined according to the arrangement of the photoelectric conversion elements.
According to another embodiment of the present invention, a solid-state imaging device includes a pixel array in which a plurality of pixel cells, each of which includes a plurality of photoelectric conversion elements, is arranged, and a controller for controlling exposure times on the photoelectric conversion elements using a ratio determined according to the arrangement of the plurality of photoelectric conversion elements, when an addition operation is performed on a plurality of signals output from the plurality of photoelectric conversion elements in the pixel array in a predetermined combination.
According to still another embodiment of the present invention, provided is a driving method for driving a solid-state imaging device having a pixel array in which a plurality of pixel cells, each of which includes a plurality of photoelectric conversion elements, is arranged, and an adder for performing an addition operation on a plurality of signals output from the plurality of photoelectric conversion elements in the pixel array in a predetermined combination. The method includes the step of causing the adder to perform the addition operation on the plurality of signals using a ratio determined according to the arrangement of the plurality of photoelectric conversion elements.
According to a further embodiment of the present invention, provided is a driving method for a solid-state imaging device having a pixel array in which a plurality of pixel cells, each of which includes a plurality of photoelectric conversion elements, is arranged, and a controller for controlling an exposure times on the plurality of photoelectric conversion elements in the pixel array. The method includes the step of causing the controller to control the exposure times using a ratio determined according to the arrangement of the plurality of photoelectric conversion elements when the addition operation is performed on the plurality of signals output from the plurality of photoelectric conversion elements in the pixel array in a predetermined combination.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram illustrating the entirety of a solid-state imaging device according to an embodiment of the present invention;
FIG. 2 is a circuit diagram illustrating a specific configuration of one pixel cell;
FIG. 3A is a conceptual diagram illustrating a technique in a known art;
FIG. 3B is a conceptual diagram illustrating an embodiment of the present invention;
FIG. 4 is a schematic diagram illustrating an example in which an embodiment of the present invention is applied to a CDS circuit in a column circuit;
FIG. 5A shows an exemplary circuit configuration used for an addition operation in the row direction;
FIG. 5B is a timing chart illustrating an addition operation in the row direction;
FIG. 6A shows an exemplary circuit configuration used for an addition operation in the column direction;
FIG. 6B is a timing chart illustrating an addition operation in the column direction;
FIG. 7 is a timing chart illustrating the differences in photoelectric conversion time between pixels to be added;
FIG. 8 is a circuit diagram illustrating different-sized differential circuits;
FIG. 9 is a conceptual diagram illustrating the addition operation on 3×3 pixels;
FIG. 10A is a conceptual diagram illustrating the addition operation on 4×4 pixels; and
FIG. 10B is a conceptual diagram illustrating the pixel centers of four pixels yielded by simple addition and averaging operations.
FIG. 11 is a schematic diagram illustrating the camera to which the present invention is applied.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiments of the present invention will be described with reference to the accompanying drawings. FIG. 1 is a schematic diagram illustrating the entirety of a solid-state imaging device according to an embodiment of the present invention.
More specifically, FIG. 1 is a block diagram illustrating an exemplary configuration of a solid-state imaging device, for example, a CMOS (Complementary Metal Oxide Semiconductor) image sensor according to an embodiment of the present invention. As shown in FIG. 1 , the solid-state imaging device includes a pixel array 2 in which a plurality of the pixel cells 1 each having a plurality of photoelectric conversion elements is two-dimensionally arranged in matrix form, a vertical scanning circuit 3 , column circuits 4 for signal processing, a horizontal transfer circuit 5 , a horizontal signal line 51 , an output circuit 6 , and so forth. In the pixel array 2 , a vertical signal line VSL is provided in connection with each vertical pixel column.
FIG. 2 is a circuit diagram illustrating a specific configuration of one pixel cell in a pixel column.
As shown in FIG. 2 , a pixel cell 1 is configured as a pixel circuit including not only a plurality of (four in this case) photoelectric conversion elements such as photodiodes 11 but also four kinds of transistors, that is, transfer transistors TRGs, a reset transistor RST, an amplifying transistor TRP and a selecting transistor SEL. In this case, N-channel MOS transistors, for example, are used as these transistors.
Each photodiode 11 performs photoelectric conversion and stores a signal charge (electrons in this case). The transfer transistor TRG transfers the signal charge to a FD (floating diffusion) portion 12 . The reset transistor RST connected between the FD portion 12 and a power supply VDD resets the potential of the FD portion 12 , in advance of the transfer of the signal charge from the photodiode 11 .
The amplifying transistor TRP supplies the vertical signal line VSL with a reset level which is the potential of the FD portion 12 reset by the reset transistor RST and also with a signal level which is the potential of the FD portion 12 after the transfer of the signal charge by the transistor TRG.
The selecting transistor SEL connected between the amplifying transistor TRP and the power supply VDD has a function to select a pixel cell 1 .
Referring back to FIG. 1 , the vertical scanning circuit 3 includes a shift resister or the like and selectively drives each pixel cell 1 in the pixel array 2 on a row-by-row basis by sequentially outputting control signals on a row-by-row basis. The control signals include a transfer signal for driving the transfer transistor TRG in the pixel cell 1 and a reset signal for driving the reset transistor RST in the pixel cell 1 .
The column circuits 4 are signal processing circuits, and each column circuit is provided for each pixel arranged in horizontal direction in the pixel array 2 , that is, for each vertical signal line VSL. For example, the column circuit 4 includes a S/H (sample and hold) circuit and a CDS (Correlated Double Sampling) circuit.
First Embodiment
FIGS. 3A and 3B are conceptual diagrams illustrating a technique in a known art and a first embodiment of the present invention, respectively. Virtual pixel centers, which are obtained by mixing two pixels of an identical color when pixels corresponding to G (green) and B (blue) are alternatively arranged in a column, are illustrated in these figures. FIG. 3A illustrates an addition operation according to the known art. Since two pixel signals, each from a single pixel of the identical color, are simply added and averaged, pitches between the centers of each pair of the adjacent virtual pixels G′ and B′ after addition are not equal.
In contrast, FIG. 3B illustrates an addition operation according to the first embodiment of the present invention. The pitches between the centers of each pair of the adjacent virtuals G′ and B′ after addition can be equalized by setting a specific value of addition ratio between the input signals in an analog signal processing. In other words, the resolution can be reduced without changing the color arrangement.
For example, when two pixel signals from two pixels of the identical color are added, an addition ratio of 3:1 is set between the pair of pixel signals G (green) and also between the pair of pixel signals B (blue), as illustrated in FIG. 3B . The pitches between the centers of the successive pairs of virtual pixels G′ and B′ can be equalized to 2 pixel pitches (pix) by using this ratio.
A technique for implementing this method will now be described by way of example. FIG. 4 is a schematic diagram illustrating an example in which the first embodiment of the present invention is applied to a CDS circuit in a column circuit. In this embodiment, a storage capacitance of a sampling portion is configured to be divisible so that the amounts of the signal charges to be averaged are controlled in accordance with the addition ratio to be obtained.
More specifically, two systems of the storage capacitances, a system Q 1 and a system Q 2 , are provided in the sampling portion. The capacitance of one system (for example, Q 2 ) is configured to be divided into two fractions: namely, one-third and two-thirds of the capacitance of the system Q 1 . For example, the capacitance of the system Q 1 and the fraction of the system Q 2 equivalent to the one-third of the capacitance of the system Q 1 side are connected so as to enable addition and averaging of the stored charges, whereby the addition and averaging operation at the addition ratio of 3:1 is performed.
This technique can effectively be used in signal processing both in the row direction and the column direction. FIGS. 5A and 5B illustrate an addition operation in the row direction. FIGS. 6A and 6B illustrate an addition operation in the column direction.
Referring to FIG. 5A , an exemplary circuit configuration used for the addition operation in the row direction will be described. When the addition operation in the row direction is performed, each signal VSL output from one of the two pixels to be added is connected to one of the two systems. A capacitor C 1 is connected to one system and a capacitor C 2 is connected to the other system. The capacitance of the capacitor C 1 is three times greater than that of the capacitor C 2 . Switches “a” and “b” are provided in one and the other systems, respectively, and a switch “c” is provided therebetween. Referring to FIG. 5B , the addition operation in the row direction will now be described. Using the configuration illustrated in FIG. 5A , the signal from a pixel in ith row is stored in the capacitor C 1 by holding the switches “a”, “b”, and “c” in the states of ON (closed), OFF (open), and OFF, respectively. Likewise, the signal from a pixel of the identical color in the jth row is stored in the capacitor C 2 by holding the switches “a”, “b”, and “c” in the states of OFF, ON, and OFF, respectively. The signals stored in the capacitor C 1 and the capacitor C 2 are then added by turning the switch “c” ON while the switches “a” and “b” are held OFF, whereby an added-averaged signal according to the capacitance ratio can be obtained.
Referring to FIG. 6A , an exemplary circuit configuration used for the addition operation in the column direction will be described. When the addition operation in the column direction is performed, a signal VSLm from a pixel cell in the mth column is connected to the capacitor C 1 and a signal VSLn from a pixel cell in the nth column is connected to the capacitor C 2 . The capacitance of the capacitor C 1 is three times greater than that of the capacitor C 2 . A switch “a” is provided for the signal VSLm, a switch “b” is provided in the signal VSLn side, and a switch “c” is provided therebetween. Referring to FIG. 6B , the addition operation in the column direction will now be described. Using the configuration illustrated in FIG. 6A , the signal from a pixel cell in mth column is stored in the capacitor C 1 and the signal from a pixel cell in nth column is stored in the capacitor C 2 by simultaneously setting the switches “a”, “b”, and “c” in the states of ON (closed), ON, and OFF, respectively, as shown in FIG. 6B . The signals stored in the capacitor C 1 and the capacitor C 2 are then added by turning the switch “c” ON while the switches “a” and “b” are held OFF, whereby an added-averaged signal according to the capacitance ratio can be obtained.
Second Embodiment
In the first embodiment, an addition operation is performed in the sampling portion in a CDS circuit. However, for an image sensor configured to have a FD portion shared between pixel cells, a charge-addition operation in the FD portion is more advantageous for high sensitivity and operational speed. In this case, addition and averaging operations for signal processing similar to those described in the first embodiment can be achieved, by adjusting an exposure time on each pixel intended for an addition operation, as shown in FIG. 7 .
Specifically, a vertical scanning circuit 3 performs a control operation, so that the time interval between ON periods (exposure time) of a transfer transistor TRG_a of a first pixel intended for an addition operation may be set to be the normal exposure time, and the time interval between ON periods of a transistor TRG_b of a second pixel intended for the addition operation may be set to be one-third shorter than that of TRG_a. This yields a ratio between the charge amounts of the first pixel and the second pixel, which corresponds to the ratio of the exposure times. These charge amounts are added in the FD portion and the result is output, whereby an added-averaged signal corresponding to the ratio of the exposure times can be obtained. Meanwhile, when performing a charge-addition operation in a charge-to-voltage converter, division on capacitance in the CDS circuit is not necessary, as with the cases of known arts.
In this embodiment, the FD portion is configured to be shared among pixels vertically arranged. A signal processing can likewise be achieved also when the FD portion is shared among pixels horizontally arranged. In addition, the technique changing an addition ratio by setting different exposure times can also be employed when FD portion is not shared.
Third Embodiment
Embodiments of the present invention may also be applicable to other signal readout configurations than the CDS circuit. For example, a signal processing technique can likewise be achieved even when a column circuit having an analog-to-digital converter (ADC) is provided for each column. For a comparison circuit in the ADC, differential circuits whose sizes i.e., amplification factors, are different from each other, e.g., Standard Size and ⅓ Size, may be connected in parallel as shown in FIG. 8 . Further, it becomes possible to switch between various output resolution modes by changing the connections of a plurality of differential circuits of various sizes appropriately.
Fourth Embodiment
In the configuration described in the second embodiment in which a FD portion is shared, an addition operation can be performed between pixels that share the FD portion. However, this addition operation is inapplicable to pixels that do not share the FD portion. For example, when the FD portion is to be shared between four pixels vertically arranged, a charge-addition operation can be performed on two pixels of each identical color. However, when an addition operation is desired with respect to three pixels of an identical color and three pixels of another identical color (3×3 pixels) or 4×4 pixels, for example, a driving method other than the one in the above described embodiment is necessary, since a unit of pixels to be added includes one or more pixels which belong to a different FD sharing unit.
As shown in FIG. 9 , in performing an addition operation with respect to 3×3 pixels, an averaging operation may be performed between a signal yielded by a charge-addition operation in a FD portion (charge-added pixel) and a signal from an adjacent pixel (non-added pixel) which has not been added, thereby obtaining an expected signal. It is to be noted, however, this operation results in two types of operational block having different orders of the charge-added pixels and the non-added pixels, as indicated by A and B in FIG. 9 . In this case, a suitable driving sequence of a transfer gate may need to be configured using an appropriate driving logic.
An operation for adding signals from 4×4 pixels will now be described with reference to FIGS. 10A and 10B , by way of example. In this case, addition is performed by adding, at a predetermined ratio, the signals which are obtained by the addition operation conducted in FDs. An addition operation on four pixels having an identical color without changing the addition ratio yields the result that, while the center of a virtual pixel G (green), expressed as an added G signal in FIG. 10A , is spaced apart by a distance corresponding to three pixel pitches from the center of the adjacent virtual pixel B (blue), expressed as added B signal, the center of the same virtual pixel G is spaced apart from another adjacent virtual pixel B by a distance corresponding to five pixel pitches, thus developing a distance ratio of 3:5. An addition operation on four pixels of an identical color is performed while taking this ratio into account. More specifically, the addition is performed by setting a ratio of 5:3 between Q 12 which is the result of the addition on the charges (Q 1 , Q 2 ) of two pixels out of the four pixels and Q 34 which is the result of the addition on the charges (Q 3 , Q 4 ) of the other two pixels. As a result of this addition operation performed at the ratio of 5:3, an equal distance or pitch, which amounts to four pixel pitches in this case, can be obtained between the centers of the successive virtual pixels B and G. As for the substantial procedure for the addition operation, one described in the first or second embodiment can be employed.
Thus, according to the embodiments of the present invention, the pitch between each pair of the adjacent apparent pixel centers of the low-resolution output signal can be equalized by the addition-averaging operation performed in the course of readout, thereby enabling high-speed output without changing any color arrangement of the pixel array. In a solid-state imaging device configured to have a charge-to-voltage converter shared among a plurality of pixels, the low-resolution signals can be output without changing the color arrangement, regardless of any difference between the unit of the pixels sharing the converter and the unit of the signals to be added.
Furthermore, according to the present invention, a solid-state imaging device may be a one-chip type solid-state imaging device, or may be a module type solid-state imaging device formed from a plurality of chips. A module type solid-state imaging device includes at least a sensor chip for imaging. The module type solid-state imaging device may further include an optical system.
FIG. 11 is a camera to which the present invention may be applied, which includes a imaging portion 71 and an optical system 72 . When the present invention is applied to a camera, the pitch between each pair of the adjacent apparent pixel centers of the low-resolution image signal can be equalized by the addition-averaging operation performed in the course of readout, thereby enabling high-speed output without changing any color arrangement of the pixel array. In a camera including a solid-state imaging device configured to have a charge-to-voltage converter shared among a plurality of pixels, the low-resolution signals can be output without changing the color arrangement, regardless of any difference between the unit of the pixels sharing the converter and the unit of the signals to be added.
It should be understood by those skilled in the art that various modifications, combinations, sub-combinations and alterations may occur depending on design requirements and other factors insofar as they are within the scope of the appended claims or the equivalents thereof.
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A driving method for a solid-state image pick up device that includes the steps of capturing an image with the pixel array, sharing at least two color pixel cells with a floating diffusion unit, adding an output signal of a first color pixel cell to an output signal of a second color pixel cell having the same color as the first color pixel cell with the floating diffusion unit in order to create a virtual pixel center, and controlling a ratio of integration time of the color pixel cells to the same colors based on pitches between virtual pixel centers with a control unit.
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BACKGROUND OF THE INVENTION
This invention relates to systems for pumping water-borne solid articles such as fish, marine crustacea and others, and is herein illustratively described by reference to the presently preferred form thereof as applied to pumping fish. It will be recognized, however, that certain modifications and changes with respect to details may be made, and that the invention may be used in other applications without departing from the essential features involved.
Fish and other food articles have been pumped with water through conduits by a variety of techniques. One in use employs a submersible on-line centrifugal pump through which the articles must pass. Such pumps are in commercial use to brail herring and other small fish from fishing nets, to transfer fish from the flooded holds of fishing vessels to receiving tanks in processing plants, and in similar applications. However, attempts to use such pumps of practical size for larger fish or more delicate forms of marine life can present problems due to flesh damage.
In air lift pumping, air under pressure is injected into the vertical run of a water primed siphoning conduit so as to lift the water and articles borne by the water through the conduit. These pumps, requiring no moving parts within the transfer path, have a gentle action. However, their pumping height capability is too limited for many applications. Attempts to achieve increased lift by lowering the inlet end of the conduit further below the water's surface is limited by physical constraints in most cases.
Water jet pumps are also in use. These pumps can move a column of water carrying solid articles to considerable heights and, like air lift pumps, operate without necessity of the articles passing through a mechanical impeller. However, article damage is nevertheless a problem with water jet pumps if attempting to achieve the lift height required for many applications because of the high degree of turbulence and the high pressure gradients within the jet injection chamber of the conduit causing flesh damage and disintegration of more delicate marine life such as shrimps and crabs.
The present invention is directed to providing an improved pumping system for such applications and, more particularly, a pumping system that effectively utilizes the lift capability of a water jet pump and, in fact, increases that capability while greatly reducing the article damage experienced in water jet pumps operated at comparable jet velocity.
A further object hereof is to devise an improved pumping system achieving the described results at relatively low cost and without unduly bulky apparatus requirements. A related object is to provide such a system which is relatively easy to install, relatively light in weight and uses components that can be made stowable and readily moved about for assembly and disassembly aboard fishing vessels, and in similar applications.
A further object hereof is to improve the efficiency of jet pumps, particularly jet pumps when used for pumping liquid-borne solid articles. It is a further object to minimize wall abrasion damage of solid articles being pumped.
SUMMARY OF THE INVENTION
In accordance with this invention as herein disclosed, the described objectives are attained by combining the effects of an air lift pump with a water jet pump mounted in the transfer conduit above the air lift pump and preferably as closely adjacent the discharge end of the transfer conduit as is practical. Aeration of the water produced by the air pump is found not only to materially increase the lifting capacity of the jet pump by reducing the average density of the column of water being raised by the jet pump, but it also serves to reduce article damage from wall abrasion and impact effect of the high-velocity water jets. Comparable results even approaching these have not been possible with either pumping system acting alone or with any other system of which applicant is aware.
At the same time, the system lends itself to further increasing the pumping height by submergence of the air ring or nozzle in the body of liquid being pumped upwardly, the depth of submergence adding proportionately and directly to the lift capability of the system. Moreover, the system is self-priming and, thus, inherently adaptable to either intermittent or continuous service.
With the improved pump system of this invention the air lift pump, aiding the jet pump both as a booster and in its otherwise unique role as an aerator, provides the effect of additional depth of submergence of the transfer conduit inlet, giving the pump system capability of pumping to increased heights above liquid surface level within given depth of submergence limitations of the installation. Despite the added energy requirements imposed to drive the air lift pump compressor, overall efficiency is maintained--even increased--by the reduction of liquid/article friction in the transfer conduit. This is especially so if the jet pump is positioned in the conduit at or near the highest point in the upward run of conduit such that liquid friction losses in the conduit are minimized where flow velocity is highest, with the air pump nozzle array located at or near the inlet. Under these conditions, article damage is kept at a minimum. In fact, with the novel system it has proven possible to elevate salmon as large as 25 pounds 15 feet or more without appreciable bruising or flesh damage, whereas smaller fish and other forms of marine life can readily be lifted to appreciably higher levels with little or no damage, feats not possible in such measure with conventional pumps.
In the preferred mode and embodiment of the invention the air lift pump nozzle array is positioned with little or no submergence. It should be recognized, however, that it can be submerged and that it will be submerged to increasing depths if and as the transfer conduit upon which it is mounted is submerged to achieve increased pumping height when the confinement limitations of the body of liquid/articles to be pumped permits it and the installation requires it. Further, the jet pump is designed without a diffuser, an advance permitted by the aerated condition of the liquid being pumped. Eliminating the usual diffuser avoids a change of cross-sectional area in the transfer path of liquid being pumped. This, together with use of reduced jet pump pressures selected to achieve correctly designed cross-sectional area ratio of jet nozzles and main channel, further reduces impact damage of the fish or other articles being pumped.
In operation, water with entrained solids or articles is drawn from an open container or enclosure, such as a fishing net, through an inlet and pumped to an elevated dischage point where it is discharged into a suitable receiver. The system is operable in a steady continuous manner or at intervals if desired. It is well suited to convenient intermittent or periodic operation because of the simplicity of the priming procedure, which is achieved by turning on the jet pump to fill the conduit and thereupon creating upward lift pressures therein, whereupon the air lift pump is activated to initiate immediate full-scale operation. All of this is accomplished very quickly without need for separate or complex equipment or procedures.
Moreover, the compact portablilty of the system, which is lent to unitized construction, like conventional jet pumps or air lift pumps, offers advantages. It can be hoisted and supported by a mast and boom on a vessel or dock and can be raised and lowered by cables, sheaves and winch apparatus so as to operate from a ship's hold flooded for the purpose or from the confines of a fishing net over the side. If desired, submersion depth adjustments, or conduit length variations needed to maintain submergence when surface level drops relatively, may be effected by any of different means including forming the transfer conduit extending between the jet pump and air lift pump from mutually telescoping sections.
These and other features, objects and advantages of the invention will become more fully evident from the description that follows by reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified vertical sectional view of a fish transfer installation depicting a system of the invention being used to transfer fish from the flooded hold of a fishing vessel to that of a larger buyer's vessel.
FIG. 2 is an enlarged sectional side elevation of the preferred jet pump shroud and nozzle unit embodied in a section of the transfer conduit.
DETAILED DESCRIPTION
As depicted, the system is shown set up to pump fish such as herring, salmon or other types from the flooded hold 14 of fishing vessel 15 to the hold 18 of a larger fish buyer's vessel 17. The specifics of controls and mounts are or may be a matter of choice or engineering to suit each of the requirements of each installation. The transfer conduit C leads upwardly from hold 14 to a dewatering chute 3 that directs the fish into hold 18 while returning the gurry-rich water back into hold 14 through pipe 12 where it aids in the foaming action within conduit C as described. Jet pump 1, which may draw water from over the side of the vessel or from hold 14, is operatively mounted between the discharge section 11 of transfer conduit C and the inlet section 4 of conduit C. Discharge section 11 includes mutually telescoping tubes 11b and 11 c interengaged in slidable relationship to permit varying the lateral reach or length of the transfer conduit between dewatering chute 3 and the upwardly directed portion of conduit C. The inlet section 4 of conduit C includes two mutually telescoping tubes 4b and 4c sealed in slidable relationship to permit varying the depth of immersion or the vertical drop of inlet 4 to reach the contents of ship's hold 14. Air lift pump 2 comprising a circular array of air discharge nozzles is mounted near the lower or inlet end of tube 4b to inject streams of air bubbles into the conduit from a plurality of circumferentially spaced points around its periphery. Nozzle 2, as thus mounted in and upon tube 4b, is adapted to be lowered to varying depths of submersion into whatever body of liquid is being pumped upwardly in conduit C.
Air lift pump 2 is supplied with air under pressure from an air compressor 9 through flexible low pressure hose 7. Jet pump 1 is supplied through pipe or hose 6 with water under pressure from pump 8. The latter preferably comprises a centrifugal water pump drawing water through hose 13, and may be operated at any of different output pressures under control of a suitable pump speed regualtor 8a. If desired, air volume from compressor 9 may also be varied by means schematically depicted as a drive speed controller 9a.
The entire assembly, conveniently manufactured as a compact and portably usable unitized system with parts that may easily be assembled for use and disassembled for shipment and stowage, may be suspended by lines from suitable supports, such as the mast 19a and boom 19b of vessel 17 with steadying and guying from mast 16a and boom 16b as well as other points of guy line securement on vessel 15.
Jet pump 1 shown in FIG. 2 is embodied in a conduit section C1 flanged and bolted serially in the conduit C. Its internal diameter matches that of the main conduit. It is surrounded by a jacketing shroud or annular plenum 1a. The plenum has a circumferentially spaced series of upwardly directed passages 1b that terminate in orifice openings 1c in the interior wall of conduit section C1, which orifices thereby produce a circumferentially distributed series of upwardly directed jets of liquid such as seawater under pressure delivered to plenum 1a by pump 8. The jet discharge directions are angled, such as at about 15°, to the conduit axis. The area ratio of the jet orifices and the interior of conduit C is determined so as to provide efficient pumping to desired heights having regard to the objective of avoiding article damage through maximizing jet flow volume at minimum jet flow velocity. As previously explained, the aerated condition of the column of water with articles being induced to flow upwardly in conduit C is created by the aeration effect of air lift pump 2. The system operates effectively in saltwater and in freshwater. When pumping fish and other marine creatures, attendant blood, slime and other protein materials tend to act as foaming agents. While foaming can prove troublesome if excessive, a normal concentration of such foaming materials in the water being pumped is acceptable and may even prove to be of aid in the avoidance of article damage.
In typical installations, depending upon types and sizes of articles to be pumped and upon pumping height and rate requirements, the conduit C may have an internal diameter in the range, for example, from 4" to 20", and may be designed in its upwardly extending length or reach dimensions to pump as high as 20 feet or more.
When pump 8 is primed and operating, conduit C fills with water, eliminating the air. Water then induced to flow upwardly in conduit C under pressure from pump 8 and aided by atmospheric pressure sucks water upwardly from hold 14 to the discharge chute 3. The air compressor 9 is then placed in operation, forcing air into the air orifice assembly 2. The air injection thereupon increases the flow rate to a significantly higher value, such that fish in hold 14 become entrained in the flow entering the inlet end of the conduit C. Upon reaching jet pump 1, additional energy imparted by the jets to the upwardly flowing mixture occurs, yet it does so without material damage or bruising of the fish. The aerated lightness of the columnar flow has a cushioning or insulating effect preventing this and also preventing abrasion damage of the fish from rubbing on the conduit walls. The air bubbles which make up nearly half the flow under an efficient operating balance in the system, act to cushion the fish.
If desired, a foot valve 10a may be mounted in the lower inlet end of conduit section 4b to close and hold water in the conduit when the pumps are shut down. This expedites priming and restarting of the system after a period of idleness.
If added pumping height is needed above that being produced under an existing set of operating conditions, or it is desired to reduce jet water flow pressure and volume, the inlet end of conduit C may be more deeply submerged in the mixture being pumped. With every foot of increased depth one added foot of above-surface pumping height is achieved.
With an 8" conduit, the average fish transfer rate achieved for essentially "dry" herring was 35 to 40 tons per hour at water shroud pressures ranging from 40 psi to 57 psi at a maximum lift height of 12 feet. Air was added at a rate to reduce aerated water column average density approximately in half. With a 10" conduit, the average transfer rate of "dry" herring was up to 100 tons per hour under similar conditions. Similarly, salmon up to 25 pounds were pumped out of fish holds to a height of 15 feet and live salmon were pumped from seine nets without damage to an equivalent height at the rate of 13,000 fish in one and a quarter hours at 20 psi water jet shroud pressure.
In practical designs, with an 8 inch conduit (internal area of 0.3474 square feet), water jet nozzle internal area (with 8 nozzles) totalled 0.0336 square feet, for an area ratio fo 0.097. For a 10 inch conduit the corresponding values proving best were 0.5456, 0.0557 and 0.10, respectively. With a 20 inch conduit, not yet tested, these values are calculated to be 2.183, 0.2176 (16 nozzles) and 0.10, respectively. Companion to those water jet area and area ratio values for the 8 inch, 10 inch and 20 inch conduits are the following air shroud design and operating values:
______________________________________ Air Hole No. of Air FlowConduit Diameter Holes Range______________________________________ 8 inch 0.25 inch 30 Up to 120 CFM at 2PSG10 inch 0.25 inch 66 Up to 150 CFM at 2PSG20 inch 0.25 inch 110 Up to 500 CFM at 2PSG______________________________________
Those values apply to the transfer mode, i.e., pumping from one fish holding tank to another. When pumping from an open net with greater submergence of the intake, more air flow was supplied to achieve equivalent results with lower jet water pressure and flow.
These and other aspects of the invention will be evident to those skilled in the field of pumping systems, particularly as applied to fish transfer applications, who will thereby appreciate the illustrative and not necessarily delimitative purpose of the foregoing disclosure of the presently preferred embodiment and application of the invention.
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An article transfer pumping system combining the effects of a jet pump and an air lift pump to minimize article damage while increasing lift capability and overall system efficiency. Air lift pump placement adjacent the pump inlet aerates the rising column of water with articles such as fish, even large salmon, being raised by the jet pump, whereas jet pump placement adjacent the discharge end of the conduit increases pump efficiency.
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BACKGROUND OF THE INVENTION
The present invention relates to a device for point feeding or servicing an electrolytic cell, in particular a cell for producing aluminum.
In the manufacture of aluminum from aluminum oxide the latter is dissolved in a fluoride melt made up for the greater part of cryolite. The aluminum which separates out at the cathode collects under the fluoride melt on the carbon floor of the cell; the surface of this liquid aluminum acts as the cathode. Dipping into the melt from above are anodes which, in the conventional reduction process, are made of amorphous carbon. As a result of the electrolytic decomposition of the aluminum oxide, oxygen is produced at the carbon anodes; this oxygen combines with the carbon in the anodes to form CO 2 and CO. The electrolytic process takes place in a temperature range of approximately 940°-970° C.
The concentration of aluminum oxide decreases in the course of the process. At an Al 2 O 3 concentration of 1-2 wt.% the so-called anode effect occurs producing an increase in voltage from e.g. 4-4.5 V to 30 V and more. At this time at the latest the crust must be broken open and the concentration of aluminum oxide increased by adding more alumina to the cell. Under normal operating conditions the cell is fed with aluminum oxide regularly, even when no anode effect occurs. Also, whenever the anode effect occurs the crust must be broken open and the alumina concentration increased by the addition of more aluminum oxide, which is called servicing the cell.
For many years now servicing the cell includes breaking open the crust of solidified melt between the anodes and the side ledge of the cell, and then adding fresh aluminum oxide. This process which is still widely practiced today is finding increasing criticism because of the pollution of the air in the pot room and the air outside. In recent years therefore it has become increasingly necessary and obligatory to hood over or encapsulate the reduction cells and to treat the exhaust gases. It is however not possible to capture completely all the exhaust gases by hooding the cells if the cells are serviced in the classical manner between the anodes and the side ledge of the cells.
More recently therefore aluminum producers have been going over to servicing at the longitudinal axis of the cell. After breaking open the crust, the alumina is fed to the cell either locally and continuously according to the point feeder principle or discontinuously along the whole of the central axis of the cell. In both cases a storage bunker for alumina is provided above the cell. The same applies for the transverse cell feeding proposed recently by the applicant (U.S. Pat. No. 4,172,018).
The numerous known point feeder systems e.g. German Pat. No. 2 135 485 and U.S. Pat. No. 3,371,026 or the elements thereof are mounted rigidly onto the cell superstructure. This has the disadvantage that repairs to the device and changing parts is often complicated and time-consuming. Furthermore, the alumina can not always be fed to the best position in the molten electrolyte.
It is therefore a principal object of the present invention to develop a device for point feeding an electrolytic cell, and namely such that the said device is easy to service i.e. feed, that it ensures the alumina is fed to the best position, and that it can be built on to existing cells without great expenditure.
SUMMARY OF THE INVENTION
The foregoing object is achieved by way of the present invention in the form of a point feeder unit which can be slid freely on a beam in the longitudinal and/or transverse direction and can be removed vertically by means of a crane, the feeder unit being made up of:
(a) a feeding device, comprising a storage bunker with a large container for alumina and a small container for additives, a dosing device and a run-out pipe which can always be extended in a telescopic manner to the place where the crust has to be broken open, and
(b) a crust breaking facility which is secured releasably to the storage bunker by a suspension means, can be raised separately in the vertical direction and comprises a pressure cylinder system, a chisel and a housing with chisel alignment means secured to a lower flange on the pressure cylinder.
Two such point feeder units on a fixed cross beam arranged on the anode supports are preferred for each cell. The freedom of movement of the units in the longitudinal and/or transverse direction is limited solely by the hooding on the cell.
The point feeder units are provided at the top with hooks. The feeder units can easily be raised with a crane and likewise can be replaced by another unit in a very short time. If necessary, the crust breaker can be removed or replaced separately.
BRIEF DESCRIPTION OF THE DRAWING
The present invention will now be explained in greater detail with the help of schematic drawings of the exemplified embodiments wherein,
FIG. 1: Is a view of a point feed unit mounted on a beam.
FIG. 2: Is a view of a feeding system with end piece of the feed pipe inside the storage bunker.
FIG. 3: Is a view of a mobile run-out pipe attached to the alignment housing.
FIG. 4: Is a view of a pressure cylinder system of a crust breaking facility in the position ready for operation, shown here partly in cross section.
FIG. 5: Is a vertical, longitudinal section with a view through part of the lower region of a crust breaker in the non-operating position, shown here with a chisel alignment device.
FIG. 6: Is a horizontal section through line VI--VI in FIG. 5.
FIG. 7: Is a view of a bell-shaped chisel with conical recess.
FIG. 8: Is a view of a bell-shaped chisel with blunted cone recess.
FIG. 9: Is a view of a fish-tail-shaped chisel with wedgeshaped recess.
FIG. 10: Is a detail A of the shape of the edge region of the chisels shown in FIGS. 7-9.
FIG. 11: Is another version of the edge region A.
FIG. 12: Is a longitudinal section through a chisel which is rectangular in cross section and has projections provided on its narrow sidewalls.
FIG. 13: Is a view of a chisel which is round in cross section and is provided with two pairs of projections at different levels on the chisel sidewall.
FIG. 14: Is a longitudinal view, shown partly n cross section, of a chisel with projections of various sizes on its sidewall.
DETAILED DESCRIPTION
FIG. 1 shows a point feeder unit which is shown later in detail as a whole. The unit can be dismounted from beam 10 and raised up by means of a crane and hooks on the storage bunker 12 which are not shown here. The crust breaking facility comprising the pressure cylinder system 24,26, the chisel 30 and the alignment housing 32 is releasably mounted on the storage bunker 12 and can also be raised separately by a crane. Below the point feeder unit are carbon anodes 38, the alumina 40 which has been poured onto the crust 42 and the molten electrolyte 44.
Also shown in FIG. 1 is a storage bunker 12 with a large container 13 for alumina and a small container 15 for additives such as e.g. cryolite, aluminum fluoride and ground electrolyte crust. Both containers are separated by a flat, vertical dividing wall 14. The alumina bunker 12 in FIG. 2 differs in its subdivision into a large container 13 and a small container 15. The small container 15 is delimited by a tube wall 54. In both cases, with the flat dividing wall or with the tube-shaped container, the volume of the small container preferably amounts to 0.5-25 vol.%, in particular 5-20 vol.% of the volume of the whole storage bunker 12.
The sliding plate valve 17 which delimits the storage bunker 12 at the bottom can be in one or two parts. The two-part plate 17 which is provided at the bottom of the dividing wall 14 can be employed for mixing the charge in that both halves can be withdrawn to varying degrees depending on the amount to be fed from each compartment of the storage bunker.
At the bottom of the storage bunker there is a flange which is connected to the dosing facility 16. This dosing facility is for example, in accordance with one of the versions described in the U.S. patent application Ser. No. 124,598 in the form of an alumina drawer. A piston arrangement pushes per stroke a specific amount of alumina or additives e.g. 1 kg into the outlet pipe 18. The material pushed out falls, via the lower, inclined part of the outlet pipe, onto the part of the crust broken open by the chisel.
Usefully the feed pipe, which is supplied with alumina and/or additives, branches just before or immediately after it enters a storage bunker which is fitted with a top sheet. One end of the branched feed pipe is situated over the large container for the alumina and is provided with a plurality of outlets. The other branch of the feed pipe terminates over the small container for the additives and is, depending on the dimensions of this small container, provided with one or more outlets. Both end pieces of the feed pipe lie preferably on a horizontal plane. At the branching point or just after that suitable diversion or blocking facilities are provided; these allow the following modes of supplying the containers in the storage bunker:
(a) the material being supplied flows through both end pieces into both containers,
(b) the material being supplied flows through one end piece into the large container,
(c) the material being supplied flows through one end piece into the large or the small container,
(d) both end pieces are closed to the material in the feed pipe.
According to the version in FIG. 2 one end of the supply pipe 46 from the pressurized chamber to the large container 13 is shown in the upper part of the storage bunker 12 which is provided with a top sheet 52.
The alumina enters the large container through outlets 50. The other end piece with the outlet over the small container is not shown here.
If the electrolyte has been depleted of additives and, for example, has become alkaline or too acidic, and both containers are full of alumina, then the sliding valve 17 is set such that only the alumina in the small container flows out. The end piece for the alumina is closed, the necessary additives charged into the pressurized chamber and passed along the supply pipe 46 into the small container 15 via the appropriate outlets. With the sliding valve 17 open for the small container the additives, if desired with some alumina, are fed to the cell via the dosing facility 16 and the outlet pipe 18. This method is, however, useful only when the volume of the small container is small compared with the volume of the storage bunker as a whole, as, otherwise, there could be a long delay before the additives reach the cell due to the length of time to empty the container.
When charging with alumina, therefore, the outlet from or the inlet opening to the small container 15 can be closed, so that all the alumina is charged to the large container 13. The small container 15 remains empty and can be used any time to supply the bath quickly with additives.
The inclination of wall 19 of the container 13 must be at least such that even the poorest flowing material will flow down it.
Any mixture of alumina and additives, if desired, can be achieved not only by means of a two-part sliding valve 17, but also by raising pipe 54.
With all versions of the storage bunker the steps in the process, for supplying alumina and additives, for setting the sliding valve 17 and for operating the dosing facility 16 are initiated and controlled by means of a central data processing unit.
The design of the storage bunker according to the present invention has the advantage that the additives can be fed to the bath at any time, quickly, in any amount desired and in a closedoff system of material flow. This means that the hooding on the cell does not need to be opened, the regular feeding from the silo is not interrupted and no separate feed pipe with separate compression chamber need be constructed.
FIG. 3 shows the connection between the movement of the working cylinder 26 and the outlet pipe 18 which is telescopic in design. The housing 32 for the alignment of the chisel 30 secured to the piston rod 28 of the pressure cylinder is mounted, preferably air-tight, on the lower flange of the pressure cylinder 26. The lower, mobile part of the outlet pipe is suspended from the mechanically stable housing 32 via a support arm 20. The upper, stationary part 56 which is attached to the dosing facility has a smaller diameter so that the mobile part 58 can be slid over it like a sleeve.
When the crust breaker is in the non-operating position--not shown in FIG. 3--the mobile part 58 of the alumina outlet pipe fits completely over the fixed, stationary pipe length 56. If the pressure cylinder 26 is lowered into the position for working the support 20 attached to the housing 32 is lowered also and with it the mobile pipe length 58 the same distance. This design ensures that the alumina is always fed to the same place and that the outlet pipe, when not in use, e.g. during anode changes, is raised out of the way. In the position ready for working--as is shown in FIG. 3--the chisel 30 is drawn up inside the housing. In the working position, however, the chisel 30, but not the housing 32, is lowered.
The crust breaking facility in FIGS. 1 and 4 comprising a pressure cylinder system with two cylinders is secured to the suspension means 22. The piston rod 60 in the positioning cylinder 24 is releasably connected to the suspension means 22 by means of an upper flange e.g. by bolts. The lower flange of the positioning cylinder 54 and the upper flange of the working cylinder 26 are likewise joined together mechanically, permanently or releasably so. Provided in the working cylinder 26 is a piston rod 28 which can be driven downwards and which carries the chisel 30 for breaking open the crust.
The sequence of operation of the crust breaker powered by the pressure cylinder system can be described schematically as follows:
1. The piston rods 60, 28 of the positioning and working cylinders respectively are in the withdrawn position when the crust breaker is not in operation. This is the position required for anode changes when the chisel 30, for physical reasons, and the working cylinder 26, for thermal reasons, must be kept as far as possible from the anodes, and for working on the crust breaker i.e. when the suspension means 22 is freed from the beam. This non-operative position is shown in FIG. 1.
2. FIG. 4 on the other hand shows the extended piston rod 60 of the positioning cylinder 24; the crust breaker is ready for operation. The piston rod 28 of the working cylinder 26 is still withdrawn but ready for working. Position A in FIG. 4 shows the starting position for maintaining an opening in the crust in order that alumina can be fed to the cell.
3. In FIG. 4, position B, the piston rod 28 of the working cylinder 26 is shown extended and the crust has been broken open by the chisel 30 which has been lowered to the end of the stroke of the working cylinder. After reaching this position, the chisel, having broken through the crust, is made to reverse its direction of movement. The return of the chisel or piston from the lower position is initiated pneumatically or by position sensors. This working sequence is repeated according to a specific program. Should the piston not reach the end position, it is returned after a predetermined interval.
In the case of the other arrangement for mounting the crust breaker--not shown here--in which the upper flange of the positioning cylinder 24 is releasably attached to the suspension means 22, the sequence of operation is in principle the same. The only difference is that the piston rod 60 is lowered and not the positioning cylinder 24 as shown in FIG. 4.
The total length of stroke between the working and non-working position of the chisel 30 on the working cylinder piston rod 28 is divided between the poitioning and working cylinders in a manner depending on the geometry of the electrolytic cell. If the total length of stroke is ca. 900 mm, the positioning cylinder can have a stroke of 300 to 500 mm and the working cylinder a stroke of 400-600 mm. FIGS. 5 and 6 show a square shaped alignment box 32 made of steel sheet. The chisel 30, in this case fish-tail-shaped, passes through this box. Two parallel alignment faces 31 on opposite broad sides of the chisel 30, which is rectangular in cross section, are at a distance of <1 mm from and come into contact with a pair of alignment rolls 34 on the sides of the alignment box 32. The relatively massive structure of the chisel 30 prevents the other sides of the chisel which are not in contact with the alignment rolls from being deflected out of line. According to another version, which is not shown here, a further pair of alignment rolls can be provided on the other sides, or the alignment rolls, preferably positioned in the middle, extend over a large part of the broad faces of the chisel.
The bearings 35 for the rolls are securely fixed to the upper side of the bottom sheet of the alignment box or housing e.g. by welding. A wiper 36 for wiping electrolyte material from the chisel is provided on the under side of the bottom sheet. This paper which extends over the whole breadth of the alignment surfaces prevents solidified electrolyte from reaching the alignment rolls when the chisel is raised. No wiper is provided on the narrow faces of the chisel 30.
In longitudinal cross section the wiper 36 is V-shaped whereby the angle α is usefully between 90° and 150°. The alignment housing 32 which is gas-tight in its upper part penetrates the hooding 62 over the cell, whereby, to achieve a more effective hooding of the cell, plates 64 which provide sealing are also provided.
FIG. 7 shows a cylindrically shaped chisel 66 which, instead of having a flat end face at the bottom, has a conical recess 68 there. The surfaces of this conical recess 68 and of the cylinder 66 form a cutting face which can be seen from below as being circular and which represents the punching or working face. The angle α formed by the faces of the conical recess 68 is preferably 15°-45°. If this angle is smaller the effect of the chisel in question as a punch diminishes progressively; angles larger than 45° are progressively less and less interesting for physical and economic reasons.
On lowering the chisel 66 a circular hole is punched in the crust of solidified electrolyte. In the process of doing this, small, outwardly directed components of force are produced. The forces developed by the faces of the conical recess are directed inwards and act therefore on that part of the crust which has to be penetrated.
If the recess in a cylindrically shaped chisel 66 is of a blunted cone shape, as in FIG. 8, the sidewall of the blunted cone acts in the same way as the sidewall 68 of the cone in FIG. 7. The horizontal surface 72 exercises its exclusively downward directed force only after the chisel has already been pushed a distance into the crust.
FIG. 9 shows a, in cross section, rectangular chisel 74 which has a wedge-shaped recess 76 on its end face instead of a horizontal flat surface. The criteria which determine the choice of the angle of inclination α of this fish-tail shape are the same as in the previous figures. The triangular shaped recess shown in FIG. 5 can, according to another version not shown here, also be trapezium-shaped, like that in FIG. 8.
FIG. 10 shows an enlarged view of one version of the punching or working edge. The recess, regardless of whether it is conical or wedge-shaped, runs first at a steep angle 78 and then changes over to a flatter angle 80. This has the advantage that the chisel can be pushed through the crust with less force. Only very hard, wear-resistant chisel materials can be used with this design.
A further version of working edge is shown in FIG. 11. The recess does not begin at the periphery of the chisel, but slightly nearer the center, as a result of which a horizontal surface 82 is formed around the edge region. The recess 84 begins at the inner edge of this horizontal surface, with the angle α preferably having the above mentioned values. This design of chisel requires more force to be applied initially when forcing its way through the crust; however, the degree of wear on the chisel is less.
FIG. 12 shows a chisel which in cross section is an elongated rectangle, in this case measuring 150×40 mm. The lower part of the chisel 74 is dipping into the molten electrolyte 44 i.e. it has completely penetrated the solidified melt 42. This lower part of the chisel is fish-tail-shaped. Although this shape can be used advantageously, all other suitable chisel end shapes can also be employed.
The lower pair of projections 86 have been pushed almost completely through the crust 42. This has resulted in a space 88 being created between the chisel 74 and the solidified melt 42 through almost the whole thickness of the crust. As indicated in FIG. 12, the alumina 40 lying on the crust 42 runs through this gap. This gap ensures that the chisel 74 is not jammed in the opening and after penetrating the crust can therefore be readily withdrawn again. The next time the cell is to be fed, which with automated systems takes place after a short interval of time, the chisel can be introduced into the hole without difficulty because of the extra space provided there by the projections on the chisel sidewalls. If the chisel is not exactly centered it pushes away, without any difficulty or large expenditure of force, the ridge 43 of solidified melt 42 left over after the previous feeding of the cell.
In versions not shown additional projections can be provided on the broader sidewalls of the chisel.
Also, the chisel can be lowered even further so that the lower pair of projections 86 push completely through the crust.
The lower face of the projections which faces downwards and which is about 1 cm 2 in cross section is undercut, preferably at an angle of up to 20°. The face of the projection inclined upwards towards the chisel sidewall causes the projections to act like teeth.
The pieces of crust and alumina pushed down into the electrolyte by the under side of the chisel are, for the sake of simplicity, not shown here.
FIG. 13 shows a chisel 66 which is round in cross section. It is to be understood that the invention is not limited to the illustrations described and shown herein, which are deemed to be merely illustrative of the best modes of carrying out the invention, and which are susceptible of modification of form, size, arrangement of parts and details of operation. The invention rather is intended to encompass all such modifications which are within its spirit and scope as defined by the claims. In this case too it holds that the conical lower part of the chisel can be of any other suitable form.
A lower pair of projections 90 extend round the greater part of the chisel periphery. Another part of projections 92 at a higher level on the other hand extend around a relatively small part of the chisel periphery.
Whereas the projections shown in FIGS. 12 and 13 are characterized not only by way of being elongated and horizontal but also by being uniformly broad, the projections on a chisel 66,74 shown in longitudinal cross section in FIG. 14 have different breadths. The lowest projection 94 which is the first to come into contact with the crust is narrow, the projection 96 above this broader and the uppermost projection 98 the broadest. This causes the space formed between the chisel and the crust when the crust breaker is lowered to be increased in stages from the bottom to the top.
Prefabricated projections can be attached to the chisel sidewalls by welding or bolting. The projections can also be deposited in the form of weld beads and, if desired, given their final shape by some suitable shaping process. Furthermore, the chisel and projections can belong to the same piece in that the latter are created e.g. by machining.
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The invention relates to a device for point feeding an electrolytic cell, in particular a cell for producing aluminum. A point feeder unit comprising a raw materials feeding device and a crust breaking facility releasably mounted on a storage bunker is mounted on a beam, can be freely displaced along and/or across the cell and can be removed in the vertical direction with a crane.
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BACKGROUND OF THE INVENTION
The present invention relates to a building structure which comprises a restaurant and an amusement area arranged such that restaurant patrons can easily view the amusement area while dining.
Previous building structures which provide for diversity of use have included arrangements as described in a number of U.S. patents. Currier, U.S. Pat. No. 4,274,233 discloses a building layout for a combined restaurant and artists work area. Restaurant patrons can view the artists at work, however, provision for the separation of the artist's areas and the dining area by the interposition of a viewing pane adjacent a structural member common to both areas is not taught or suggested by Currier. Yuter, U.S. Pat. No. 5,193,648 discloses a restaurant construction system whereby an order-taking person at an order-taking post can see a patron at a table located on a lower terraced level. Obata, U.S. Pat. No. 3,002,233 discloses an auditorium which can be used as a single large space or partitioned into several smaller spaces through the use of movable partition walls.
SUMMARY OF THE INVENTION
The present invention provides a building structure within which a setting is maintained which allows restaurant patrons to enjoy dining out while allowing primarily children accompanying the adult patrons the opportunity of playing in an adjacent play center without disturbing the adult patrons. The adult patrons, however, can view the children and any other amusement area patrons, allowing monitoring of the children's activity while simultaneously enjoying the view of the children at play and enjoying their meal.
In one embodiment there is provided a building structure which houses a restaurant and an amusement area, comprising an enclosed space defining a dining area, further comprising a doorway for access thereto, an enclosed space defining an amusement area, further comprising a doorway for access thereto and a viewing pane disposed adjacent a wall common to the dining area and the amusement area, whereby patrons of the dining area can view the amusement area.
In another embodiment the building structure further comprises an enclosed space defining a food preparation area accessible to the dining area.
In a further embodiment a second viewing pane is provided.
In another embodiment the viewing pane disposed adjacent a wall common to the dining area and the amusement area comprises a surface area in a range of from about 20% to about 100% of a surface area of the common wall.
In still another embodiment the viewing pane disposed adjacent a wall common to the dining area and the amusement area comprises a surface area in a range of from about 20% to about 50% of a surface area of the common wall.
In still another embodiment the viewing pane disposed adjacent a wall common to the dining area and the amusement area comprises a surface area in a range of from about 50% to about 100% of a surface area of the common wall.
In one embodiment sound proofing material is disposed adjacent the dining area and the amusement area.
In another embodiment of the building structure the enclosed space defining a dining area further comprises movable walls disposed between a first dining area and a second dining area. A movable wall can be disposed between the dining area and a coffee shop area.
In a further embodiment a means of access between the enclosed space defining a dining area and the enclosed space defining an amusement area is provided.
In one embodiment of the building structure the doorway for access to the space defining an amusement area houses a revolving door.
In another embodiment the amusement area can further include video games.
In another embodiment the amusement area can further include means for engaging in a virtual reality experience.
In another embodiment the amusement area can include one of any or all of: a non-video game, a toy, an amusement park ride, a climbing structure which can further be resilient to allow for bouncing. The amusement area can further include a tunnel, a video game and a means for engaging in a virtual reality experience.
In one embodiment there is provided a building structure which comprises: a) a first structural member enclosing a food preparation area, a dining area, an amusement area, and a lobby area, the lobby area in communication with an exterior of the building structure; b) a doorway in communication with the amusement area disposed adjacent a second structural member interposed between the lobby area and the amusement area, the amusement area including an amusement park ride housed therein; c) a third structural member interposed between the dining area and the amusement area; d) a doorway disposed adjacent the first structural member; e) a second doorway disposed adjacent the third structural member; and f) and a viewing pane disposed adjacent the third structural member interposed between the dining area and the amusement area; whereby patrons of the dining area can view the amusement area.
In one embodiment of the invention the amusement area can contain permanent or semi-permanent amusement park type rides, e.g. an astronaut ride, a jet plane ride.
In another embodiment the building structure further comprises a second viewing pane.
In yet another embodiment the building structure with a viewing pane disposed adjacent a third structural member interposed between a dining area and an amusement area comprises a surface area in a range of from about 20% to about 100% of a surface area of the third structural member.
In still another embodiment the building structure with a viewing pane disposed adjacent a third structural member interposed between a dining area and an amusement area comprises a surface area in a range of from about 20% to about 50% of a surface area of the third structural member.
In still another embodiment the building structure with a viewing pane disposed adjacent a third structural member interposed between a dining area and an amusement area comprises a surface area in a range of from about 50% to about 100% of a surface area of the third structural member.
In another embodiment the building structure further comprises a doorway disposed adjacent the third structural member interposed between the dining area and the amusement area.
In a further embodiment the building structure further comprises a gift shop and a coffee shop which can be combined or separate.
In yet another embodiment the building structure further comprises a stage adjacent the amusement area.
In still another embodiment the building structure further comprises sound proofing material disposed adjacent the dining area and the amusement area.
In one embodiment the building structure having an enclosed space defining a dining area further comprises movable members disposed between a first dining area and a second dining area.
In another embodiment the building structure wherein a doorway in communication with the amusement area disposed adjacent a second structural member interposed between the lobby area and the amusement area comprises a revolving door.
In another embodiment the amusement area can further include video games.
In another embodiment the amusement area can further include means for engaging in a virtual reality experience.
In another embodiment the amusement area can include one of any or all of: a non-video game, a toy, an amusement park ride, a climbing structure which can further be resilient to allow for bouncing thereon. The amusement area can further include a tunnel, a video game and a means for engaging in a virtual reality experience.
Other features and advantages of the invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings which illustrate, by way of example, various features of preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE FIGURES
The detailed description of the invention will be made with reference to the accompanying drawings, where like numerals designate corresponding parts of the figures.
FIG. 1 illustrates one particular embodiment of a layout of the building structure of the present invention.
FIG. 2 illustrates a particular embodiment of a rotatable doorway of the present invention.
FIG. 3 illustrates a particular embodiment of a viewing pane of the present invention.
FIG. 4 illustrates another embodiment of a viewing pane of the present invention.
FIG. 5 depicts an art projector area.
FIG. 6 illustrates a particular embodiment of a mine area.
FIG. 7 illustrates one particular embodiment of an interior of a mine area.
FIG. 8 illustrates a rocket ride.
FIG. 9 depicts a moonwalk bounce ride.
DETAILED DESCRIPTION OF THE INVENTION
It is to be understood that the Figures are illustrative of only one particular embodiment of the present invention and other configurations of areas or the nature of types of areas and/or particular combinations of amusement rides, games and the like are within the contemplation of the present invention.
FIG. 1 illustrates a building structure 10, having a doorway 1 2 allowing access from an exterior of building structure 10 to a lobby area 13. Building structure 10 includes a first structural member 11 enclosing a food preparation area 34, a dining area 26, an amusement area 41, and a lobby area 13. First structural member 11 includes a wall or walls and a roof within which the designated areas are located. The wall or walls and roof can define any shape including but not limited to a cube, a pyramid, a geodesic dome, a cylinder, a rectangular prism or combinations thereof. The wall or walls and roof can be formed of different structural elements which are joined as is known in the building arts. They can be constructed on site or off site and transported to the location at which the building structure will be erected. The first structural member accordingly encompasses any structure or technique as is known in the building arts for enclosing an interior space comprised of separate functional areas. In one embodiment first structural member 11 along a length enclosing amusement area 41 is substantially opaque. First structural member 11 can enclose fewer areas or more areas than set forth above.
Lobby area 13 is an area adjacent an exterior of building structure 10 through which access to one or more others areas can be gained. Lobby area 13 is accessible to an exterior of building structure 10 such that lobby area 13 either directly or indirectly allows one to exit building structure 10.
A gift shop 14, containing a gift shop counter 15 can be accessed through lobby area 13 or through a rocket slide 40 disposed within an amusement area 41. The terms "gift shop" and "coffee shop" are used as commonly defined. There can be a play area disposed adjacent coffee shop 18. In a further embodiment there can be an exercise area 44 adjacent coffee shop 18. Gift shop 14 and/or coffee shop 18 can be disposed adjacent to lobby area 13. Coffee shop 18 can contain a counter 20, tables 22 and chairs 24 is located adjacent lobby area 13.
A second structural member 17 can be disposed between lobby area 13 and amusement area 41. A revolving doorway 16 disposed adjacent second structural member 17 can allow for access between lobby area 13 and amusement area 41. Revolving door 16 can be in one aspect, for example, a standard revolving door with multiple partitions. In a specific embodiment a curved member bridging an entrance to an area can be rotated to allow entrance and/or exit to the area, somewhat similar to those devices which allow access to and from a darkroom without allowing light to enter.
Second structural member 17 is similar to first structural member 11, differing in that a roof is not considered an element of second structural member 17 and second structural member 17 encompasses any structure or technique as is known in the building arts for dividing an interior space comprised of separate functional areas. A doorway 37 provides access to dining area 26, which contains tables 28 and chairs 30. Door 33 provides access to and from amusement area 41, through a third structural member 35. Third structural member 35 interposed between dining area 26 and amusement area 41 is, for example, a wall separating these areas. The definition given for second structural member 17 applies to third structural member 35. However, in some embodiments, a viewing pane 31 can comprise about 100% of the surface area of third structural member 35, accordingly the definition as to viewing pane 31 would then apply to third structural member 35. Further, the third structural member can span more than one story of building structure 10, either contiguously or by position above or below third structural member 35 on a given story of a multi-story structure. Such a third structural member is still a wall in common between two areas, such as dining area 26 and amusement area 41.
A viewing pane 31 allows for monitoring of amusement area 41 from dining area 26 and vice versa. The viewing pane 31 can be disposed adjacent third structural member 35 interposed between dining area 26 and amusement area 41 to permit one to look from one area to the other. Viewing pane 31 can be a single aperture or multiple apertures in third structural member 35 between the two areas. Preferably, a material is interposed between the two areas within the aperture or apertures to allow for viewing. The material is preferably transparent, however, translucent materials or non-opaque materials or combinations thereof are within the scope of the invention so long as some images are visible from one area to the next. Viewing pane 31 interposed between dining area 26 and amusement area 41 can particularly comprise various materials such as glass, plastic or other transparent substances as are in compliance with any relevant building regulations. The materials can be optically neutral and transmit the image from one area to the next substantially unaltered or the materials can enlarge, diminish or distort the images transmitted from one area to the other. In a particular embodiment, one way mirrors or glass can be utilized. Viewing pane 31 can comprise the entirety of a common wall between dining area 26 and amusement area 41. Alternatively, viewing pane 31 can comprise some lesser area thereof. The shape of viewing pane 31 is not limited to any particular geometric shape or any combination of geometric shapes.
A second viewing pane can be provided in addition to a first viewing pane regardless of size or shape, except where the first viewing pane comprises 100% of the surface area of a structural member interposed between the dining area 26 and amusement area 41. The second or additional viewing pane can be of the same size and shape or different size and shape from the first viewing pane or from each other. In one embodiment, the size of the viewing pane or panes is not limited to any particular range of the surface area of an area perpendicular to and in common between the border of dining area 26 and amusement area 41. So long as a view of one area from the other is available, it is within the scope of the present invention. In a preferred embodiment, one can view substantially all of one area from substantially anywhere in the other area.
In one embodiment, the viewing pane can comprise a surface area in a range of from about 20% to about 100% of a surface area of the third structural member such that about 20% to about 100% of the surface area, as measured by, for example, multiplying the height by the width of, for example, a wall in common between the border of the dining area and amusement area, and which can be load bearing or not, comprises material which allows for a view from the dining area to the amusement area and vice versa.
In another embodiment, the viewing pane can comprise a surface area in a range of from about 20% to about 50% of a surface area of the third structural member such that about 20% to about 50% of the surface area, as measured by, for example, multiplying the height by the width of, for example, a wall in common between the border of the dining area and amusement area, and which can be load bearing or not, comprises material which allows for a view from the dining area to the amusement area and vice versa.
In yet another embodiment, the viewing pane can comprise a surface area in a range of from about 50% to about 100% of a surface area of the third structural member such that about 50% to about 100% of the surface area, as measured by, for example, multiplying the height by the width of, for example, a wall in common between the border of the dining area and amusement area, and which can be load bearing or not, comprises material which allows for a view from the dining area to the amusement area and vice versa.
In one embodiment viewing pane 31 can be located on a different level, for example the second or higher story of a structure, and allow for viewing of an area located on a lower or higher story.
Movable members 32a and 32b allow the dining area to be partitioned into more than one area such as areas 27 and 29. In a preferred embodiment the dining area can be partitioned into three sections. The movable members 32a and 32b can contain elements permanently affixed to some area of the dining room such as a floor, a wall a ceiling or the like and can slide, roll, compress and expand or otherwise be movable such that the dining area can be partitioned. Alternatively, the entire movable member 32a and/or 32b can be carried into place where it acts to partition or can be moved into place and can slide, roll, compress and expand or otherwise be further movable such that the dining area can be partitioned. Such means would be known to those of ordinary skill in the art. In one embodiment of the present invention a movable member 32a and/or 32b can be disposed adjacent dining area 26 and coffee shop 18.
An enclosed space defining a food preparation area 34 is accessible to a dining area through a door 39. The food preparation area 34 is an area where food can be prepared such as a kitchen, a barbecue grill area and the like. Generally a kitchen will contain running water, a sink(s), an oven(s), a refrigerator(s), food preparation utensils, and means for storing those utensils, food supplies and means for storing those supplies and the like. In a preferred embodiment the kitchen is suited to the commercial demands of a restaurant. The dining area 26 is an area containing; for example, but not limited to, counters, tables or tables and chairs and counters and stools, where food is served. Non-traditional dining areas, from a Western perspective, such as, but not limited to, the Japanese style where one sits on the floor are within the contemplation of this invention. The amusement area 41 is an area containing any one of a non-video game, a toy, an amusement park ride, a climbing structure which can further be resilient to allow for bouncing thereon. Further, the amusement area can include a tunnel, a video game and a means for engaging in a virtual reality experience. In a preferred embodiment a number of permanent or semi-permanent amusement park type rides, e.g. an astronaut ride, a jet plane ride and a number of video and non-video games are contained within the amusement area. Such amusement park rides can be obtained from commercial suppliers as would be readily ascertainable. Alternatively or additionally, custom rides can be created for use in the amusement area. These custom rides can be combinations of commercially available components or can be entirely fabricated according to custom specifications. In preferred embodiments the amusement area is enclosed and separated from other areas within the building structure, apart from access means; such as, but not limited to doors. The doorway in communication with amusement area 41 provides a means of entering and exiting amusement area 41. The doorway can or need not contain a door. The door can be a conventional door or a revolving door or other doors as are known in the art. The door can be opaque, semi-opaque or transparent. However, the interior of amusement area 41 is preferably easily viewable from at least dining area 26, as described in greater detail above. In a most preferred embodiment, the amusement area is accessible through a traditional revolving door. In a specific embodiment a curved member bridging an entrance to the amusement area can be rotated to reveal the entrance, somewhat similar to those devices which allow access to and from a darkroom without allowing light to enter.
In one embodiment sound proofing material can be added to the structural members enclosing the amusement area and/or the structural members themselves can have sound proofing properties. For example, the sound proofing material can be either directly incorporated in or on, in whole or in part, the third structural member interposed between dining area 26 and amusement area 41 and can be disposed in and around additional areas, if necessary, such as the ceiling, other internal walls and the like. Sound proofing materials are materials that either are generally used building materials used to the extent that the sound level of the amusement area is dampened so as not to interfere with normal conversation, or specially designed sound proofing materials as would be known to those of ordinary skill in the building arts can be used for a similar purpose, or a combination thereof can be used.
In one embodiment access to amusement area 41 can be provided by access means connecting dining area 26 and amusement area 41. In another embodiment access can be provided only directly to amusement area 41 or from another area which is not dining area 26, such as lobby area 13. In another embodiment access can be provided by any combination of the above. For example, as illustrated in FIG. 1, there is provided an enclosed space defining an amusement area 41 which furthers comprises a doorway for access thereto. Amusement area 41 contains amusement rides 36a and 36b, video games 42, a moonwalk bounce ride 46, a stage 48 and a mine area 45. The video games include electronic entertainment games with a video display which allow for interaction with the video display by some type of control means, for example, driving a car, flying a jet, shooting at objects and the like. In one embodiment a multiple screen display, for example, three screens, can display images of, for example, a rocket launch and a journey to the planets. A seat positioned to view the screens can be movable to simulate a feeling of motion, preferably in accordance with the image or images displayed on the screens. Such video games can be obtained from commercial suppliers as would be readily ascertainable. Alternatively, custom video games can be created for use in the amusement area. These custom video games can be combinations of commercially available components or can be entirely fabricated according to custom specifications. The means for engaging in a virtual reality experience include equipment such as a visored helmet which contains a video display and or gloves and/or a full body suit which contain sensors that allow for the representation of actions made by a person wearing such equipment on the video display. The result of wearing this equipment is the sensation of engaging in an activity in a highly realistic way, such as, storming a castle, while in actuality the person is merely sitting in a room. This term also encompasses all definitions as are in common usage. Further, the means for engaging in a virtual reality experience are not meant to be limited to existing technologies, but any means which provide for a virtual reality experience which can be developed. Such means for engaging in a virtual reality experience can be obtained from commercial suppliers as would be readily ascertainable. Alternatively or additionally, custom means for engaging in a virtual reality experience can be created for use in the amusement area. These custom means for engaging in a virtual reality experience can be combinations of commercially available components or can be entirely fabricated according to custom specifications.
The stage 48 can be adjacent amusement area 41 and provides an area or a platform for musical, dramatical, theatrical or dance performances and the like and is located in or is viewable from amusement area 41, and preferably also the dining area. Mine area 45 can contain objects such as costume jewelry or faux jewels, and toy creatures such as spiders, which can be available for sale in a gift shop area. An exercise area 44 is accessible to the amusement area through a doorway 47, which can be slidable. An art projector area 38 having a projection surface 64, as further described in FIG. 5 can be provided.
In one embodiment of the present invention, dining area 26 or another area can be located on a second or higher story of building structure 10. The viewing panes can still allow for a view of one area from another area, even when such areas are on different stories from each other.
FIG. 2 illustrates a particular embodiment of a rotatable doorway 16 having a rotatable side member 51 and a top member 52, which allows access from lobby area 13, in communication with doorway 12, to amusement area 41, through second structural member 17 disposed between lobby area 13 and amusement area 41. Arrows b and c illustrate access routes to and from amusement area 41 and lobby area 13. Arrow a illustrates a direction of rotation of rotatable door 16. Rotation in the opposite direction is within the scope of the present invention.
FIG. 3 illustrates dining area 26 containing tables 28 and chairs 30. Amusement area 41 containing video game 42 and amusement rides 36a and 36b are visible through multiple viewing panes 31a-e.
FIG. 4 is similar to FIG. 3, however it illustrates another embodiment of the present invention, comprising a single larger viewing pane 31f.
FIG. 5 illustrates art projector area 38. A drawing console 60 allows a patron to make a drawing at the console 60 and project an image of it 62 on a projection surface 64.
FIG. 6 illustrates a particular embodiment of the mine area 45 depicted in FIG. 1. A door 70 provides access to mine area 45.
FIG. 7 illustrates one particular embodiment of an interior 72 of mine amusement area 45, having futuristically designed support members 74.
FIG. 8 illustrates in more detail rocket slide 40, adjacent access steps 80 to slide tube 81.
FIG. 9 illustrates in more detail moonwalk bounce ride 46.
While the description above refers to particular embodiments of the present invention, it will be understood that many modifications can be made without departing from the spirit thereof. The accompanying claims are intended to cover such modifications as would fall within the true scope and spirit of the present invention.
The presently disclosed embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims, rather than the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
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The present invention provides a building structure within which a setting is maintained which allows restaurant patrons to enjoy dining out while allowing primarily children accompanying adult patrons the opportunity of playing in an adjacent amusement area without disturbing the adult patrons. The adult patrons, however, can view the children and any other amusement area patrons, allowing monitoring of the children's activity while simultaneously enjoying the view of the children at play and enjoying their meal. Preferably sound proofing is disposed between the two areas. Additionally, other areas, such as an exercise area, a play area, a coffee shop, gift shop, art projection area and the like can be contained within the building structure.
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This application claims the benefit of Danish Application No. PA 2006 00113 filed Jan. 26, 2006 and PCT/DK2006/000457 filed Aug. 23, 2006, which are hereby incorporated by reference in their entirety.
The present invention relates to a portable catalytic heating system for off grid application.
DESCRIPTION OF THE PRIOR ART
Infra-red radiation is the part of the electromagnetic spectrum that comprises wave-lengths between 0.76 and 100 μm of which only radiation up to 10 μm is being applied industrially. The spectrum can be divided into three “bands”:
short-wave IR radiation: 0.76-2 μm medium-wave IR radiation: 2-4 μm, and long-wave IR radiation: 4-10 μm
Outside the infra-red area, to one side of the radiation spectrum we have the visible light (shorter wavelengths); to the other side (longer wavelengths) we are approaching the radio wave area.
The wavelengths of the IR radiation correspond to the weak photons (<4.10-19 J), which is not suspected to weaken materials by modification of the molecular structure, in contrast to radiation with higher energy levels: UV, X and gamma. Accordingly, the infra-red radiation has a pure thermic effect.
A catalytic heater produces heat without generation of a flame. Catalytic infra-red radiation is produced in a process that is called an oxidation-reduction-reaction. When hydrocarbon is combined with oxygen in the presence of a heated catalyst, the exothermic reaction releases infra-red energy and produces CO2 and water vapour.
Catalytic heaters are described in the American U.S. Pat. No. 4,420,462 by Clyde for heating of liquid, which flows through pipes near the heater, and in the American U.S. Pat. No. 5,215,076 by Oglesby et al. primary for soldering.
Catalysis occurs in the temperature range 370-425° C. These temperatures correspond to IR wavelengths about 3-7 μm, which basically coinciding with the maximal absorption spectrum of water, which is in the range of 3-7 μm. Consequently, IR heating is well suited for heating of water in sundry materials. Thus, it is known that catalytic heaters can be used in hair curlers, by way of example as described in the American U.S. Pat. No. 4,416,298 by Berghammer.
The function of a catalytic heater can be described in the following way. In a gas-fired catalytic infra-red heating panel gas is feed through the catalytic medium. The IR element primary consists of a catalytic material with an evenly distributed mesh or a fibre structure, which offers a maximal surface area and allows the catalyst to react with optimum efficiency.
In catalytic infra-read heating is applied a catalytic reaction between fuel, oxygen and heat for generation of infra-red radiation. The catalytic reaction is generated by application of a substance (catalyst), which creates a thermodynamical reaction between the substance and the heat. Or stated more simply: Changes and acceleration in the chemical reaction that is triggered by the substance (the catalyst), which in itself remains unchanged.
The burning process normally (i.e. without a catalyst) starts at about 500° C. When the catalyst is added the process occurs faster and at a lower temperature. At 250° C. the oxidization can occur, provided that the other conditions are met, however, it concerns oxidization without fire (ignition) and flame.
When the catalyst, by preheating, has reached a temperature at 150° C., as an example, the gas passes by the heated catalytic material. The gas gets into contact with the warm catalyst and reacts with the oxygen of the air, by which the temperature of the catalyst is raised to between 175 and 440° C., at the same time as it emits infra-red energy. Efficiency tests have shown that up to 72% of the energy in the gas is converted to infra-red heat energy. Since the reaction temperature is much lower than the ignition temperature for gas (above 700° C.) the reaction is flameless. The catalytic reaction can be established few seconds after the gas has reached the panel.
OBJECT OF THE INVENTION
It is the object of the invention to provide a catalytic heater for heating of water and watery liquids and watery masses, in which the heat is easy to transport and meet the needs required by individuals that stay in the nature/outdoors and that need a dependable and efficient off grid heating system for their food and beverages. The target group is i.a. military units, special units, hikers, trekkers and families with children.
This object is achieved by a portable catalytic heating system for off grid application, in which the heating system comprises a heating unit with a handle and an, in extension hereof arranged, heating pipe containing a catalytic burner for catalytic combustion of gases for providing infra-red radiation, where the heating pipe is produced in a material that is transparent for infra-red radiation and fluid-proof for immersion in liquids. It is constructed in such a manner that it can be applied in all positions. It means that the handle may be placed both below and above the medium that has to be heated.
Catalytic heating systems are in general known as being dependable, robust and to have a high degree of efficiency. Accordingly, a relatively small and light apparatus may be produced, which makes it suitable to carry it at a trek or at a military operation. Hence, it is also beneficial to apply it in third-world countries due to the robust form of construction and because of low manufacturing costs. It may for instance be used for sterilization of water.
This invention makes it possible to avoid the use of cooking vessels and pots in the process of off grid heating of canned goods, ready-prepared drinks, watery liquids or freeze-dried food. This opportunity means that one obtain a much better hygiene and state of health, because there will not occur a contamination of the cooking vessel or the pot and the need for washing-up is largely reduced compared with the heating systems available today, since the heating unit is self-disinfectant. The system layout permits furthermore that the heating system can be applied as heater and hot-water bottle.
The heating element comprises a catalytic IR-burner, which gives off its heat, to the medium that is to be heated, via a combination of infra-red radiation and thermal convection.
In practice a catalytic IR-burner will give off up to about 70% of its energy in the form of radiant heat, while the remaining about 30% will be given off partly to the off-gas as convection heat (20%) and partly as visible and UV-light etc. (ca. 10%), why the invention has large energy efficiency and very low damaging emission values.
The catalytic heating system applies combustion of gas (natural gas—propane, butane gas or mixtures hereof) in a catalytic element, which may comprise a cylindrical or flat catalytic element of a ceramic, metal or filtering material.
In comparison with conventional heating systems for field rations etc. applied in the nature, the primarily difference in the operational principle and the efficiency, that the conventional heating is provided from the outside and into the material and there is a rather low efficiency, typically about 18-20% due to the huge emission of heat to the surroundings.
By a catalytic infra-red heating combined with convection heating the heating is provided both from the inside of and out of the material as well as from the outside and into the material. This involves a more regular heating of the medium to be heated. This effect is furthermore utilised by having the heating element immerged and placed centrally in the medium that is to be heated. The efficiency is typically over 70%.
Catalysis occurs in the temperature range 370-425° C. These temperatures corresponds to a IR wavelength of 3-7 μm, which means that this IR-radiation emission spectrum is substantially coinciding with the maximal absorption spectrum of water, which is in the range 3-7 μm. Accordingly, Catalytic IR heating is well suited for heating of materials with a relatively high water content, which is characteristic for food products and beverages.
Since this heating system is intended to be immerged directly into the medium to be heated, there has to be provided a water-proof separation between the medium to be heated and the catalytic heating element. In order to enhance the efficiency of the transmission of the IR radiation there has to be provided a partition wall made in a material that can be optimised with regard to both transmission of IR radiation and transfer of convection heat. The partition wall may comprise either aluminium, copper or quartz glass or a combination of these.
Catalytic infra-red heating is approved by Factory Mutual for Class 1, Division 2, Group D, and Canadian Standards Association for Class 1, Division 1, Group D hazardous locations.
A flameless catalytic heating element is suitable for being operated in dangerous areas such as chemical or petrochemical storing sites and places, with inflammable or explosive gases or steams. A flameless catalytic heating element can also be safely operated in areas with highly flammable dust or metal dust and in building areas, where gas-powered vehicles are being maintained, stored or parked.
In a concrete embodiment there is provided a venturi system for mix of fuel gas and air in between the gas tank and the catalytic burner. A venturi system is robust and dependable and may be manufactured in a great number for low costs, which for a system according to the invention is a huge advantage because is considered to be distributed among many users.
In another embodiment a counter-flow heat exchanger is provided between a pipeline for air supply and a pipeline for vent gases for heat exchange between vent gas and supplied air.
For use in the military the heating system according to the invention has the advantage that it is more difficult to trace in use than conventional heating methods. The heating system according to the invention entail that there is not occurring any form of visible flame in use. The system layout secures that the heating unit that comprises the IR burner is surrounded by the medium, which has to be heated, coincident with that the exhaust gas is cooled to the maximum via a cross-flow heat exchanger, which secures that the heat from the exhaust gas partly is transferred to the gas tank, which uses heat as the gas is converted from being a liquid to being gaseous for combustion and partly to the intake air to the catalytic burning.
Accordingly, there is only a weak thermal profile in use. The concept layout secures furthermore, that the sound level is very low and that no smoke is formed.
Moreover, between a gas tank in the heating system and a pipeline for vent gases there may by provided a heat exchanger, optionally identical to the previously mentioned heat exchanger. Thereby it is secured that the apparatus also can be applied at very cold conditions.
Due to the high efficiency, which is more than 3 times better than the off grid heating systems with cooking vessels and pots used today, this heating system is both energy-efficient and environmentally benign. The energy consumption is very low, namely only about 10-12 gram gas per liter water heated to 80 degrees Celsius. By way of example a propellant as natural gas, propane gas, butane gas, isobutene gas or a mixture hereof is being used. According to all prognoses it should be possible to supply butane gas for the next 100 years. Heating units may in practice also apply hydrogen as propellant without significant changes.
Therefore, the application of a heating system according to the invention is associated with a number of advantages. Firstly, catalytic combustion is based on technologies that are far less polluting than the present off grid heating methods. Furthermore, the heating system of the invention and its energy medium is lighter and takes up less space than the present off grid systems. Catalytic combustion has been known and used for more that hundred years in other applications why the technology is thoroughly tested and safe.
It is moreover possible to provide the heating system with an internal piezoelectric ignition system to start the catalytic combustion in all weather conditions also in the heavy snow storms and tropical storms and heavy rainfalls without preparation or requirements regarding temperature or the physical surrounding. The unit does not make demands on the base or any other kind of preparation, which is why it can be started and operated by one hand. The system layout permits that the heating unit can be carried by the user in use, which is why it is possible to start and heat during motion, march or military work.
That heating system, to witch the invention is related, can directly be incorporated in the delivery channels, supplier channels and distribution channels that is used today, because a standard propellant and available raw materials and semi-finished products is applied, which is why it will not be difficult to establish a full delivery system with delivery of a propellant in standard units and servicing of the equipment. Hence the heating system according to the invention may comprise an exchangeable gas tank, arranged in the handle if desired.
The invention relates to a robust, energy efficient and thoroughly tested principle, which takes up less space and is lighter than the existing systems, which are based on external heating of cooking vessels/pots by means of for instance spirit tablets, multi-fuel burners, spirit boilers or gas flames. Basically there is no wear on the system, why service and maintenance is reduced to an absolute minimum.
The typical user can by the invention achieve i.a. the following advantages: faster and much easier heating of i.a. field rations, emergency rations, water, milk and baby food. There will be no problems regarding washing-up in those cases where the packaging is used as cooking vessel. It will always be possible to have access to hot drinks and sterilization of water and there is no requirements to the surroundings at all, because the heating system function without problems in all the places, in which the user can cary out his service also regarding transport. The heating system can, furthermore, also be applied as a hot-water bottle and finger heater and generally as heater against frost-bites.
The concept, the system layout and the applied combustion technology in the heating system according to the invention secure all together the user a greater safety, comfort and user friendliness.
A portable catalytic heating system according to the invention, where the handle is provided with an adapter for fluid-proof attachment of the heating unit to a tank with a corresponding adapter.
A portable catalytic heating system according the invention, where gas supply to the catalytic burner in the heating pipe is provided between the catalytic burner and the inner wall of the heating pipe. By this way, the temperature of the supplied gas is reduced and secures a good catalytic combustion with high degree of efficiency.
BRIEF DESCRIPTION OF THE DRAWING
The invention is described further refereeing to the drawing, where
FIG. 1 shows a heating unit according to the invention together with a protective tank
a) removed and b) mounted.
FIG. 2 is a detailed sketch of the heating system,
FIG. 3 shows an embodiment, in which the heating unit is fitted directly to the threaded bottleneck of a canteen,
FIG. 4 illustrates the application in connection with heating of a medium in a tin,
FIG. 5 shows the heating unit submerged in a tin that is provided with a corresponding adapter,
FIG. 6 shows an illustration in connection to the replacement of the gas tank/energy cell,
FIG. 7 shows a hand-operated valve, which a) can open and b) close the air intake and the exhaust of the heating unit respectively,
FIGS. 8 a and 8 b show alternative embodiments designed especially for use in connection to bottles, feeding bottles and glass for infants,
FIG. 9 shows the alternative heating unit packed together for storing and transport.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a heating system 1 according to the invention. The heating system 1 comprises a heating unit 2 and a protective tank 3 . The heating unit 2 has a handle 4 for attachment of the heating unit 2 and a heating pipe 5 that transmits heat radiation from the catalytic element contained in the heating pipe 5 . The heating pipe 5 can be fitted into a protective tank 3 , when the heating system is not in use. The tank 3 may also be used for storing of fluids or other materials such as powder, as an example in connection to heating with the heating pipe 5 or in order to constitute a storage of fluid or other materials in during transport. The tank 3 may by way of example comprise hot fluid and function as a thermos bottle or for heating of the hands. The tank 3 is isolated in order to reduce the output of energy to the surroundings.
The tank 3 is open in its upper extremity 6 and by the edge provided with a thread 7 corresponding to an internal thread (not shown) in an adapter 8 in one extremity of the handle 4 . FIG. 1 a shows the heating unit 2 and the tank 3 separated from each other, while FIG. 1 b shows the heating unit 2 and the tank 3 in a situation, in which they are screwed together.
It should be noted that the tank may have other shapes than the one showed in FIG. 1 , and the heating system 1 according to the invention may be provided with a number of other tanks for heating of fluids or other materials. It would be beneficial to provide such other tanks with internal or external thread 7 in their open extremity 6 , so that they may be screwed together with the adapter 8 for heating of the material therein. In connection to heating of fluid or another material in the tank 3 , it is up to the user to take into account any pressure rise in the closed tank that could occur during the heating. In order to prevent damage to the material and/or the personnel in case of over-pressure in the tank due to the heating, the heating system 1 according to the invention may advantageously be provided with a safety valve connected to the interior of the tank 3 , in order to provide a passage for equalization of pressure relative to the atmosphere in case of over-pressure in the tank 3 . Accordingly, it is not necessary that a fluid-filled tank is screwed together with the adapter 8 during the heating process. The heating system 1 may, near the handle 4 , furthermore be provided with a pivotal bow 9 for suspension of the system 1 , by way of example suspension in a belt on a uniform.
The heating pipe 5 is closed in the lower extremity in order to prevent fluid from surging up in the pipe. Accordingly, there is no entry of fluid from the tank 3 into the handle 4 or into the pipe 5 . The safety valve, which must carry out the equalization of pressure, may also be located in the adapter 8 .
In the pipe 5 there is installed a catalytic burner that is supplied with gas to the process from a gas tank/energy cell in the handle 4 . Between the gas tank and the catalytic burner in the pipe 5 there is provided a valve, which can be controlled by use of a regulator via a button 11 . In order to make the catalytic process start, it is necessary to heat the catalyst. This can be done by pushing a push button 10 as shown in FIG. 1 b . The push button 10 both ignites and opens for the gas so that the heating unit 2 may be operated with one hand. Air suction and exhaust of gas is provided via openings in the upper part of the handle, in which there in FIGS. 1 a and 1 b is shown the air suction opening 12 , while the exhaust opening on the opposite side of the handle is not show in this figure. Such suction openings 12 and exhaust openings may be provided with a regulation valve 13 for regulation of the volume of intake air and exhaust gas, respectively, through the openings.
In FIG. 2 is shown a specific embodiment of the more general heating system 1 shown in FIG. 1 . The sketch in FIG. 2 shows the handle 4 with the heating pipe 5 inserted into the built-on tank 3 . The handle 4 comprises a gas tank 14 , from which gas is released via a regulator 15 , for example by operating a button 11 as shown in FIG. 1 a , and fed into a nozzle 16 . Such nozzle 16 is preferably part of a venturi system 17 , so that the gas carries air and hence oxygen along with it, when the gas is fed out of the tank 14 . This air is provided via the pipeline 18 that is connected to the inlet port 12 . The gas and air mixture is fed through a transport pipe 19 between the venture system 17 and a catalytic element 20 . The transport pipe 19 is on the same level as the catalytic burner 20 , which may be provided with apertures or an adjusted length in interaction with a special shaped bottom that forms the closing section of the catalytic element 21 in order to ensure a smooth flow and gas-air distribution in the catalytic burner 20 . After the catalytic process, in which the fuel gas is converted to carbon monoxide and water vapour, these exhaust gases are fed through another pipe system 22 to an exhaust opening 23 in the opposite section of the handle 4 .
The catalytic burner 20 can have different geometrical shapes depending on the intended application and efficiency. As an example it may comprise or be comprised of two plane units or of one or more curved units, for instance cylindrical units. By way of example the burner may be comprised of more plates with gas supply in the periphery of the burner in order to ensure a lower temperature of the gas and a larger heating surface per unit area of the catalytic burner, which all things being equal should ensure an even higher efficiency than with the cylindrical heating surface.
The catalytic process produces a great amount of infra-red radiation, which is being transmitted through the material of the heating pipe 5 and into the tank 3 , which is closed upwardly with a partition wall 29 . The medium in the tank 3 is being exposed to the infra-red radiation that especially heats the water in the tank 3 . In order to ensure an effective utilization of the infra-red radiation, the tank 3 may be provided with a reflective coating on the inside, in order to reduce the emission of heat through the wall of the tank 3 . It is furthermore possible to construct the tank 3 with a general heat insulating wall, optionally with a multi-layered structuring as known from thermos bottles.
With a heat insulating tank 3 and a handle that is not heated, it is difficult to trace the use of such heating system 1 according to the invention in relation to military actions, because the emission of heat, by this way, is minimised. A certain kind of emission of heat that imply a potential risk of tracing during application, is associated to the heated emissions (gas, water vapour) from the known catalytic process through the exhaust opening 23 . To reduce the temperature of the exhaust gases there is provided a counter flow heat exchanger 25 that, at least in part, encloses the gas tank 14 in order to trans-form heat from the exhaust emissions to the gas in the gas tank. Moreover, the pipe-line 22 for the exhaust gas is, at least in part, surrounded by the pipeline 18 for the intake air through the inlet port 12 . Accordingly, heat is transferred from the emission gases to the gas tank and to the intake air, which contributes towards an optimal combustion. In this connection it should be mentioned, that the gas from the gas tank 14 during expansion after the nozzle 15 in the venturi system 17 entails a cooling of the gas so that absorption of substantial amounts of heat from the exhaust is possible.
Emission of heat from the exhaust gas to the intake gas and the gas tank 14 contributes towards to ensure an expedient function of the heating system 1 according to the invention also in very cool surrounding. Therefore, the heating system 1 according to the invention is well suited for use both in hot and cool areas and due to its robust nature it is well suited for use in the military sector.
In the case of heating of fluids or another medium 24 in the tank 3 , when it is mounted on the adapter 8 , a possibly generated over-pressure in the tank 3 due to the heating induces a risk for the heating system 1 and for the user of it. In order to reduce the risk for damage of the apparatus and the personnel, the heating unit 1 is provided with a safety valve 25 between to the interior of the tank 3 and the atmosphere outside the tank. The safety valve opens a passage between the interior of the tank 3 and the surrounding atmosphere for equalization of pressure. The over-pressure valve is in the figure located in the adapter 8 , but it is possible to provide a over-pressure valve in other appropriate places in the apparatus.
To be even easier to operate, the heating unit 2 may furthermore be provided with a heat sensor 26 , which, by use of the infra-red radiation emitted by the medium 24 , can measure the temperature of the medium 24 .
Alternatively, such heat sensor 26 may comprise a thermometer that measures the temperature of the medium while being submerged into the medium. However, this embodiment is not shown in FIG. 2 .
Thus, the heat sensor may be connected to a temperature indicator on the handle (not shown) or to an acoustic device that indicates when the medium 24 has reached a certain preset temperature. It may, as an example, be possible to set this temperature on a unit on the handle or the temperature may be preset, so that it is indicated when a certain temperature is reached, for instance by a sound or light indication on the handle. Hence, it may also be considered to use installed light indicators in different colours or a number of light indicators that is turned on depending on the temperature reached in order to indicate to the user the temperature reached or exceeded.
As a further alternative a thermo valve that regulates the gas flow directly to the catalytic burner may be inserted. If the temperature in the catalytic burner exceeds a preset temperature, this thermo valve will regulate the gas flow downwards until the temperature come down below the level that is permitted in the catalytic burner.
The gas tank/energy cell 14 is arranged in the upper part of the handle 4 to facilitate the replacement of it, which also is illustrated in FIG. 6 , or to facilitate refuelling of gas to the gas tank 14 .
In FIG. 3 is shown an embodiment, in which the heating unit 2 is fitted directly to the threaded neck of the canteen 3 ′, which may have other shapes and sizes than the one showed. The canteen 3 ′ may, depending on the selected degree of insulation, be applied directly for heating of water, moist masses or beverages or as a hot-water bottle or hand heater. It is possible to mount the heating unit directly on other kinds of canteens, water tanks, drinking bottles, thermos bottles and the like by adjusting the adapter 8 . Likewise, the adapter 8 may be manufactured with both internal thread and external thread for adjustment to specially developed fluid tanks.
In FIG. 4 is shown an application in connection to heating of a medium in a tin. The heating pipe may, at the same time, function as a spoon and a high-efficient heating element.
In FIG. 5 the heating unit is emerged into a tin that is provided with a thread corresponding to the adapter so that the heating unit may be screwed together with the adapter, which fits tightly to the upper edge of the packing. The adapter may be provided with a skirt made in soft rubber, for instance approved by the American FDA, so that it covers the entire casing of the packing. Hereby the adapter will also be insulating and contribute to a fast heating, because the heat loss to the surroundings, all things being equal, will be reduced.
In FIG. 6 is shown an illustration in connection to a replacement of the gas tank/energy cell.
In FIG. 7 is shown a hand operated valve 27 that can open and close for the air intake 12 and exhaustion of the heating unit, respectively. The valve 27 is shown in open position in FIG. 7 a and in closes position in FIG. 7 b.
FIG. 8 a shows an alternative embodiment special designed for use for parents that have young children and wishes to be able to heat milk and baby food directly in the packing. FIG. 8 b shows the same heating system, however, with a replaceable adapter intended for attachment to e.g. a standard feeding bottle or a standard baby food packing. Hereby it is possible for the minder of children to put the feeding bottle/baby food in the pocket while the person for instance consoles the hungry child in the middle of the nature.
FIG. 9 shows the alternative heating unit packed together for storing and transport. Air intake 12 and exhaustion of gas 28 is provided on the end face and may have a colour indication that depends on whether they are open or closed. A red marking communicates as an example to the user that the air intake 12 and exhaustion 28 of the heating unit are closed and accordingly protects against ingress of unwanted foreign objects.
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A portable catalytic heating system for off grid application, in which the heating system comprises a heating unit with a handle ( 4 ) and an, in extension hereof arranged, heating pipe ( 5 ) containing a catalytic burner ( 20 ) for catalytic combustion of gases for providing infra-red radiation, where the heating pipe ( 5 ) is produced in a material that is transparent for infra-red radiation and fluid-proof for immersion in liquids.
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This application is a continuation of application Ser. No. 07/071,698, filed Jul. 9, 1987, now abandoned, which is a continuation-in-part of U.S. application Ser. No. 942,196 filed 16 Dec. 1986, also now abandoned.
BACKGROUND OF THE INVENTION
The invention pertains to the field of sample preparation systems, and more particularly, to the field of control systems for automated sample preparation systems.
In many industrial production facilities and laboratories, there is a need to assay sample chemicals being prepared, analyzed or otherwise processed. Such samples can come in many different forms. For example, they may be solid, liquid, two phase liquid or liquid-solid, and may or may not be highly viscous. Many types of assay systems require liquid samples of known viscosity and concentration. An example would be a liquid chromatography system.
Obviously, there is a need for systems which can prepare many different types of samples for assay by such machines. Preferably such systems are automatic in the sense that after the user defines the type of sample preparation needed, the system automatically carries out this processing on samples until told to stop or until the sample preparation runs out of samples.
Because of the many different types of sample formats and because of the many different types of sample preparation processes which exist for various types of assays, there is a need for flexibility and programmability in a control system for an automated sample preparation system. The user must be provided the facility with which the particular types of samples he or she intends to process may be prepared in a process for which the steps and sequence of steps are defined by the user. In this way the user can tailor the automatic sample preparation system for use in the environment peculiar to that particular user.
Prior art automatic sample preparation systems exist in the form of robots. One particular type of robot of which the applicants are aware is a robot manufactured by Zymark. These robots may be programmed to emulate all the movements a human being would make in doing a sample preparation process manually. Unfortunately, such systems are complicated and expensive and difficult to use because of the complexity of the mechanical machinery and control computers and software needed. Thus, a need has arisen for a control system for a sample preparation system which is flexible, programmable, easy to use, and relatively inexpensive to manufacture.
SUMMARY OF THE INVENTION
In accordance with the teachings of the invention, there is provided a control system for a sample preparation system to fully automate the system and allow users to program their own sample preparation procedures or to use preprogrammed procedures. Further, the control system allows a user acting as a system manager to define the necessary sample preparation procedures for various types of samples likely to be encountered. Then the system manager may lock out users without system manager privileges to prevent them from altering the procedures while allowing such users to use the procedures programmed for them by the system manager.
The control system of the invention allows user interaction with the system at three levels. At the first level, users may only give the sample identification (in embodiments with no bar code reader), the sample weight, the user initials, the date and time, the lot number to run, and the method of sample preparation to be followed. These methods of sample preparation will have been programmed into nonvolatile memory before the control system is obtained by the user or will have been previously programmed in by the system manager.
The next level of user interaction is a high level language level. At this level, the user has various high level sample preparation system control commands at his disposal. Such commands include fill, mix, isolate, flush, dilute, inject, wash, etc. Each of these commands represents a predetermined sequence of events which will be caused by the control system to happen in the sample preparation system when the particular command is executed in the course of performing a sample preparation procedure. The user at this level may string a series of such high level commands together into a sample preparation procedure and give it a name. Upon selection of a high level command, the control system would prompt the programmer for any necessary variables or parameters, such as solvent selection, volumes, flow rates, mixing times, etc. Thereafter, by identifying the particular procedure the user wishes to run, the same sequences of events may be caused to occur in the sample preparation system of the invention. Some of the high level commands have parameters which are accessible to the user and may be set to accommodate the particular needs of the user. These parameters allow the user to control, for example, the amount of time a mixing step is carried out and the level of energy that is input to the mixer by the homogenizer.
The key to breaking up sample preparation procedures into a series of standard preparation steps, which can be chained or re-chained together in any useful sequence the user needs to accomplish his desired sample preparation procedure, is to design the hardware and software control logic to allow each standard preparation step and each programmed series of standard preparation steps to be completely independent of the preceding or following step or series of steps. For example, upon completion of a dilution sequence or cup wash cycle, the diluent or wash solvent from a prior dilution or rinse should not be left in the instrument connecting tubings or modules. If there is such leftover solvent etc, it may inadvertently contaminate the next dilution or wash with the wrong or an undesired solvent. If this undesired solvent could not be removed from all tubings and connections prior to the next step or sequence of steps, the next step would be restricted to using a solvent deemed compatible with the undesired solvent and thereby place undesired restrictions on the next step.
At the most detailed level, the control system according to the invention provides the user access to and programmability for elemental operations of the type that are combined into the sequences which make up each high level command. Such elemental operations control individual events in the system such as the opening and closing of a particular valve, the turning on of the homogenizer, setting of the power level of the homogenizer, etc. The user may program the system at this level by stringing together sequences of these detailed level commands. These sequences may be thought of as user definable high level commands, or "macros." The user may string any number of macros together to form a procedure which may then be labelled and executed by referring to it by its name.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is block diagram of the hardware of the control system and the system electromechanical devices which are read and controlled by the control system.
FIG. 2 is a schematic diagram of a typical sample preparation system which may be controlled by the control system of the invention.
FIG. 3 is a schematic diagram of another embodiment of a sample preparation system which may be controlled using the control system of the invention.
FIG. 4 is a flow diagram of the overall control flow of the control system software.
FIG. 5 is a flow diagram of the various routines of the control system of the invention.
FIG. 6 is a flow diagram of the create, modify and delete routine of the control system of the invention that the allows a user to create new sequences of commands at either of two levels of detail and complexity.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 is a block diagram of the electronics of the control system in accordance with the teachings of the invention. The control system is centered around a CPU 20 which could be a microprocessor, personal computer, minicomputer, or mainframe. Included within the CPU block is RAM memory for storing programs and data while the computer is running. Mass storage of data, programs, and other information such as data bases, macros, user defined parameters, user defined sample processing routines, etc., is performed by mass storage unit 22. This unit could be a disk drive, tape transport, bubble memory, or any other bulk storage device with sufficient access speed and storage capacity for the particular application involved. The user controls the computer 20 through a terminal comprised of keyboard 24 and any type of display 26.
The computer 20 is coupled to the various operating units in the sample preparation system by bus 28. This bus 28 is actually comprised of the address, data, and control signal lines of the computer 20. The bus is coupled to the ports for addresses, data, and control signals such as read/write, interrupt, ready, etc. on the various drivers and interfaces to the various functional elements of the system. A more complete description of the sample preparation system for which the control system is intended to be used with is given in the following U.S. patent applications: "System for Preparation of Samples for Analysis" by Nau, Metzger, Orimm, Nohl, Ser. No. 942,197, filed 12/16/86 and "Sample Preparation Chamber with Mixer/Grinder and Sample Aliquot Isolation" by Nau, Metzger, Grimm, Andre, and Nohl, Ser. No. 942,198, filed 12/16/86, both of which are hereby incorporated by reference.
Because the sample preparation system is intended for use in applications where either the samples will be brought into the system in cups or other containers with bar codes thereon or pumped into the cup through a 6-way valve, a bar code reader 30 is provided. This allows sample identification data such as lot number and batch number or other types of information pertaining to the incoming samples to be read from bar codes on the sample containers. This information may then be read by the computer 20 and stored in the mass storage unit 22 for later correlation with the test results for that group of samples. Bar code readers are known and systems for moving sample containers by bar code readers so that the bar codes may be read are also known.
In the preferred embodiment, a network interface controller 32 is provided to allow other computers and units on a network in the user facility such as terminals in the offices of scientists to offices, program the system or inquire as to the status of a particular sample preparation routine. Further, the users may have access to the data which resulted from a particular sample run. For the network interface, this user can have the sample data resulting from the assay of a particular lot of sample communicated directly into the data based in the other computer.
A sample loader 34 functions to mechanically load samples arriving in containers. The particular design of the sample loader is not critical to the invention. It may load sample from one or more containers brought in by the user such as a tray of test tubes into the sample preparation chamber. In such a system, the sample from each test tube would be loaded into the sample preparation chamber, homogenized, diluted, and pumped through the assay system. At some point in the process, the sample would be identified either by the user keying in the identification data or by the bar code reader 30 reading the bar code on the test tube. The analysis data from the assay would then be stored in the mass storage unit 22 along with the corresponding identification data. The sample loader would then load the sample from the next test tube into the sample preparation chamber, and the process would be completed for the sample from the next text tube. The design of such a sample loader is known and a commercially available unit which could be programmed to do the job would be the PRO/GROUP(tm) automatic assay machine available from Cetus Corporation in Emeryville, Calif. In alternative embodiments, the sample loader 34 could be any mechanical system which could take a cup like that used in the sample preparation chamber described in the patent applications incorporated by reference and attach it to the cap. Any mechanical arrangement that can load a cup from a tray, conveyor belt, or carousel of cups into mechanical, sealing engagement with the cap of the sample preparation chamber described in the patent applications incorporated by reference will suffice. In some embodiments, this unit may be omitted altogether where sample is pumped in from a process stream or injected from a 6-way valve coupled to a sample vat. The design of suitable sample loaders which will suffice to practice this aspect of the invention is known.
There are also provided electronic scales 36 in the preferred embodiment. These provide the facility for weighing of solid samples or samples which are too viscous to pump into the sample preparation chamber where such samples are placed manually in the sample preparation chamber. The purpose of weighing such samples is to provide the user with an indication of the amount of sample that has been placed in the sample preparation chamber. This is important because the samples will later be diluted with solvents or diluent to a user defined concentration. In order to do this properly, the weight of sample in the sample preparation chamber prior to addition of the diluent must be known. The electronic scales also provide an RS232 or parallel interface to the computer 20 via the bus 28 so that the computer 20 may read the sample weight directly. The electronic scales may be eliminated in some embodiments. Without the electronic scales, if the user is dealing with a solid sample, the weight of sample placed in the sample preparation chamber must be keyed in by the user through the keyboard 24. A suitable electronic scale 36 would be the Mettler AE160 available from Mettler in Switzerland.
A pump interface 38 provides the facility for the computer 20 to control the reversible pump used in the sample preparation chamber. The pump motor may be a stepper motor or a D.C. servo motor with an optical or other type of encoder so that the pump interface circuit 38 can determine the position of the motor shaft at all times. Any type of motor with sufficient power and a system to positively control the pump shaft position or otherwise control the exact volume pumped will suffice. The pump interface obviously needs to be designed to interface between the particular type of pump motor and pump chosen and the particular type of computer 20 chosen.
FIG. 2 shows one embodiment of a sample preparation system with which the control system of the invention may be used. In this embodiment of the sample preparation system, the details of the structure and operation of which are as described in the patent applications incorporated herein by reference, two manifolds 39 and 41 are used as central terminals in what amounts to a fluid switching multiplexer. Each manifold is coupled to various sources of material or various destinations in the system by a plurality of remotely controllable valves of which valves 43 and 45 are typical. These valves are typically solenoid operated or pneumatically operated under the control of the computer 20. The purpose of the valve interface 40 in FIG. 1 is to electrically translate the address, data, and control signals on the bus 28 into the proper electrical or pneumatic control signals to cause the proper valve in the system to assume the proper state. Such interface circuits are well known for either solenoid operated valves or pneumatically operated valves. For example, in the case of solenoid operated valves, a motor controller chip can decode the address on the bus 28 and a data word indicating whether the valve is to be opened or closed along with an active write signal. All these signals define an action desired for a particular valve. The address specifies which valve is to be operated, and the active write signal indicates when the computer 20 is addressing a particular valve. The data word defines whether the valve is to be opened or closed or which of its multiple states to assume in the case of a multistate valve.
The motor controller chip then activates a particular output signal line coupled to a solenoid driver such as a relay or a triac in such a manner as to cause the desired change in the state of the addressed valve.
In the case of pneumatic valves, the address, data and control signals are decoded, as above, but the activated output signal from the motor controller chip is used to control a pneumatic pressure source to either apply pneumatic pressure or remove it from the particular valve addressed.
FIG. 3 shows the preferred embodiment of the sample preparation system with which the control system in accordance with the teachings of the invention is used. The difference between this sample preparation system and the sample preparation system of FIG. 2 is that the manifolds 39 and 41 and the associated valves such as valves 43 and 45 are replaced with two rotary, multistate valves 47 and 49. All other details of the system structure and operation are as described in the patent applications incorporated by reference herein. Each of these valves has a central input pipe, pipes 51 and 53 respectively, which is connected to only one of a plurality of output ports coupled to various sources of material or destinations in the system. A stepper motor or D.C. servo motor with optical encoder is used to drive the valve to its various states. In such an embodiment, the valve drivers 40 are the interface circuits needed to control the stepper motors or D.C. servo motors.
Integrated circuits for stepper motor control are commonly available. These circuits allow the computer 20 to send address and data words to the stepper motor controllers after enabling the chip with a proper chip select signal. The address signals indicate which of the two rotary valves is being addressed, and the data words indicate the desired state in which the rotary valve is to be placed. Typically, these integrated stepper motor controllers have a command set. Typical commands include commands to start and stop the controlled motor, commands to control the acceleration and deceleration profiles to use, commands to control the step number to which the controlled motor's shaft is to be moved, and commands to read the particular step at which the controlled motor's shaft is currently resident. Such chips may be used to control the stepper motors used to drive the rotary valves 47 and 49. In the preferred embodiment of the sample preparation system, these rotary valves 47 and 49 are manufactured by Hamilton Company of Reno, Nev.
A typical D.C. servo motor which could be used to drive the rotary valves 47 and 49 is manufactured by Galil Motion Control, Inc. of Mountain View, Calif., under the model designation DMC 100. These servo motors have optical encoders which are used to provide feedback as to the shaft position to an interface board for the Galil motor plus motor controller chips for the other remotely controlled valves in the system.
The RS232 port interface 42 may be a simple commercially available UART. The analyzer 48 may be coupled to the computer 20 through the RS232 interface 42, or the network interface 32.
The mixer 55 in FIGS. 1 and 2 may be an ultrasonic mixer such as is made by Sonic and Materials of Danbury, Connecticut under the trademark VIBRA CELL. In alternative embodiments, a high speed homogenizer could be used such as are made by Brinkman (shroud with a high speed rotating shaft therein rotating at 28,000 RPM, thereby creating a high shear in the liquid and disintegrating particles therein). These units come with their own interfaces which may be used for the mixer interface 44. The basic control functions needed to control the mixer are the time of mixing and the power level which controls the amount of turbulence generated in the liquid. The mixer interface will be necessary electronics to interface with the mixer control circuit for the selected mixer. The details of how to interface the computer 20 to the interface circuits that come with the mixers will be apparent to those skilled in the art. A good reference for interfacing computers such as the computer 20 to control external instrumentalities is Libes and Garetz, Interfacing S-100/IEEE 696 Microcomputers, (Osborne/McGraw Hill 1981) which is hereby incorporated by reference. An auxiliary interface 46 is provided to allow the computer 20 to control external instrumentalities such as valves, solenoids, etc. which are outside the sample preparation system. Typically, this interface will be digital, programmable ports such as are commonly available in integrated circuit form where the characteristics of the ports may be set by the user.
FIG. 4 is a high level functional diagram of the control program in the computer 20 which allows users to program and run their own sequences of events to be performed in the sample preparation system under control by the control system of the invention. The control program runs the user defined sequences by generating the proper control signals to cause the desired sequence of events to occur in said sample preparation system.
At power up in some embodiments, the system will perform a self test to verify the integrity of the system prior to performing any operations. This is symbolized by block 50. Next, the system displays a user identification request/sample identification request screen as symbolized by block 52 (hereafter references to blocks will be understood to mean reference to those source code computer instructions organized as routines and subroutines in the control program which perform the function indicated in the block referred to). The purpose of block 52 is to supply query fields on the terminal or display 26 for the user to respond to by filling in the requested data via the keyboard 24. The requested data is to identify the user, to give various data items regarding the sample, to give the date and the time and to identify the sequence the user desires to run. The data items regarding the sample to be filled in may include the sample ID, the sample weight, and the lot number from which the sample came. The user identification number is used by the control system to determine the access privileges which the user has.
The control system has three levels of access. At the simple level, the user may only run sequences that have been previously programmed by the system manager. At the high level, users having access privileges at this level may program their own sequences of events using commands from a high level language command set. These commands represent predetermined building block functions which are necessary to perform sample preparation. Such building block functions include: mix, isolate known sample volume, flush the remaining liquid out of the sample preparation chamber, release the isolated sample volume, dilute the sample volume with a user defined volume of a user identified solvent, pump the diluted sample to the analyzer, etc. At the expert level, users having access to this level may program their own "macros" using system commands at a more detailed level than the high level commands identified above. These more detailed commands allow the user to control the system at a finer level of resolution. For example, a typical command may be an individual action to be taken by one of the electromechanical devices, such as open valve #1" or "rotate multiport valve #2 to state #3." Each of the high level commands is comprised of a predetermined sequence such actions, i.e., of expert level commands.
The identification data entered by the user in block 52 via the keyboard 24 is stored on the mass storage device 22 in block 54. Next the system, in block 56, determines the access privileges of the user by comparing the user ID to the list of ID numbers supplied by the system manager for each level of access.
Block 58 represents the step of displaying an option menu by which the user, by selecting an option, may express a request regarding what the user wishes the system to do or what the user desires to do with the system. Typical menu options include: start, status, method, directory, report, load, print, system, control, defaults, functions, and options. The meaning of these options will be explained more below.
After the user has entered his or her request via the keyboard 24, the control system verifies that the user has the access privilege necessary to perform the function requested in block 60. If so, the control system branches to the routine which performs the desired function or provides the facility requested by the user in block 62. If the user does not have the required access privilege, a message to that effect is displayed in block 64, and processing proceeds to block 58.
FIG. 5 is a flow chart of the various routines which are available for selection by the user in Step 58 of FIG. 4. The first routine, symbolized by block 67, is a routine which allows the user to create, modify, or delete an operation sequence. An operation sequence is a collection of commands which are executed by the central processing unit in order to generate control signals to control the electromechanical devices in the system. The control signals cause them to perform a physical sequence of events to process a sample where the sequence is defined by the particular sequence of commands in the program. The routine of block 67 allows the user to program his own sequences of commands at either of two levels of complexity. At a first level of complexity, the user may have access to a set of commands each of which represents a specified function that the system is capable of performing and each of which causes a predetermined sequence of events to occur in the proper order to cause the physical event symbolized by that command. The second level of complexity allows the user to have access to a set of commands which are very detailed. These commands each represent a single action or a very small group of actions that one or a very small group of electromechanical devices performs. Essentially, the commands at this second level are the component commands which are grouped together in a predetermined sequence to implement one of the commands on the first level. Essentially, then, the commands on the first level are macros which are collections of commands on the second level but arranged in a predetermined sequence for each particular command on the first level.
Block 66 is a routine which allows the user to print a hard copy of a sequence which has been programmed by the user.
Block 68 is a routine which allows the user to load a predetermined sequence, i.e., a method of sample preparation which has been preprogrammed by the system manager. The system manager is a user which has access to all functions of the system. That is, the system manager can define the access privileges of all the other users on the system, and he may program preprogrammed sequences which are available for certain users who are not allowed to program their own sequences. Block 68 is the routine which the user calls when one of these preprogrammed sequences is to be loaded.
Block 70 is a routine which allows the user to print a directory of all the methods or sequences which are stored in the system and available for execution. Block 72 represents a routine which allows the user to start the selected sample preparation routine and which causes the CPU to begin generating the control signals which cause the physical actions to occur.
Block 74 represents a routine which displays the system status. Block 76 is a routine which allows the user to print the system status which is displayed in the routine of Block 74.
Block 78 is a routine which allows the user to change the system default parameters. Typically, each command on either the first or second programming level will have parameters or arguments associated therewith. These arguments are variable values which define the specific manner in which the command is to be performed. For example, a mix command may have as an argument the power level at which the mix is to be performed, the time duration of the mix, and the RPM that the mixer is to use.
The routine represented by block 80 allows the user to have access to the various valve and relay controls such that the user may open certain valves or close certain relays manually by causing the CPU to generate the proper command to cause the proper operation of the valve, relay or other electromechanical device.
Block 82 represents a routine which allows the system manager to create new system functions.
Block 84 is a routine which allows the user to print a report. Such reports may consist of reports of user activity, the sequences which have been run, the volume of activity for a particular sequence, and so on. Block 86 is a routine which allows the user to change the print parameters. This routine allows the format of the report to be set such as margins, spacing, headers, and other types of formatting commands common to database report routines.
Block 88 is a routine which displays for the user the system options which have been elected and which are operable.
Block 90 is a routine which allows the user to use the print mode of the system for various functions.
Block 92 is a routine which allows the system manager access to certain system functions.
Referring to FIG. 6 there is shown a more detailed flow diagram of the create, modify and delete routine of block 67 in FIG. 5. The first step when the user elects to program his own sequence is to inquire whether the user wishes to program on the first level or on the second level noted above. The first level will be called the high level for purposes here, and this level will provide the user access to the macro commands. The second level will be called the expert level and grants the user access the detailed commands which essentially allow the user to define each valve opening and closing and each operation of each motor or other electromechanical device individually. The levels are named the high level and the expert level for purposes of indicating the relative amounts of skill needed to program on these levels. Programming at the high level is similar to calling subroutines or macros on any computer. Programming on the expert level is similar to programming in source code and requires a some programming skill and a great deal of knowledge regarding the hardware aspects of the system being programmed.
The process of determining which level the user wishes to have access to is symbolized by step 94. This step also determines the user's access privilege by checking the user's identification code and comparing it to a table or other such database defined by the system manager which indicates which users have access to the high level command set and which users have access to the expert level programming command set. If the user elects to program at the high level, the next step is symbolized by block 100. In this step, the user is prompted for a name for the sequence which he is about to program. After the sequence has been named, step 102 is performed wherein the user selects the first high level command which is to be executed in the sequence. In some embodiments, the list of high level commands from which the user may choose may be displayed and the user may simply choose a command by positioning the cursor on the proper command and pressing a select key. In other embodiments, the user may be required to know the high level commands and select the particular command desired by an acronym.
As noted above, most commands have certain parameters or arguments. Step 104 represents the process of prompting the user for parameter values for the command selected in step 102. Each command will have default parameters which are set by the user in step 78 of FIG. 5. If the user wishes to use the default parameters, he need do nothing in step 104. If however, the user wishes to define the specific manner in which the particular command is to be executed, then the parameters for that command may be adjusted in step 104.
After step 104 is performed, the control software causes the central processing unit to prompt the user to determine if the command just defined is the last command in the sequence. This step is symbolized by block 106 in FIG. 6. If the user is done picking commands, the processing proceeds to step 108 where the method is stored in permanent storage such as on a floppy disk or hard disk. Processing then returns to the main menu symbolized by block 58 in FIG. 4.
If the user is not finished programming, then processing proceeds from block 106 to block 110 where the user is prompted to select the next high level command in the sequence. Processing then proceeds to block 112 where the parameters for the command selected in block 110 are displayed and the user is prompted for new values for these parameters. If the user responds with new parameters, these are stored with the command as a permanent part of the sequence being programmed. After step 112 is performed, step 114 is performed to again to test for completion of programming. Step 114 represents the process of prompting the user to determine if the user is done programming. If he is, then processing continues at step 108 as described above to store the method. If the user is not done programming as determined in step 114, then processing returns to step 110 where the user is prompted to select the next command in the sequence.
Returning again for a moment to step 94 in FIG. 6, if the user is determined to have no access to either the high level or expert level programming command sets, then step 94 vectors processing to a step 96 wherein a "no access privilege for selected level" message is displayed on the terminal. Thereafter, in step 98, processing is returned to the main menu of step 58 in FIG. 4.
If the user selects the expert level for programming, a similar sequence of events occurs starting with step 116. There the user is prompted to name the sequence he is about to define. The next step, 118, prompts the user to select the first expert level command to be executed in the sequence. Then, in step 120, the user is prompted to select new parameters for the expert level command selected in step 118. Again, the expert level commands also have default values which may be altered by the user in step 120. Step 122 represents a test to determine if programming has been completed. If it has, then step 108 is performed as described above. If programming is not completed, processing proceeds to step 124. There the user is prompted to select the next expert level command and define the parameters for that command.
Step 126 represents a test to determine whether the user is done programming. If he is, then step 108 is performed and control is returned to the main menu. If the user is not done programming, then control returns to step 124 where the user is prompted to select the next expert level command.
Although the invention has been described in terms of the preferred and alternative embodiments detailed herein, those skilled in the art will appreciate that many modifications may be made. All such modifications are intended to be included within the scope of the claims appended hereto.
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The two levels of programming complexity include a high level and an expert level. The command set on the high level includes a plurality of commands which comprise sequences of more detailed commands from the expert level. The expert level commands comprise single actions or operations, or small groups of operations, to be performed by the electromechanical devices, such as valve openings or closures. User access privileges are definable by a system manager to restrict different classes of users to one or more of the levels of complexity.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority to and the benefit of Korean Patent Application No. 10-2012-0013470 filed in the Korean Intellectual Property Office on Feb. 9, 2012 respectively, the entire contents of which are incorporated herein by reference.
TECHNICAL FIELD
[0002] The present invention relates to a secondary battery, and more particularly, to a redox flow secondary battery that uses an electrode in which a porous metal is coated with carbon.
BACKGROUND
[0003] Electricity storage technologies are important technologies for efficiently maximizing performance in areas such as efficient use of electricity, improvement of ability or reliability of a power supply system, expansion of introducing renewable energy in which a range of changes depending on time is large, energy recuperation of a moving object, and the like, throughout an entire energy industry, and their development possibilities to meet demands for social contribution are being gradually increased.
[0004] In order to adjust a supply-demand balance of a semi-autonomous local power supply system such as a microgrid, appropriately distribute non-uniform output of development of the renewable energy such as wind power or solar energy generation, and control an influence of voltage and frequency changes generated by a difference from a conventional electric power system, studies on secondary batteries are being actively conducted, and expectations with respect to the utilization of the secondary batteries are being increased in these fields.
[0005] Referring to characteristics required for a secondary battery to be used for storing of high-capacity power, the secondary battery should have a high energy storage density, and thus a redox flow secondary battery is being spotlighted as the secondary battery having a high capacity and high efficiency, which is the most appropriate to these characteristics.
[0006] The redox flow secondary battery is formed so that a cell frame forms an outline of an entire cell, a center of the cell is divided by an ion exchange layer, and an anode and a cathode are located at both sides of the ion exchange layer.
[0007] Further, the redox flow secondary battery is formed to include a bipolar plate and a current collector for externally conducting electricity from each of the electrodes provided, an anode tank and a cathode tank, which store electrolytes, an inlet in which the electrolytes flow in, and an outlet in which the electrolytes flow out.
[0008] Various studies are being conducted on such the redox flow secondary battery to develop to an increase in both output and energy efficiency. Recently, a non-aqueous electrolyte rather than an aqueous electrolyte has been mainly used.
[0009] As described above, in order to develop the redox flow secondary battery to which the non-aqueous electrolyte is applied, use of the electrode in which affinity with the non-aqueous electrolyte is high and having excellent electrical conductivity is required, and thus research and development of the electrode in which these requirements are satisfied are urgently needed.
[0010] In the case of a carbon-based material used for an energy electrode material of a commercial redox flow secondary battery, since affinity with the non-aqueous electrolyte is very low as well as conductivity is significantly reduced compared to a metal electrode, improvement in energy efficiency is limited when applied to a non-aqueous redox flow secondary battery.
[0011] Various studies for development of the metal electrodes are being conducted to improve an electrochemical characteristic of the non-aqueous redox flow secondary battery. However, there is a limit on increase of a specific surface area of the metal electrode in a manufacturing process, and thus these studies are not proposing a fundamental solution to an improvement of energy efficiency of the non-aqueous redox flow secondary battery.
SUMMARY
[0012] The present invention is directed to providing a redox flow secondary battery capable of ensuring conductivity of an electrode using a porous metal having excellent conductivity.
[0013] The present invention is also directed to providing a redox flow secondary battery using a porous metal electrode uniformly coated with carbon having a large specific surface area to improve energy efficiency.
[0014] The present invention is also directed to providing a redox flow secondary battery in which a porous metal electrode is coated with carbon having a large specific surface area and thus reactivity is improved.
[0015] One aspect of the present invention provides a redox flow secondary battery including a unit cell, a pair of current collectors, and a pair of cell frames. The unit cell is formed of a porous metal, and includes a pair of electrodes formed at a surface of the porous metal coated with carbon. The pair of current collectors are bonded to both outer surfaces of the unit cell. The pair of cell frames are attached to each outer surface of the current collectors.
[0016] In the redox flow secondary battery according to the present invention, the amount of carbon coated on the surface of the porous metal may be 50 wt % or less compared to a weight of the porous metal.
[0017] In the redox flow secondary battery according to the present invention, the porous metal may be any one selected from nickel (Ni), copper (Cu), iron (Fe), molybdenum (Mo), titanium (Ti), platinum (Pt), and iridium (Ir).
[0018] In the redox flow secondary battery according to the present invention, the coating may be performed using any one selected from a dip coating method and a spray coating method.
[0019] In the redox flow secondary battery according to the present invention, a carbon content of coating slurry for the coating may be 50 wt % or more.
[0020] In the redox flow secondary battery according to the present invention, the unit cell includes an ion exchange layer, the pair of electrodes each bonded to both surfaces of the ion exchange layer and including an anode and a cathode, and a pair of plates in which one surface is bonded to an outer surface of each of the pair of electrodes and the other surface is bonded to the current collector.
[0021] In the redox flow secondary battery according to the present invention, the unit cell generates electricity according to an oxidation-reduction reaction through the ion exchange layer between the electrodes.
[0022] The redox flow secondary battery according to the present invention may further include anode and cathode tanks, pumps, inlets, and outlets. The anode and cathode tanks are disposed at left and right sides of cell frame, respectively, and configured to store an electrolyte to flow the electrolyte. The pumps each are connected to the anode and cathode tanks, and supplies the electrolyte. The inlet connects the pump to the cell frame so that the electrolyte flows into the unit cell through the cell frame. The outlet connects to the cell frame so that the electrolyte flowed out from the unit cell flows into the anode and cathode tanks.
[0023] Another aspect of the present invention provides a redox flow secondary battery including at least one unit cell having at least one pair of electrodes formed of a porous metal coated with carbon.
[0024] Still another aspect of the present invention provides a redox flow secondary battery including a pair of cell frames formed to face and to be spaced apart from each other, a pair of current collectors each attached to inner surfaces of the pair of cell frames, and at least two unit cells formed between the pair of current collectors, wherein the unit cell includes at least one pair of electrodes formed of a porous metal coated with carbon.
[0025] According to the present invention, a redox flow secondary battery using a porous metal electrode uniformly coated with carbon is provided, and thus conductivity of the electrode is improved.
[0026] Further, a surface of the porous metal electrode is uniformly coated with a carbon layer having a large specific surface area, and thus reactivity can be improved.
[0027] Therefore, capacity of the redox flow secondary battery and energy efficiency can be improved and resistance of a cell can be effectively reduced. Further, the electrode is uniformly coated with the carbon layer, and thus corrosion resistance can also be improved.
BRIEF DESCRIPTION OF DRAWINGS
[0028] FIGS. 1 and 2 are views for describing a redox flow secondary battery according to an embodiment of the present invention.
[0029] FIG. 3 is images for comparing the morphology of an electrode according to the present invention with comparative examples.
[0030] FIGS. 4 and 5 are graphs for comparing cyclic voltammetry (CV) characteristics of embodiments of the electrode according to the present invention with comparative examples.
[0031] FIG. 6 is a graph for comparing energy efficiency of the embodiment of the electrode according to the present invention with the comparative example.
[0032] FIGS. 7 and 8 are views for describing a redox flow secondary battery according to another embodiment of the present invention.
DETAILED DESCRIPTION
[0033] Before detailed description of embodiments of the present invention, terms and words used in this specification and claims should not be interpreted as limited to commonly used meanings or meanings in dictionaries and should be interpreted with meanings and concepts which are consistent within the technological scope of the invention based on the principle that the inventors have appropriately defined concepts of terms in order to describe the invention in the best way. Therefore, since the embodiments described in this specification and configurations illustrated in drawings are only exemplary embodiments and do not represent the overall technological scope of the invention, it is understood that the present invention covers various equivalents, modifications, and substitutions at the time of the filing of this application.
[0034] Hereinafter, exemplary embodiments of the invention will be described in detail with reference to the accompanying drawings. The same reference numbers will be used throughout this specification to refer to the same or like parts. However, detailed descriptions of well-known functions or configurations that unnecessarily obscure the gist of the invention in the following explanations and accompanying drawings will be omitted. For the same reason, some components are exaggerated, omitted or schematically shown in the drawings, and a size of each component is not entirely reflected as an actual size.
[0035] Hereinafter, exemplary embodiments of the inventive concept will be described in detail with reference to the accompanying drawings.
[0036] First, a redox flow secondary battery according to an embodiment of the present invention will be described. FIGS. 1 and 2 are views for describing the redox flow secondary battery according to the embodiment of the present invention. Here, FIG. 1 is an exploded view showing disassembled components of the redox flow secondary battery according to the embodiment of the present invention, and FIG. 2 is a cross-sectional view showing a cross section of the redox flow secondary battery according to the embodiment of the present invention.
[0037] Referring to FIGS. 1 and 2 , the redox flow secondary battery according to the embodiment of the present invention is a secondary battery charged or discharged using an oxidation-reduction reaction of a metal ion in which valency is changed. Further, the redox flow secondary battery according to the embodiment of the present invention may be driven in a voltage range of 0 to 3.0 V.
[0038] The redox flow secondary battery according to the embodiment of the present invention may be formed to have a unit cell 100 having a multi-layer structure in a plate shape, a pair of current collectors 40 bonded to both outer surfaces of the unit cell 100 and formed in a plate shape, and cell frames 50 attached to outer surfaces of the current collectors 40 , respectively and formed in a plate shape.
[0039] Here, the unit cell 100 includes an ion exchange layer 10 , electrodes 20 , and bipolar plates 30 (hereinafter, abbreviated as “plates”), of which each have a plate shape, and has a structure in which the electrodes 20 , in which an anode is opposite a cathode as a pair, each are bonded to both surfaces of the ion exchange layer 10 based on a center of the ion exchange layer 10 , and the plates 30 each are bonded to outer surfaces of the anode and the cathode of the electrodes 20 . Meanwhile, although not shown, a gasket may be selectively interposed between the electrode 20 and the ion exchange layer 10 .
[0040] As described above, the ion exchange layer 10 , the electrodes 20 , and the plates 30 , of which each have a plate shape, form a unit cell 100 in a multi-layer structure.
[0041] The oxidation-reduction reaction of the metal ion in which valency is changed occurs in the unit cell 100 . In this case, the oxidation-reduction reaction occurs between the anode and the cathode of the electrodes 20 through the ion exchange layer 10 , and thus electricity is generated by the oxidation-reduction reaction.
[0042] When the electricity is generated at the anode and the cathode of the electrodes 20 of the unit cell 100 , the plates 30 and the current collectors 40 collect the generated electricity. The cell frames 50 maintains and supports a shape of the ion exchange layer 10 , the pair of electrodes 20 , the pair of plates 30 , and the pair of current collectors 40 described above.
[0043] Further, the redox flow secondary battery according to the embodiment of the present invention may further include an anode tank 60 , a cathode tank 70 , pumps 61 and 71 , inlets 63 and 73 , and outlets 65 and 75 .
[0044] The anode tank 60 and the cathode tank 70 store an anodic electrolyte and a cathodic electrolyte, respectively, to flow when required. It is preferably that the anode tank 60 and the cathode tank 70 respectively use non-aqueous electrolytes as the anodic electrolyte and the cathodic electrolyte, however, aqueous electrolytes may also be used. Such the anode tank 60 and the cathode tank 70 each are disposed on the both outer surfaces of the unit cell 100 corresponding to the anode and the cathode of the electrode 20 of the unit cell 100 described above.
[0045] Further, the anode tank 60 and the cathode tank 70 are connected to the cell frames 50 through the inlets 63 and 73 and the outlets 65 and 75 , respectively. The inlets 63 and 73 are paths through which the electrolytes of the anode tank 60 and the cathode tank 70 flow into the unit cell 100 , and the outlets 65 and 75 are paths through which the electrolytes flow from the unit cell 100 . Further, the pumps 61 and 71 are provided to flow the electrolytes from the anode tank 60 and the cathode tank 70 and supply the electrolytes to the unit cell 100 , and are interposed between the anode tank 60 and the inlet 63 and between the cathode tank 70 and the inlet 73 , respectively.
[0046] Therefore, the electrolytes flowed out from the anode tank 60 and the cathode tank 70 may be supplied to the unit cell 100 through the pumps 61 and 71 , the inlets 63 and 73 , the cell frames 50 , and the current collectors 40 , respectively and in the reverse order, flowed and stored in the anode tank 60 and the cathode tank 70 .
[0047] In the redox flow secondary battery configured according to the embodiment of the present as described above, the ion exchange layer 10 may be formed of Nafion. Further, the plates 30 may be formed of graphite.
[0048] As described above, the electrodes 20 are bonded to inner surfaces of the plates 30 , respectively. Such the electrodes 20 each have a characteristic in which a surface of a porous metal is uniformly coated with a carbon layer. According to the embodiment of the present invention, the electrodes 20 are formed at the porous metal thereof is uniformly coated with carbon.
[0049] Here, the porous metal may be any one selected from nickel (Ni), copper (Cu), iron (Fe), molybdenum (Mo), titanium (Ti), platinum (Pt), and iridium (Ir).
[0050] Further, it is preferable that the porous metal is coated so that the amount of carbon coated on the surface of the porous metal is 50 wt % or less compared to a weight of the porous metal. Further, it is preferable that a dip coating method or a spray coating method is used as a coating method. When a carbon coating slurry for the coating is manufactured, the coating slurry is manufactured to have a carbon content of 50 wt % or more.
[0051] As described above, the porous metal electrode uniformly coated with carbon is used on surfaces of an aqueous or a non-aqueous redox flow secondary battery and a stacked type battery that will be described below, and thus capacity of the non-aqueous redox flow secondary battery and energy efficiency may be enhanced, and a corrosion characteristic may be improved.
[0052] Next, a morphology of the electrode according to embodiments of the electrode of the present invention will be compared with comparative examples. FIG. 3 is images for comparing the morphology of the electrode according to the present invention, and field emission scanning electron microscope (FESEM) images of the comparative examples and the embodiments of the electrode of the present invention are disclosed.
[0053] Referring to FIG. 3 , it may be determined that the electrodes 20 of the embodiments in which the surfaces of the porous metals are uniformly coated with carbon. Details of the comparative examples and the embodiments are as the following [Table 1].
[0000]
TABLE 1
Amount of Carbon
Metal type
Pore Size
Coating
Comparative
Ni
800
0 wt %
Example 1
Comparative
Cu
800
0 wt %
Example 2
Embodiment 1
Ni
800
5 wt %
Embodiment 2
Cu
800
5 wt %
[0054] The electrodes 20 of Embodiments 1 and 2 of the present invention are coated using a spray coating method, after slurry having a composition of Super-P:binder:N-methylpyrrolidinone (NMP)=2.5:2.5:95 is manufactured, when the surface of the porous metal is coated with carbon. The amount of coated carbon (amount of carbon coating) was measured as a weight ratio of the coating before and after.
[0055] A cyclic voltammetry (CV) characteristic of the electrode of the present invention will be compared through the embodiment of the electrode of the present invention and the comparative examples. FIGS. 4 and 5 are graphs for comparing CV characteristics of the embodiments of the electrodes according to the present invention with the comparative examples. Here, the CV characteristic evaluation was performed on Comparative examples 1 and 2 of [Table 1] described above and the embodiments of the porous metal electrode coated with carbon using a spray coating method of a propylene carbonate (PC)-based organic electrolyte.
[0056] In FIGS. 4 and 5 , in order to evaluate an electrochemical characteristic of the porous metal electrode coated with carbon, a CV measurement was performed in various non-aqueous electrolytes. In this case, the measurement was performed under a condition of a scan rate of 1 mV/s in a potential area in a range of −1.8 to 0.0 V compared to Ag/Ag + . FIG. 4 is a graph showing the CV characteristics of the comparative examples and the embodiments in a Co(bpy) + PC electrolyte, and FIG. 5 is a graph showing the CV characteristics of the comparative examples and the embodiments in an Ni(bpy) + PC electrolyte.
[0057] As shown in FIGS. 4 and 5 , referring to CV results of the comparative examples and the embodiments, when copper (Cu) and nickel (Ni) porous metal electrode coated with carbon is applied in various PC-based non-aqueous electrolytes, it may be determined that reactivity of the embodiments is significantly increased compared to that of the comparative examples. That is, it may be determined that a current value to be used for oxidation of the ion was increased. The increase of the current value is due to improvement of conductivity of the electrode using the porous metal, and also because the carbon coated on the surface of the porous metal efficiently provides a redox reaction site.
[0058] Next, energy efficiency characteristics of the electrode of the present invention will be compared through the embodiment of the electrode of the present invention and a comparative example. FIG. 6 is a graph for comparing energy efficiency of the embodiment of the electrode according to the present invention with a comparative example. Here, energy efficiency of cells to which Comparative examples 1 and 2 are applied as an anode and a cathode, and energy efficiency of cells to which Embodiments 1 and 2 are applied as an anode and a cathode was compared.
[0059] Referring to FIG. 6 , it may be determined that the cells which are coated with carbon according to applications of Embodiments 1 and 2 show enhanced Coulomb efficiency and energy efficiency. In the case of the applied embodiments, the initial energy efficiency is 82% which is a better characteristic than 77% of the energy efficiency of the applied comparative examples. Further, the Coulomb efficiency was increased from 93% to 95% through carbon coating on the surface of the porous metal electrode.
[0060] FIGS. 7 and 8 are views for describing a redox flow secondary battery according to another embodiment of the present invention. Here, FIG. 7 is an exploded view showing disassembled components of the redox flow secondary battery according to another embodiment of the present invention. FIG. 8 is a cross-sectional view showing a cross section of the redox flow secondary battery according to another embodiment of the present invention.
[0061] Referring to FIGS. 7 and 8 , the redox flow secondary battery according to another embodiment of the present invention is a secondary battery charged or discharged using oxidation-reduction reaction of a metal ion in which valency is changed. Further, the redox flow secondary battery according to another embodiment of the present invention may be driven in a voltage range of 1.5 to 3.0 V.
[0062] The redox flow secondary battery according to another embodiment of the present invention includes a pair of cell frames 50 , a pair of current collectors 40 , and a plurality of unit cells 100 .
[0063] The pair of cell frames 50 are spaced apart from each other by a predetermined distance and opposite each other. As described above, the pair of current collectors 40 are bonded to inner surfaces of the pair of cell frames 50 facing each other, respectively. The plurality of unit cells 100 are interposed between the pair of current collectors 40 . As described above, the plurality of unit cells 100 each include an ion exchange layer 10 , electrodes 20 including an anode and a cathode, and plates 30 . As shown, the plurality of unit cells 100 are connected to each other in series and share the plates 30 connected to each other. For example, the redox flow secondary battery in which three unit cells 100 are formed is shown in FIGS. 7 and 8 . As shown, since the three unit cells 100 share the two connected plates 30 , there are four plates 30 . Such the redox flow secondary battery according to another embodiment of the present invention is a stacked type battery in which the three unit cells 100 are stacked in series.
[0064] As described above, in a structure in which the plurality of unit cells 100 are connected to each other in series, the electrodes 20 each have a characteristic in that a surface of a porous metal thereof is uniformly coated with a carbon layer as disclosed in FIG. 3 . Since each electrode 20 has the same configuration as the electrode of the redox flow secondary battery according to the embodiment of the present invention, detail descriptions will be omitted.
[0065] Further, although not shown in FIGS. 7 and 8 , the redox flow secondary battery according to another embodiment of the present invention further includes an anode tank 60 , a cathode tank 70 , pumps 61 and 71 , inlets 63 and 73 , and outlets 65 and 75 as the same as the redox flow secondary battery according to the embodiment of the present invention.
[0066] The anode tank 60 and the cathode tank 70 store an anodic electrolyte and a cathodic electrolyte, respectively, to be flowed when required, and use a non-aqueous electrolyte as the anode and cathode electrolytes. Such the anode tank 60 and the cathode tank 70 each are disposed at left and right sides of the unit cell 100 corresponding to the anode and the cathode of the electrode 20 of the unit cell 100 described above. Further, the anode tank 60 and the cathode tank 70 are connected to the cell frames 50 through the inlet 63 and 73 and the outlet 65 and 75 , respectively. Further, the pumps 61 and 71 are provided to flow the electrolytes from the anode tank 60 and the cathode tank 70 and supply the electrolytes to the unit cells 100 , and are interposed between the anode tank 60 and the inlet 63 and between the cathode tank 70 and the inlet 73 , respectively. That is, the electrolytes flowed out from the anode tank 60 and the cathode tank 70 may be supplied to the unit cells 100 through the pumps 61 and 71 , the inlets 63 and 73 , the cell frames 50 , and the current collectors 40 , respectively and in the reverse order, flowed and stored in the anode tank 60 and the cathode tank 70 .
[0067] Meanwhile, in the above-described embodiments, it was described for coating on the porous metal using only a dip coating method or a spray coating method. However, the embodiment of the present invention is not limited thereto. That is, various methods such as a vapor deposition method, a sputtering method, a chemical vapor deposition method, and the like may be selectively or complexly used if necessary.
[0068] Further, in the above-described embodiments, it was described in an example for a case in which the electrode is formed of a porous metal. However, the embodiment of the present invention is not limited thereto, and the metal may be formed in a mesh shape. Further, a type in a flat plate shape, such as a conventional type, may also be possible when appropriately coated with carbon.
[0069] Further, in the above-described embodiments, it was described in an example for a case in which the coating layer is formed on the electrode of the non-aqueous redox flow secondary battery. However, the embodiment of the present invention is not limited thereto, and may also be applied to the electrode of the aqueous redox flow secondary battery.
[0070] In addition, in the above-described embodiments, it was described as an example as to the electrode provided in the redox flow secondary battery. However, the embodiment of the present invention is not limited thereto; the electrode may be widely applied to a battery including the electrode accommodated in an electrolyte, and specifically, to a stacked type battery.
[0071] In this specification, exemplary embodiments of the present invention have been classified into the first, second and third exemplary embodiments and described for conciseness. However, respective steps or functions of an exemplary embodiment may be combined with those of another exemplary embodiment to implement still another exemplary embodiment of the present invention.
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The present invention relates to a redox flow secondary battery. The redox flow secondary battery of the present invention comprises a unit cell including a pair of electrodes made of a porous metal, wherein the surface of the porous metal is coated with carbon. According to the present invention, a redox flow secondary battery using porous metal electrodes uniformly coated with carbon is provided, thus improving conductivity of the electrodes, and the electrodes have surfaces uniformly coated with a carbon layer having a wide specific surface area, thus improving reactivity. As a result, capacity of the redox flow secondary battery and energy efficiency can be improved and resistance of a cell can be effectively reduced. Further, the electrodes are uniformly coated with a carbon layer, thus also improving corrosion resistance.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to the field of synthetic cables. More specifically, the invention comprises a cable termination which allows a cable to freely flex without placing excessive stress on the cable strands.
[0003] 2. Description of the Related Art
[0004] Devices for mounting a termination on the end of a cable are disclosed in detail in copending U.S. Application Ser. No. 60/404,973 to Campbell, which is incorporated herein by reference.
[0005] The individual components of a wire rope are generally referred to as “strands,” whereas the individual components of synthetic cables are generally referred to as “fibers.” For purposes of this application, the term “strands” will be used generically to refer to both.
[0006] Some type of fitting must typically be added to a cable in order to transmit a load to the cable. An old example of this idea is to wrap one end of a cable back upon itself—usually around an “eye” or “thimble” device—then clamp the cable to itself with one or more U-bolts. The resulting assembly on the end of the cable is referred to as a “termination.”
[0007] It is known to terminate the strands of a synthetic cable by locking them into an anchor. The strands can be locked in place using a mechanical clamp, solidified potting compound, or other known approaches. The use of potting compound is perhaps the most common. For this approach, the strands are typically splayed into a diverging pattern and infused with liquid potting compound (using a variety of known techniques). The liquid potting compound is any substance which transitions from a liquid to a solid over time. The most common example would be a cross-linking adhesive such as an epoxy. Those skilled in the art know that such adhesives use two separate liquids which cross-link when mixed together. Such a liquid is mixed just prior to wetting the strands.
[0008] The wetted strands are at some point placed in a cavity within the anchor (in some cases prior to wetting and in some cases after wetting), so that when the liquid potting compound hardens the strands will be locked to the anchor. The anchor and the portion of cable locked therein are then collectively referred to as a termination.
[0009] FIG. 1 shows a prior art termination 14 for a synthetic cable (in a sectional view). Anchor 18 features an expanding cavity 28 joined to a straight portion 38 . The hardened potting compound forms potted region 16 , in which the strands are locked rigidly in place. The portion of cable 10 below the anchor (with respect to the orientation shown in the particular view) is relatively free to flex. The transition from the freely flexing portion of the cable to the portion locked within the potting compound is denoted as potting transition 20 .
[0010] The reader should at this point consider the differences between traditional wire rope strands and modern synthetic cable strands. Wire rope strands are relatively large, relatively stiff, and have a moderate surface coefficient of friction. Synthetic cable strands are, in comparison, quite small, have very little stiffness, and have a very low coefficient of friction. Synthetic strands are analogous to human hair in terms of size and stiffness. These differences mean that termination techniques traditionally used for wire rope cannot be used for synthetic cables—or at least not without substantial modification.
[0011] Those skilled in the art will know that the maximum theoretical stress a cable can withstand (force per unit area) is 100% of the maximum theoretical stress an individual strand can withstand. In practice, of course, the cable as a whole never reaches 100% of the strand strength. In wire rope applications, an ultimate cable stress of 70% of the individual strand stress is quite good.
[0012] Of course, numerous other factors degrade the ultimate stress a cable can withstand. Bending of the cable is perhaps the most significant of these. A cable is ideally loaded while in perfect alignment. Deviations from this alignment degrade the performance. One particularly worrisome situation is where a cable is fixed at one end within an anchor and the freely flexing portion is then bent with respect to the anchor. FIG. 9 shows such a situation.
[0013] Wire ropes tolerate this condition fairly well. Their strand stiffness—the strands are typically steel—preserves the cable's circular cross section as it passes through an arcuate bend. The stiffness—as well as the internal friction between the strands—means that the strands stay well organized. Thus, the loss of ultimate tensile strength a wire rope experiences when undergoing a bend is manageable.
[0014] This is not true for synthetic cables. FIG. 2 shows a synthetic cable termination undergoing a significant bend. Flexible region 30 of cable 10 has been pulled to one side, forming a first kink 22 where the cable exits the anchor and a second kink 72 where the cable exits the potted region. These two kinks—which may be significantly different in nature—place considerable stress on the individual strands, and may even break or cut some strands. The cable has also flattened substantially in the region of second kink 72 . The result is that the majority of the load is carried by a relatively small number of strands.
[0015] FIG. 3 shows another type of prior art anchor 18 . The version shown does not include a straight portion. A relatively sharp corner is present proximate potting transition 20 . This sharp corner exacerbates the problem seen in FIG. 2 , since the sharp corner may actually cut synthetic strands which are forced against it (Solidified potting compound often creates a very sharp edge).
[0016] FIG. 3A shows a greatly magnified view of potting transition 20 . The portion of the strand 32 lying within potted region 16 is held in alignment. Where it exits the hardened potting compound, however, it undergoes an immediate sharp bend. This bend produces stress concentration 66 . FIG. 3A represents a very uniform (“good”) potting transition. However, the reader will perceive how substantial stress concentration in individual strands can nevertheless occur.
[0017] FIG. 4 shows the kinking of the individual fibers against a sharp corner where they exit an anchor. Strands at this point are subject to axial compression and bending compression. Such lateral loading are often cyclic in nature, resulting in “flex fatigue” (a condition of accumulating plastic deformation or outright breakage of the individual cable strands).
[0018] The strands actually forced against the corner may even be cut. Synthetic cable strands have little cut resistance in comparison to wire rope strands. This fact represents yet another difference between synthetic cables and wire ropes. Strand cutting is a much larger concern for synthetic cables.
[0019] Looking now at FIG. 5 , the reader will note that the potting transition 20 is typically irregular in shape, since the infusion of the liquid potting compound through the strands may not be uniformly planar. A portion of hardened potting compound can extend into the freely flexing region of cable near the cable's centerline. This portion often breaks free when the cable is flexed laterally. The existence of the solid region—even when broken free—tends to kink and abrade the cable's strands.
[0020] Some prior art anchors have included features which could mitigate the aforementioned problems somewhat (at least insofar as they reduce an edge actually cutting into the cable). These features are typically the result of manufacturing convenience or cosmetics, rather than any specific attempt to address the problem of flexural loads. FIG. 6 shows an anchor 18 having a small fillet 24 around its lower edge (the fillet joins the lower surface and, in this case, the wall of straight portion 38 ). (Throughout this disclosure, directional terms such as “upper” and “lower” will be understood to refer only to the orientation shown in the view. The devices disclosed will obviously function in any orientation).
[0021] FIG. 7 shows an anchor 18 having a small chamfer 26 around its lower edge. Such a chamfer is sometimes added to prevent a sharp corner existing at the bottom of expanding cavity 28 (For an anchor having no straight portion, this feature can be particularly important). Such fillets and chamfers have traditionally been added to facilitate machining of the anchors on a lathe or automatic screw machine. Those skilled in the art will know that a sharp corner at the mouth of a bore is undesirable for such machining.
[0022] While some flex-mitigating features are found in the prior art terminations, they do not readily accommodate substantial lateral flexing of the cable. Thus, when such terminations are attached to an object, the attachment must allow the anchor to move freely so that it remains aligned with the cable. Suitable attachments include ball and socket joints. However, it is often desirable to attach the anchor to an object without allowing any movement. An example would be an externally threaded anchor which is threaded into a hole in a plate. Once installed, the anchor will be rigidly held.
[0023] The prior art includes certain strain-relieving devices. FIG. 16 shows the addition of a soft boot 44 encircling the portion of cable 10 which is immediately adjacent to anchor 18 . Made of a pliable material—such as a hard rubber—the soft boot can reduce strand kinking. FIG. 17 shows another type of boot—designated as external boot 46 . This version attaches to the outside surface of anchor 18 , while still surrounding the portion of the cable which is adjacent to the anchor.
[0024] Unfortunately, it is difficult to design a soft boot which can accommodate the different loads and different bending angles which can be placed on a cable. FIG. 18 shows a soft boot using a relatively stiff material. The cable tends to bend near the exit of the boot, causing bend point 48 . Thus, the unwanted bend has merely been shifted downward rather than eliminated.
[0025] In order to reduce this phenomenon, the designer will often substitute a more pliable compound. Such a pliable compound has been used in FIG. 19 . However, at higher loads or angles, a bend point 48 still results, albeit in a higher location. The reader will thereby appreciate the difficulty in optimizing the boot stiffness using the prior art approach. Thus, while the prior art devices can reduce problems associated with the lateral flexing of a cable, a more advanced solution is desirable.
BRIEF SUMMARY OF THE PRESENT INVENTION
[0026] The present invention comprises terminations having features which reduce and control stress in the transition between the portion of the cable locked within the termination and the freely flexing region of a cable when the cable flexes laterally with respect to the anchor. Several favorable geometries are disclosed.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0027] FIG. 1 is a sectional perspective view, showing a prior art termination.
[0028] FIG. 2 is a sectional perspective view, showing bending in a prior art termination.
[0029] FIG. 3 is a sectional perspective view, showing a common prior art anchor.
[0030] FIG. 3A is a detail view, showing the bending of an individual strand.
[0031] FIG. 4 is a detail view, showing strands bending around a corner.
[0032] FIG. 5 is a sectional perspective view, showing an irregular potting transition.
[0033] FIG. 6 is a sectional perspective view, showing manufacturing features of the prior art.
[0034] FIG. 7 is a sectional perspective view, showing manufacturing features of the prior art.
[0035] FIG. 8 is a sectional perspective view, showing one embodiment of the present invention.
[0036] FIG. 9 is a sectional elevation view, showing one embodiment of the present invention.
[0037] FIG. 10 is a sectional elevation view, showing one embodiment of the present invention.
[0038] FIG. 11 is a sectional elevation view, showing one embodiment of the present invention.
[0039] FIG. 12 is a sectional elevation view, showing one embodiment of the present invention.
[0040] FIG. 13 is a sectional elevation view, showing one embodiment of the present invention.
[0041] FIG. 14 is a sectional elevation view, showing one embodiment of the present invention.
[0042] FIG. 15 is a sectional elevation view, showing one embodiment of the present invention.
[0043] FIG. 16 is a sectional perspective view, showing a prior art boot.
[0044] FIG. 17 is a sectional perspective view, showing a prior art boot.
[0045] FIG. 18 is a sectional perspective view, showing a prior art boot.
[0046] FIG. 19 is a sectional perspective view, showing a prior art boot.
[0047] FIG. 20 is a sectional elevation view, showing one embodiment of the present invention.
[0048] FIG. 21 is a sectional elevation view, showing one embodiment of the present invention.
[0049] FIG. 22 is a sectional elevation view, showing one embodiment of the present invention.
[0050] FIG. 23 is a sectional elevation view, showing one embodiment of the present invention.
[0051] FIG. 24 is a sectional elevation view, showing one embodiment of the present invention.
[0052] FIG. 25 is a sectional elevation view, showing one embodiment of the present invention.
[0053] FIG. 26 is a sectional elevation view, showing one embodiment of the present invention.
[0054] FIG. 27 is a sectional perspective view, showing one embodiment of the present invention.
[0055] FIG. 28 is a sectional perspective view, showing one embodiment of the present invention.
[0056] FIG. 29 is a sectional perspective view, showing an intermediate termination.
[0057] FIG. 30 is a sectional perspective view, showing one embodiment of the present invention.
[0058] FIG. 31 is a sectional perspective view, showing one embodiment of the present invention.
REFERENCE NUMERALS IN THE DRAWINGS
[0059]
10
cable
14
termination
16
potted region
18
anchor
20
potting transition
22
kink
24
fillet
26
chamfer
28
expanding cavity
30
flexible region
32
strand
34
circular expansion
36
parabolic expansion
38
straight portion
40
linear expansion
42
buffer material
44
soft boot
46
external boot
48
bend point
50
smooth expansion
52
angular range
54
shoulder
56
relieved portion
58
step relief
60
jacket
62
slotted expansion
64
intermediate termination
66
stress concentration
68
middle expansion
70
expansion bell
72
second kink
DESCRIPTION OF THE INVENTION
[0060] FIG. 8 shows a sectional view of an anchor 18 made according to the present invention (Those skilled in the art will know that such anchors are generally radially symmetric). It features an expanding cavity 28 and a straight portion 38 as in the prior art. Circular expansion 34 is added to the bottom of straight portion 38 . The radius of this circular expansion is quite large, being at least equal to the radius of the cable to be locked into the anchor.
[0061] FIG. 9 is an elevation sectional view through the anchor of FIG. 8 , with a cable being installed and flexed laterally. In this particular example, the cable has been locked in the anchor via potting. The reader should bear in mind that the particular method of locking the cable strands into the anchor is not particularly important to the present invention. The invention can function for terminations where the strands are mechanically clamped in place within the anchor. Because potting is a very common approach, however, potting is used as the means of locking the strands within the anchor throughout the illustrations. Throughout this disclosure, the reader should bear in mind that other methods of locking the strands within the anchor could be substituted.
[0062] Those skilled in the art will also realize that the inventive features disclosed are not dependent upon the use of a particular expanding cavity 28 . A linear expansion profile (conical) is shown. A curved expansion could just as easily be used. By the same token, the potted region can be locked to the anchor by using a straight cavity having threads, serrations, or other mechanically interlocking features.
[0063] In FIG. 9 , potted region 16 occupies the expanding cavity and a portion of the straight portion. Potting transition 20 lies well inside the anchor, near the commencement of expanding cavity 28 (though it can lie higher up—well into the expanding cavity—or lower down in the straight portion). The present invention incorporates a smooth expansion proximate the potting transition on the side of the freely flexing portion of the cable (distal to the potted region). This smooth expansion can assume many forms.
[0064] The version shown in FIG. 9 includes a simple arcuate expansion, denoted as circular expansion 34 . If the flexible region 30 of the cable is flexed laterally as shown, circular expansion 34 provides a smooth “bending shoulder” around which the cable can bend. Since the circular expansion is radially symmetric, it allows the cable to flex laterally in any direction. The reader will also note that potting transition 20 , while still irregular, has been moved significantly away from the point where the cable bends.
[0065] The inclusion of the circular expansion reduces or prevents the kinking of the cable's strands, as well as reducing axial compression and radial compression. Stress concentrations are thereby minimized, meaning that the load is spread more uniformly throughout the cable's cross section. The circular expansion shown in FIG. 9 is a simple arc having a fixed radius. This radius of the circular expansion should be at least equal to the radius of the cable, though for stiffer cables (or cables having poor resistance to flexural fatigue) it may need to be up to 45 times the radius of the cable.
[0066] The use of the structure shown in FIG. 9 ensures a uniform bending radius for the cable. If, as an example, the cable is bent 5 degrees off the anchor's centerline, the bending radius will be equal to the radius of circular expansion 34 . If, on the other hand, the cable is bent 45 degrees (as actually shown in FIG. 9 ) the bending radius will still be equal to the radius of circular expansion 34 . The length of contact between the cable and circular expansion 34 obviously varies, with the length being far less for the 5 degree bend than the 45 degree bend. The bending radius remains the same, though. This fact allows the cable designer to know what bending radius the completed assembly must endure (within a reasonable range). Since this knowledge allows the prediction of ultimate strength, flexural resistance, etc., it allows the design of a much more predictable cable termination.
[0067] Other types of smooth expansions work as well. FIG. 10 shows an anchor 18 having a parabolic expansion 36 . As for FIG. 9 , the potting transition can be placed within the straight portion or up within the lower portion of expanding cavity 28 . FIG. 11 shows an anchor having another parabolic expansion 36 , wherein the defining parabola has different coefficients. Those skilled in the art will know that many different parabolas could be applied.
[0068] The term “smooth expansion” is not intended to be limited to tangential curves. FIG. 12 shows an anchor 18 having linear expansion 40 . Again, the potting transition can be placed within the straight portion or up within the lower portion of expanding cavity 28 . The linear expansion allows the cable to flex laterally proximate the potting transition. While not so effective as the tangential curves, the linear expansion may be easier to manufacture, and may be suitable where only limited lateral flexing is needed.
[0069] Linear expansion 40 can be improved by filleting its intersection with the straight portion. Such an embodiment is shown in FIG. 13 , where a fillet 24 has been added to this intersection (where the fillet may be a simple arc, a parabolic arc, or a higher-order curve). This fillet again provides a bending shoulder for the laterally flexing cable.
[0070] Those skilled in the art will know that the addition of fillets can be helpful at many points within the anchor. FIG. 14 shows the addition of a fillet 24 at the bottom of linear expansion 40 . Of course, fillets can be added in both locations (the location shown in FIG. 13 and the location shown in FIG. 14 ). Ideally, these fillets should conform to the size constraints stated previously (i.e., having a radius at least as large as the radius of the cable).
[0071] The preceding examples have shown the smooth expansion only extending out to the lower surface of the anchor (with “lower” again being understood in the context of the orientation shown in the views). The smooth expansion can be carried further. It can, in fact, be carried around the bottom of the anchor and up the outside surface. FIG. 15 shows an anchor having a circular expansion 34 extending around to the outside surface. Such an expansion extends the “bending shoulder” so that a cable can be bent all the way around the anchor (up to 180 degrees). If the shoulder is carried over the top of the anchor, the bending angle could even exceed 180 degrees. Applications for such a termination are uncommon, but they do exist. As one example, a cable termination attached to the end of a cylinder rod may extend to the point where it bends the cable back over the anchor as shown.
[0072] The anchor geometry can be optimized for a given amount of anticipated lateral cable flexing. FIG. 20 shows an anchor 18 having a lower expanding portion designated as smooth expansion 50 (which can be a simple arc, a parabola, or higher-order curve). The angular measurement is denoted as angular range 52 , which defines the maximum (positive and negative) flexure which can be accommodated before the cable is pressed against a sharp corner. For the embodiment shown in FIG. 20 , angular range 52 measures 119.6 degrees. Extreme examples are possible. FIG. 24 shows a version having an angular range 52 of only 7.2 degrees, while FIG. 25 shows a version having an angular range of 180 degrees (90 degrees per side).
[0073] FIG. 21 shows an embodiment having an angular range 52 measuring only 59.8 degrees. It uses similar geometry, but altered dimensional values. The reader will therefore understand that a given anchor geometry can be optimized for a particular application by using a specific angular range.
[0074] More complex geometry can also be used. FIG. 22 shows an anchor 18 which includes a relieved portion 56 immediately below a first circular expansion 34 and above a second circular expansion 34 . This embodiment allows a completely free movement of the cable until it bends far enough to contact the circular expansion
[0075] For some applications, it may be desirable to have the anchor wall contact the cable at multiple points. FIG. 23 shows such an embodiment, which includes step reliefs 58 . These provide point contacts as the cable bends over against shoulder 54 . The size and shape of the step reliefs can be varied to produce many different effects.
[0076] The previous embodiments used a straight portion immediately above the expanding portion where the cable exits the anchor. This straight portion need not be entirely straight. FIG. 26 shows an anchor having a “straight” portion 38 which is not purely cylindrical. Parabolic expansion 36 actually extends all the way up to expanding cavity 28 . The portion right next to expanding cavity 28 is almost flat (It asymptotically approaches the vertical). It then smoothly blends into a rapidly expanding portion near the bottom of the anchor. The nearly-vertical portion of the parabolic side wall serves the purpose of the straight portion found in the other versions.
[0077] FIG. 27 shows a cable 10 which is encased by an jacket 60 . Smooth expansion 50 allows the jacket to bend without abrading or kinking. Such a jacket binds the cable strands together to preserve the circular cross-sectional shape when the cable is flexed. This binding helps to eliminate the problem of uneven load sharing between strands and the creation of stress concentrations (The reader will recall illustrations of this scenario in FIGS. 2 and 3 ).
[0078] Of course, the jacket does not provide a smooth transition acting alone. It is the combination of the jacket—which substantially maintains the circular cross section—and the smooth expansion 50 , around which the jacketed cable bends. Thus, these elements must be sized to interact appropriately. The radius of the smooth expansion is ideally greater than the radius of the cable. The jacket material is preferably pliable enough to bend around the expansion without kinking.
[0079] The term “jacket” can include a tape wrap, a shrink wrap tubing, an extruded plastic, a stranded braid (“over-braid”), an over-molded polymer, a string wrap, or other known binding techniques. The jacket can be applied over the length of the entire cable, over a short length in the proximity of the termination, or any length in between.
[0080] Although the illustrations show radially symmetric terminations, the reader should note that not all embodiments of the present invention need to be radially symmetric. In some applications, it will be apparent that the cable will flex only in one plane. It may even be desirable to inhibit flexing out of this plane. FIG. 28 shows an anchor having an expansion which is not radially symmetric. Slotted expansion 62 allows the cable to flex freely in only one plane.
[0081] The preceding examples disclose a termination placed on an end of a cable. The principles disclosed apply equally to terminations placed somewhere between the two ends of a cable. FIG. 29 shows intermediate termination 64 . The central portion of the cable is potted into the termination. It has two circular expansions 34 , one on each end. The two circular expansions allow both the exiting cable segments to flex laterally with respect to intermediate termination 64 .
[0082] Finally, those skilled in the art will realize that the expanding portion of the passage through the anchor could be made as a separate piece in order to accommodate manufacturing concerns. FIG. 31 shows such an embodiment, with expansion bell 70 being made as a separate piece from anchor 18 . The expansion bell can include a circular expansion, a parabolic expansion, or any other shape disclosed in the preceding.
[0083] Thus, the reader should rightly view all the preceding embodiments as providing examples of the invention claimed. The scope of the invention should therefore be fixed by the following claims, and not by the examples provided.
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Cable terminations having features which reduce stress in the transition between the potted region and the freely flexing region of a cable when the cable flexes laterally with respect to the anchor. Several favorable geometries are disclosed. The use of a supplemental buffer material to reduce stress is also disclosed.
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FIELD OF THE INVENTION
This invention relates generally to paper-making machines and more particularly to the nozzle means, of a paper-making apparatus, through which flows a stream of pulp stock.
BACKGROUND OF THE INVENTION
Heretofore it has been known to provide nozzle means, for the breast box of a paper-making machine, wherein the nozzle means comprises an opening or gap, through which pulp stock is flowed, and wherein such opening or gap is comprised of a lower disposed lip or lip surface and an upper disposed lip or lip surface. Further, in such prior art structures a shutter means or member, operatively carried as at a downstream position of such upper lip, can be moved, generally, upwardly and downwardly as to thereby selectively determine the effective height of such opening or gap. Such reciprocal movement of the shutter is usually effected as by a plurality of threaded spindles which operatively engage the shutter and which are operated as by, for example, handwheels or the like.
The thusly selected width of the gap or opening of the breast box nozzle therefore determines the thickness of the stream of pulp stock emerging from the nozzle.
In such arrangements the shutter projects downwardly some amount into the stream of pulp stock and consequently experiences a considerable pressure thereagainst, at the upstream side of the shutter, applied by such flowing stream of pulp stock. Such pressure causes some degree of deflection in the shutter which, in turn, results in uncontrolled variations in the effective width of the nozzle gap causing defects in the resulting paper web.
The prior art has been aware of the problem of such undesired shutter deflection, and the defects in the resulting paper web, and has attempted to solve such problem as by, for example: significantly increasing the thickness of the shutter, which is usually constructed as in the form of a steel straight-edge member; dividing the shutter member into separate sections which are, generally, functionally aligned as to span the entire longitudinal length of the nozzle gap or opening; and providing for a more sensitive adjustment of the threaded adjustment spindles as to thereby, hopefully, offset the effects of the upstream created pressure on the shutter means and eliminate the resulting surface-weight fluctuations occurring in the subsequent paper web, paper, strips and the like. None of such prior art attempts has proven to be successful and such defects and surface-weight fluctuations of the paper web and paper product continued.
In the embodiments of breast box nozzles heretofore employed, a support is provided as to lie directly against, what may be termed, the downstream side of the straight-edge type of shutter. Such support was intended to hold the shutter in such a way as to prevent deformation of the shutter due to the upstream pressure created by the flow of pulp stock. However, despite efforts, the prior art has been unable to manufacture a shutter so dimensionally accurate as to assure that the said support would always rest flush, throughout its length, against the shutter member. The manufacturing tolerances, in order to attain the required flatness, surface parallelism, etc., are extremely critical (and for all practical purposes unattainable) since the slightest undesired curvature or warping of the shutter edge exerts a damaging influence on the quality of the stream of pulp stock and the resulting paper web. Consequently, because of the unattainable dimensional accuracy, the said support, instead of lying flush (along its entire functional length) against the shutter actually engages the shutter only at what amounts to spaced points. Such, of course, only further encourages the undesired bowing or deflection of the shutter. Even with manufacture to close tolerances, due to the considerable temperature fluctuations arising in the area of the shutter, internal and applied material stresses are released which, again, result in the non-flush contact as between the shutter and said support.
The invention as herein disclosed and claimed is primarily directed to the solution of the aforestated and other related and attendant problems.
SUMMARY OF THE INVENTION
According to the invention, a breat box nozzle comprises a nozzle opening extending generally laterally, the nozzle opening being at least in part comprised of an upper disposed lip portion, a shutter operatively carried as to extend across the lateral extent of said opening, said shutter being adjustably positionable relative to said upper lip portion as to thereby selectively adjust the effective height of said opening and thereby select the thickness of the stream of pulp stock flowing through said opening, and support means effective to apply a force against said shutter along the downstream side of said shutter counter to the force created by the pressure of the flow of the paper stock acting against the upstream side of said shutter, said support means comprising force reaction means and elastomeric means, said elastomeric means being generally interposed between said force reaction means and said shutter whereby said elastomeric means is effective to apply to said shutter at least a portion of the force along the downstream side of said shutter.
An object of the invention is to provide a breast box nozzle of the general type described in which irregularities in the stream of pulp stock and defects in the paper web resulting therefrom, particularly surface-weight fluctuations across the paper web, are substantially if not totally eliminated.
Other general and specific objects, advantages and aspects of the invention will become apparent when reference is made to the following detailed description considered in conjunction with the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWING
The single drawing, wherein for purposes of clarity certain details and/or elements may be omitted, illustrates in general vertical cross-section, a breast box nozzle employing a shutter in accordance with the teachings of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now in greater detail to the drawing, as is generally well known, a source of pulp stock supplies a generally fluid stream of such pulp stock to the nozzle means of the drawing wherein the said nozzle is illustrated as comprising upper disposed lip means 2 and lower disposed lip means 1 which cooperate to define a passageway 10 therebetween (in conjunction with opposite end wall means not shown but well known) for the flow therethrough of said stream of pulp stock. In the embodiment shown, the passageway between lip means 1 and 2 converges as it approaches what could be considered to be the downstream end 12 of upper lip or passage wall 2.
A shutter 3 is placed as against a surface 14, formed as on upper lip structure 2, and is operatively connected to a beam 3a and to related adjustment means which may take the form of threaded spindles one of which is typically illustrated at 5. The purpose of such adjustment means, as is well known in the art, is to enable the selective adjustable positioning of the shutter 3 in directions depicted generally by both arrows 16 and 18. In so doing, of course, shutter 3 will move relative to surface 14 and, depending upon the direction of travel, will bring the horizontally extending edge 20 of shutter 3 closer to or further away from the surface of lower lip structure 1 thereby selectively establishing the height, or width, of the discharge opening of nozzle passageway 10 which would otherwise be determined by the distance between end 12 of upper lip structure 2 and lower lip structure 1.
The shutter 3 is, in turn, held in its selectively adjusted position against surface means 14 as by support means 22 which, in the preferred embodiment, is depicted as comprising a support member 4, suitably secured as to the upper lip structure 2, and elastomeric means 6 situated generally between the support member 4 and the shutter 3. In the preferred embodiment, the elastomeric means 6 would extend, generally horizontally, across the functional length of the shutter 3 as to be effective for applying a force, or pressure, thereto counter to that created by the stream of pulp stock flowing in nozzle passageway 10.
Further, in the preferred embodiment of the invention, the elastomeric means 6 comprises an elastomeric hose-like or tubular member which, in turn, is filled with a fluid. Still further, in the preferred embodiment of the invention, the elastomeric hose-like or tubular member 6 is in fluid communication with associated supply conduit means 7, which may comprise pressure regulating valve means 24, leading to a suitable source of fluid pressure 26.
As depicted in the drawing, the elastomeric member 6 may be carried as within a groove-like recess 28 which may be formed in an end surface or portion of support member 4 with such recess being of a relative dimension as to enable the extension of the side of the elastomeric means 6 beyond the end surface 30 of support member 4.
Shutter 3 and beam 3a extend, preferably horizontally, across the length of the discharge opening of nozzle passageway 10. Shutter 3 is connected to beam 3a by screws (not shown) and by pins, one of which is illustrated at 13. Support member 4 is connected to upper lip structure 2 by support screws one of which is illustrated at 32. It should be noted that spaces or gaps 8 and 9 exist between the end face 30 of support member 4 and shutter 3 besides the elastomeric means 6 and that a further space 11 exists between support member 4 and beam 3a. Thus, the invention assures that all counter force is transmitted through elastomeric means 6 and that inspite of said transmission of force the shutter may be adjusted during operation of the breast box nozzle.
OPERATION OF THE INVENTION
Support member 4 may cause an elastomeric deflection of elastomeric means 6 against shutter 3 thereby applying thereto a counter pressure and force generally oppositely directed to that pressure or force existing against the shutter 3 and created by the stream of pulp stock.
That is, as should now be apparent, as the flow of pulp stock is forced through nozzle passageway 10 (from right to left as viewed in the drawing) the stream of pulp stock flows against the depending portion of the upstream side of the shutter means 3 and in so doing applies a pressure thereagainst the resulting force of which tends to bow or move the shutter means in a direction generally away from surface 14 and thereby result in the product defects hereinbefore described.
The invention, by providing what amounts to as an intermediate elastomeric means 6 for the application of a counter pressure (and resulting counter force) uniformly across the functional length of the shutter prevents the occurrence of such undesired movement by the shutter means throughout its entire functional length. The elastomeric means 6, of course, functions to transmit the entire force exerted by the support member 4 to the shutter means 3 with such transmission of force occurring in a manner as to apply it to the shutter means 3 uniformly along its functional length without adverse influence because of such factors as uneven surface conditions on the shutter means against which the elastomeric means 6 is acting.
As previously indicated, in the preferred embodiment, the elastomeric means 6 is of a hose-like or tubular configuration and, further, is in fluid communication with a source of fluid pressure. Accordingly, as generally depicted in the drawing, with the support member 4 positioned as illustrated, fluid under superatmospheric pressure can be directed to the interior of the elastomeric tubular means 6 and in so doing even increasing the pressure and resulting counter force against the shutter means 3.
Also, further various embodiments and modifications of the invention are contemplated. For example, in the drawing only a single elastomeric means 6 is illustrated. It should be made clear that a plurality of such elastomeric means 6 may be employed. For example, there may be a plurality of relatively shorter segments of such elastomeric means generally functionally aligned over the span of the shutter means 3 and situated in selected areas thereof as to thereby be able to variably influence certain selected points or areas of the shutter means independently of the influence exercised on other points or areas of the shutter means. In such an arrangement where fluid pressure were to be employed for pressurizing the plurality of elastomeric segments, it would be possible, of course, to have the pressure in each elastomeric segment controlled as by a respective separate pressure regulating means or valve as generally depicted at 24.
Further, it would, of course, be possible to provide two or more elastomeric means 6 or portions thereof at respectively different elevations. That is, referring to the drawing, it would be possible to, for example, provide a second portion of such elastomeric means 6 or even a second elastomeric means 6 at an elevation generally above that at which the single elastomeric means 6 is depicted in the drawing. Such elevated additional elastomeric means could, of course, be in accordance with any of the embodiments, or modifications thereof, hereinbefore described with reference to the preferred embodiment of the invention.
Although the elastomeric means 6, in the preferred embodiment, is comprised of rubber, any suitable elastomeric material may, of course, be employed.
It should be pointed out that the prior art, as disclosed by the Federal Republic of Germany Letters Patent No. 1,461,176 teaches a breast box construction in which the front wall thereof is braced against a support with the interposition of a pneumatic cushion. However, the breast box of said German Letters Patent is of a construction and type other than that as concerns this invention. That is the breast box of said German Letters Patent is the type wherein the interior of the entire breast box is subjected to a high magnitude superatmospheric pressure and wherein the entire structurally heavy front wall thereof has to be held straight. In contrast, in the case of the invention, the problem involved is the maintaining of an extremely sensitive setting of an important individual element with such being the shutter.
Although only a preferred embodiment and certain other embodiments and modifications of the invention have been disclosed and described, it is apparent that other embodiments and modifications of the invention are possible within the scope of the appended claims.
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A breast box nozzle for a paper making machine or the like is shown as having an adjustably positionable shutter member which can be moved generally further and lesser into the path of flow of a stream of pulp stock as to thereby determine the thickness of the discharged stream of pulp stock. A support arrangement applies a pressure to the shutter member as against a downstream side thereof in order to counter the forces generated by the stream of pulp stock upstream of the shutter member and applied as against the upstream side thereof tending to undesirably deform the shutter member. The support arrangement includes an elastomeric member generally interposed between a relatively fixed support member and a downstream side of the shutter member.
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FIELD OF THE INVENTION
[0001] The present invention relates to the field of mineral and metallurgical processes, to disintegrating in general and to disintegrating by tumbling mills, and more particularly to a method and arrangement for determining a degree of fullness of a large grinding mill drum, and to a large grinding mill drum.
BACKGROUND OF THE INVENTION
[0002] One of the most common processes in mining and metallurgy is the comminution processing or disintegrating of ore. When processing material for the selective or collective recovery of valuable material components, the processes concerned are preceded by comminution processing i.e. mechanical crushing or disintegration of the material in a manner to free the valuable components, one from the other. Comminution is particle size reduction of materials. Comminution is achieved by blasting, crushing and grinding. After comminution the components are then mutually isolated with the aid of known separation methods, this isolation being contingent on differences in color, shape, density or in differences in their respective surface active and magnetic properties, or other properties.
[0003] In comminution processing first ore or rock is excavated, broken down or removed by blasting. Blasting is the controlled use of explosives and other methods in mining, quarrying and civil engineering. Typically blasting produces particles in the size having a diameter of 500 mm or more.
[0004] Crushing is particle size reduction of ore or rock materials by using crushing devices i.e. crushers. Crushers e.g. jaw crushers, gyratory crushers or cone crushers are used to reduce the size, or change the form, of materials so that pieces of different composition can be differentiated. In the crushing process the crushing devices hold material being crushed between two parallel or tangent solid surfaces of a stronger material and apply sufficient force to bring said surfaces together. Typically in a crushing process particles having a diameter up to 1000 mm are crushed to particles having a diameter of 5 mm or more.
[0005] Grinding is particle size reduction of ore or rock materials in grinding mills. In hard rock mining and industrial mineral operations the demands for rotating mineral and metallurgical processing equipment such as grinding mills are very high both in terms of grinding efficiency and energy consumption. Typically in a grinding process particles having a diameter up to 1000 mm are grinded to particles having a diameter of 0.010 mm or more. This conventional grinding of materials results in considerable wear on the grinding bodies present in the mill, due to the hardness of the rock concerned, therewith also resulting in considerable costs for the provision of such grinding bodies.
[0006] The rotating mineral and metallurgical processing equipment such as grinding mills are typically very large, having a diameter of several meters. The grinding mills may be trunnion-supported or shell-supported. Trunnion support is the most common way of supporting a mill in a mineral processing application, especially in very large grinding mills. In a bearing arrangement of a trunnion-supported grinding mill the support bearings have a relatively small bearing diameter and the trunnion journals have a high consistent stiff journal surfaces, this facilitating the formation of a good bearing lubricant film distribution. The shell-supported grinding mills are more compact, occupy less floor space and require simpler foundations than comparable trunnion-supported grinding mills. Because the end plates of the shell-supported grinding mill do not support the structure, the feed and discharge openings may be sized to meet process conditions without being constrained by trunnion bearing limitations.
[0007] A ball mill is a typical type of fine grinder. However, the rotating mineral and metallurgical grinding mills are today very often autogenous grinding mills or semi-autogenous grinding mills designed for grinding or primary crushed ore. Autogenous grinding mills are so-called due to the self-grinding of the ore. In an autogenous grinding mill a rotating drum throws larger rocks of ore in a cascading motion which causes impact breakage of larger rocks and compressive grinding of finer particles. In autogenous grinding the actual material itself, i.e. the material to be ground, forms the grinding bodies.
[0008] Semi-autogenous grinding mills are similar to autogenous mills, but utilize grinding balls e.g. steel grinding balls to aid in grinding like in a ball mill. Attrition between grinding balls and ore particles causes grinding of finer particles. Semi-autogenous grinding mills typically use a grinding ball charge of 8 to 21%, sometimes a grinding ball charge of 5 to 60%. A semi-autogenous grinding mill is generally used as a primary or first stage grinding solution. Semi-autogenous grinding mills are primarily used at gold, copper and platinum mines with applications also in the lead, zinc, silver, alumina and nickel industries.
[0009] Autogenous and semi-autogenous grinding mills are characterized by their large diameter and short length as compared to ball mills. The rotating mineral and metallurgical processing equipment such as autogenous and semi-autogenous grinding mills are typically driven by ring gears, with a 360° fully enclosing guard.
[0010] The inside of an autogenous or semi-autogenous grinding mill is lined with mill linings. The mill lining materials typically include cast steel, cast iron, solid rubber, rubber-steel composites or ceramics. The mill linings include lifters, e.g. lifter bars to lift the material inside the mill, where it then falls off the lifters onto the rest of the ore charge.
[0011] Rotating mineral and metallurgical processing equipment that is provided with internal lifters is typically difficult to control. For example, in autogenous grinding mills or semi-autogenous grinding mills the feed to the mill also acts as a grinding media, and changes in the feed have a strong effect on the grinding efficiency. The change in the feed properties is a normal phenomenon that needs to be considered in in controlling the rotating mineral and metallurgical processing equipment.
[0012] In autogenous or semi-autogenous grinding mills, the existing mineral deposits seldom have a homogenous structure and a homogenous mechanical strength. Material properties such as hardness, particle size, density and ore type also change constantly and consequently a varying energy input is required.
[0013] Conventionally grinding has been controlled on the basis of the mill power draw, but particularly in autogenous and semi-autogenous grinding, the power draw is extremely sensitive to changes in feed parameters. It has been discovered that the degree of fullness in the mill as percentages of the mill volume is a quantity that is remarkably more stable and much more descriptive as regards the state of the mill. But because the degree of fullness is difficult to infer in an on-line-measurement, the measurement of the load mass is often considered sufficient. However, the mass measurement has its own problems both in installation and in measurement drift. Moreover, there may be intensive variations in the load density, in which case changes in the mass do not necessarily result from changes in the degree of fullness.
[0014] As a summary, the degree of fullness is an important parameter that describes the state of the grinding mill. The main challenge with the degree of the fullness is that the parameter is difficult to measure online. One prior art method for determining the degree of fullness of a large grinding mill drum has been to measure the weight of a large grinding mill drum and use the measured weight to calculate the degree of fullness of a large grinding mill drum. In this prior art method the weight of the grinding charge has been used as the deciding parameter for controlling the mill. This method is cost demanding, however, because of the weighing equipment needed to register continuously the changes in the weight of the grinding charge that occur during operation of the mill, which enables the steps necessary in order to improve prevailing operating conditions to be carried out as quickly as possible. Also the water content of the mill changes constantly, the density, hardness and particle size of the grinding charge changes constantly. Furthermore the mill linings typically constitute up to 30-50% of total weight of the mill. As these linings wear off in time this has a considerable effect on the weight of the mill. Therefore the weight of the grinding mill drum is not a good indication the degree of fullness in the grinding mill drum. All in all it has been discovered that the weight of the grinding charge does not correlate good enough with the degree of fullness in the grinding mill drum as percentages of mill volume.
[0015] Another prior art method for determining the degree of fullness of a large grinding mill drum has been to measure and analyze the power consumption or the power intake signal of a large grinding mill and use the measured power consumption to calculate the degree of fullness of a large grinding mill drum. However, particularly in autogenous and semi-autogenous grinding mills, the power consumption is extremely sensitive to changing parameters. The energy or power requirement of a large grinding mill depends on several factors, such as the density of the grinding charge, a mill constant, the extent of mill charge replenishment, or the instant volume of charge in the grinding mill, relative mill speed, length and diameter of the grinding mill. Furthermore, it has been discovered that the grinding mill power consumption or the power intake signal does not correlate enough with the degree of fullness in the grinding mill drum as percentages of mill volume.
[0016] The above presented two prior art methods are off-shell-device type methods for determining the degree of fullness of a large grinding mill drum. That is, the measuring devices are installed on the side of the grinding mill on the surrounding structure. A third off-shell-device type prior art method for determining the degree of fullness of a large grinding mill drum has been to measure acoustic wave properties of a large grinding mill and use the measured acoustic wave properties, i.e. sound pressure and/or sound intensity to estimate the degree of fullness of a large grinding mill drum. In the third prior art method the off-shell-device type acoustic wave property measurement sensors may be a single microphone or a series of microphones or microphone mats that are measuring acoustic wave properties coming from the large grinding mill. Also here, it has been discovered that the off-shell-device measured grinding mill acoustic wave properties provide only a rough estimate on the degree of fullness.
[0017] In the following, the prior art will be described with reference to the accompanying FIG. 1 , which shows a cross-sectional view of a large grinding mill drum according to the prior art.
[0018] FIG. 1 shows a cross-sectional view of a large grinding mill drum according to the prior art. In FIG. 1 the grinding mill has a drum casing 1 , which drum casing 1 is provided with linings. The linings of the drum casing 1 comprise lifting bars 2 , which lifting bars 2 lift the grinding charge material inside the mill, where it then falls off the lifting bars 2 onto the rest of the grinding charge. The angle in which the grinding charge material inside the mill first hits a lifting bar 2 is called “toe angle” φ k . Respectively the angle in which the grinding charge material inside the mill first falls off a lifting bar 2 is called “shoulder angle” φ s .
[0019] Over the recent years there has also been a lot of development around on-mill-shell type of devices. In U.S. Pat. No. 6,874,364 a system for monitoring mechanical waves from a moving machine has been presented in which system a sensor arrangement is located on an exterior surface of the grinding mill drum. The presented sensor arrangement has an acoustic wave sensor for measuring acoustic wave properties and an accelerometer for measuring mechanical waves, i.e. vibrational events and low frequency events, event spatial localization, and events occurring on the ends of the mill. The presented mechanical wave monitoring method may also include a step of monitoring volumetric load in the machine based on the measured mechanical waves. However, even the presented on-mill-shell type device measured grinding mill acoustic wave properties do not correlate adequately enough with the degree of fullness in the grinding mill drum as percentages of mill volume.
[0020] In U.S. Pat. No. 5,360,174 an arrangement for registering the instant grinding charge volume of a grinding drum has been presented in which arrangement there is integrated a tension sensor on a flexible bar inside a rubber or steel-cap lifter bar of the grinding mill drum. In the U.S. Pat. No. 5,360,174 patent specification there is in FIG. 1 presented a point A where a lifting device will engage the grinding charge, said point A also commonly referred to a toe position or toe angle. Similarly in FIG. 1 of said patent specification there is presented a point B where a lifting device will leave its engagement with the grinding charge, said point B also commonly referred to a shoulder position or shoulder angle. The tension sensor arrangement presented in the U.S. Pat. No. 5,360,174 patent specification detects a tension on a lifter bar caused by the grinding charge load. However, the presented tension sensor arrangement requires customized lifter bars of the grinding mill drum.
[0021] In U.S. Pat. No. 7,699,249 there is presented a method for defining the degree of fullness in a mill is calculated on the basis of the measured toe angle, the rotation speed of the mill and the geometrical dimensions of the mill. However, the presented sensor arrangement does not consistently enough provide straightforward and adequate measurement sensitivity required for a precise monitoring of the degree of fullness in the grinding mill drum as percentages of mill volume.
[0022] In general, there are some problems with the prior art solutions for measuring the degree of fullness of a large grinding mill drum. So far, the measuring solutions are relatively complex and difficult in order to provide reliable information. Also the measurement accuracy and reliability with the prior art measuring solutions has not been adequate enough.
[0023] The problem therefore is to find a solution for measuring the degree of fullness of a large grinding mill drum which can provide reliable measurement data for the determination of the degree of fullness of a large grinding mill drum with better measurement accuracy and reliability.
[0024] There is a demand in the market for a method for determining a degree of fullness of a large grinding mill drum which method would be more reliable and have a better measurement sensitivity when compared to the prior art solutions. Likewise, there is a demand in the market for an arrangement for determining a degree of fullness of a large grinding mill drum which arrangement would be more reliable and have a better measurement sensitivity when compared to the prior art solutions; and also a demand for a large grinding mill drum having such characteristics.
BRIEF DESCRIPTION OF THE INVENTION
[0025] An object of the present invention is thus to provide a method and an apparatus for implementing the method so as to overcome the above problems and to alleviate the above disadvantages.
[0026] The objects of the invention are achieved by a method for determining a degree of fullness of a large grinding mill drum which method comprises the steps of:
measuring force measurement data from reactions caused by the grinding material, said reactions subjected to an at least one lifting bar and to an at least one lifting bar bolt of the grinding mill, using at least one force transducer attached to said at least one lifting bar bolt; and calculating the degree of fullness of the grinding mill from said force measurement data.
[0029] Preferably, in the step of measuring also position/angle measurement data on the position and/or the angle or rotation of the at least one lifting bar bolt of the grinding mill, using at least one accelerometer) and/or inclinometer attached to or arranged next to said at least one lifting bar bolt; and that in the step of calculating also said position/angle measurement data is utilized.
[0030] Alternatively, in the step of calculating a toe angle φ k and/or a shoulder angle φ s of the grinding mill drum is first calculated.
[0031] Furthermore, the objects of the invention are achieved by an arrangement for determining a degree of fullness of a large grinding mill drum, having a sensor arrangement attached to at least one lifting bar bolt of an at least one lifting bar of the grinding mill, said sensor arrangement having an at least one force transducer attached to said at least one lifting bar bolt.
[0032] Preferably, said sensor arrangement has an at least one accelerometer and/or inclinometer attached to said at least one lifting bar bolt. Alternatively, said sensor arrangement has an at least one accelerometer and/or inclinometer arranged next to said at least one lifting bar bolt.
[0033] Further preferably, said arrangement further comprises:
a data processing and transmitting unit arranged on the grinding mill drum casing surface, said data processing and transmitting unit connected to said sensor arrangement; a data receiving unit arranged outside the mill drum on any fixed surrounding structure outside the mill drum; and a data processing device.
[0037] Preferably, said data processing and transmitting unit comprises a signal acquisition module for receiving the measurement signals from the sensor arrangement and a transmitter for transmitting the measurement data wirelessly to said data receiving unit. Preferably, said data processing and transmitting unit comprises a relay for switching the data processing and transmitting unit on wirelessly. Preferably, said data processing and transmitting unit further comprises a power supply and/or a regulator and/or an amplifier.
[0038] Preferably, said sensor arrangement is attached to one lifting bar bolt on the grinding mill drum casing surface. Alternatively, said several sensor arrangements are attached to the several lifting bar bolts in one row on the grinding mill drum casing surface. Alternatively, said several sensor arrangements are attached to the several lifting bar bolts in several rows on the grinding mill drum casing surface.
[0039] Furthermore, the objects of the invention are achieved by a large grinding mill drum, which comprises an arrangement for determining a degree of fullness of a large grinding mill drum, having a sensor arrangement attached to at least one lifting bar bolt of an at least one lifting bar of the grinding mill, said sensor arrangement having an at least one force transducer attached to said at least one lifting bar bolt.
BRIEF DESCRIPTION OF THE DRAWINGS
[0040] FIG. 1 shows a cross-sectional view of a large grinding mill drum according to the prior art;
[0041] FIG. 2 shows a partial cross-sectional view of a one embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention;
[0042] FIG. 3 shows a partial cross-sectional view of a another embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention;
[0043] FIG. 4 shows a perspective view of a third embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention;
[0044] FIG. 5 shows a schematic diagram of one embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention;
[0045] FIG. 6 shows a perspective view of a fourth embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention;
[0046] FIG. 7 shows a perspective view of a fifth embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention.
[0047] The prior art drawing of FIG. 1 has been presented earlier. In the following, the invention will be described in greater detail by means of preferred embodiments with reference to the accompanying drawings of FIGS. 2 to 7 .
DETAILED DESCRIPTION OF THE INVENTION
[0048] The present invention relates to a method and an arrangement for registering the instant volume or the instant level of the charge in an ore-grinding drum of the kind that is provided with internal lifting means.
[0049] FIG. 2 shows a partial cross-sectional view of a one embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention. In FIG. 2 the grinding mill has a drum casing 3 , which drum casing 3 is provided with linings 4 . The linings 4 of the drum casing 3 comprise lifting bars 5 , 6 , which lifting bars 5 , 6 have been attached to the drum casing 3 of the grinding mill with lifting bar bolts 7 , 8 .
[0050] In the presented embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention said determining arrangement has at least one lifting bar bolt 7 , which has been provided with a force transducer 9 . In the presented embodiment of a determining arrangement said force transducer 9 has been attached to the said at least one lifting bar bolt 7 with the help of a shim 10 and a nut 11 . The force transducer 9 is used to measure reactions caused by the grinding material said reactions subjected to the lifting bar 5 and to the said at least one lifting bar bold 7 of the grinding mill. The determining arrangement according to the presented embodiment of the present invention may also have an accelerometer and/or an inclinometer arranged next to the said at least one lifting bar bolt 7 of the grinding mill.
[0051] FIG. 3 shows a partial cross-sectional view of another embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention. In FIG. 3 the grinding mill has a drum casing 3 , which drum casing 3 is provided with linings 4 . The linings 4 of the drum casing 3 comprise lifting bars 5 , 6 , which lifting bars 5 , 6 have been attached to the drum casing 3 of the grinding mill with lifting bar bolts 7 , 8 .
[0052] In the presented another embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention said determining arrangement has an at least one lifting bar bolt 7 , which has been provided with a force transducer 9 and an accelerometer 12 and/or an inclinometer. In the presented another embodiment of a determining arrangement said force transducer 9 has been attached to the said at least one lifting bar bolt 7 with the help of a shim 10 and a nut 11 . Furthermore in the presented another embodiment of a determining arrangement said accelerometer 12 and/or inclinometer has been attached to the said at least one lifting bar bolt 7 .
[0053] The force transducer 9 is used to measure reactions caused by the grinding material to the lifting bar 5 and to the said at least one lifting bar bolt 7 of the grinding mill. The accelerometer 12 and/or inclinometer is used to measure the position and the angle or rotation of the said at least one lifting bar bolt 7 of the grinding mill and of the force transducer 9 attached to the said at least one lifting bar bolt 7 . The accelerometer 12 and/or inclinometer is used to synchronize the output of the force transducer 9 to the mill rotation and to define the phase angle of the lifting bar with respect to the earth gravity.
[0054] FIG. 4 shows a perspective view of a third embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention. The third embodiment of a determining arrangement comprises a sensor arrangement 13 attached to one lifting bar bolt on the grinding mill drum casing surface 3 and a data processing and transmitting unit 14 arranged on the grinding mill drum casing surface 3 , said data processing and transmitting unit 14 connected to said sensor arrangement 13 . Said data processing and transmitting unit 14 may also be attached to the one or more lifting bar bolts on the grinding mill drum casing surface 3 . Furthermore the third embodiment of a determining arrangement comprises a data receiving unit 15 and a data processing device 16 , e.g. a personal computer (PC) 16 , said data receiving unit 15 and said data processing device 16 being arranged outside the mill drum on any fixed surrounding structure outside the mill drum. The data processing and transmitting unit 14 is responsible for handling raw measurement signals obtained from the sensor arrangement 13 , and transmitting those wirelessly to the data receiving unit 15 and further to the data processing device 16 . With apparatus having a sensor arrangement 13 consisting of one force transducer and one accelerometer it is possible to measure the degree of fullness in one mill cross section.
[0055] FIG. 5 shows a schematic diagram of one embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention. The one embodiment of a determining arrangement shown in FIG. 5 comprises a data processing and transmitting unit 17 arranged on the grinding mill drum surface and a sensor arrangement 18 attached to the said at least one lifting bar bolt on the grinding mill drum surface.
[0056] The data processing and transmitting unit 17 of the determining arrangement according to an embodiment of the present invention comprises a signal acquisition module 19 for receiving the measurement signals from the a sensor arrangement 18 ; a transmitter 20 for transmitting the measurement data wirelessly to a data receiving unit 15 arranged outside the mill drum on any fixed surrounding structure outside the mill drum; and a relay 21 for switching the data processing and transmitting unit 17 on wirelessly.
[0057] The data processing and transmitting unit 17 of the determining arrangement according to an embodiment of the present invention may also comprise a power supply 22 for providing electrical power to the determining arrangement; a regulator 23 for providing regulated voltage to the sensor arrangement 18 ; and an amplifier 24 for providing regulated power to a force transducer 25 of the sensor arrangement 18 and amplifying the signal from said force transducer 25 of the sensor arrangement 18 to a signal acquisition module.
[0058] The sensor arrangement 18 of the determining arrangement according to an embodiment of the present invention comprises a force transducer 25 for measuring reactions caused by the grinding material to a lifting bar bolt of the grinding mill; and an accelerometer 26 and an inclinometer 27 for measuring the position and the angle or rotation of a lifting bar bolt of the grinding mill and of the force transducer 25 attached to the said lifting bar bolt. The accelerometer 26 and an inclinometer 27 is used to synchronize the output of the force transducer 25 to the mill rotation and to define the phase angle of the lifting bar with respect to the earth gravity. The force transducer 25 may be any kind of force transducer 25 suitable for measuring reactions on a lifting bar bolt such as e.g. a strain gage type transducer. The accelerometer 26 may be any kind of accelerometer 26 suitable for measuring the position and the angle or rotation of a lifting bar bolt such as e.g. a capacitive accelerometer. The force transducer 25 may also be based on a force sensor, on a pressure sensor, on a strain gauge or on a piezoelectric sensor.
[0059] FIG. 6 shows a perspective view of a fourth embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention. The fourth embodiment of a determining arrangement comprises several sensor arrangements 28 attached to the several lifting bar bolts in one row on the grinding mill drum casing surface 3 and a data processing and transmitting unit 14 arranged on the grinding mill drum casing surface 3 , said data processing and transmitting unit 14 connected to said several sensor arrangements 28 . Said data processing and transmitting unit 14 may also be attached to the one or more lifting bar bolts on the grinding mill drum casing surface 3 . Furthermore the fourth embodiment of a determining arrangement comprises a data receiving unit 15 and a data processing device 16 , e.g. a personal computer (PC) 16 , said data receiving unit 15 and said data processing device 16 being arranged outside the mill drum on any fixed surrounding structure outside the mill drum. The data processing and transmitting unit 14 is responsible for handling raw measurement signals obtained from the sensor arrangements 28 , and transmitting those wirelessly to the data receiving unit 15 and further to the data processing device 16 . With apparatus having several sensor arrangements 28 consisting of several force transducers and several accelerometers it is possible to measure the degree of fullness in several mill cross sections. In addition an apparatus with several force transducers and several accelerometers becomes more reliable.
[0060] FIG. 7 shows a perspective view of a fifth embodiment of an arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention. The fifth embodiment of a determining arrangement comprises several sensor arrangements 29 , 30 attached to the several lifting bar bolts in several rows on the grinding mill drum casing surface 3 and a data processing and transmitting unit 14 arranged on the grinding mill drum casing surface 3 , said data processing and transmitting unit 14 connected to said several sensor arrangements 29 , 30 . Said data processing and transmitting unit 14 may also be attached to the one or more lifting bar bolts on the grinding mill drum casing surface 3 . Furthermore the fourth embodiment of a determining arrangement comprises a data receiving unit 15 and a data processing device 16 , e.g. a personal computer (PC) 16 , said data receiving unit 15 and said data processing device 16 being arranged outside the mill drum to on any fixed surrounding structure outside the mill drum. The data processing and transmitting unit 14 is responsible for handling raw measurement signals obtained from the sensor arrangements 29 , 30 , and transmitting those wirelessly to the data receiving unit 15 and further to the data processing device 16 . With apparatus having several sensor arrangements 29 , 30 consisting of several force transducers and several accelerometers it is possible to provide a three dimensional picture of the conditions and the state inside the grinding mill. In addition an apparatus with several force transducers and several accelerometers becomes more reliable.
[0061] In the method and arrangement for determining a degree of fullness of a large grinding mill drum according to the present invention there is measured force measurement data on reactions caused by the grinding material to an at least one lifting bar bolt of the grinding mill as well as measurement data on the position and the angle or rotation of the at least one lifting bar bolt of the grinding mill. With the help of this force measurement data the degree of fullness of a large grinding mill is then calculated. In this calculation there can be the toe angle φ k and/or the shoulder angle φ s first calculated.
[0062] In the method and arrangement according to the present invention the degree of fullness of a large grinding mill may be calculated e.g. as explained in the following. In the analysis of the measurement results the phase 6 of the force or power oscillation caused by the lifter bars is calculated by using a sample data P(n) that is equidistant in relation to the angle of rotation and is obtained e.g. on the basis of the mill power draw of one rotation cycle, according to the following formula:
[0000]
θ
=
arg
[
∑
n
=
0
N
-
1
P
(
n
)
exp
(
-
2
π
nN
n
N
)
]
[0063] where i=√{square root over (−1)}=imaginary unit
[0000]
arg
z
=
arctan
Im
z
Re
z
=
the
polar
angle
,
[0064] i.e. argument, of a complex number z,
[0065] N=number of samples in a sample data P(n),
[0066] N n =number of lifter bars in the mill,
[0067] n=number of sample, and
[0068] θ=the phase of the oscillation caused by the lifter bars.
[0069] The toe angle is calculated from the phase e of the power oscillation caused by the lifter bars as follows, according to the following formula:
[0000]
Φ
k
=
2
π
(
k
n
+
1
)
-
θ
N
n
+
Φ
n
[0070] where k n =number of lifter bars, remaining in between the lifter bar located nearest to the axis x and the lifter bar located nearest to the toe position,
[0071] φ k =toe angle, and
[0072] φ n =angle from the axis x to the lifter bar located nearest to the axis x, so that it has a positive value in the rotation direction of the mill.
[0073] The degree of fullness is calculated from the toe angle and the rotation speed of the mill by means of various mathematical models, such as the model defined in the Julius Kruttschitt Mineral Research Center (JKMRC). Said model is described in more detail for example in the book Napier-Munn, T., Morrell, S., Morrison, R., Kojovic, T.: Mineral Comminution Circuits, Their Operation and Optimisation (Julius Kruttschnitt Mineral Research Centre, University of Queensland, Indooroopilly, Australia, 1999). The calculation formula of the JKMRC model for the degree of fullness in a mill is given in the following formula:
[0000]
{
n
c
,
i
+
1
=
0
,
35
(
3
,
364
-
V
i
)
V
i
+
1
=
1
,
2796
-
Φ
toe
-
π
2
2
,
5307
(
1
-
-
19
,
42
(
n
c
,
i
+
1
-
n
p
)
)
,
[0074] where the degree of fullness is defined by iterating the degree of fullness of the mill in relation to the interior volume of the mill. In the above formula, n c is an experimentally calculated portion of the critical speed of the mill, in which case centrifugation is complete, n p is the rotation speed of the mill in relation to the critical speed, V i is the previous degree of fullness of the mill, and V i+1 is the degree of fullness to be defined, in relation to the interior volume of the mill.
[0075] The solution for determining a degree of fullness of a large grinding mill drum according to the present invention provides a direct measurement of the reactions caused by the grinding material. The degree of fullness of the grinding mill drum can therefore be determined irrespective of possible stops and interruptions. With the help of the arrangement according to the present invention consisting of several force transducers and several accelerometers it is possible to provide a three dimensional image of the conditions inside the grinding mill.
[0076] As the measurement according to the present invention is a direct measurement of the phenomena and related measurement of the reactions caused by the grinding material, there is no need for calibration. As the position and the angle of the sensors are continuously known online there is no need for external trigger to determine the rotation. This is of particular importance in the analysis and calculation, as this simplifies calculations substantially and makes the result more reliable. As the measurement solution with sensor arrangements is quite simple and straightforward also installation and maintenance is easy.
[0077] With the help of the solution according to the present invention the manufacturers of large grinding mill drums will be able to provide grinding mill with a measurement arrangement producing more reliable measurement data for the determination of the degree of fullness of a large grinding mill drum with said measurement arrangement having better measurement sensitivity. The solution according to the present invention may be utilised in any kind of large grinding mill having lifter bars inside the grinding mill drum.
[0078] It will be obvious to a person skilled in the art that, as the technology advances, the inventive concept can be implemented in various ways. The invention and its embodiments are not limited to the examples described above but may vary within the scope of the claims.
|
The present invention relates to the field of mineral and metallurgical processes, to disintegrating in general and to disintegrating by tumbling mills, and more particularly to a method and arrangement for determining a degree of fullness of a large grinding mill drum, and to a large grinding mill drum. An arrangement for determining a degree of fullness of a grinding mill drum has a sensor arrangement attached to at least one lifting bar bolt of an at least one lifting bar of the grinding mill. The sensor arrangement includes at least one force transducer attached to the at least one lifting bar bolt. With the help of the measurement arrangement, more reliable measurement data can be provided for the determination of the degree of fullness of a grinding mill drum.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a division of our copending application Ser. No. 582,646, filed June 2, 1975, now U.S. Pat. No. 4,022,833 which is a division of our copending application Ser. No. 332,267, filed Feb. 14, 1973, now U.S Pat. No. 3,928,427, which is a continuation-in-part of our copending application Ser. No. 123,097, filed Mar. 10, 1971 and now abandoned.
FIELD OF THE INVENTION
This invention relates to compositions of matter classified in the art of organic chemistry as N,N'-bridged-bis-[(O and/or N-substituted)-2-alkyl-2-hydroxyethylamines] and to a process for preparing them.
SUMMARY OF THE INVENTION
In its composition of matter aspect our invention provides N,N'-(X)-bis[N-(R')-2-(R)-2-(ZO)-ethylamine] of the formula ##STR3## wherein: R is alkyl of three to fifteen carbon atoms or cycloalkyl of four to seven ring carbon atoms;
R' is hydrogen or atertiary alkyl of one to four carbon atoms;
X is alkylene of two to twelve carbon atoms with bonds to the nitrogen atoms at different carbon atoms or X'--Y--X", wherein X' and X" are alkylene of one to four carbon atoms with bonds to Y and to the nitrogen atoms at the same or different carbon atoms and Y is cycloalkylene of four to seven ring carbon atoms with bonds to X' and X" at the same or different carbon atoms, phenylene, vinylene or ethynylene;
The sum of the number of carbon atoms of R and X is at least nine;
Z is hydrogen or, when R' is atertiary alkyl of one to four carbon atoms, N-phenylcarbamoyl or N-phenylcarbamoyl substituted in the benzene ring by one to three members selected from the group consisting of atertiary alkyl of one to four carbon atoms, halo and atertiary alkoxy of one to four carbon atoms or by a member selected from the group consisting of trifluoromethyl, acetamido, nitro, and methylsulphonyl;
acid-addition salts thereof; and,
when R' is atertiary alkyl of one to four carbon atoms and Z is hydrogen, N,N'-dioxides, N,N'-di(atertiary alkyl of one to four carbon atoms)diammonium quaternary salts and N,N'-dibenzyldiammonium quaternary salts thereof.
The compounds of Formula I and acid-addition salts, N,N'-dioxides and N,N'-diammonium quaternary salts thereof have antibacterial activity in vitro and are useful as antibacterial agents.
In its process aspect our invention provides the process for preparing N,N'-(X)-bis[N-(R')-2-(R)-2-(ZO)-ethylamine] of Formula I, wherein Z is hydrogen, which comprises condensing an epoxide of the formula ##STR4## with a diamine of the formula
R'NH--X--NHR' (Formula III),
wherein R of Formula II and R' and X of Formula III have the same meanings ascribed thereto in Formula I.
DETAILED DESCRIPTION OF THE INVENTION
When R is alkyl of three to fifteen carbon atoms, it is normal alkyl or branched alkyl as illustrated by propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl and pentadecyl. Since R and ethyl are integral, they are named integrally when R is alkyl. Thus, the illustrated alkyls become respectively, pentyl, 3-methylbutyl, hexyl, 4-methylpentyl, 2-methylpentyl, 3,3-dimethylbutyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl and heptadecyl.
When R is cycloalkyl of four to seven ring carbon atoms, it is cyclobutyl, cyclopentyl, cyclohexyl or cycloheptyl.
When R' is atertiary alkyl of one to four carbon atoms, it is methyl, ethyl, propyl, isopropyl, butyl, isobutyl or sec-butyl.
When X is alkylene of two to twelve carbon atoms with bonds to the nitrogen atoms at different carbon atoms, it can be unbranched or branched. If unbranched, X is 1,2-ethylene, 1,3-propylene, 1,4-butylene, 1,5-pentylene, 1,6-hexylene, 1,7-heptylene, 1,8-octylene, 1,9-nonylene, 1,10-decylene, 1,11-undecylene or 1,12-dodecylene. If branched, X is, for example, 1,2-propylene, 2,4-butylene, 2,10-dodecylene, or 2-methyl-1,4-butylene.
When X is X'--Y--X", X' and X" can be the same or different and can be unbranched or branched alkylene of one to four carbon atoms with bonds to Y and to the nitrogen atoms at the same or different carbon atoms as illustrated by methylene, ethylene, ethylidene or 1,4-butylene. When Y is cycloalkylene of four to seven ring carbon atoms with bonds to X' and X" at the same or different carbon atoms, it is, for example, cyclobutylidene, 1,4-cyclohexylene or 1,2-cycloheptylene. When Y is cycloalkylene or vinylene, the bonds to X' and X" can be cis or trans. Thus, X'--Y--X" is, for example, 1,3-cyclobutylenebis-methyl, 1,4-cyclohexylenebismethyl, cis-1,4-cyclohexylenebis-methyl, trans-1,4-cyclohexylenebismethyl, 1,2-cycloheptylene-bismethyl, cyclohexylene-1-methyl-4-(2-ethyl), cyclohexylene-1-methyl-4-(1-ethyl), cyclohexylene-1-methyl-4-(4-butyl), 1,4-phenylenebismethyl, trans-1,4-(2-butenylene) and 1,4-(2-butynylene).
When Z is N-phenylcarbamoyl substituted in the benzene ring, it is, for example, N-(o-tolyl)carbamoyl, N-(p-bromophenyl)carbamoyl, N-(m-methoxyphenyl)carbamoyl, N-(4-chloro-o-tolyl)carbamoyl, N-(5-chloro-2,4-dimethoxyphenyl)carbamoyl, N-[m-(trifluoromethyl)phenyl]carbamoyl, N-(p-acetamidophenyl)carbamoyl, N-(m-nitrophenyl)carbamoyl, or N-[p-(methylsulfonyl)phenyl]carbamoyl. Named as substituted carbanilates the illustrated substituted N-phenylcarbamoyls are, respectively, o-methylcarbanilate, p-bromocarbanilate, m-methoxycarbanilate, 2-methyl-4-chlorocarbanilate, 5-chloro-2,4-dimethoxycarbanilate, m-(trifluoromethyl)carbanilate, p-acetamidocarbanilate, m-nitrocarbanilate and p-(methylsulfonyl)carbanilate. When N-phenylcarbamoyl is substituted in the benzene ring by halo, halo is fluoro, chloro, bromo or iodo.
In N,N'-diammonium quaternary salts of the compounds of Formula I wherein R' is alkyl, atertiary alkyl of one to four carbon atoms can be methyl, ethyl, propyl, isopropyl, butyl, isobutyl or sec-butyl.
The manner and process of making and using the invention and the best mode of carrying it out will now be described so as to enable any person skilled in the art to which it pertains to make and use it.
The preferred method for carrying out the process of condensing an epoxide of Formula II with a diamine of Formula III is the use of a solvent inert under the reaction conditions, for example, acetonitrile, benzene, chloroform, N,N-dimethylformamide, ethanol, methanol or tetrahydrofuran at a temperature in the range of 0° to 100° C. Methanol is the preferred solvent and room temperature is the preferred temperature.
Compounds of Formula I in which R' is methyl are also prepared by methylating the corresponding compounds of Formula I in which R' is hydrogen with formaldehyde and formic acid.
Phenylcarbamoylation and phenylthiocarbamoylation of compounds of Formula I wherein R' is alkyl and Z is hydrogen, formation of acid-addition salts of the compounds of Formula I, and N,N'-dioxidation and N,N'-diquaternerization of the compounds of Formula I wherein R' is alkyl are all accomplished by standard methods.
The phenylisocyanates and phenylisothiocyanates required for phenylcarbamoylation and phenylthiocarbamoylation are known classes of compounds, some of which are commercially available. Those (substituted-phenyl)isocyanates which are not commercially available can be prepared, for example, by passing carbonyl chloride into hot solutions of the corresponding anilines in toluene, saturated with hydrogen chloride. Those (substituted-phenyl)isothiocyanates which are not commercially available can be prepared, for example, by treating the corresponding ammonium (substituted-phenyl) dithiocarbamates, prepared in turn from the corresponding substituted anilines, carbon disulfide and ammonia, with lead nitrate.
Acid-addition salts of the compounds of Formula I can be prepared with any pharmaceutically acceptable inorganic (mineral) or organic acid. If inorganic, the acid can be, for example, hydrochloric acid, hydrobromic acid, nitric acid, phosphoric acid or sulfamic acid. If organic, the acid can be, for example, acetic acid, glycolic acid, lactic acid, quinic acid, hydrocinnamic acid, succinic acid, tartaric acid, citric acid, methanesulfonic acid or benzenesulfonic acid.
N,N'-diammonium quaternary salts of compounds of Formula I wherein R' is alkyl can be prepared with any pharmaceutically acceptable atertiary one-to-four-carbon alkyl or benzyl ester of a strong inorganic or organic acid, for example, methyl chloride, methyl iodide, ethyl p-toluenesulfonate, propyl bromide, isobutyl iodide or benzyl bromide.
That the acid and the alkyl ester be pharmaceutically acceptable means that the beneficial properties inherent in the free base not be vitiated by side effects ascribable to the anions.
Although pharmaceutically acceptable salts are preferred, all salts are within the scope of the invention. A pharmaceutically unacceptable salt may be useful, for example, for purposes of identification or purification or in preparing a pharmaceutically acceptable salt by ion-exchange procedures.
The intermediate epoxides of Formula II are a known class of compounds. Their preparation is accomplished by epoxidation of the corresponding 1-alkenes and vinylcycloalkanes by any of several well-known methods, for example, by the use of peracetic acid buffered with sodium acetate. The 1-alkenes and vinylcycloalkanes are known compounds, some of which are commercially available.
The intermediate diamines of Formula III are also a known class of compounds, some of which are commercially available. Preparation of those which are not commercially available is accomplished by well-known methods, for example, by reductive amination of the corresponding diketone or dialdehyde, amination of the corresponding dihalide or dialcohol p-toluenesulfonate diester or reduction of the corresponding dinitrile, dioxime, diamide, diazide or other di-higheroxidation-state nitrogen compound. Unsymmetrical diamines can be prepared from unsymmetrical starting materials.
The compounds of Formula I and acid-addition salts, N,N'-dioxides and N,N'-diammonium quaternary salts thereof are purified by distillation or by recrystallization. Their structures follow from their route of synthesis and are corroborated by infrared spectral analysis and by the correspondence of calculated and found values of elemental analysis of representative samples.
As stated above the compounds of Formula I and acid-addition salts, N,N'-dioxides and N,N'-diammonium quaternary salts thereof have antibacterial activity in vitro, which was determined by a standard serial dilution test. In this test the concentration of compound arresting the growth of the microorganism is the bacteriostatic concentration and is expressed in parts per million (p.p.m.). The concentration of compound preventing growth of the microorganism after further incubation is the bactericidal concentration and is also expressed in parts per million.
The compounds of Formula I and acid-addition salts, N,N'-dioxides and N,N'-diammonium quaternary salts thereof are useful as antibacterial agents and are especially useful for disinfecting and sanitizing living and non-living surfaces by conventional swabbing, padding, spraying, immersing, rinsing and the like techniques. Depending on the particular purpose involved, the compounds are used in aqueous solution, in aqueous detergent solutions or in solutions in organic solvents.
The following examples illustrate specific embodiments of our invention without limiting the latter thereto.
EXAMPLE 1
A solution of 1-undecene oxide (88.8 g.), hexamethylenediamine (1,6-hexanediamine, 30.3 g.) and methanol (400 ml.) was allowed to stand at 0° C. overnight, then at room temperature over the weekend. The solid was collected and recrystallized from ethanol, affording N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = (CH 2 ) 6 ; Z = H)(m.p. 122.6°-129.0° C.).
Hydrogen bromide was bubbled through a solution of N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine] (5 g.) in methanol (100 ml.). The resulting solid was collected (4.6 g.) and recrystallized from methanol, affording N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dihydrobromide (2.4 g., m.p. 299°-301° C.).
A solution of N,N'-(1,6-hexylene-bis[2-hydroxyundecylamine] (5 g.), glycolic acid (1.66 g.) and methanol was heated until the solids dissolved, then evaporated to dryness. Recrystallization of the solid from acetone afforded N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine] diglycolate (4.6 g., m.p. 88.2°-94.6° C.).
In a similar manner using acetic acid and lactic acid instead of glycolic acid there were obtained, respectively, N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine] diacetate (m.p. 113°-120.6° C.) and N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dilactate (m.p. 102.0°-104.0° C.).
Using hydrochloric acid, nitric acid, phosphoric acid, sulfamic acid, quinic acid, hydrocinnamic acid, succinic acid, tartaric acid, citric acid methanesulfonic acid and benzenesulfonic acid, there are obtained, respectively:
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dihydrochloride;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dinitrate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] diphosphate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] disulfamate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] diquinate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dihydrocinnamate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] succinate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] tartrate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dicitrate;
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dimethanesulfonate; and
N,n'-(1,6-hexylene)-bis[2-hydroxyundecylamine] dibenzenesulfonate.
Table I shows the results of the antibacterial testing in vitro of N,N'-(1,6-hexylene)-bis[2-hydroxyundecylamine].
Table I______________________________________ Bacteriostatic con- Bactericidal con-Microorganism centration (p.p.m.) centration (p.p.m.)______________________________________Staphylococcus 2.5 5aureusEberthella typhi 5 5Clostridium welchii 10 10Pseudomonas 7.5 25aeruginosa______________________________________
EXAMPLE 2
Condensation of 1-pentene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxypentylamine] (I: R = CH 3 (CH 2 ) 2 , R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 3
Condensation of 3-methyl-1-butene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-3-methylbutylamine] (I: R = (CH 3 ) 2 CH, R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 4
Condensation of 1-hexene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxyhexylamine] (I: R = CH 3 (CH 2 ) 3 , R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 5
Condensation of 4-methyl-1-pentene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-4-methylpentylamine] (I: R = (CH 3 ) 2 CHCH 2 , R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 6
Condensation of 3-methyl-1-pentene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-3-methylpentylamine] (I: R = CH 3 CH 2 (CH 3 )C, R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 7
Condensation of 3,3-dimethyl-1-butene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-3,3-dimethylbutylamine] (I: R = (CH 3 ) 3 C, R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 8
In a manner similar to that of Example 1, condensation of 1-heptene oxide (71.8 g.) and hexamethylenediamine (32 g.) and recrystallization of the resulting product from ethanol gave N,N'-(1,6-hexylene)-bis[2-hydroxyheptylamine] (I: R = CH 3 (CH 2 ) 4 , R' = H, X = (CH 2 ) 6 , Z = H) (16.5 g., m.p. 131.2°-134.2° C.).
EXAMPLE 9
In a manner similar to that of Example 1, condensation of 1-octene oxide (42 g.) and hexamethylenediamine (19.05 g.) and recrystallization of the resulting product from methanol gave N,N'-(1,6-hexylene)-bis[2-hydroxyoctylamine] (I: R = CH 3 (CH 2 ) 5 , R' = H, X = (CH 2 ) 6 , Z = H) (17.2 g., m.p. 124.0°-127.4° C.).
EXAMPLE 10
In a manner similar to that of Example 1, condensation of 1-nonene oxide (97.4 g.) and hexamethylenediamine (39.8 g.) and recrystallization of the resulting product (67 g.) from ethanol afforded N,N'-(1,6-hexylene)-bis[2-hydroxynonylamine] (I: R = CH 3 (CH 2 ) 6 , R' = H, X = (CH 2 ) 6 , Z = H) (67 g., m.p. 122°-129.2° C.).
Treatment of N,N'-(1,6-hexylene)-bis[2-hydroxynonylamine] (4 g.) with lactic acid (2.12 g.) in methanol and recrystallization of the resulting salt from acetone gave N,N'-(1,6-hexylene)-bis[2-hydroxynonylamine] dilactate (3.3 g., m.p. 103.0°-104.6° C.).
EXAMPLE 11
In a manner similar to that of Example 1, condensation of 1-decene oxide (50 g.) and hexamethylenediamine (18.6 g.) and recrystallization of the resulting product from methanol gave N,N'-(1,6-hexylene)-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = (CH 2 ) 6 , Z = H) (25.4 g., m.p. 118.0°-126.8° C.).
EXAMPLE 12
In a manner similar to that of Example 1, condensation of 1-dodecene oxide (50 g.) and hexamethylenediamine (15.8 g.) and recrystallization of the resulting product from ethanol gave N,N'-(1,6-hexylene)-bis[2-hydroxydodecylamine] (I: R = CH 3 (CH 2 ) 9 , R' = H, X = (CH 2 ) 6 , Z = H) (35 g., m.p. 123.6°-128.0° C.).
EXAMPLE 13
Condensation of 1-tridecene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxytridecylamine] (I: R = CH 3 (CH 2 ) 10 , R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 14
In a manner similar to that of Example 1, condensation of 1-tetradecene oxide (91.8 g.) and hexamethylenediamine (25 g.) and recrystallization of the resulting product (71 g., m.p. 118°-121° C.) from ethanol gave N,N'-(1,6-hexylene)-bis[2-hydroxytetradecylamine] (I: R = CH 3 (CH 2 ) 11 , R' = H, X = (CH 2 ) 6 , Z = H) (55.3 g., m.p. 122°-126° C.).
EXAMPLE 15
In a manner similar to that of Example 1, condensation of 1-pentadecene oxide (81.7 g.) and hexamethylenediamine (21 g.) and recrystallization of the resulting product (74.3 g.) from isopropyl alcohol gave N,N'-(1,6-hexylene)-bis[2-hydroxypentadecylamine] (I: R = CH 3 (CH 2 ) 12 , R' = H, X = (CH 2 ) 6 , Z = H) (m.p. 117.4°-124.0° C.).
EXAMPLE 16
Condensation of 1-hexadecene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxyhexadecylamine] (I: R = CH 3 (CH 2 ) 13 , R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 17
Condensation of 1-heptadecene oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxyheptadecylamine] (I: R = CH 3 (CH 2 ) 14 , R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 18
Condensation of vinylcyclobutane oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-2-cyclobutylethylamine] (I: ##STR5## R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 19
Condensation of vinylcyclopentane oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-2-cyclopentylethylamine] (I: ##STR6## R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 20
Condensation of vinylcyclohexane oxide and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-2-cyclohexylethylamine] (I: ##STR7## R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 21
Condensation of vinylcycloheptane and hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[2-hydroxy-2-cycloheptylethylamine] (I: ##STR8## R' = H, X = (CH 2 ) 6 , Z = H).
EXAMPLE 22
A. N,N'-(1,6-Hexylene)-bis[2-hydroxyundecylamine] (25.6 g.) was added in portions to a solution of formic acid (98%, 25 ml.) and formaldehyde (60%, 15 ml.) held at 70° C. When the addition was complete the resulting solution was refluxed (9 hr.), then basified with sodium hydroxide solution (35%). The solid was collected and treated with methanolic potassium hydroxide. The mixture was diluted with water and extracted with ether. Concentration of the ether extract and distillation of the residue under vacuum afforded an oil (16 g., b.p. 208°-214° C./0.05 mm.). Hydrogen bromide was bubbled through an ethereal solution of the oil. The resulting solid was recrystallized from etherisopropyl alcohol, affording N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine] dihydrobromide (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) (m.p. 186.4°-189.8° C.).
B. Condensation of 1-undecene oxide and N,N'-dimethylhexamethylenediamine and treatment of the resulting product with hydrogen bromide also affords N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine] dihydrobromide.
Table II shows the results of the in vitro antibacterial testing of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine] dihydrobromide.
Table II______________________________________ Bacteriostatic con- Bactericidal con-Microorganism centration (p.p.m.) centration (p.p.m.)______________________________________Staphylococcus 2.5 7.5aureusEberthella typhi 5 5Clostridium welchii 5 5Pseudomonas 25 50aeruginosa______________________________________
EXAMPLE 23
Condensation of 1-undecene oxide and N,N'-diethylhexamethylenediamine affords N,N'-(1,6-hexylene)-bis[N-ethyl-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 CH 2 , X = (CH 2 ) 6 , Z = H).
EXAMPLE 24
Condensation of 1-undecene oxide and N,N'-dipropylhexamethylenediamine affords N,N'-(1,6-hexylene)-bis[N-propyl-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 (CH 2 ) 2 , X = (CH 2 ) 6 , Z = H).
EXAMPLE 25
Condensation of 1-undecene oxide and N,N'-di(isopropyl)hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[N-isopropyl-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = (CH 3 ) 2 CH, X = (CH 2 ) 6 , Z = H).
EXAMPLE 26
Condensation of 1-undecene oxide and N,N'-dibutylhexamethylenediamine affords N,N'-(1,6-hexylene)-bis[N-butyl-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 (CH 2 ) 3 , X = (CH 2 ) 6 , Z = H).
EXAMPLE 27
Condensation of 1-undecene oxide and N,N'-di(isobutyl)hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[N-isobutyl 2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = (CH 3 ) 2 CHCH 2 , X = (CH 2 ) 6 , Z = H).
EXAMPLE 28
Condensation of 1-undecene oxide and N,N'-di(secbutyl)hexamethylenediamine affords N,N'-(1,6-hexylene)-bis[N-(sec-butyl)-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 CH 2 (CH 3 )CH, X = (CH 2 ) 6 , Z = H).
EXAMPLE 29
In a manner similar to that of Example 22, methylation of N,N'-(1,6-hexylene)-bis[2-hydroxyheptylamine] (35.7 g.) treatment of a portion (18.0 g.) of the resulting product (35.6 g.) with hydrogen bromide and recrystallization of the resulting salt from acetone gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyheptylamine] (I: R = CH 3 (CH 2 ) 4 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) dihydrobromide (15.5 g., m.p. 147.0°-149.0° C.).
EXAMPLE 30
In a manner similar to that of Example 22, methylation of N,N'-(1,6-hexylene)-bis[2-hydroxyoctylamine] (35 g.) and treatment of the resulting product (b.p. 177°-182° C./l mm.) with hydrogen bromide gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyoctylamine] (I: R = CH 3 (CH 2 ) 5 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) dihydrobromide (19.1 g., m.p. 167.0°-168.8° C.).
EXAMPLE 31
In a manner similar to that of Example 22, methylation of N,N'-(1,6-hexylene)-bis[2-hydroxynonylamine] (36 g.) and treatment of the resulting product (25 g., b.p. 172°-176° C./0.05 mm.) with hydrogen bromide gave N,N'-(1,6-hexylene)-bis-[N-methyl-2-hydroxynonylamine] (I: R = CH 3 (CH 2 ) 6 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) dihydrobromide (26.3 g., m.p. 176.0°-177.0° C.).
EXAMPLE 32
In a manner similar to that of Example 22, methylation of N,N'-(1,6-hexylene)-bis[2-hydroxydecylamine] (36.7 g.), treatment of the resulting product (17.5 g., b.p. 204°-206° C./0.03 mm.) with hydrogen bromide and recrystallization of the resulting salt from isopropyl alcohol gave N,N'-(1,6-hexylene)bis[N-methyl-2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) dihydrobromide (8.4 g., m.p. 186.0°-187.6° C.).
EXAMPLE 33
In a manner similar to that of Example 22, methylation of N,N'-(1,6-hexylene)-bis[2-hydroxydodecylamine] (25 g.), treatment of the resulting product (b.p. 217°-228° C./0.02 mm.) with hydrogen bromide and recrystallization of the resulting salt from isopropyl alcohol gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydodecylamine] (I: R = CH 3 (CH 2 ) 9 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) dihydrobromide (9.6 g., m.p. 197.0°-198.4° C.).
EXAMPLE 34
In a manner similar to that of Example 22, methylation of N,N'-(1,6-hexylene)-bis[2-hydroxytetradecylamine] (30 g.) gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxytetradecylamine] (I: R = CH 3 (CH 2 ) 11 , R' = CH 3 , X = (CH 2 ) 6 , Z = H) as a brown oil (28.2 g.).
EXAMPLE 35
In a manner similar to that of Example 1, condensation of 1-decene oxide (100 g.) and ethylenediamine (19.2 g.) and recrystallization of a portion (20 g.) of the resulting solid (45 g.) from ethanol gave N,N'-ethylenebis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = (CH 2 ) 2 , Z = H) (13.6 g., m.p. 140.0°-145.8° C.).
EXAMPLE 36
In a manner similar to that of Example 1, condensation of 1-undecene oxide (40 g.) and ethylenediamine (7.07 g.) and two recrystallizations of the resulting solid (14.9 g.) from ethanol gave N,N'-ethylenebis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = (CH 2 ) 2 , Z = H) (12.4 g., m.p. 130.2°-137.8° C. ).
EXAMPLE 37
In a manner similar to that of Example 1, condensation of 1-dodecene oxide (100 g.) and ethylenediamine (16.3 g.) and recrystallization of part (20 g.) of the resulting product (55.3 g.) from methanol gave N,N'-ethylenebis[2-hydroxydodecylamine] (I: R = CH 3 (CH 2 ) 9 , R' = H, X = (CH 2 ) 2 , Z = H) (13.4 g., m.p. 137.0°-142.0° C.).
EXAMPLE 38
In a manner similar to that of Example 22, methylation of N,N'-ethylenebis[2-hydroxydecylamine] (15 g.) and treatment of the resulting product with hydrogen bromide gave N,N'-ethylenebis[N-methyl-2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = (CH 2 ) 2 , Z = H) dihydrobromide (4.0 g., m.p. 152.0°-164.0° C.).
EXAMPLE 39
In a manner similar to that of Example 22, methylation of N,N'-ethylenebis[2-hydroxyundecylamine] (30 g.), treatment of the resulting product with hydrogen bromide and recrystallization of the resulting salt from isopropyl alcohol gave N,N'-ethylenebis[N-methyl-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 , X = (CH 2 ) 2 , Z = H) dihydrobromide (12.8 g., m.p. 151.0°-162.0° C.).
EXAMPLE 40
In a manner similar to that of Example 22, methylation of N,N'-ethylenebis[2-hydroxydodecylamine] (35 g.), treatment of the resulting product with hydrogen bromide and recrystallization of the resulting salt from isopropyl alcohol gave N,N'-ethylenebis[N-methyl-2-hydroxydodecylamine] (I: R = CH 3 (CH 2 ) 9 , R' = CH 3 , X = (CH 2 ) 2 , Z = H) dihydrobromide (4.6 g., m.p. 162.0° C.).
EXAMPLE 41
In a manner similar to that of Example 1, condensation of 1-nonene oxide (120 g.) and 1,3-propanediamine (31.2 g.) and two recrystallizations of the resulting product from methanol gave N,N'-(1,3-propylene)-bis[2-hydroxynonylamine] (I: R = CH 3 (CH 2 ) 6 , R' = H, X = (CH 2 ) 3 , Z = H) (13.2 g., m.p. 107.0°-109.0° C.).
EXAMPLE 42
In a manner similar to that of Example 1, condensation of 1-decene oxide (58 g.) and 1,3-propanediamine (13.8 g.) and three recrystallizations of the resulting product from methanol gave N,N'-(1,3-propylene)-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = (CH 2 ) 3 , Z = H) (8.5 g., m.p. 104.0°-107.6° C.).
EXAMPLE 43
In a manner similar to that of Example 1, condensation of 1-undecene oxide (104.6 g.) and 1,3-propanediamine (22.7 g.) and two recrystallizations of the resulting product from methanol gave N,N'-(1,3-propylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = (CH 2 ) 3 , Z = H) (29.0 g., m.p. 94.0°-103.0° C.).
EXAMPLE 44
In a manner similar to that of Example 1, condensation of 1-dodecene oxide (100 g.) and 1,3-propanediamine (20.1 g.) and three recrystallizations of the resulting product from isopropyl alcohol gave N,N'-(1,3-propylene)-bis[2-hydroxydodecylamine] (I: R = CH 3 (CH 2 ) 9 , R' = H, X = (CH 2 ) 3 , Z = H) (11.9 g., 96.0°-106.0° C.).
EXAMPLE 45
In a manner similar to that of Example 22, methylation of N,N'-(1,3-propylene)-bis[2-hydroxynonylamine] (14 g.), treatment of the resulting product with hydrogen bromide and two recrystallizations of the resulting salt from acetonitrile gave N,N'-(1,3-propylene)-bis[N-methyl-2-hydroxynonylamine] (I: R = CH 3 (CH 2 ) 6 , R' = CH 3 , X = (CH 2 ) 3 , Z = H) dihydrobromide (9.1 g., m.p. 175.0°-189.0° C.).
EXAMPLE 46
In a manner similar to that of Example 22, methylation of N,N'-(1,3-propylene)-bis[2-hydroxydecylamine] (21.4 g.), treatment of the resulting product with hydrogen bromide and four recrystallizations of the resulting salt from ethyl acetate-isopropyl alcohol gave N,N'-(1,3-propylene)-bis[N-methyl-2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = (CH 2 ) 3 , Z = H) dihydrobromide (9.0 g., m.p. 174.2°-184.0° C.).
EXAMPLE 47
In a manner similar to that of Example 22, methylation of N,N'-(1,3-propylene)-bis[2-hydroxyundecylamine] (16 g.), treatment of the resulting product with hydrogen bromide and recrystallization of the resulting salt from acetone gave N,N'-(1,3-propylene)-bis[N-methyl-2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = CH 3 , X = (CH 2 ) 3 , Z = H) dihydrobromide (12.9 g., m.p. 176.0°-189.0° C.).
EXAMPLE 48
Condensation of 1-undecene oxide and 1,4-butanediamine affords N,N'-(1,4-butylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = (CH 2 ) 4 , Z = H).
EXAMPLE 49
Condensation of 1-undecene oxide and 1,5-pentanediamine affords N,N'-(1,5-pentylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = (CH 2 ) 5 , Z = H).
EXAMPLE 50
Condensation of 1-heptene oxide and 1,7-heptanediamine affords N,N'-(1,7-heptylene)-bis [2-hydroxyheptylamine] (I: R = CH 3 (CH 2 ) 4 , R' = H, X = (CH 2 ) 7 , Z = H).
EXAMPLE 51
In a manner similar to that of Example 1, condensation of 1-heptene oxide (52 g.) and 1,8-octanediamine (32.8 g.) and two recrystallizations of the resulting product from methanol gave N,N'-(1,8-octylene)-bis[2-hydroxyheptylamine] (I: R = CH 3 (CH 2 ) 4 , R' = H, X = (CH 2 ) 8 , Z = H) (17.2 g., m.p. 128.0°-132.8° C.).
EXAMPLE 52
In a manner similar to that of Example 22, methylation of N,N'-(1,8-octylene)-bis[2-hydroxyheptylamine] (16.9 g.), treatment of the resulting product with hydrogen bromide and two recrystallizations of the resulting salt from isopropyl alcohol gave N,N'-(1,8-octylene)-bis[N-methyl-2-hydroxyheptylamine] (I: R = CH 3 (CH 2 ) 4 , R' = CH 3 , X = (CH 2 ) 8 , Z = H) dihydrobromide (15.9 g., m.p. 177.0°-190.0° C.).
EXAMPLE 53
Condensation of 1-hexene oxide and 1,9-nonanediamine affords N,N'-(1,9-nonylene)-bis[2-hydroxyhexylamine] (I: R = CH 3 (CH 2 ) 3 , R' = H, X = (CH 2 ) 9 , Z = H).
EXAMPLE 54
In a manner similar to that of Example 1, condensation of 1-hexene oxide (34.8 g.) and 1,10-decanediamine (30 g.) and recrystallization of the resulting product from isopropyl alcohol gave N,N'-(1,10-decylene)-bis[2-hydroxyhexylamine] (I: R = CH 3 (CH 2 ) 3 , R' = H, X = (CH 2 ) 10 , Z = H) (8.9 g., m.p. 127.0-137.0° C.).
EXAMPLE 55
Condensation of 1-pentene oxide and 1,11-undecanediamine affords N,N'-(1,11-undecylene)-bis[2-hydroxypentylamine] (I: R = CH 3 (CH 2 ) 2 , R' = H, X = (CH 2 ) 11 , Z = H).
EXAMPLE 56
Condensation of 1-pentene oxide and 1,12-dodecanediamine affords N,N-(1,12-dodecylene)-bis[2-hydroxypentylamine] (I: R = CH 3 (CH 2 ) 2 , R' = H, X = (CH 2 ) 12 , Z = H).
EXAMPLE 57
Condensation of 1-undecene oxide and 1-methyl-1,2-ethanediamine affords N,N'-(1,2-propylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = CH(CH 3 )CH 2 , Z = H).
EXAMPLE 58
Condensation of 1-undecene oxide and 1,2-dimethyl-1,2-ethanediamine affords N,N'-(2,4-butylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = CH(CH 3 )CH(CH 3 ), Z = H).
EXAMPLE 59
Condensation of 1-pentene oxide and 1,10-dimethyl-1,10-decanediamine affords N,N'-(2,10-dodecylene)-bis[2-hydroxypentylamine] (I: R = CH 3 (CH 2 ) 2 , R' = H, X = CH(CH 3 )(CH 2 ) 8 CH(CH 3 ), Z = H).
EXAMPLE 60
Condensation of 1-undecene oxide and 2-methyl-1,4-butanediamine affords N,N'-(2-methyl-1,4-butylene)-bis[2-hydroxyundecylamine] (I: R = CH 3 (CH 2 ) 8 , R' = H, X = CH 2 CH(CH 3 )CH 2 CH 2 , Z = H).
EXAMPLE 61
In a manner similar to that of Example 1, condensation of 1-octene oxide (50g.) and 1,4-cyclohexylenebis(methylamine) (27.8g.) and recrystallization of the resulting product from acetone gave N,N'-(1,4-cyclohexylenebismethyl)-bis[2-hydroxyoctylamine] (I: R = CH 3 (CH 2 ) 5 , R' = H, X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H), (12 g., m.p. 90.0°-96.2° C.).
EXAMPLE 62
In a manner similar to that of Example 1, condensation of 1-decane oxide (two runs, 50 g. each) and 1,4-cyclohexylene-bis(methylamine) (22.8 g. each run) and two recrystallizations of the products from acetone gave N,N'-(1,4-cyclohexylenebismethyl)-bis[2-hydroxydecylamine] (R = CH 3 (CH 2 ) 7 , R' = H, X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H) (18.4 g., m.p. 92.0°-98.8° C.).
EXAMPLE 63
In a manner similar to that of Example 1, condensation of 1-decene oxide (96.6 g.) and cis-1,4-cyclohexylenebis(methylamine) (44.2 g.) and two recrystallizations of the resulting product from acetone gave N,N'-(cis-1,4-cyclohexylenebismethyl)bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = cis-CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H) (13.5 g., m.p. 72.6°-77.4° C.).
EXAMPLE 64
In a manner similar to that of Example 1, condensation of 1-decene oxide (98.9 g.) and trans-1,4-cyclohexylenebis(methylamine) (45.2 g.) and recrystallization of the resulting product from acetone gave N,N'-(trans-1,4-cyclohexylenebismethyl)bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = trans-CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H) (23.3 g., m.p. 101.0°-102.8° C.).
EXAMPLE 65
In a manner similar to that of Example 22, methylation of N,N'-(1,4-cyclohexylenebismethyl)-bis[2-hydroxydecylamine] and two recrystallizations of the resulting product from methanol gave N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl-2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H) (8.9 g., m.p. 66°-69° C.).
EXAMPLE 66
In a manner similar to that of Example 1, condensation of 1-dodecene oxide (50 g.) and 1,4-cyclohexylenebis(methylamine) (19.3 g.) and recrystallization of the resulting product from methanol gave N,N'-(1,4-cyclohexylenebismethyl)-bis[2-hydroxydodecylamine] (I: R = CH 3 (CH 2 ) 9 , R' = H, X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H) (9.5 g., m.p. 93.0°-96.0° C.).
EXAMPLE 67
Condensation of 1-decene oxide and cyclobutylidene-bis(methylamine) affords N,N'-(cyclobutylidenebismethyl)-bis [2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, ##STR9##
EXAMPLE 68
Condensation of 1-decene oxide and 1,2-cycloheptylene-bis(methylamine) affords N,N'-(1,2-cycloheptylenebismethyl)bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, ##STR10##
EXAMPLE 69
Condensation of 1-decene oxide and 1-(aminomethyl)-4-(2-aminoethyl)cyclohexane affords N,N'-[cyclohexylene-1-methyl-4-(2-ethyl)]-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = CH 2 CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H).
EXAMPLE 70
Condensation of 1-decene oxide and 1-(aminomethyl)-4-(1-aminoethyl)cyclohexane affords N,N'-[cyclohexylene-1-methyl-4-(1-ethyl)]-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = CH(CH 3 )CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H).
EXAMPLE 71
Condensation of 1-decene oxide and 1-(aminomethyl)-4-(4-aminobutyl)cyclohexane affords N,N'-[cyclohexylene-1-methyl-4-(4-butyl)[-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = (CH 2 ) 4 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = H).
EXAMPLE 72
Condensation of 1-decene oxide and 1,4-phenylenebis(methylamine) affords N,N'-(1,4-phenylenebismethyl)-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = 1,4--CH 2 C 6 H 4 CH 2 , Z = H).
EXAMPLE 73
Condensation of 1-decene oxide and trans-1,4-(2-butenylene)diamine affords N,N'-[trans-1,4-(2-butenylene)]-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = trans--CH 2 CH═CHCH 2 , Z = H).
EXAMPLE 74
Condensation of 1-decene oxide and 1,4-(2-butynylene)diamine affords N,N'-[1,4-(2-butynylene)[-bis[2-hydroxydecylamine] (I: R = CH 3 (CH 2 ) 7 , R' = H, X = CH 2 C.tbd.CCH 2 , Z = H).
EXAMPLE 75
A mixture of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine[ (3.6 g.), phenyl isocyanate (1.78 g.), pyridine (seven drops) and benzene (45 ml.) was heated under reflux (for 3 hr.), then filtered. The filtrate was diluted with hexane (10 ml.), and the resulting product (2.4 g.) was recrystallized from methanol, affording N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] dicarbanilate (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 5 ) (m.p. 74°-76° C).
EXAMPLE 76
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and o-tolyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl-2hydroxydecylamine] bis(o-methylcarbanilate) (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 4 CH 3 --o).
EXAMPLE 77
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and p-bromophenyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl-2-hydroxydecylamine] bis(p-bromocarbanilate) (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 4 Br-p).
EXAMPLE 78
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and 4-chloro-o-tolyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl-2-hydroxydecylamine] bis(2-methyl-4-chlorocarbanilate) (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 3 CH 3 --2--Cl--4).
EXAMPLE 79
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and 5-chloro-2,4-dimethoxyphenyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] bis(5-chloro-2,4-dimethoxycarbanilate) (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 2 (OCH 3 ) 2 --2,4--Cl--5).
EXAMPLE 80
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and m-(trifluoromethyl)phenyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)bis-[N-methyl-2-hydroxydecylamine] bis[m-(trifluoromethyl)carbanilate] (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 4 CF 3 --m).
EXAMPLE 81
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and p-acetamidophenyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl2-hydroxydecylamine] bis(p-acetamidocarbanilate) (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 4 --NHCOCH 3 --p).
EXAMPLE 82
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and m-nitrophenyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl-2-hydroxydecylamine] bis(m-nitrocarbanilate) (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 4 NO 2 --m).
EXAMPLE 83
Condensation of N,N'-(1,4-cyclohexylenebismethyl)bis[N-methyl-2-hydroxydecylamine] and p-(methylsulfonyl)phenyl isocyanate affords N,N'-(1,4-cyclohexylenebismethyl)-bis[N-methyl-2-hydroxydecylamine] bis[p-(methylsulfonyl)carbanilate] (I: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = CH 2 CH(CH 2 CH 2 ) 2 CHCH 2 , Z = CONHC 6 H 4 SO 2 CH 3 --p).
Examples 84-90 are N,N'-dioxides of the formula ##STR11##
EXAMPLE 84
Hydrogen peroxide (30%, 164 ml.) was added dropwise with stirring to a solution of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine] (51.6 g.) in alcohol (200 ml.). The temperature was maintained at about 25° C. with cooling during the addition. The solution was allowed to stand overnight at room temperature. A small amount of palladium-on-carbon was added and the mixture was allowed to stand overnight again. The mixture was filtered and the solvents were stripped from the filtrate, leaving an oil. Crystals which separated from an acetone solution of the oil were recrystallized from acetone, affording N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine]N,N'-dioxide (IV: R = CH 3 (CH 2 ) 8 , R' = CH 3 , X = (CH 2 ) 6 )(3.2 g., m.p. 168.0°-170.6° C.).
Table III shows the results of the antibacterial testing in vitro of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine]N,N'-dioxide.
Table III______________________________________ Bacteriostatic con- Bactericidal con-Microorganism centration (p.p.m.) centration (p.p.m.)______________________________________Staphylococcus 10 25aureusEberthella typhi >100 --Clotridium welchii 10 10Pseudomonas 100 >100aeruginosa______________________________________
EXAMPLE 85
In a manner similar to that of Example 84, oxidation of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyheptylamine] (20.2 g.) and two recrystallizations of the resulting product from acetone gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyheptylamine] N,N'-dioxide (IV: R = CH 3 (CH 2 ) 4 , R' = CH 3 , X = (CH 2 ) 6 ) (6.0 g., m.p. 148.0°-152.4° C.).
EXAMPLE 86
In a manner similar to that of Example 84, oxidation of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyoctylamine] (30.3 g.) and recrystallization of the resulting product from acetonitrile gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyoctylamine] N,N'-dioxide (IV: R = CH 3 (CH 2 ) 5 , R' = CH 3 , X = (CH 2 ) 6 ) (26.1 g., m.p. 143.8°-145.5° C.).
EXAMPLE 87
In a manner to that of Example 84, oxidation of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxynonylamine] and recrystallization of the resulting product from acetonitrile gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxynonylamine] N,N'-dioxide (IV: R = CH 3 (CH 2 ) 6 , R' = CH 3 , X = (CH 2 ) 6 ) (19.3 g., m.p. 155.0°-157.6° C.).
EXAMPLE 88
In a manner similar to that of Example 84, oxidation of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydecylamine] (31.7 g.) and two recrystallizations of the resulting product from acetone-methanol gave N,N'-(1,6-hexylene)-bis[N-methyl2-hydroxydecylamine] N,N'-dioxide (IV: R = CH 3 (CH 2 ) 7 , R' = CH 3 , X = (CH 2 ) 6 ) (4.0 g., m.p. 162.0°-166.0° C.).
EXAMPLE 89
In a manner similar to that of Example 84, oxidaton of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydodecylamine] (40 g.) and two recrystallizations of the resulting product from acetone-methanol gave N,N'-(1,6-hexylene)-bis(N-methyl-2-hydroxydodecylamine] N,N'-dioxide (IV: R = CH 3 (CH 2 ) 9 , R' = CH 3 , X = (CH 2 ) 6 ) (10.4 g., m.p. 163.6°-166.0° C.).
EXAMPLE 90
In a manner similar to that of Example 84, oxidation of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxytetradecylamine] (28.2 g.) and two recrystallizations of the resulting product from acetone-methanol gave N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxytetradecylamine] N,N'-dioxide (IV: R = CH 3 (CH 2 ) 11 , R' = CH 3 , X = (CH 2 ) 6 ) (8.8 g., m.p. 150.0°-155.0° C.).
Examples 91-98 are N,N'-diammonium quaternary salts of the formula ##STR12##
EXAMPLE 91
A mixture of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyundecylamine] (10 g.), methyl chloride (34 g.) and acetonitrile (30 ml.) was heated in a bomb (60°-65° C., 4 hr.). The resulting product (3.6 g.) was recrystallized from acetonitrile affording N,N'-(1,6-hexylene)-bis[N,N-dimethyl-2-hydroxyundecylammonium]dichloride (V: R = CH 3 (CH 2 ) 8 , R' = R" = CH 3 , X = (CH 2 ) 6 , Y = Cl) (7.0 g., m.p. 171.0°-174.8° C.).
Table IV shows the results of the antibacterial testing in vitro of N,N'-(1,6-hexylene)-bis[N,N-dimethyl-2-hydroxyundecylammonium]dichloride.
Table IV______________________________________ Bacteriostatic con- Bactericidal con-Microorganism centration (p.p.m.) centration (p.p.m.)______________________________________Staphylococcus 2.5 2.5aureusEberthella coli 50 50Pseudomonas 50 >100aeruginosaProteus vulgaris >100______________________________________
EXAMPLE 92
In a manner similar to that of Example 91, quaternerization of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydecylamine] (two runs, 10 g. each) with methyl chloride (40 ml. one run, 28 g. other run) and recrystallization of the combined products from acetonitrile gave N,N'-(1,6-hexylene)-bis[N,N'-dimethyl-2-hydroxydecylammonium]dichloride (V: R = CH 3 (CH 2 ) 7 , R' = R" = CH 3 , X = (CH 2 ) 6 , Y = Cl) (18.7 g., m.p. 171.0°-174.0° C.).
EXAMPLE 93
Quaternerization of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydecylamine] with methyl iodide affords N,N'-(1,6-hexylene)-bis[N,N-dimethyl-2-hydroxydecylammonium]dichloride (V: R = CH 3 (CH 2 ) 7 , R' = R" = CH 3 , X = (CH 2 ) 6 , Y = I).
EXAMPLE 94
Quaternerization of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydecylamine] with ethyl p-toluenesulfonate affords N,N'-(1,6-hexylene)-bis[N-ethyl-N-methyl-2-hydroxydecylammonium] bis(p-toluenesulfonate) (V: R = CH 3 (CH 2 ) 7 , R' = CH 3 , R" = CH 3 CH 2 , X = (CH 2 ) 6 , Y = SO 3 C 6 H 4 CH 3 --p).
EXAMPLE 95
Quaternerization of N,N'-(1,6-hexylene)-bis[N-methyl-N-propyl-2-hydroxydecylamine] with propyl bromide affords N,N'-(1,6-hexylene)-bis[N-methyl-N-propyl-2-hydroxydecylammonium] dibromide (V: R = CH 3 (CH 2 ) 7 , R' = CH 3 , R" = CH 3 (CH 2 ) 2 , X = (CH 2 ) 6 , Y = Br).
EXAMPLE 96
Quaternization of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydecylamine] with isobutyl iodide affords N,N'-(1,6-hexylene)-bis[N-isobutyl-N-methyl-2-hydroxydecylammonium] diiodide (V: R = CH 3 (CH 2 ) 7 , R' = CH 3 , R" = (CH 3 ) 2 CHCH 2 , X = (CH 2 ) 6 , Y = I).
EXAMPLE 97
In a manner similar to that of Example 91, quaternerization of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxydodecylamine] (10 g.) with methyl chloride (34 g.) and recrystallization of the resulting product from acetonitrile gave N,N'-(1,6-hexylene)bis[N,N-dimethyl-2-hydroxydodecylammonium]dichloride (V: R = CH 3 (CH 2 ) 9 , R' = R" = CH 3 , X = (CH 2 ) 6 , Y = Cl)(8.5 g., m.p. 176.6°-180.0° C.).
EXAMPLE 98
A mixture of N,N'-(1,6-hexylene)-bis[N-methyl-2-hydroxyheptylamine] (5 g.), benzyl bromide (4.7 g.) and hexane (60 ml.) was heated under reflux (for 5 hr.). Acetonitrile (20 ml.) was added and refluxing was continued (for 5 hr.). The solvents were stripped and the residue was recrystallized from ethylene dichloride, affording N,N'-(1,6-hexylene)-bis[N-benzyl-N-methyl-2-hydroxyheptylammonium]dibromide (V: R = CH 3 (CH 2 ) 4 , R' = CH 3 , R" = C 6 H 5 CH 2 , X = (CH 2 ) 6 , Y = Br) (3.5 g., m.p. 127.0 °-129.0° C.)
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N,N'-Bridged-bis[(O and/or N-substituted)-2-alkyl-2-hydroxyethylamines] of the formula ##STR1## are prepared by condensing an epoxide of the formula ##STR2## and a diamine of the formula R'NH--X--NHR'. The products and dicarbanilates, acid-addition salts, N,N'-dioxides and N,N'-diammonium quaternary salts derived therefrom have antibacterial activity in vitro and are useful as antibacterial agents.
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BACKGROUND OF THE INVENTION
The invention concerns a calender, in particular a supercalender, on whose frame a set of rolls is mounted, which is shaped as a stick of rolls placed one above the other and which comprises an upper roll, a lower roll and several intermediate rolls placed between the upper roll and the lower roll, the rolls being supported on the frame by the intermediate of the base parts as vertically displaceable along guides provided in the frame, of which at least the base parts of the intermediate rolls can be positioned in the vertical direction by means of lifting spindles provided in the frame and by means of spindle nuts provided on the spindle.
The system of rolls in a conventional supercalender comprises a number of rolls, which are arranged one above the other as a stack of rolls. The rolls placed one above the other are in nip contact with each other, and the paper web to be calendered is arranged to run through the nips between the rolls. The rolls in the system of rolls are normally mounted rotatably in bearing housings, which are again attached to base parts that are fitted to glide on vertical guides provided in the frame of the calender. Moreover, the base parts are provided with stop parts, which are fitted on vertical lifting spindles provided in the frame of the calender. Thus, one of the functions of the lifting spindles is to act as guides so as to keep the rolls in the system of rolls in the correct position. Thus, the bearing housings of the rolls in the system of rolls are not fixed rigidly to the calender frame, but the bearing housings, and consequently also the rolls, can move vertically. Since the masses of the bearing housings of the rolls and the auxiliary devices attached to the housings are quite large, in conventional supercalenders this causes the considerable drawback that these masses of the bearing housings and of the auxiliary devices attached to the bearing housings cause distortions in the distributions of the linear loads in the nips Thus, the linear load in the nips is not uniform, but it is substantially higher at the ends of the nips than at the middle. Since in the systems of rolls of supercalenders there are several rolls placed one above the other, as was already stated above, this further results in the linear loads in individual nips being cumulated and causes a considerably large error in the overall linear load. This defective distribution of the linear load deteriorates the quality of the calendered paper.
With a view to solving the problem described above, in the Applicant's earlier FI patent application No. 880137 it is suggested that the system of rolls be provided with lightening devices, which are supported on the base parts of the rolls, on one hand, and on the spindle nuts provided on the lifting spindles, on the other hand, so that by means of these lightening devices, the distortions caused by the weight of the bearing housings and of auxiliary devices attached to the housings, e.g. takeoff rolls, in the lateral areas of the profiles of linear loads between the rolls can be eliminated. Also, for conventional machine calenders, a solution is known in the prior art wherein the rolls of the machine calender are provided with a lightening system, in particular with hydraulic lightening cylinders for elimination of concentrated loads arising from the bearing housings of the rolls and from auxiliary devices. It is a simple matter to provide machine calenders with such relief devices, because the rolls in the system of rolls of a machine calender are mounted on the frame of the calender by the intermediate use of levers with articulated joints. It is, however, quite difficult to use devices corresponding to the machine calenders in supercalenders because of the constantly varying diameters of the fiber rolls and because of the large number of rolls in supercalenders.
Owing to their construction, which was described above, conventional supercalenders also have a further drawback, which is concerned with the vertical movement of the rolls in the system of rolls. As was already explained above, the bearing housings of the rolls in the system of rolls are mounted on base parts, which is vertically mobile along glides provided in the frame of the calender. This further drawback is related to the friction at the guides, which is effective between said guides and the base parts. Under these circumstances, owing to the friction at the guides, the rolls in the system of rolls cannot move or be positioned in the vertical direction completely freely, which may cause disturbances in the operation of the calender as well as considerable local errors in the distributions of the linear loads. With a view to eliminating the frictions at the guides, in supercalenders it would be possible to think of using the solution described above, commonly known from machine calenders, wherein the rolls are mounted on the calender frame by the intermediate use of lever systems provided with articulated joints. The use of such an arrangement in supercalenders is, however, limited by the fact that the system of rolls in a supercalender includes several fiber rolls, whose diameter may vary to a considerable extent. Thereby, owing to the variations in the diameters of the rolls, the rolls must be able to move vertically to a considerable extent. If the rolls were mounted to the frame of the calender by the intermediate structure of lever systems with articulated joints, in such a case a vertical shifting of the rolls would also cause a considerable shifting in the transverse direction.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a solution by means of which the above drawbacks found in the prior art are avoided, especially in connection with supercalenders. A more specific object of the invention is to provide a solution by whose means friction at the guides can be eliminated and by whose means the journal loads arising from the bearing housings and from auxiliary equipment in the system or rolls can be relieved so as to align the distribution of the linear loads. With a view to achieving this, and other objects of the invention which will become apparent hereinafter the invention is mainly characterized in that the base parts of the intermediate rolls are supported on the lifting spindles as vertically displaceable by means of pressure-medium operated relief devices arranged between the base parts and the spindle nuts to reduce the journal loads on the rolls and that the bearing housings of the intermediate rolls are attached to the base parts as pivotable relative to an articulation shaft parallel to the axes of the rolls and supported on the base parts and/or on the calender frame by means of attenuation devices so as to equalize the forces resulting from movements of the nips between the rolls and to attenuate oscillation of the rolls.
Of the advantages of the invention as compared with the prior art solutions, among other things, the following should be stated. By means of the solution of the invention, the profiles of linear loads in the nips in the system of rolls can be made even, owing to which the quality of the calendered paper becomes better and more uniform across the entire width of the paper web. Moreover, by means of the solution in accordance with the invention, disturbances resulting from friction at the guides for the operation of the calender can be eliminated. Further, by means of the solution in accordance with the invention, the tendency of detrimental oscillations to occur in the rolls in the system of rolls can be reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematical side view of a calender provided with an apparatus in accordance with the invention, with the system of rolls closed.
FIG. 2 shows a calender as shown in FIG. 1, with the system of rolls opened.
FIG. 3 is an enlarged view of a detail of FIG. 1.
FIGS. 4 to 6 show embodiments alternative to the solution shown in FIG. 3.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1 and 2 are schematical illustrations of a supercalender, whose frame is denoted with the reference numeral 1 and the system of rolls with the reference numeral 2. To further clarify the illustration, in FIGS. 1 and 2, the auxiliary devices included in the calender, such as takeoff rolls and their equivalent, have been omitted. As is shown in FIGS. 1 and 2, the system or rolls 2 in the supercalender comprises an upper roll 3, a lower roll 4, as well as a number of intermediate rolls 5 arranged one above the other between the upper roll and the lower roll, these rolls being arranged in such a way that they are in nip contact with one another. In the usual way, the upper roll 3 is provided with an upper cylinder 32 placed at each end of the roll and attached to the frame 1 of the calender, the piston 33 of said upper cylinder 32 acting upon the bearing housing 31 of the upper roll so as to load the system or rolls 2 to reach the desired level of linear load. In the usual way, the lower roll 4 is also provided with a lower cylinder 45 placed at each end of the roll, the piston 46 of said lower cylinder 45 acting upon the bearing housing 44 of the lower roll. By means of the lower cylinders 45, the system of rolls 2 can be opened in the usual way. In FIGS. 1 and 2 it is shown that the lower roll 4 is a variable-crown roll, which comprises a revolving roll mantle 41, which is supported in the nip plane on a non-revolving roll axle 42 by means of hydraulic loading members 43 The lower roll 4 is a so-called floating roll, whose roll mantle 41 can move in the direction of the nip plane in relation to the roll axle 42. The intermediate rolls 5 in the system of rolls 2, of which only the lowest intermediate roll is provided with detailed reference numerals in FIGS. 1 and 2, are at both of their ends mounted rotatably in bearing housings 51.
In the normal way, the calender frame 1 is provided with guides 7 as well as, at each side of the calender frame, with lifting spindles 6. The drive gear of the lifting spindle 6, which is placed in the top portion of the frame 1 in the customary way and by means of which the lifting spindle 6 is rotated and displaced in the vertical direction, is not shown in the figures in the drawing. Thus, when the lifting spindle 6 is rotated by means of the drive gear, at the same time it moves a certain distance upwards or downwards. The bearing housing 31 of the upper roll 3 is attached to the base part 34 of the upper roll, which is arranged to be displaceable along the guide 7 in the vertical direction. The base part 34 is provided with a stop part 35, through which the lifting spindle 6 extends and which stop part 35 moves on the spindle 6 in a longitudinal direction. On the lifting spindle 6, below the stop part 35, a spindle nut 36 is fitted, which is, in the situation shown in FIG. 1, when the system of rolls 2 is closed, placed at a distance of the gap b from the stop part 35.
On the contrary, the bearing housings 51 of the intermediate rolls 5 are attached to the base parts 54 of the intermediate rolls pivotally by the intermediate of lever parts 52 and articulation shafts 53. These base parts 54 of the intermediate rolls 5 are also arranged on the frame 1 of the calender as vertically displaceable along the guides 7. In a way corresponding to the base part 34 of the upper roll 3, the base parts 54 are provided with stop parts 55, through which the lifting spindle 6 extends. Underneath the stop parts 55, at a distance from them, spindle nuts 56 are fitted on the spindle 6. Each spindle nut 36, 56 is advantageously provided with an adjustable friction member, by means of which adequate friction is provided between the spindle nuts 36, 56 and the lifting spindle 6. Moreover, each spindle nut 36, 56 is provided with a locking device (not shown), by whose means, when necessary, the corresponding spindle nut 36, 56 can be locked in its position. When the spindle nut 36, 56 is not locked by means of the locking device, the spindle nut revolves, when the lifting spindle 6 is rotated, by the effect of the friction member of the spindle nut 36, 56, along with the lifting spindle 6. On the contrary, when locked, the spindle nut 36, 56 remains in its position when the lifting spindle 6 revolves. The locking device (not shown) may be, e.g., a dual-action pneumatic cylinder, by means of which the corresponding spindle nut 36, 56 can be locked as non-revolving when necessary. Between the stop parts 55 provided in the base parts 54 of the intermediate rolls 5 and the spindle nuts 56, a pressure-medium operated relief device 57 is provided, whose construction is also shown in more detail in FIGS. 3 to 6.
The relief device comprises a body 57, which is arranged to be mounted on the spindle nut 56. Above the body 57, a plate 58 is fitted, which reaches contact with the lower face of the stop part 55. The body 57 of the relief device is provided with pressure-medium operated power units 59, the plate 58 being raised apart from the body 57 by feeding a pressure medium into the power units 59. The power units 59 comprise cylindrical bores formed into the body 57 of the relief device, into which bores pistons have been fitted which are directed upwards and which rest against the lower face of the plate 58 placed above the body 57 of the relief device.
In FIG. 1 a situation is shown wherein the system of rolls 2 of the calender is closed, i.e. the nips N 1 . . . N 4 are closed, and correspondingly FIG. 2 shows a situation wherein the nips N 1 . . . N 4 are opened, e.g., for replacement of a roll, in which case there are gaps a, c between the rolls 3,4,5 in the system of rolls. When the system of rolls 2 is closed, there is a gap b between the stop part 35 of the upper roll 3 and the spindle nut 36, this gap being closed in accordance with FIG. 2 when the system of rolls 2 is opened. When the system of rolls is in the closed position, the power units 59 are in operation, i.e. a hydraulic/pneumatic pressure medium has been fed into them so that the pistons of the power units 59 push the plates 58 upwards and against the stop parts 55.
In order that an equally large gap a could be obtained between the upper roll 3 and the uppermost intermediate roll 5 and, on the other hand, between the other intermediate rolls when the system of rolls 2 is in the opened position, the stroke lengths of the pistons in the power units 59 have been chosen so that, as is shown in FIG. 1, the stroke length in the power units 59 of the uppermost intermediate roll 5 has a magnitude of b+a, and in the subsequent intermediate rolls 5 the stroke length is always by the dimension a larger as compared with the preceding intermediate roll 5. This comes from the circumstance that instantaneous opening of the system of rolls 2 is carried out exactly by means of the power units 59 discharging the pressure out of the power unit and by means of the lower cylinder 45, lowering the lower roll 4 while the base part 47 of the lower roll glides down along the guide 7. Since the bearing housings 51 of the intermediate rolls 5 are attached to the base parts 54 by means of the lever parts 52 and the pivot shafts 53 with articulated joints, attenuation devices 10 are provided between said lever parts 52 and the base parts 54, said attenuation devices 10 supporting the lever parts 52 in relation to the base parts 54 during running. A first embodiment of the attenuation devices 10 is illustrated in FIGS. 1 to 3, and their operation and significance for the invention will be described in more detail later.
In this connection it should, however, be ascertained that, when the system of rolls 2 is opened, the pressure is discharged out of the attenuation devices 10 of the type of a cylinder-piston device. Thereby, when the system of rolls 2 is opened, the base parts 54 of the intermediate rolls 5 rest completely on the spindle nuts, and the lever parts 52 are pivoted down around the articulation shaft 53 so that the bottom edge of the lever part 52 reaches contact with the base part 54, which, thus, operates as a limiter of the pivoting of the lever part 52. In the figures in the drawing, the gap between the bottom edge of the lever part 52 and the base part 54 has been exaggerated. From the opened position the system of rolls 2 is closed so that first the system of rolls 2 is run into the closed position by means of the lower cylinder 45, whereupon the attenuation devices 10 and the power units 59 are pressurized.
For the purpose of regulation of the system of rolls 2, it is necessary to make the spindle nuts 56 free in order that the lifting spindle 6 could be rotated. In a calender in accordance with FIGS. 1 and 2 this is accomplished so that the pressure is released out of the upper cylinder 32 and out of the power units 59, whereupon the bearing housings 44 of the lower cylinder and the whole roll 4 are raised by means of the lower cylinders 45. It is also possible that the roll mantle 41 is raised in relation to the axle 42 by means of the loading members 43 of the lower roll 4. The attenuation devices 10, which are of the cylinder-piston type in the embodiment of FIG. 1, are not affected in this state, but they are kept under pressure. Thereby the intermediate rolls 5 rise one at a time so that first the lever parts 52 pivot around the articulation shafts 53 upwards until the upper edges of the lever parts 52 reach contact with the base parts 54, whereby the base parts 54 rise along with the rolls 5. The relief devices 57 are provided with members which prevent falling down of the body parts 57 of the relief devices when the power units 59 are free of pressure. Thus, these body parts 57 rise along with the base parts 54 off the top of the spindle nuts 56, whereby it is possible to adjust the lifting spindle 6.
After the regulation has been completed and when the whole system of rolls 2 is together, pressures are admitted into the power units 59, and the mantle 41 of the lower roll is lowered somewhat. Thereby, the power units 59 keep the base parts 54 in their positions, and the lever parts 52 pivot around the articulation shafts 53 downwards so that gaps are formed between both the upper edges and the lower edges of the lever parts 52 and the base parts 54. In such a situation the centers of the intermediate rolls 5 are in a horizontal plane substantially at the level of the articulation shafts 53.
Since the base parts 54 move along with the intermediate rolls 5 both in connection with the raising and in connection with the opening of the system of rolls 2, the change in the angles of the lever parts 52 in relation to the base parts 54 is quite little. Moreover, this change in the angle is substantially equally large in the case of all intermediate rolls 5, so that the intermediate rolls 5 remain in line with each other. In supercalenders, commonly an abundance of steam is used, which is supplied through steam-moistening pipes into nips or into pockets formed by the paper web, rolls, and the takeoff. However, steaming has the drawback that it promotes gathering of dirt in the constructions of a calender, e.g. the guides 7. This might result, e.g., in jamming of the base parts 54 in the guides 7. Since, in the solution in accordance with the invention, the base part 54 moves constantly along with the roll 5 when the system of rolls 2 is being opened and regulated, such jamming cannot occur.
As was already ascertained once above, attenuation devices 10 are arranged to be effective between the lever parts 52 and the base parts 54 of the intermediate rolls 5, these attenuation devices 10 supporting the bearing housing 51 in relation to the base part 54. In the embodiment shown in FIGS. 1 to 3, the attenuation device comprises a preferably hydraulic or pneumatic cylinder-piston device, which, by the effect of the pressure medium, produces a force that pivots the bearing housing 51 relative to the articulation shaft 53, by means of which force the loads arising from the bearing housing 51 and from a takeoff roll possibly attached to same are relieved, which forces would, in the contrary case, attempt to deflect the profile of the roll 5, because the loading of the roll 5 would be higher in the lateral areas of the roll than in the middle part. The journal loads arising from the base parts 54 on the rolls are additionally relieved by means of a power unit 59, by whose means the base part 54 is raised in relation to the spindle nut 56. In addition to the relieving of the journal loads, the attenuation device 10 attenuates and equalizes the forces and oscillations arising from the movements of the nips N 1 . . . N 4 efficiently.
FIG. 4 shows an embodiment alternative to the solution shown in FIG. 3. In the solution shown in FIG. 4, double attenuation devices 20 are fitted between the lever part 52 and the base part 54 of the intermediate roll 5 at opposite sides of the articulation shaft 53, these devices 20, thus, acting upon the bearing housing 51 so as to pivot it in opposite directions relative to the articulation shaft 53. The solution shown in FIG. 4 is highly advantageous, because by means of the attenuation member placed below the articulation shaft 53, a relieving of the journal loads is obtained that is similar to that described above in relation to FIG. 3. In the solution shown in FIG. 4, the attenuation member 20 placed above the articulation shaft 53 operates as a highly efficient attenuator of oscillation, which equalizes the forces arising from movement of the nip and attenuates oscillations.
In the embodiment shown in FIG. 5, the cylinder-piston devices 10, 20 shown in FIGS. 3 and 4 have been substituted for by attenuation members 60 fitted between the lever part 52 and the base part 54, which are preferably made of an elastic material. Thus, the solution shown in FIG. 5 is simpler and has a lower cost of manufacture as compared with the embodiments shown in FIGS. 3 and 4. In the embodiment shown in FIG. 5, in respect of their material and physical properties, the attenuation devices 60 have been manufactured so that, when the base part 54 has been placed at the correct level in relation to the spindle nut 56 by means of the power units 59, the lower attenuation member 60 in FIG. 5, when compressed, produces a sufficiently high force by means of which the journal loads on the roll 5 are relieved. In the solution shown in the figure, the upper attenuation member 60 operates exclusively as an attenuator of oscillations.
It is possible to depart from the embodiment of FIG. 5 so that the upper attenuation member 60 is omitted completely. This procedure is possible particularly when no large external forces are supported on the bearing housing 51, but the bearing housing 51 carries the roll 5 only. Moreover, it is possible to combine the embodiments shown in FIGS. 3, 4, and 5, for example, so that the attenuation device below the articulation shaft 53 is, e.g., a cylinder-piston device 10 shown in FIG. 3, whereas the upper attenuation device is an attenuation member 60 shown in FIG. 5 this member being, in such a case, functional to attenuate oscillations.
FIG. 6 shows a further embodiment, which differs from those described above in the respect that in this embodiment the attenuation device 70 is supported on the lever part 52 at one end, and on the front face 8 of the guide 7 at the opposite end. In respect of its operation and construction, the attenuation device 70 may be, e.g., a cylinder-piston device corresponding to the attenuation device 10 shown in FIG. 3. In the embodiment shown in FIG. 6, it is also possible to install an attenuation member similar to that shown in FIG. 5 above the articulation shaft 53 between the lever part 52 and the base part 54.
To summarize the above, the following can be stated. By means of the relief devices 57 fitted between the base parts 54 of the intermediate rolls 5 and the spindle nuts 56, relieving of the journal loads applied to the intermediate rolls can be carried out efficiently and, moreover, by means of said relief devices 57, an instantaneous opening of the system of rolls 2 is carried out in the way described above. The loads arising from the bearing housings 51 and from additional loads that may be supported on them, such as takeoff rolls, are relieved in the solution in accordance with the invention by means of attenuation devices 10, 20, 60 fitted between the base part 54 and the lever part 52. This relieving can also be arranged so that the attenuation device 70 is arranged between the lever part 52 and the calender frame 1.
During operation, i.e. when the system of rolls 2 is in the closed position, the base parts 54 of the intermediate rolls 5 are kept in their positions in relation to the spindle nuts 56 by means of relief devices 57. On the contrary, during raising and lowering of the system of rolls 2, the base parts 54 move along with the rolls 5. Raising of the system of rolls 2 for the purpose of regulation of the system of rolls can be arranged, with the solution in accordance with the invention, by means of a lower roll 4 of the floating type, and instantaneous opening of the system of rolls 2 is carried out by means of the relief device 57, as was stated above.
Above, the invention has been described by way of example with reference to the figures in the accompanying drawing. This is, however, not supposed to restrict the invention to the exemplifying embodiments illustrated in the figures along, but many variations are possible within the scope of the inventive idea defined in the accompanying patent claims.
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The invention concerns a calender, in particular a supercalender, on whose frame (1) a set of rolls (2) is mounted, which comprises an upper roll (3), a lower roll (4), and several intermediate rolls (5) placed between the upper roll and the lower roll. The rolls (3, 4, 5) are supported on the frame (1) by the intermediate structure of the base parts (34, 47, 54) being vertically displaceable along guides (7) provided in the frame. Of the base parts, at least the base parts (54) of the intermediate rolls can be positioned in the vertical direction by means of lifting spindles (6) provided in the frame (1) and by means of spindle nuts (56) provided on the spindle. The base parts (54) of the intermediate rolls are supported on the lifting spindles (6) being vertically displaceable by means of pressure-medium operated relief devices (57) arranged between the base parts (54) and the spindle nuts (56) to reduce the journal loads on the rolls (5). The bearing housings (51) of the intermediate rolls are attached to the base parts (54) being pivotable relative to an articulation shaft (53) parallel to the axes of the rolls (3, 4, 5) and supported on the base parts (54) by means of attenuation devices (10) to equalize the forces resulting from movements of the nips (N 1 , N 2 , N 3 , N 4 ) between the rolls and to attenuate oscillations of the rolls (5).
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This application is a divisional application of U.S. patent application Ser. No. 12/495,914, filed Jul. 1, 2009, the disclosure of which is herein incorporated by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates to a composition that improves recovery of aluminum values from the aluminum hydroxide production process such as the Bayer process. In particular, the invention relates to the compositions and methods providing the increase of particle size of aluminum hydroxide product.
BACKGROUND OF THE INVENTION
Aluminum hydroxide is produced on an industrial scale by well-established methods such as the Bayer process. The precipitation process operators optimize their methods so as to produce the greatest possible yield from the aluminate process liquors while trying to achieve a particular crystal size distribution of aluminum hydroxide product. It is desirable in most instances to obtain the product of relatively large crystal size and to correspondingly limit the amount of very fine crystals since this is beneficial in subsequent processing steps required to produce aluminum metal. Production is often limited by processing conditions under which the crystallization and precipitation is conducted. These processing conditions vary from one plant to the next and include, but are not limited to, temperature profiles, seed charge, seed crystal surface area, purge of carbon dioxide or flue gases, liquor loading, liquor purity, and the like.
Extensive efforts have been invested into finding chemical additives and methods limiting the factors negatively affecting particle size in order to achieve the optimal economic recovery of aluminum hydroxide product.
Despite the continuous and ongoing development worldwide, the industry demands for more economical resolution of the above-described process needs remain. A method of such resolution suitable for obtaining aluminum hydroxide crystals with increased particle size is provided by the present invention.
SUMMARY OF THE INVENTION
To satisfy the industry needs identified above, a method and compositions for obtaining aluminum hydroxide crystals with increased particle size have been developed.
According to the method of the present invention, the suitable compositions are blended and introduced into the process in an amount effective to obtain the changes desired. The compositions are introduced in their primary form without any further preparation.
The principal embodiment of the present invention is a crystal growth modifier composition represented by an emulsion having hydrocarbon oil content of more than 15%. The other key ingredient of such an emulsion is a surfactant, or a blend of surfactants, with the remaining ingredient being water.
DETAILED DESCRIPTION OF THE INVENTION
The following are definitions that apply to the relevant terms as used throughout this specification.
A: Stands for aluminum concentration expressed as g/L Al 2 O 3
C: Stands for sodium hydroxide or caustic concentration expressed as g/L Na 2 CO 3
S: Stands for total alkali concentration expressed as g/L Na 2 CO 3
A/C: Refers to the alumina to caustic ratio
CGM: This acronym stands for “crystal growth modifier.”
Oil carrier: Describes a hydrophobic liquid that can be comprised of the aliphatic or aromatic compounds such as paraffinic oils, naphthenic oils, or fuel oils.
Also, bottoms or residual waste materials remaining from the production of aliphatic alcohols represent a suitable hydrophobic liquid.
The materials suitable as an oil carrier can be used neat or as a mixture of any proportion. The oil carrier needs only be a solvent for the surfactant or blend of surfactants and have a boiling point safely above the temperature of the hot aluminate liquor undergoing precipitation (about 80° C., 176° F.).
Weight percent ratio: The total weight fraction of one reagent within 100 grams of the composition or mixture.
Increase in Percent+45 μm fraction (−325 mesh): The response in all samples is the increase in the percent+45 μm fraction of the alumina trihydrate product (the size commonly monitored across the industry). The greater the increase, the better the CGM performance in producing the large size crystals.
Effective amount: An effective amount is deemed any dosage of any additive that affords an increase in the particle size distribution as measured by a change in the percent+45 μm fraction of the alumina trihydrate product.
Precipitation liquor: Refers to aluminate containing liquor in an aluminum hydroxide precipitation step of an alumina production process. The aluminate liquor may be referred to as various terms known to those of ordinary skill in the art, for example, pregnant liquor, green liquor, and aluminum hydroxide precipitation feed. The Bayer process is one example of an alumina production process.
The term precipitation liquor may also include the aluminate solution directed to decomposition in a sintering-carbonation process or combined Bayer-sintering process as accomplished by the methods well known to those skilled in the art as described, for example, in U.S. Pat. Nos. 4,256,709 and 3,642,437, and RU Pat. Nos. 2,184,703, 2,257,347, and 2,181,695, which are herein incorporated by reference.
As described in U.S. Pat. No. 4,737,352, assigned to Nalco, the invention in practice is unaffected by different proprietary precipitation techniques involving proprietary process parameters. This is of great significance because it establishes that regardless of the proprietary processing parameters maintained inside the precipitating tank, the present invention for actual practice only requires blending of the proposed treatment.
Precipitation feed liquor: refers to the precipitation liquor that flows into a precipitator of an aluminum hydroxide precipitation process.
While the invention is susceptible of embodiment in many different forms, this disclosure will describe in detail preferred embodiments of the invention with the understanding that the present disclosure is to be considered as an exemplification of the principles of the invention and is not intended to limit the broad aspect of the invention to the embodiments illustrated.
The CGM emulsions of the present invention incorporate three basic ingredients:
A1: Surfactant or a blend of surfactants
A2: Oil carrier in the amount greater than 15%.
A3: Water.
Additional components may also be present in various concentrations however these three basic components constitute the key ingredients for such CGM emulsions.
The preferred surfactant in Ingredient A1 is tall oil fatty acid, but there are a host of equivalents. Thus, the surfactant may be a fatty acid having at least a saturated or unsaturated four carbon alkyl backbone, with or without one or more carboxylic acid, ester, anhydride or sulfate surfactant functional groups attached directly or by a succinic alkyl linkage. Advantageously the fatty acid may contain at least an eight-carbon backbone with at least one of the above functional groups attached.
Ingredient A1 may include C8-C35 unsaturated or saturated fatty acids with a straight or branched carbon chain or their blends.
Among the unsaturated acids preferable are palmitoleic, oleic, linoleic, linolenic, ricinoleic, eleostearic, docosahexaenoic acids, elcosapentaenoic acid, and the likes. Any combination of the unsaturated monobasic acids listed above may be used. Among the saturated fatty acids the acids with a straight chain are preferred, such as octadecanoic (stearic) acid, hexadecanoic (palmitic) acid, octadecanedioic acid and hexadecandioic acid, their blend, or blends with other saturated (and/or unsaturated) fatty acids with the hydrocarbon chains of 8-35 carbon atoms. In the formulations, the fatty acids can also be used as their esters with C1-C4 alcohols, including but not limited to methyl ester or ethyl esters.
Additionally, natural esters of the fatty acids can be utilized as Ingredient A1, which include crude or processed triglyceride oils of vegetable or animal origin such as soybean oil, linseed oil, castor oil, dehydrated castor oil, corn oil, safflower oil, sunflower oil, canola oil, fish oils, lard oil, beef oil, oiticica oil, tung oil, and tall oil, or their combinations. The suitable processed oils can be those processed by means of refining, heat polymerization, isomerization-conjugation, boiling, blowing, epoxidation, dehydration, copolymerization with ethylenic monomers selected from but not limited to the group of acrylate, methacrylate, styrene, acrylamide, acrylonitrile, vinyl carboxylate esters and vinyl halides, mixtures thereof, and salts thereof. In an exemplary embodiment, the suitable oils may be the crude and refined oils available, for example, from Archer Daniels Midland Company, Decatur, Ill., USA; blown, and boiled plant oils available, for example, from Cargill Inc., Minn., USA; epoxidized oils available, for example, under the trade name Vikoflex® from ATOFINA Chemicals, Inc., Pa., USA; dehydrated castor oil available, for example, under the trade name Castung from G.R. O'Shea Company, Ill., USA; acrylated soybean oil available, for example, from Sartomer Company, Pa., USA.
The fatty acid amides of Ingredient A1 are preferably represented by the condensation products of fatty acids with alkyl polyamines. The suitable alkyl polyamines can be exemplified by but are not limited to ethylene diamine, diethylene triamine, and triethylene tetramine.
Ingredient A1 may also comprise other ionic and nonionic surfactants or mixtures of thereof. The ionic surfactants may include anionic, zwitterionic, and cationic surfactants.
In an exemplary embodiment one may assist the formation of instant emulsions by “salting out” the hydrolysable surfactants of Ingredient A1 using a base, such as ammonia, amine, or alkali, whereby increasing the pH of the emulsion formulation to higher than 7.
A co-solvent may be added to the present emulsions to increase their stability. The suitable co-solvents can be selected from the group that includes but is not limited to polyoxyalkylene homopolymers and copolymers, straight chain or branched mono and polyhydric aliphatic or aromatic alcohols, and their monomeric, oligomeric, or polymeric alkoxylates.
In the principal embodiment of the present invention, the instant CGM compositions are prepared as water-in-oil or oil-in-water emulsions.
For a successful application, CGM composition must be homogeneously distributed in the precipitation environment to ensure its unimpeded contact with the fine particulate. Traditional waterless CGM formulations are prepared as solutions of functional ingredients in an oil carrier. The oil carrier is essential for helping distribute the CGM product in the green liquor or seed slurry stream. Still, to homogeneously blend an oil formulation into water based precipitation liquor significant mechanical energy is required. In this way, the emulsions of the present invention have a distinct advantage over the waterless formulations. The functional ingredients of these emulsions are already dispersed in water environment due to chemical forces. These chemical forces aid the mechanical forces to faster and more uniformly distribute the CGM product within the process stream. The availability of these chemical forces makes it also possible to reduce the amount of carrier oil present in CGM formulations without sacrificing performance. This in turn is beneficial for the plants concerned with the amount of external hydrocarbons added to their precipitation circuit.
Longer chain saturated fatty acids, such as stearic acid, are solid at room temperature and thus difficult to formulate into a liquid. The same applies to other suitable materials such as fatty amides that are not water or oil soluble, but when used in emulsion can be incorporated into a CGM product in a broad range of concentrations.
The instant CGM formulations prepared as microemulsions are preferred. Microemulsions are significantly different in structure from regular emulsions. Regular emulsions are comprised of separate oil droplets in water or water droplets in oil with a sharp transition between the two phases. Microemulsions have a particle size in the range from 10 to 600 nm, so that they appear as clear or opalescent one-phase formulations.
Unlike regular emulsions, microemulsions are thermodynamically stable. This means that microemulsions form spontaneously when the components are brought together and stay stable as long as the components are intact. Thus, their manufacturing may be reduced to simple kneading without the need for expensive high energy mixing. Also, microemulsions are not prone to separation or settling, which results in their long storage stability. Only gentle mixing is required to restore microemulsions upon their freezing or high temperature exposure.
The emulsions of the present invention are designed to incorporate more than 15% oil carrier. Earlier investigators, e.g., U.S. Pat. No. 6,168,767, found that CGM compositions can be prepared from blends of surfactants that may contain water but preferably contain substantially no water, while incorporating not more than 15% by weight of oil carrier. A thorough investigation of this contention is presented in the examples below. It reveals that the presence of more than 15% oil carrier is essential for a high performance of a CGM formulation.
The emulsified crystal growth modifier may be introduced into the precipitation liquor via various routes. In one embodiment, the emulsified crystal growth modifier is added to the precipitation liquor at the following steps of a Bayer process: a) to a precipitation feed liquor, b) to a seed slurry or other input stream to a precipitation tank, c) directly into a precipitation tank, and d) a combination thereof.
The emulsified crystal growth modifier can be added to the precipitation liquor via various modes of addition such as an in-line injection of the composition.
The amount of crystal growth modifier required to produce desirable effect depends upon the precipitation process parameters. Most often, this amount is determined by the surface area of available hydrated alumina solids in the precipitation liquor. The solids comprise the aluminum hydroxide introduced as seed or originated as new crystals or agglomerates during the decomposition of precipitation liquor. The suitable amount of crystal growth modifier can range from about 0.01 to about 30 mg per square meter of the available aluminum hydroxide seed area, and preferably, from about 0.1 to about 15 mg per square meter. Commonly, less than about 8 mg per square meter of CGM can be used.
In case the available aluminum hydroxide area may not be reliably determined, the precipitation operators can dose the crystal growth modifier in relation to liquor flow by volume. In this case, the crystal growth modifier amount may range from about 0.01 to about 400 mg/liter of precipitation liquor, preferably from about 0.05 to about 200 mg/liter of precipitation liquor. Commonly less than about 100 mg/liter of CGM can be used.
The addition of the crystal growth modifier product to the precipitation liquor reduces the percent of alumina trihydrate crystal fines formed in the Bayer process substantially and thereby increases the yield of alumina trihydrate crystals of optimal particle size.
The examples below are offered to aid in understanding the present invention and are not to be construed as limiting the scope thereof.
EXAMPLES
The foregoing may be better understood by reference to the following examples, which are intended to illustrate methods for carrying out the invention and are not intended to limit the scope of the invention.
Precipitation Test Procedure:
Each set of tests was run using either fresh pregnant liquor obtained from an alumina plant or using reconstituted pregnant liquor prepared by adding alumina trihydrate the plant spent liquor. Typical starting A/C ratio for liquors used in all tests was in the range 0.66-0.72 to 0.66-0.75.
All precipitation tests were performed in 250-mL Nalgene® bottles rotated end-over-end, at approximately 10-15 rpm, in an Intronics temperature-controlled water bath. Approximately 200 mL of liquor was accurately weighed into a series of bottles. The additive, where required was dosed to the appropriate bottles and all the bottles were then placed in the rotating bath for equilibration at the given test temperature (˜20 minutes). After equilibration, the bottles were removed, quickly charged with the required quantity of seed and immediately returned to the water bath. The bottles were rotated for the given test duration.
On completion of the test, the bottles were removed from the bath and 10 mL of a sodium gluconate solution (400 g/L) was added to the remaining slurry and mixed well to prevent any further precipitation. The solids were collected by vacuum filtration and were thoroughly washed with hot deionized water and dried at 110° C. The particle size distribution was determined on a Malvern Particle Sizer using a method of laser diffraction that is well known in the art. The effect of CGM on the particle size distribution is inferred from the increase of the percent of particles sized greater than 45 μm in the precipitation product relatively to an undosed control sample.
Example 1
The tests used the precipitation procedure as described above. The liquor was fresh pregnant liquor with A/C=0.711. The CGM dose was 50 ppm. The charge of the standard seed was 75 g/L. The seed was DF225 alumina trihydrate obtained from R.J. Marshall Company, Southfield, Mich. The five-hour test was conducted at 75° C.
Table 1 lists the composition and performance of the instant microemulsions employing different amounts of oil carrier. The surfactant, oil and other components are the same for all formulations listed. The %+45 μm fraction data listed is the average of triplicate samples.
TABLE 1
Effect of increasing oil content on the
performance of CGM emulsion formulations.
Composition
Other
Treatment
Surfactant
Oil
Water
components
% + 45 μm
Undosed Control
60.2
Emulsion A
15
0
71
14
62.2
Emulsion B
15
15
56
14
65.2
Emulsion C
15
30
41
14
67.7
Emulsion D
15
45
26
14
67.3
Emulsion E
15
60
11
14
67.4
The results indicate that Emulsion A employing no oil carrier provides the lowest increase in %+45 μm fraction relative to the undosed control sample and as a result is the least active CGM formulation. Surprisingly, the oil, despite having no activity in coarsening trihydrate precipitation when used alone, results in increased CGM activity when emulsion formulations contain increased concentrations of oil.
Example 2
This example demonstrates that maximizing the amount of oil component by eliminating the water content of the formulation (formulation 1) results in an effective CGM that increases the %+45 μm fraction relative to the undosed control sample. However, emulsion formulas containing significantly less oil but having the three vital components of surfactant, oil and water in appropriate proportions are found to be equally effective.
All emulsions in this example were prepared as clear microemulsions comprised of the same surfactant, oil and additional components. The waterless formulation 1 also used the same surfactant and oil as that used in the emulsions.
The tests used the precipitation procedure as previously outlined. The liquor was fresh pregnant liquor, A/C=0.707. The CGM dose was 50 ppm. The test was conducted using the same seed type and charge, holding time, and temperature as in Example 1. The %+45 μm fraction data listed is the average of triplicate samples.
TABLE 2
Performance of Emulsions as compared
to a Waterless Formulation.
Composition
Other
Treatment
Surfactant
Oil
Water
components
% + 45 μm
Undosed Control
65.3
Formulation 1
15
85
0
0
71.2
Emulsion F
15
20
41
24
71.5
Emulsion G
15
20
36
19
71.2
Example 3
A series of CGM emulsion compositions were tested under the same conditions as in the previous example using a different batch of fresh pregnant liquor, A/C=0.707. The test was conducted using the same seed type and charge, holding time, and temperature as in Example 1. The %+45 μm fraction data listed in Table 3 is the average of triplicate samples.
Table 3 presents the compositions of the emulsions as compared to the waterless Formulation 2. The emulsions were prepared using a different surfactant to that used in the waterless Formulation 2. However, despite the lower oil content the emulsion formulas are shown to be equal to or more effective at coarsening the precipitated product, resulting in a greater increase in the %+45 μm fraction compared to the undosed control sample.
TABLE 3
Performance of Emulsions as compared to a Waterless formulation.
Composition
Other
Treatment
Surfactant
Oil
Water
components
% + 45 μm
Undosed Control
67.0
Formulation 2
15*
85
0
0
74.2
Emulsion L
15
20
41
24
74.2
Emulsion M
15
20
36
19
76.2
*Surfactant in formulation 2 is different to that used in emulsions L and M.
Example 4
A series of CGM formulations were tested using the same general conditions as previously described. The test was conducted using fresh plant liquor and the same seed type as in earlier examples. Seed charge was 150 g/l, holding time was 4 hours and temperature was 80° C. The start liquor A/C=0.75 and the %+45 μm fraction data listed in Table 4 is the average of triplicate samples for the control and duplicate samples for dosed treatments.
This example further demonstrates that an emulsion of this invention containing a blend of surfactants (to a total composition of 15%), water and oil can be produced and that such a formulation is more effective than a waterless formulation. Note that the waterless formulations in this case are not exclusively surfactant/oil mixtures but also contain other non-water components. The results below indicate that Emulsion N containing 35% water, together with the surfactant and oil components provided much more effective coarsening than Formulations 3 and 4.
TABLE 4
Performance of an emulsion product
compared to Waterless formulations.
Composition (% w/w)
Other
Treatments
Surfactant
Oil
Water
components
% + 45 μm
Undosed Control
80.0
Formulation 3
2
95
0
3
83.8
Formulation 4
5
92
0
3
84.0
Emulsion N
15*
17
35
33
86.0
*Surfactant blend
Example 5
CGM formulations were tested using the same general conditions as previously described. The test was conducted using the same seed type as in earlier examples. Seed charge was 75 g/l, holding time was 4 hours and temperature was 78° C. The %+45 μm reaction data listed in Table 5 is the average of triplicate samples all treatments.
This example again demonstrates that the performance of emulsions containing more than 15% oil, together with water and surfactant, are effective CGMs and perform equal to or better than a waterless Formulation 5.
All emulsions in this example were prepared as clear microemulsions
TABLE 5
Performance of emulsion products compared
to a Waterless formulation.
Composition (% w/w)
Other
Treatments
Surfactant
Oil
Water
components
% + 45 um
Undosed Control
63.5
Formulation 5
10
90
0
0
69.0
Emulsion P
15
16
44
25
67.9
Emulsion Q
15
25
35
25
69.5
Emulsion R
15
25
37.5
22.5
69.7
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The present invention relates to compositions and methods to increase the output of a high quality product from the precipitation liquor crystallization process exemplified through the aluminum hydroxide recovery processes such as the Bayer process. The invention is a method of increasing the size of precipitates from a liquor. The invention in one embodiment relates to the use of a crystal growth modifier compositions added to the precipitation process to increase the particle size distribution of the precipitated alumina trihydrate.
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BACKGROUND OF THE INVENTION
The field of the invention pertains to windows for buildings and in particular to means for controlling the passage of sunlight through windows and means for improving the resistance to heat flow through windows.
Double glazing is a common construction technique for improving the resistance of windows to the transfer of heat therethrough. The panes of glazing, commonly glass or plastic, are typically separated by an air gap of one quarter of an inch to one inch. The double glazing may be provided by separate storm windows or by permanently installed double panes. To provide additional insulation a third pane of glazing separated by a second air gap may be added. Heavy drapes, movable insulating blankets or louvers may be positioned adjacent the glazing on the inside of the structure. Such techniques are commonly employed for windows regardless of the compass direction the windows face.
Movable louvers may be positioned against skylights to control the heat and light gain. However, the other techniques noted above are not practical for skylights. The devices above control heat gain and light transmission into the immediate interior area adjacent the window or skylight but do not necessarily take advantage of the compass direction the window or skylight faces.
Examples of insulated movable louvers to control light and heat flow through glazing are the "SUN MOVER," Solar Technology Corporation, Denver, Colo. and the "SKYLID," Zomeworks Corp., Albuquerque, N. Mex. These devices comprise pivotably mounted louvers positioned inside the glazing of the window or skylight.
SUMMARY OF THE INVENTION
The invention comprises a double glazing construction having foldable insulating louvers attached to and located between the glazing panels. The louvers are positioned horizontally for south facing windows and vertically for east and west facing windows. The louvers include internal insulating means and dual hingeing means permitting the louvers to be closed and opened as one of the glazing panels is moved relative to the other. Typically, the interior pane of glazing is moved relative to a permanently affixed exterior pane.
The panes include either integral extruded channels or separate extruded channels affixed to the panes in opposed relationship between the panes. Extruded louvers including integral hinges are inserted into the channels. The louvers are opened or closed by moving the interior pane of glazing relative to the exterior pane.
The extruded louvers are formed with a double wall creating an internal insulating air space therein. Alternatively, the air space may be filled with insulating foam. When the louvers are closed the combination with the exterior and interior glazing panes creates triple insulating air spaces between the exterior and interior panes. The exterior surfaces of the louvers are covered with a heat and light reflective coating to further enhance the insulating effectiveness of the louvers when shut. The heat and light reflective coating on the louvers enables incoming sunlight and heat to be redirected inside the building interior for an improved distribution of natural lighting and heat gain. To achieve the improved light and heat distribution, south facing windows are equipped with horizontal louvers and east and west facing windows are equipped with vertical louvers.
The particular design of the louvers including the hingeing means permits extrusion from very inexpensive plastic materials and fabrication techniques of sufficient simplicity to permit the sale of kits for retrofitting existing windows by relatively unskilled persons.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a vertical cross-section of a south facing window according to the invention;
FIG. 2 is a vertical cross-section of the window of FIG. 1 in closed insulating position;
FIG. 3 is a cross-section of the window installed in an east or west facing position;
FIG. 4 is a partial perspective view of one of the insulating louvers for the windows;
FIG. 5 is a partial perspective view of an alternative construction for the insulating louver of FIG. 4.
FIG. 6 is a partial cross section view of the window and latching means for the window;
FIG. 7 is a cutaway view of the window and the latching means.
FIG. 8 is a cutaway view of an attachment modification for the alternative embodiment of FIG. 5; and,
FIG. 9 is a cross-section of the window modified for use as a skylight.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1 a typical vertical cross-section of a south facing window embodying the invention is illustrated. The window assembly is positioned between a lower sill 10 and upper sill 12 with window lower frame member 14 and upper frame member 16 attached thereto respectively. An exterior stationary glazing pane 18 is inserted into slots 20 in the upper and lower frame members 14 and 16. Spaced from the exterior pane 18 is a movable glazing pane 22 that is supported by a plurality of horizontal louvers 24.
As shown in FIG. 1 the louvers 24 are fully open to permit the passage of light through the window as well as maximum direct heat gain to the interior of the structure. In FIG. 2 the louvers 24 and movable glazing 22 are shown in the fully closed position preventing the passage of light therethrough and completely covering the exterior glazing 18.
Referring to FIGS. 6 and 7 a latch mechanism 26 comprising a ball detent 28 is attached to the movable pane 22 at the edge of the pane. The ball detent 28 is adapted to engage any one of a plurality of sockets 30 spaced along an arcuate path 31 in the window jamb 29. The movable pane 22 and louvers may be opened, closed or set in an intermediate position by grasping the handle 27 and moving the movable pane 22 to the desired ball detent socket 30. A piece of weatherstrip 25 is adhesively attached to the pane 22 to provide a movable sliding seal with the jamb 29.
Opposed dovetail channel mullions 34 and 36 extend from the exterior glazing 18 and the movable interior glazing 22. Inserted in the channel mullions 34 and 36 are dovetail tongues 38 and 40. The tongues 38 and 40 form integral longitudinal edges of the louvers 24. The dovetail tongues 38 and 40 are attached to the central portion of the louver 24 by continuous hinges 42 and 44. The central portion of the louver 24 is filled with insulating foam 46. Optionally, the louver 24 can be left hollow to provide an insulating air gap between the walls of the louver. Thus, either triple air gaps or double air gaps separated by an insulated louver are provided between the double glazing.
The exterior surfaces of the louvers 24 may be coated or covered with a heat and light reflective material. The coating produces additional resistance to the transmission of heat when the louvers 24 are closed. When the louvers 24 are open, the light, in particular, as shown by the arrow 48 can be reflected off the louvers and off the interior ceiling 50 to provide increased daylighting to the interior of the building.
With the louvers 24 set in an intermediate position such as that shown ghosted at 32 in FIG. 1, light and heat (arrow 49) can be directed toward the floor adjacent the window. Thus, the heat and light gain to the building interior can be selectively controlled by adjusting the angular position of the louvers.
The louvers are preferably formed by extruding a suitable plastic material such as polyethylene, polypropylene or other material suitable for extrusion. In FIG. 4 the tongues 38 and 40 and hinges 42 and 44 are preferably formed as an integral flexible part of the extrusion. The use of a material such as polypropylene is suitable for such an integral flexible "living" hinge. Alternatively, mechanical hinges such as piano hinges might be substituted where the material of the louver 24 is not suitable for a flexible extruded "living" hinge. A urethane foam or other foam insulation is expanded inside the louver and the exterior coated with a suitable reflective material. Alternatively, aluminum foil may be adhered to the louver exterior.
The exterior glazing 18 and movable glazing 22 may be formed from extruded clear or translucent plastic with the dovetail mullions 34 and 36 formed as integral parts thereof. Alternatively, the glazing 18 and 22 may be formed of flat plate glass or plastic and the dovetail mullions 34 and 36 formed by extrusion and adhesively fastened to the glazing.
The extruded construction of the louvers and mullions permits the window structure to be manufactured very economically. The extrusions need only be cut to the proper length and then assembled by snapping or sliding the dovetail mullions and tongues together.
FIG. 5 illustrates an alternative construction for the louvers 24. The central portion 52 of the louver is formed from rigid foam insulation sheet that is covered on one or both sides with a heat and light reflective material. Such rigid foam insulation is available in one half inch and other thicknesses in retail building supply stores. The insulation is cut into strips of required width and length for the particular window installation. Attached to the rigid foam 52 are a pair of extruded hinge and attachment strips 54. The strips may be extruded from polyethylene or polypropylene. The strips include a U-section 56 that engages the rigid foam 52 and a dovetail tongue 58 joined to the U-section 56 by the integral hinge 60. The tongue 58 is engageable with dovetail channel mullion 62 also preferably formed by plastic extrusion. The back 64 of the extruded mullion 62 is adhesively fastened to the glazing (not shown). The U-section 56 may be adhesively attached to the central portion 52 or as shown in FIG. 8 the U-section 56' of the strip 54' may be serrated or grooved 57' to prevent extraction of the central portion 52 after insertion into the U-section.
Returning to FIG. 2 the louvers in the closed position nest together with the lower end 64 of the movable glazing pane 22 adjacent the lower frame 14. The integral flexible hinges 42 and 44 and a thin weatherstrip 43 effectively prevent the circulation of air through the louvers or vertically between the louvers and the exterior glazing 18. The weatherstrip 43 is formed as a thin flap integral with the louver 24 in the extrusion process.
FIG. 3 illustrates the use of the movable glazing and louvers in an east or west facing window. The basic construction of the window assembly is similar to that shown for the south facing window, however, the orientation of the louvers is vertical. With the louvers 24 fully open there can be mostly direct gain of heat and light as shown by arrow 66 or mostly indirect heat and light gain as shown by arrow 68 depending on the time of day and specific orientation of the window. By adjusting the position of the louvers to an intermediate location such as that shown in dashed outline 69 a portion of the light and heat (arrow 70) can be reflected back out through the exterior glazing 18. The light and heat gain can be thereby controlled and adjusted as the sun moves during the day.
The vertical louver orientation also can be installed in south facing windows rather than the horizontal louver orientation. The vertical orientation may be preferred where it is desired to follow the sun as it moves from east to west during the day rather than to follow the sun as it rises and falls during the day.
In FIG. 9 the movable glazing and louvers are shown in a skylight installation. Again the basic construction of the assembly is similar to that shown above, however, the louvers 24 and interior glazing 22 are suspended from the glazing 18 and mullions 34. With this configuration interior glazing 22 of plastic is to be preferred over heavy glass. The louvers 24 are opened and closed fully as above, however, the supporting ceiling structure 72 is tapered back permitting the louvers 24 to be rotated beyond the fully open position to the position shown ghosted at 74. A greater range of adjustment to accommodate the direction of the sun light is thereby provided for the skylight as illustrated by the arrows 76, 78 and 80. Arrow 76 indicates sunlight and heat passing through the normal full open position of the louvers and arrow 78 indicates the reflection of sunlight and heat from the partially closed position of the louvers as above. Arrow 80 indicates the extended open position to allow direct heat and sunlight gain despite a low sun angle to the skylight. The configuration permits a wide range of adjustment for direct gain, indirect gain or reflection despite the low altitude of the sun in the winter sky. To retain the louvers in the extended open position additional ball detents are added in an extended arcuate path in the skylight frame for the additional range. The range of adjustment for the vertical louver window illustrated in FIG. 3 can also be extended by tapering back the window jamb in the same manner.
The embodiments of the louvered window or skylight are particularly suitable for green houses with sloping or flat roofs in addition to other structures with windows in sloping or flat roofs as well as the walls. The low cost manufacture of the louvers, mullions and glazing by extrusion renders the invention of particular advantage for green houses with great expanses of glazing.
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The invention comprises a double glazing construction having foldable insulating louvers attached to and located between the glazing panels. The louvers include internal insulating means and dual hingeing means permitting the louvers to be closed and opened as one of the glazing panels is moved relative to the other. The specific configuration of the louvers and the means for attaching the louvers to the glazing permit the louvers, the hingeing means and the glazing to be manufactured from extruded plastic components. The louvers may be coated with a heat and light reflective material to further improve the insulating effectiveness when the louvers are closed and to direct sunlight deeper within a building interior when the louvers are opened.
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CROSS-REFERENCE TO RELATED PATENT APPLICATIONS
This application claims the benefit of Korean Patent Application No. 10-2006-0124937, filed on 8 Dec. 2006, in the Korean Intellectual Property Office, the disclosure of which is incorporated herein in its entirety by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a cosmetic case for containing an oily or watery tint-care cosmetic, more particularly, to a cosmetic case having a content transmitting path to a nozzle tip for discharging a cosmetic contained in a container and for rubbing the discharged cosmetic to a desired portion of the skin. The nozzle tip may be closed or opened in accordance with covering or uncovering of a cap, which also protects the nozzle tip from being loosened when dispensing the cosmetic.
2. Description of the Related Art
For the purpose of skin protection of beauty, ladies usually makeup with a tint-care cosmetic such as foundation, lipstick/lip gloss, eye cream, eye gel, ball touch, concealer, etc, after makeup with a skin-care cosmetic.
Not only appropriate structure of a container for maintaining the tint-care cosmetic differs from each other according to the usage and the component of the tint-care cosmetic but also the way how to makeup differs from each other according to the structure of the container.
There is one type of tint-care cosmetic for which a separate instrument for example, a powder puff, is used to makeup while there is another type which is contained in a container, is discharged through a nozzle and then rubbed on a desired portion of the skin by using the nozzle tip to makeup.
For example, tint-care cosmetics that are rubbed on a desired portion of the skin to makeup include lipstick, lip gloss, foundation, eye cream, etc, can be referred to.
Because those tint-care cosmetics are of oily gel type, it is possible to makeup by rubbing discharged tint-care cosmetic through the nozzle tip on the skin directly. Also because the discharged tint-care cosmetic is rubbed on the skin when performing makeup, not only it can permeate through the skin easily but also an effective makeup can be performed even with a small amount.
Because those tint-care cosmetic to be rubbed on the skin when makeup, including lipstick, lip gloss, ball touch, foundation, eye cream, eye gel, etc, are of oily gel type, it is preferable to prevent oil component from evaporating and to prevent the contained tint-care cosmetic in the container from contacting with the air.
In a conventional tube-type cosmetic case that discharges an oily gel-type tint-care cosmetic through a nozzle tip, a switching pole which is provided at the inside bottom portion of a cap is inserted into a discharging hole of the nozzle tip so that the content is blocked from being contacted with the air and an oily component of the content is blocked from being evaporated.
However, in such a conventional tube-type cosmetic case the switching pole may be bent and break if the pole is not aligned properly and inserted into the discharging hole when putting the cap on.
If the switching pole, which is provided at the inside bottom of the cap, is broken, it becomes impossible to block the discharging hole. Thus, air can be introduced into the container where the tint-care cosmetic is contained so that the tint-care cosmetic becomes hardened because the oily component which is contained in the tint-care cosmetic can evaporate.
Further, if the discharging hole remains open due to the broken switching pole, various problems can happen. For example, the content can spill out from the container when the container is pressed by an outer force or the container is placed upside down, the inside of the cap can become dirty with the discharged content, the unnecessarily discharged content becomes useless if it gets hardened, etc.
Further in the conventional cosmetic case with the nozzle tip, an opening portion of the container is deformed easily by the shock from the outside because the container, in which content is contained, is made by a soft tube in order that the content can be discharged easily through the nozzle tip.
If the nozzle tip is loosened from the container, air can be introduced through a connecting part and oily component of the content can evaporate thereby the content becomes hardened. Further the content can leak out from the container thereby the leaked content can stick to articles in the carrying bag and the interior of the carrying bag can become dirty.
To solve the problems of the conventional tube-type cosmetic case as described above, the applicant of the present invention have disclosed a cosmetic case capable of blocking outside air from being contacted to the oily gel-type tint-care cosmetic, which is contained in the container, so that not only the problem that the tint-care cosmetic gels harden but also other problems those can be occurred due to the opened discharging hole of the nozzle tip can be solved through the Korean registered utility invention No. 385091.
The registered invention has a container, in which the content is contained, a content outlet which is located at the opening part of the case through of an outer body, a switching adjustment part having a switching knob which is provided to open or close the content outlet selectively, an outer body on which a nozzle tip is provided at the upper portion and which is assembled to the outside of the switching adjustment part, and a cap to press the switching knob, which is protruded from the side of the outer body, in order to block the content outlet.
The registered invention opens or closes the content outlet selectively by the cap which is separated or installed with respect to the container.
If the cap is installed to the container, the switching knob of the switching adjustment part at the inside of the cap is restrained to close up inwardly so that a pressing pole of the switching knob presses the content outlet to be blocked.
Thus, the tint-care cosmetic in the case is protected from being contacted with the air and from becoming hardened.
When makeup using the tint-care cosmetic which is contained in the case stably, because the content outlet is blocked, the cap should be separated from the cosmetic case.
If the cap is separated from the cosmetic case, the switching knob of the switching adjustment part, which has been pressed by the inside of the cap, is set to free and the pressing pole is detached from the content outlet because the switching knob is protruded by the inherent elastic force.
If the pressing pole of the switching knob is detached, the content outlet is restored to an original state to open the content transmitting path because it is made by an elastic material (for example, rubber).
If the content transmitting path of the content outlet is opened, the content which is contained in the cosmetic case can be discharged through the nozzle tip and makeup can be performed by rubbing the discharged content to the desired portion of the skin with the nozzle tip.
When discharging the content in the container through the nozzle tip, the content is discharged from the nozzle tip with the cosmetic case placed upside down.
When the container is of a soft tube-type capable to press to discharge, the content is discharged by pressing the container.
After finishing makeup, the content outlet is blocked with the cap covered over the nozzle tip to maintain.
The registered invention is advantages in that the oily gel-type tint-care cosmetic can be used stably because the air is protected from being introduced into the inside of the cosmetic case where the tint-care cosmetic is contained. However, large number of the parts of the nozzle tip reduces productivity according to an assembling process and causes the cost increased.
Thus, it is necessary to simplify the structure in order to reduce the cost as well as to perform airtight process stably.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a cosmetic case capable of solving the problem that the oily or watery tint-care cosmetic is unnecessarily leaked out and hardened when it is carried or maintained.
Another object of the present invention is to provide a cosmetic case capable of improving credibility of product because it can make the customer who uses the product feel the sense that he/she felt at first purchase without evaporation of the oily or watery component by effectively blocking the content in the container from being contacted with the air.
Still another object of the present invention is to provide a cosmetic case capable of improving productivity in accordance with assembly process by simplifying the structure of the nozzle tip and reduction of the cost can be also expected accordingly.
Still another object of the present invention is to provide a cosmetic case capable of improving the durability of the opening portion 31 by installing ratchet projection 33 at the opening portion 31 of the soft tube type container 30 .
Still another object of the present invention is to provide a cosmetic case capable of protecting the content from becoming harden due to contact with the air or evaporation of the oily or watery component because the elastic ratchet projection 16 , which is provided on the connecting part 23 of the nozzle tip 20 , is engaged with the ratchet projection 33 , which are provided on the opening portion 31 , so that loosening cannot happen even if a rotating force in the screw-loosening direction at the installed nozzle tip 20 is applied.
Still another object of the present invention is to provide a cosmetic case capable of improving consumer's credibility of the cosmetic case with the nozzle tip because the content is protected from being leaked to lose and the interior of a carrying case is protected from getting dirty as the leaked content sticks to other articles.
The cosmetic case according to the present invention includes a container 30 whose opening portion 31 for discharging the contained content is formed in layers, a thread is provided on a lower outer circumference portion so that a nozzle tip connecting part 10 can be installed by screwing and a ratchet projection 33 is provided on an upper circumference portion; a nozzle tip connecting part 10 where an elastic ratchet projection 16 , which is supported in the screw-loosening direction with respect to the ratchet projection 33 of the container 30 , is provided in parallel with the outer side of a content path 15 ; a spiral guiding rail 41 which ensures a nozzle tip 20 elevated upwardly or downwardly is provided and a spiral supporting rail 12 is provided in parallel over the spiral guiding rail 11 on the outer circumference portion; and a switching pole 13 is provided on the inner content transmitting path 15 through a rib 14 ; a nozzle tip 20 having a discharging tube 21 where a content transmitting path 22 , which is connected to a discharging hole 22 a , is provided inside; a connecting part 21 which is provided at the bottom portion of the discharging tube 21 ; an elevating rail 24 , which is guided along a spiral guiding rail 11 and supported by a spiral supporting rail 12 , is provided on the interior side of the connecting part 21 ; and a groove 27 which is provided on the outer circumference portion; and a cap 40 where a key projection 42 which is inserted into the groove 27 of the nozzle tip 20 ; and a guiding projection 41 which is guided along the cap closing guiding rail 17 of the nozzle tip connecting part 10 are provided.
Additional aspects and/or advantages of the present invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other features and advantages of the present invention will become more apparent by describing in detail preferred embodiments thereof with reference to the attached drawings in which:
FIG. 1 is a disassembled perspective view illustrating a cosmetic case according to the present invention;
FIG. 2 is an assembled sectional view of the cosmetic case according to the present invention;
FIG. 3 is a disassembled perspective view of a nozzle of the cosmetic case according to the present invention, illustrating a supporting thread of a screw which is provided in a connecting part;
FIG. 4 is a disassembled perspective view illustrating a content transmitting tube of the nozzle tip of the cosmetic case according to the present invention;
FIG. 5 is a sectional view illustrating the state that a content transmitting path is achieved in the cosmetic case according to the present invention;
FIG. 6 is a sectional view illustrating the initial state of the process that blocks the transmitting path of the nozzle tip 20 in the cosmetic case according to the present invention;
FIG. 7 is a sectional view illustrating the intermediate state of the process that blocks the transmitting path of the nozzle tip 20 in the cosmetic case according to the present invention;
FIG. 8 is a sectional view illustrating the final state of the process that blocks the transmitting path of the nozzle tip 20 in the cosmetic case according to the present invention;
FIG. 9 is a sectional view illustrating the state that an elastic ratchet projection, which is provided on a nozzle tip connecting part, is being supported by the ratchet projection of the cosmetic case according to the present invention; and
FIG. 10 shows another embodiment of the nozzle in the cosmetic case according to the present invention.
BRIEF DESCRIPTION OF NUMERALS IN DRAWINGS
10:
nozzle tip connecting part
11:
spiral guiding rail
11a:
tilted guiding side
11b:
settling side
11c:
stopper
11d:
ledged side
12:
spiral supporting rail
13:
switching pole
14:
rib
15:
content transmitting path
16:
elastic ratchet projection
20:
nozzle tip
17:
cap closing guiding rail
17a:
locking groove
21:
discharging tube
22:
content transmitting tube
22a:
discharging hole
22b:
tube-widening portion
23:
connecting part
24:
elevating rail
25:
guiding projection
26:
supporting thread
27:
groove
30:
container
31:
opening portion
32:
upper circumference portion
33:
ratchet projection
40:
cap
41:
guiding projection
42:
key projection
DETAILED DESCRIPTION OF THE INVENTION
Reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the like elements throughout. The embodiments are described below to explain the present invention by referring to the figures. For the sake of clearness and conciseness, technology related to the present invention that is not novel and is well known in the art to which present invention pertains will not be described herein.
As shown in FIG. 1 through FIG. 9 , the cosmetic case according to the present invention has a container 30 in which the content is contained, a nozzle tip connecting part 10 which is installed to the opening portion of the container 30 , a nozzle tip 20 which is installed to the nozzle tip connecting part 10 and elevates upwardly or downwardly, and a cap 40 to protect the nozzle tip 20 .
The container 30 is of a soft tube-type so that the contained content is pressed to discharge and the opening portion 31 is formed in layers so that it can be classified into a larger external diameter and a smaller external diameter.
Threads are provided on the outer circumference portion with the larger external diameter of the opening portion 31 in order that the nozzle tip connection part 10 can be installed by screwing it onto the opening portion 31 .
Further ratchet projection 33 is provided on both sides of the upper circumference portion 32 with the smaller outer diameter of the opening portion 31 .
The ratchet projection 33 is formed in order that the nozzle tip connecting part 10 can be rotated toward a screw-tightening direction while it is prevented from being rotated toward a screw-loosening direction.
An elastic ratchet projection 16 is provided so that it can be climbed over the ratchet projection 33 of the opening portion 31 when the nozzle tip connecting part 10 is installed to the position neighboring to the outside of the content transmitting path 15 whilst it is engaged with the ratchet projection 33 of the opening portion 31 when a rotating force is applied to the opening portion 31 toward a screw loosening direction.
Basically, the elastic ratchet projection 16 performs a role to block the nozzle tip connecting part 10 from being rotated in the screw loosening direction. But the elastic ratchet projection 16 is configured to be modified elastically in order to climb over the ratchet projection 33 which are provided on the opening portion 31 of the container 30 when the nozzle tip connecting part 10 is rotated with a large force in the screw loosening direction.
Threads are provided on the inside of the nozzle tip connecting part 10 and a spiral guiding rail 11 is provided on the upper circumference portion 32 in order that it can be screwed to connect to the opening portion 31 of the container 30 .
The spiral guiding rail 11 has a tilted guiding side 11 a , which is protruded from the outer circumference portion in order to guide a elevating rail 24 of the nozzle tip 20 , a setting side 11 b on its upper portion, on which a shorter guiding projection 25 b of guiding projection 25 of the elevating rail 24 of the nozzle tip 20 is settled, and a stopper 11 c , which is protruded upwardly and restrains the movement of the longer guiding projection 25 b , neighboring to the settling side 11 b.
The spiral guiding rail 11 is formed on the outer circumference portion in opposite directions.
A spiral supporting rail 12 is provided on the upper portion of the spiral guiding rail 11 . The upper portion of the elevating rail 24 of the nozzle tip 20 is supported to guide in the parallel direction with respect to the spiral guiding rail 11 .
The spiral supporting rail 12 is formed on the outer circumference portion in opposite directions.
A switching pole 13 is provided on the content transmitting path, which is provided in the nozzle tip connecting part 10 , through a rib 14 . The switching pole 13 is inserted into the content transmitting path 22 of the nozzle tip 20 to switch the content transmitting path 22 selectively.
A cap closing guiding rail 17 is provided at the lower portion of the spiral guiding rail 11 of the nozzle tip connecting part 10 in opposite directions. The guiding projection 41 of the cap 40 is guided by the cap closing guide rail 17 .
A camping groove 17 a is provided at the lower portion of the cap closing guiding rail 17 . The installment of the cap 40 is maintained by the cap closing guide rail 17 .
The nozzle tip 20 , which is installed to the nozzle tip connecting part 10 , is configured with a discharging tube 21 and a connecting part 23 .
The content transmitting path 22 , by which the cosmetic is transmitted, is provided in the discharging tube 21 and the content transmitting path 22 is connected to the discharging hole 22 a.
The content transmitting path 22 has a tube-widening portion 22 b and the inner diameter of the tube-widening portion 22 b is larger than the outer diameter of the switching pole 13 of the content transmitting path 22 .
The connecting part 23 is provided at the lower portion of the discharging tube 21 and an elevating rail 24 is provided at the inner side of the connecting part 23 .
The guiding projection 25 is provided at the bottom of the one end of the elevating rail 24 and the guiding projection 25 is guided to climb over the spiral guide rail 11 of the nozzle tip connecting part 10 .
The guiding projection 25 has a shorter guiding projection 25 b and a longer guiding projection 25 a . The shorter guiding projection 25 b is contacted tightly to the tilted guiding side 11 a of the spiral guiding rail 11 and will be placed on the setting side 11 b when the nozzle tip 20 is elevated upwardly until the content can be discharged to use. The a longer guiding projection 25 a is supported on the ledged side 11 d when the nozzle tip 20 is elevated downwardly until the content transmitting path 22 is blocked air tightly.
A supporting thread 26 is provided at the elevating rail 24 . The supporting thread 26 is extended from the guiding projection 25 and supported to guide by the lower portion of the spiral supporting rail 12 .
A groove 27 is provided on the outer circumference portion of the nozzle tip 20 so that a key projection 42 of the cap 40 is inserted.
The discharging tube 21 of the nozzle tip 20 can be replaced with one of brush, rubber, TEFLON (trademark of DuPont. Another name for “POLYTETRAFLUOROETHYLENE”), sponge, puff and flocking ball 21 a.
The key projection 42 , which is inserted into the groove 27 of the nozzle tip 20 , and a guiding projection 41 , which is guided along the cap closing guiding rail 17 of the nozzle tip connecting part 10 , is provided on the inner side of the cap 40 which protects the nozzle tip 20 .
When it is desired to discharge the tint-care cosmetic through the nozzle tip of the cosmetic case according to the present invention, the cap 40 , which is covered to protect the nozzle tip 20 , should be separated.
After then, content is discharged through the nozzle tip 20 to makeup.
FIG. 5 shows the state that the cap 40 is separated from the nozzle tip 20 .
As shown in FIG. 5 , the nozzle tip 20 is separated from the nozzle tip connecting part 10 when the nozzle tip rotates in the screw-loosening direction because the guiding projection 41 of the cap is guided along the cap closing guiding rail 17 of the nozzle tip connecting part 10 when the cap 40 is pulled out to separate.
The cap 40 and the nozzle tip 20 rotate together when the cap 40 is separated because the key projection 42 of the cap 40 is inserted into the groove 27 of the connecting part 23 of the nozzle tip 20 .
The nozzle tip 20 is moved together in the screw-loosening direction by the rotating cap 40 .
If the nozzle tip 20 rotates, the nozzle tip 20 is elevated upwardly because the shorter guiding projection 25 b of the guiding projection 25 of the elevating rail 24 , which is provided on the inner side of the connecting part 23 of the nozzle tip 20 in opposite directions, are guided along the tilted guiding side 11 a of the spiral guiding rail 11 of the nozzle tip connecting part 10 .
If the shorter guiding projection 25 b of the elevating rail 24 , which is provided at the nozzle tip 20 , climbs on upwardly along the tilted guiding side 11 a of the spiral guiding rail 11 of the nozzle tip connecting part 10 , the switching pole 13 , which has blocked the content transmitting path 22 , is located at the tube-widening portion 22 b so that the content transmitting path 22 , through which the tint-care cosmetic can be discharged, is achieved as shown by an arrow in FIG. 5 .
If the transmitting path is provided in the content transmitting tube 22 , the shorter guiding projection 25 b of the guiding projection 25 of the elevating rail 24 of the nozzle tip 20 is settled on the settling side 11 b of the spiral guiding rail 11 of the nozzle tip connecting part 10 and contacted to the stopper 11 c so that the nozzle tip cannot rotate any more.
In the meantime, the nozzle tip 20 can elevate upwardly stably without departing from the nozzle tip connecting part 10 when the elevating rail 24 of the nozzle tip 20 is guided toward the spiral guiding rail 11 of the nozzle tip connecting part 10 because the supporting thread 26 is guided toward the spiral supporting rail 12 , which is provided at the upper portion of the spiral guiding rail 11 .
If the content transmitting path 22 of the discharging tube 21 is opened as the nozzle tip 20 elevates upwardly, the content, which is contained in the container 30 , can be discharged through the discharging hole 22 , which is provided on the upper side of the discharging tube 21 of the nozzle tip 20 , and then the discharged content can be rubbed to apply to the desired portion of the skin to makeup by using the nozzle tip 20 .
The content of the container 30 can be discharged through the discharging hole 21 a of the nozzle tip 20 when the case placed upside down.
If the case is of a soft tube-type, the content can be discharged by squeezing the case.
After makeup, the content in the container 30 should be maintained in order that the content should not be hardened by contacting with air.
For blocking the content from being contacted with the air, the nozzle tip 20 , which is elevated upwardly, should be elevated downwardly.
To elevate the nozzle tip 20 downwardly, the nozzle tip 20 should be rotated in the screw-closing direction.
The nozzle tip 20 can be rotated in the screw-closing direction by covering the cap 40 over the nozzle tip 20 .
The process to airtight the nozzle tip 20 by covering the cap 40 over the nozzle tip 20 will be described taken with accompanied drawings of FIG. 7 through FIG. 8 .
FIG. 6 is a sectional view illustrating the initial state of the process that the transmitting path of the nozzle tip 20 is blocked in the cosmetic case according to the present invention.
FIG. 7 is a sectional view illustrating the intermediate state of the process that the transmitting path of the nozzle tip 20 is blocked in the cosmetic case according to the present invention.
FIG. 8 shows a sectional view illustrating the final state of the process that the transmitting path of the nozzle tip 20 is blocked in the cosmetic case according to the present invention.
Firstly, the guiding projection 41 , which is provided on the inner side of the cap 40 , is positioned to the cap closing guiding rail 17 , which is provide on the nozzle tip connecting part 20 as shown in FIG. 6 .
If the guiding projection 41 is inserted into the cap closing guiding rail 17 after the guiding projection 41 is positioned at the cap closing guiding rail 17 , the key projection 42 is inserted into the groove 27 , which is provided on the connecting part 23 of the nozzle tip 20 .
If the cap 40 is pressed downwardly after the key projection 42 is inserted into the groove 27 of the connecting part 23 of the nozzle tip 20 , the cap 40 rotates in the screw-closing direction while the guiding projection 41 of the cap 40 is guided along the cap closing guiding rail 17 .
If the cap rotates in the screw-closing direction, the nozzle tip 20 , wherein the key projection 42 of the cap 40 is inserted into the groove 27 , is moved in accordance with the movement of the cap 40 .
The process to block the nozzle tip 20 by the cap 40 , which covers the nozzle tip 20 , is described in more detail.
If the nozzle tip 20 is rotated in the screw-closing direction as described above, the shorter guiding projection 25 b of the guiding projection 25 of the elevating rail 24 of the nozzle tip 20 , which is placed at the settling side 11 b of the spiral guiding rail 11 of the nozzle tip connecting part 10 , escapes from the setting side 11 b and elevates downwardly along the tilted guiding side 11 a.
If the guiding projection 25 b is guided along the tilted guiding side 11 a , the nozzle tip 20 is moved downwardly toward the nozzle tip connecting part 10 because the supporting thread 26 of the elevating rail 24 is guided toward the spiral supporting rail 12 , which is provided at the upper side of the spiral guiding rail 11 .
If the nozzle tip 20 is moved downwardly, the content transmitting path 22 is blocked air tightly because the switching pole 13 , which is provided through the rib 14 on the content transmitting path 15 of the nozzle tip connecting part 10 , is inserted in to the content transmitting path 22 , as shown in FIG. 8 .
In the meantime, the state in which the content transmitting path 22 is blocked by the switching pole 13 can be maintained stably because the longer guiding projection 25 a of the guiding projection 25 of the elevating rail 24 is supported on the ledged side 11 d of the nozzle tip connecting part 10 and the supporting thread 16 is supported by the spiral supporting rail 12 at the same time.
Because the content transmitting path 22 is blocked air tightly by the switching pole 13 , not only leakage of the content while carrying but also intrusion of air can be blocked effectively.
Further the nozzle tip 20 is blocked more stably because the guiding projection 41 of the cap 40 , which blocks the nozzle tip 20 , is positioned at the locking hole 17 a of the cap closing guiding rail 17 of the nozzle tip connecting part 10 .
As described above, the present invention can discharge the content to be used or block the nozzle tip 20 as the nozzle tip 20 rotates. The present invention can prevent the nozzle tip connecting part 10 from being loosened even though excessive rotating force is applied in the screw-loosening direction because the nozzle connecting part 10 is installed to the container 30 while the elastic ratchet projection 16 , which is provided on the inner side of the nozzle tip connecting part 10 , is engaged with the ratchet projection 33 , which is provided on the opening portion 31 of the container 30 .
FIG. 10 shows another embodiment of the nozzle tip in the cosmetic case according to the present invention.
In the embodiment shown in FIG. 10 , the discharging tube 21 of the nozzle tip 20 is made by one of brush, rubber, TEFLON (trademark of DuPont. Another name for “POLYTETRAFLUOROETHYLENE”), sponge, puff, flocking ball 21 a so that various needs of customer can be met.
As described above, the present invention can solve the problem that the oily or watery tint-care cosmetic is unnecessarily leaked out and hardened because the content transmitting path 22 , which forms the discharging tube 21 of the nozzle tip 20 , is blocked air tightly by the movement of the cap 40 , which covers the nozzle tip 20 , with respect to the switching pole 13 , which is provided on the content transmitting path 22 of the nozzle tip connecting part 10 , which is connected to the opening portion 31 of the container 30 through the rib so that the content can be discharged through the content transmitting path 22 .
Further the present invention can improve credibility and consistency of the product because it can ensure that the user will feel the sense that he/she felt at first purchase without evaporation of the oily or watery component by effectively blocking the content in the container from being contacted with the air.
Still further the present invention can improve productivity in accordance with assembly process because the structure of the nozzle tip is simplified.
Reduction of the cost can be also expected accordingly.
Still further the present invention can improve the durability of the opening portion 31 by installing ratchet projection 33 at the opening portion 31 of the soft tube type container 30 .
Still further the present invention can protect the content from becoming harden due to contact with the air or evaporation of the oily or watery component because the elastic ratchet projection 16 , which is provided on the connecting part 23 of the nozzle tip 20 , is engaged with the ratchet projection 33 , which are provided on the opening portion 31 , so that loosening cannot happens even if a rotating force in the screw-loosening direction at the installed nozzle tip 20 is applied.
Still further the present invention can protect the content.
Still further the present invention can improve consumer's credibility of the cosmetic case with the nozzle tip because the content is protected from being leaked to lose and the interior of a carrying case is protected from getting dirty as the leaked content sticks to other articles.
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A cosmetic dispenser including a container, a dispensing part connected to the container through a connecting part, and a cap removably covering the dispensing part. The cap is rotatable to rotate the dispensing part therewith thereby moving the dispensing part between a closed position in which a switching pole of the connecting part blocks an opening inside the dispensing part, and an open position in which the opening is moved away from the switching pole and the content stored inside the container is able to be transmitted to the dispensing part.
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BACKGROUND OF THE INVENTION
The present invention relates generally to bridge construction techniques and more particularly to a method for building the deck structure of a cable-stayed girder bridge. The invention is particularly intended for utilization with the type of construction technique which involves formation of the deck girder section of a bridge in sequential stages with adjacent sections of the deck girder being successively formed. In the type of construction technique to which the present invention relates, a form carrier which is movable along the bridge during its formation is utilized. As each successive bridge section is formed, the form carrier is moved to extend in a cantilevered arrangement from a previously formed bridge section in order to thereby provide support for a successive bridge section during its formation.
The successively formed deck girder of the bridge consists of reinforced or prestressed concrete. With the formation of each segment of the deck girder, anchoring of the bridge support cables is effected and the anchored cables are tensioned prior to formation of a next section.
In bridges constructed from reinforced or prestressed concrete, it has been known to build the bridge superstructure in the form of two projecting arms which extend from a pier toward opposite sides and which consist of concrete cast in situ or of precast concrete units. The production occurs in successive cantilevered segments from a form carrier which is secured on a completed section of the bridge superstructure and which projects beyond the end thereof. Such a form carrier is moved on rollers along the bridge superstructure to enable formation of the next respective cantilever segment.
In the construction of bridge superstructures in a cantilever form of construction, a problem arises during the construction stage of the bridge with regard to adaption, to the fullest extent possible, of the static principle system of the unfinished bridge to the static system of the finished bridge. Only in this way can there be avoided problems such as the receipt by individual members of loads which are higher during the construction stage of the bridge than when the bridge is in its finished state. Also, in this manner, there may be avoided additional measures which might be required to absorb loads which occur only during the relatively short period of bridge construction, which measures might include the provision of additional reinforcements, auxiliary supports or the like.
A cable-stayed girder bridge usually consists of a deck girder which is carried by abutments and piers and additionally by a system of straight cables which extend obliquely from the approaches by way of one or more pylons to the main span or spans. The cables extend generally in vertical planes, either in a plane within the longitudinal axis of the bridge or on either side along the edges of the deck's girder. As the loads of a cable-stayed girder bridge are supported essentially by oblique cables, the deck girder does not have a great deal of bending strength. For this reason, cantilevering of a cable-stayed girder bridge, though possible in principle, presents difficulties because, due to the low bending strength of the deck girder, the pouring loads of the respective front cantilevered sections can be shifted back only to the previously produced section so that this section and the cable anchored therein are under greater load than in the final state of the bridge.
The present invention is aimed at overcoming many of the aforementioned problems. With utilization of the present invention, there may be obtained in the building of a cable-stayed girder bridge formed in successive cantilever sections, a better adaptation of the static principle system in the building stage of the bridge relative to the final system of the finished bridge whereby making possible a more economic production method for such a bridge.
Briefly, the present invention may be described as a process for the construction of a cable-stayed girder bridge which has a concrete deck girder including longitudinally extending stiffening girders and a laterally extending deck. The process is performed by sequential formation of the deck girder in successive adjacent sections utilizing a form carrier movable along the bridge and adapted to be cantilevered from a previously formed deck girder section to provide support for a successive deck girder section during its formation. The bridge of the type to which the present invention relates is supported from pylons anchored in the earth. Cables extend from the pylons to the longitudinal stiffening girders of the deck girder. The particular improvement of the present invention involves formation of the deck girder by first forming the longitudinal stiffening girders with the cables embedded therein. The longitudinal stiffening girders are permitted to set and harden and the cables embedded therein are subsequently tensioned between pylons and the formed stiffening girders. As a result, the cables may be utilized to provide additional support for the partially formed deck girder. During the pouring of the stiffening girders, the form carrier is arranged to extend in cantilever fashion from a previously formed deck girder. After formation of the stiffening girders, the form carrier is connected to the formed stiffening girders to thereby enable additional support to be provided for the section being constructed. Finally, the laterally extending deck portion of the deck girder may be formed and this stage of the construction of the bridge may be effected with the advantage that the cables enhance the support which would otherwise be provided only by the form carrier.
The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and specific objects attained by its use, reference should be had to the accompanying drawings and descriptive matter in which there are illustrated and described a preferred embodiment of the invention.
DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a side view showing an overall bridge construction produced by utilization of the present invention;
FIG. 2 is a sectional side view of the bridge of FIG. 1 taken along the lines II--II;
FIGS. 3a and 3b are transverse sectional views of a bridge formed in accordance with the present invention showing an initial stage of bridge construction, with FIG. 3a being a view looking in the direction of the arrows IIIa -- IIIa and FIG. 3b being a view looking in the direction of the arrows IIIb -- IIIb of FIG. 4;
FIG. 4 is a longitudinal sectional view of the bridge depicted in FIG. 3 taken along the line IV-- IV;
FIGS. 5a and 5b are transverse sectional views showing the bridge in a subsequent phase of construction with FIG. 5a being a view looking in the direction of the arrows Va --Va of FIG. 6 while FIG. 5b is a view looking in the direction of the arrows Vb--Vb of FIG. 6; and
FIG. 6 is a longitudinal sectional view of the bridge structure depicted in FIG. 5b taken along the line VI--VI.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, there is depicted a cable-stayed girder bridge which is supported from piers 1 extending to below the surface of a body of water which is to be spanned by the bridge structure and which are anchored in the earth. Pylons or towers 2 extend upwardly from the piers 1. The bridge comprises a deck girder 3 which is formed of prestressed concrete and which comprises two longitudinally extending stiffening girders 4 in which cables 5 are anchored. The cables 5 extend between the pylons 2 and the stiffening girders 4. Between the stiffening girders 4 a lateral deck portion 6 of the deck girder 3 is provided. The cables 5 extend from the pylons 2 in generally parallel relationship relative to one another and they are, in the finished bridge structure, maintained in tension between the pylons 2 and the stiffening girders 4.
FIGS. 3a and 3b are partial sectional views taken transversely of the bridge structure each showing the bridge when viewed in opposite directions. In FIG. 3a, there is depicted a portion of the bridge looking rearwardly toward previously constructed sections. FIG. 3b shows the bridge structure when viewed forwardly in the direction in which construction is occurring. Thus, with respect to FIG. 4, which shows a longitudinal sectional views of the bridge, the construction of the bridge takes place in a direction extending rightwardly of the view of FIG. 4. In the construction of the bridge in cantilevered segments, the deck girder is produced in sequentially formed successive segments. The segments of the deck 6 are marked 6a, 6b, 6c etc. and those of the two outer stiffening girders 4, in which the cables are anchored are marked 4a, 4b, 4c, etc. The deck girder 3 is produced in individual cantilever segments 3a, 3b, 3c etc., each having one cable or two cables 5a, 5b, 5c etc. assigned thereto.
In the bridge structure depicted in the drawings, a cantilever segment 3b of the overal deck girder has been completed and a cable 5b is embedded therein. After formation of the segment 3b, a form carrier 8 is placed in position for the production of the next successive cantilever segment 3c which is to have attached thereto a cable 5c.
The form carrier 8 consists of two longitudinal girders 9 which are arranged proximate and below the stiffening girders 4. The longitudinal girders 9 are connected by cross girders 10. Thus, the form carrier 8 essentially consists of a girder grate which rests upon shuttering 11 for the deck girder 3.
During the formation of the successive deck girder segment 3c, the form carrier 8 is supported at its rear end upon the front end of the cantilever segment 3b by wheels 13 which engage rails 14 provided on the top of the stiffening girder 4. To relieve the carriage during concrete pouring, tendons 15 are provided which may be tensioned by hydraulic jacks 16. The form carrier 8 is braced on the back of the longitudinal girders 9 against the underside of the stiffening girders 4 by rollers 17.
FIGS. 3a and 3b show transverse sections through the cantilever segment 3c which is to be produced in a state in which the stiffening girder members 4c have just been formed. The illustration has been selected so that the left half, i.e. FIG. 3a, shows a section looking rearwardly while the right half, i.e. FIG. 3b, shows a section looking forwardly. It will be noted that during this initial stage of formation, the stiffening girders 4c have been formed but the laterally extending deck portion 6c has not as yet been formed.
After setting of the concrete forming the stiffening girders 4c, the cables 5c anchored therein are tensioned. Thus, the cables 5c will be loaded between the pylons 2 and the stiffening girders 4c. At this point, the form carrier 8 may be secured at the front end of the longitudinal girders 9 over additional tendons 18 with interposition of hydraulic jacks 19 at the stiffening girder members 4c thus enabling a direct bearing of the loads of the member 6c by the cables 5c.
Accordingly, by initially forming the stiffening girders 4c, the support for the subsequently formed lateral deck portion may be enhanced by utilization of the cables 5c. As a result, the deck girder segment being formed will be supported not only by the form carrier 8 but there will also be applied to the end of the form carrier 8 additional support by means of the cables 5c.
If, as in the examples shown in the drawings, the stiffening girders are produced only to the height of the lower edge of the deck 6, as is favorable for reasons of weight, it becomes necessary to bridge the missing portion of the height for the support of the jacks 19 by a spacer 20 which may, for example, be a tube section, a block or the like.
After the initial stage of formation depicted in FIGS. 3a, 3b and 4, the subsequent stage of formation depicted in FIGS. 5a, 5b and 6 may be achieved. With the cable 5c extending to support the deck girder segment being formed, the concrete for the lateral deck 6c may be poured. Such pouring may be done with greater facility by virtue of the fact that the added structural support previously described has been afforded. After the setting of the concrete of the member 6c of the deck, as shown in FIGS. 5a or 5b, the anchorings of the tendons 15 and 18 may be released whereby the form carrier 8 supported upon the rails 14 by the wheels 13 may be moved forwardly to enable production of the next successive segment of the bridge deck girder.
In the formation of bridges of the type depicted in the drawings, it is ordinarily necessary to construct the deck structure by proceeding in directions away from the pylons 2. Thus, a first deck girder is normally formed adjacent a pylon 2 and successive deck girders 3 may then be formed utilizing the techniques of the present invention by proceeding from the first deck girder thus formed in a direction away from the pylon. The procedure for forming such a first deck girder may be in accordance with techniques known in the prior art and thus a detailed description thereof is not deemed necessary for a complete understanding of the present invention.
From the foregoing it will be seen that the present invention provides a method which overcomes many of the problems of the prior art discussed hereinbefore. Each cantilever section is produced by first forming the part of the deck girder situated in the zone of the cable plane or planes with the cables being anchored therein. After this portion of the deck girder has set and hardened, the cable or cables anchored therein may be tensioned and a form carrier may be additionally supported through the cables embedded therein. Thereafter, the remaining portion of the deck girder may be produced.
With the method according to the present invention, much better adaptation of the static principle system of the bridge in its construction stage to the final system may be obtained. This is achieved in that there is first formed only a part of the deck girder with the aid of the projecting form carrier with this initially formed part being that part in which the oblique cables are anchored. These cables may be installed very early and under very low load of the previously produced portion of the bridge superstructure. For the absorption of the weight of the remaining portion of the deck girder to be produced in the second building segment, even though it is usually the greater portion, there are then available in each cantilever segment the cables already anchored therein so that not only these cables but also the previously connected cables may be stressed during stages of construction in the same manner and in approximately the same amount as in the final bridge structure.
An advantage of the present invention involves the fact that in the projecting state, the form carrier is required to carry only a small part, about 1/4 to 1/3, of the load of the total cantilever segment being formed. Thus, not only may the production steps be carried out more easily but there is enabled the formation of longer individual cantilever segments of the deck girder. This, in turn, has a favorable effect upon construction time and profitability of the entire construction process.
While a specific embodiment of the invention has been shown and described in detail to illustrate the application of the inventive principles, it will be understood that the invention may be embodied otherwise without departing from such principles.
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A cable-stayed girder bridge having a concrete deck girder which includes longitudinally extending stiffening girders having cables embedded therein and a laterally extending deck portion is constructed by sequential formation of said deck girder in successive adjacent sections. The longitudinally extending stiffening girder portions of said deck girder are first formed, support cables are embedded therein and subsequently tensioned. After hardening of the stiffening girders, the laterally extending deck portion of the duck girder is formed. A form carrier movable along the bridge during its construction extends in a cantilevered arrangement from a previously formed deck girder section to provide support for a successive deck girder section during formation thereof.
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FIELD OF THE INVENTION
[0001] The present invention relates to a portable, temporary guard rail support and, more particularly, to a novel guard rail support for use in the erection of a safety barrier or fence at sites under construction such as office buildings, high rise apartments or the like.
BACKGROUND TO THE INVENTION
[0002] Modern construction techniques, particularly those commonly employed in high rise apartment and office building construction, require that safety barriers or guard rails be erected around the perimeter of all uncompleted floors (i.e. along the drop-off edges of concrete floor slabs) for two reasons: Firstly, personal safety requires the erection of at least a single rail at about waist height around the exterior of such uncompleted floors. Secondly, it is also necessary that a retaining kick board be erected at floor level so as to prevent the accidental dislodgement of articles which would otherwise cause a substantial safety hazard to workmen on the floors below and around the construction site. In certain cases, the provision of a weather barrier, such as a plastic tarpaulin or the like, may be necessary so as to protect the site under construction as well as workmen from inclement weather conditions.
[0003] The general practice in the erection of such safety barriers involves the use of lengths of lumber stock such as long boards of the 2″×4″ variety (commonly referred to as “two-by-fours”). Such boards are cut to length and then nailed together in varying patterns in order to provide the desired guard railings. After such railings have served their purpose they are knocked down, the longer boards typically reserved for future use in the piecing together of future guard railings. The shorter boards are not always reusable. Furthermore, the longer lengths of lumber frequently become damaged by splitting or otherwise due to the application thereto of repeated impact blows and different nail placements. While such makeshift such guard railings meet safety requirements, they require more than one person and a fair amount of time to construct and often result in the destruction of the materials used when they are disassembled after completion of work at a construction site. Obviously, the additional labour and cost of materials used will add to the expense of the job. Many such railings also fail to pass the rigidity requirements of safety inspectors.
[0004] As a result, various structures have been proposed to aid in the construction of temporary safety barriers which prevent workmen from accidental falls and which meet strict safety guidelines. To a large extent, however, most of the proposed structures are impractical, expensive and too complicated to use. Furthermore, structures that are too complicated to use will not be used efficiently and/or properly by workmen at a construction site, thereby posing a safety risk.
[0005] Consequently, a need exists for a portable and simple guard rail system which is effective in preventing accidental falls, meets safety guidelines and which can be assembled and disassembled in an efficient manner.
SUMMARY OF THE INVENTION
[0006] A portable guard rail support and assembly for use in erecting a safety barrier to provide a safe work area for workmen working at dangerous heights, particularly in the construction industry, is provided.
[0007] In accordance with a first aspect of the present invention, a guard rail support for use in erecting a temporary safety barrier is provided wherein the guard rail support comprises a substantially flat bottomed base plate, an upright column affixed to the flat bottomed base plate, at least one guard rail support bracket affixed to the upright column, a kick board retaining flange affixed to the flat bottomed base plate in spaced proximal relationship to the upright column, an angular brace affixed to the upright column and the flat bottomed base plate and a safety tie-off ring affixed to the upright column and the flat bottomed base plate.
[0008] In accordance with a further aspect of the present invention, a concrete-filled steel base is also provided that is adapted to receive the portable guard rail support in circumstances where anchoring of the portable guard rail support to a floor or ground surface is not possible. The concrete-filled steel base has a retaining groove formed in a bottom surface thereof for slidably receiving the substantially flat bottomed base plate of the portable guard rail support. The steel base further comprises a channel integrally formed therein extending from a top surface of the steel base to the retaining groove and wherein the channel is in perpendicular relation to the retaining groove and dimensioned so as to be able to receive at least one kick-board.
[0009] In accordance with another aspect of the present invention, a portable safety barrier for use about a drop-off edge of a floor surface is provided comprising at least first and second portable guard rail supports located in spaced relation to one another along the drop-off edge and wherein each of the at least first and second portable guard rail supports comprises a substantially flat bottomed base plate, an upright column affixed to the substantially flat bottomed base plate, at least one guard rail support bracket affixed to the upright column, a kick board retaining flange affixed to the substantially flat base plate in spaced proximal relationship with the upright column, an angular brace affixed to the upright column and the substantially flat bottomed base plate, a safety tie-off ring affixed to the upright column and the substantially flat bottomed base plate, and wherein the at least one guard rail support bracket and the retaining flange of the at least first and second portable guard rail supports fixedly retain guard rails and kick boards.
[0010] Other aspects and features of the present invention will become apparent to those ordinarily skilled in the art upon review of the following description of specific embodiments of the invention in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] A better understanding of the invention will be obtained by considering the detailed description below, with reference to the following drawings in which:
[0012] FIG. 1 is a front perspective view of a portable guard rail support in accordance with the present invention.
[0013] FIG. 2 illustrates a rear perspective view of the portable guard rail support according to FIG. 1 .
[0014] FIG. 3 is a side view of the portable guard rail support according to FIG. 1 .
[0015] FIG. 4 depicts a portion of a safety barrier constructed with overlapping wooden guard rails in accordance with a preferred embodiment of the present invention.
[0016] FIG. 5 depicts a portion of a safety barrier constructed with wooden guard rails in accordance with another embodiment of the present invention.
[0017] FIG. 6 is a perspective view of a portable guard rail support having a concrete-filled steel base in accordance with an alternate embodiment of the present invention.
[0018] FIG. 7 depicts a portion of a safety barrier constructed with a safety mesh in accordance with a further aspect of the present invention.
DETAILED DESCRIPTION
[0019] Throughout the following detailed description, the same reference numerals are used to denote the same features in all of the drawings.
[0020] FIGS. 1 and 2 depict front and rear isometric views, respectively, of a guard rail support 10 according to a preferred aspect of the present invention. The guard rail support 10 consists of a rectangular upright column 12 , the lower end of which is affixed to a substantially flat rectangular metallic base plate 14 in a central symmetric axis thereof. The flat base plate 14 is provided with at least two bores or holes 24 a and 24 b for receiving suitable fastening means (not shown) in order to anchor or secure the guard rail support 10 to a floor or ground surface (not shown). In a preferred embodiment, the fastening means comprises expansion anchors well known to those skilled in the art. However, any suitable fastening means (e.g. screws) may be used. First and second L-shaped rail supporting brackets 16 are affixed one above the other to the upright column 12 as shown to provide supporting means for wooden guard rails (not shown). A retaining flange 17 , spaced apart from the upright column 12 , is affixed to the baseplate 14 of the guard rail support 10 in order to receive and secure a kick board (not shown) in position. The rail supporting brackets 16 and the retaining flange 17 have bores 19 formed therein for receiving fasteners to secure wooden guard rails within the rail supporting brackets 16 and the retaining flange 17 . An angle brace 20 is affixed between the upright column 12 and the base plate 14 in the manner shown to provide for structural stability of the guard rail support 10 . Finally, a fall protection (or safety) tie-off ring 22 is affixed to the lower end of the upright column 12 and to the base plate 14 .
[0021] Preferably, the L-shaped rail supporting brackets 16 and retaining flange member 17 are dimensioned to accommodate two adjacent, overlapping wooden rails which may be secured to each other and within the brackets 16 and retaining flange 17 by suitable fastening means such as nailing or the like. In a preferred embodiment, the wooden rails would be comprised of stock lumber such as lengths of two-by-four (2×4). In this case, the brackets would be dimensioned so as to accommodate two 2×4's i.e. a width, 2 w, of 4 inches and a height, h, of at least 4 inches. Thus, it may be seen that the rail supporting brackets 16 and retaining flange 17 may be dimensioned in any appropriate manner, 2 w×h, to accommodate any size, w×h, of stock lumber desired.
[0022] In order to implement a guard rail assembly (safety barrier) at a construction site according to a first aspect of the invention, a plurality of guard rail supports 10 are located at set distances apart (preferably slightly less than the length of stock lumber to be used for the guard rails) along the outer edge or perimeter of a floor undergoing construction. The guard rail supports 10 are secured to the floor via suitable fasteners driven through the bores 24 a , 24 b formed in the base plate 14 of each guard rail support 10 . Lengths of stock lumber (at least spanning the distance between the corresponding rail supporting brackets 16 and retaining flanges 17 of consecutively aligned guard rail supports 10 ) may then be positioned and secured within the corresponding rail supporting brackets 16 and retaining flanges 17 of adjacent guard rail supports 10 so as to form a guard rail assembly (safety barrier) consisting of upper and lower wooden guard rails and a kick board. The configuration of such a guard rail assembly is discussed further in relation to FIG. 4 .
[0023] As seen in FIGS. 1 and 2 , the fall protection tie-off (safety) ring 22 has the preferred shape of a sideways “U” with one end portion affixed to the lower end of the upright column 12 and the other end affixed to the base of the upright column 12 and the flat base plate 14 . The fall protection tie-off ring 22 provides for numerous advantages. Firstly, the fall protection tie-off ring 22 may serve as retaining and attachment means for a safety cable which is frequently used by workers at sites undergoing construction. In this respect, a continuous safety cable may be run through the fall protection tie-off rings 22 of consecutively aligned guard rails supports comprising a guard rail assembly (see FIG. 4 ) constructed in accordance with the present invention. A workman may then “tie off” to such a safety cable at any desired location thereby providing protection from accidental falls. Alternatively, a workman may tie off to the actual fall protection tie-off ring 22 of an individual guard rail support 10 , if desired. Secondly, the fall protection tie-off rings 22 of individual guard rail supports 10 comprising a guard rail assembly may be used to fasten weatherproof tarpaulins or the like (not shown) to protect workmen and the site under construction from inclement weather conditions.
[0024] FIG. 3 is a side view of the guard rail support 10 in FIGS. 1 and 2 wherein like features are denoted by like numerals.
[0025] FIG. 4 depicts a portion of a guard rail assembly or safety barrier 40 assembled along the perimeter of a floor 33 under construction in accordance with one aspect of the present invention. In FIG. 4 , first and second guard rail supports 10 a and 10 b are located at a set distance d apart and secured along an outer floor edge 34 via expansion anchors 31 driven through the corresponding bores 24 a , 24 b of each guard rail support 10 a , 10 b into the floor 33 . Upper and lower wooden rails 36 a and 37 a , (e.g. suitable lengths of 2×4) span at least the distance between corresponding rail supporting brackets 16 on the guard rail supports 10 a , 10 b . Similarly, kick board 39 a spans at least the distance between the retaining flanges 17 on the guard rail supports 10 a , 10 b . In a preferred embodiment, the distance d between guard rail supports 10 a and 10 b is slightly less than the lengths of 2×4 comprising the wooden rails such that the upper and lower wooden rails 36 a , 37 a and kick board 39 a will have some overshoot at each rail supporting bracket 16 or retaining flange 17 .
[0026] Considering guard rail support 10 a , upper and lower wooden rails 36 a , 37 a and kick board 39 a are secured with overlapping wooden rails 36 b , 37 b and 39 b within the corresponding rail supporting brackets 16 and retaining flange 17 via suitable fasteners 23 placed through bores 19 . Suitable fasteners 23 may include nails, screws, rivets or the like. Similarly, upper and lower wooden rails 36 a , 37 a and kick board 39 a are secured with overlapping wooden rails 36 c , 37 c and 39 c within the corresponding rail supporting brackets 16 and retaining flange 17 of guard rail support 10 b via suitable fasteners 23 placed through corresponding bores 19 . As shown, the left end of upper wooden rail 36 a overlaps with the right end of upper wooden rail 36 b at the uppermost rail supporting bracket 16 of the first guard rail support 10 a . Similarly, the right end of upper wooden rail 36 a overlaps with the left end of upper wooden rail 36 c at the uppermost rail supporting bracket 16 of the second guard rail support 10 b . It should be understood that the configuration described above for the upper wooden rails 36 holds for lower wooden rails 37 and kick boards 39 . It will further be appreciated that upper wooden rails 36 b and 36 c , lower wooden rails 37 b and 37 c and kick board 39 b and 39 c span the distance to other respective guard rail supports 10 (not shown) and may be secured within the corresponding rail supporting brackets and retaining flanges of the other guard rail supports 10 in the same manner as described above.
[0027] In cases where it is not desired or possible to use the overlapping wooden rail scheme depicted in FIG. 4 , for whatever reason, an alternative configuration may be used at each guard rail support 10 of the present invention to construct a safety barrier 50 as shown in FIG. 5 . In this case, a short stub 35 of the same stock lumber used for the wooden guard rails (e.g. 2×4) may be used at the rail supporting brackets 16 and retaining flange 17 of each guard rail support 10 in order to firmly secure the upper and lower wooden guard rails 36 , 37 and kickboard 39 in place. As before, at the rail supporting brackets 16 and retaining flange 17 of each guard rail support 10 , the upper and lower wooden rails 36 , 37 and kick board 39 may be secured to their corresponding short wooden stubs 35 and to the rail supporting brackets 16 and flanges 17 via suitable fasteners 23 such as nails or the like.
[0028] It will further be appreciated that the safety barrier configuration 50 depicted in FIG. 5 also represents the configuration present at the guard rail supports defining the ends of the safety barrier 40 constructed in accordance with the embodiment of FIG. 4 . As can be envisioned, at each guard rail support defining an end of the safety barrier 40 , there will be no overlapping wooden rail scheme at the rail supporting brackets 16 and retaining flange 17 . Thus, short stubs of stock lumber (preferably of the same type used for the wooden rails) will be needed to firmly secure the wooden rails within their respective brackets and retaining flanges.
[0029] FIG. 6 depicts a guard rail support 60 in accordance with a further aspect of the present invention. Again, like numerals are used to denote like features with the guard rail support 10 of FIGS. 1 and 2 . As can be seen, the guard rail support 60 comprises the guard rail support 10 of FIGS. 1 and 2 , slidably received within a concrete-filled steel base 68 . The steel base 68 provides for greater stability and adequate support in cases where it is not possible, for whatever reason, to secure the base plate 14 of the guard rail support 10 to a floor surface via fasteners (e.g. expansion anchors or screws) placed through holes 24 a , 24 b . As shown, the concrete-filled steel base 68 is constructed so as to have a groove formed on the bottom surface thereof for slidably receiving the base plate 14 of the guard rail support 10 . The groove extends to an open end 66 of the steel base 68 in order to provide means for allowing the guard rail support 10 to slide into the steel base 68 . It will be appreciated that the groove terminates before reaching an opposite end 69 of the steel base 68 such that the guard rail support 10 may only be slidably received within and removed from the steel base 68 at the open end 66 .
[0030] The concrete-filled steel base 68 has a first channel or cavity 67 formed along its central longitudinal axis and dimensioned accordingly to receive angular brace 20 , retaining flange 17 and tie-off ring 22 of the guard rail support 10 . Furthermore, the steel base 68 has a pass-through channel or cavity 64 formed therein proximal the flange 17 and dimensioned to correspond to the distance between the flange 17 and the upright column 12 . The pass-through cavity 64 advantageously provides for pass-through of kick board rails (not shown), as appropriate.
[0031] In the embodiment of FIG. 6 , the guard rail support 10 is securely maintained within the concrete-filled steel base 68 due to the precise tongue-groove type of fitting of the base plate 14 within the groove and the weight of the steel base 68 . Advantageously, the substantial weight afforded by the concrete-filled base 68 provides the necessary stability and support to maintain the guard rail support 10 in a fixed and upright position. It will be appreciated that a resilient, non-slip pad 63 may also be fastened by suitable adhesive means to the underside of the concrete-filled steel base 68 to provide a frictional wear resistant non-slip surface for contacting and engaging a floor surface. A plurality of such guard rail supports 60 may then be located along the outer edge of a floor under construction and a safety barrier constructed in the manner shown by either of FIG. 4 or 5 .
[0032] In accordance with a further aspect of the present invention, a mesh-like fence structure may be used in conjunction with any of the guard rail supports 10 or 60 described in relation to FIGS. 1 and 2 or 6 to form a mesh-like (or fence) safety barrier at any desired site under construction. For example, a portion of a fence-like safety barrier 79 constructed in accordance with the present invention is depicted in FIG. 7 . Again, like features are denoted by like numerals. As shown, a framed mesh 80 includes three projecting U-beams 78 affixed to opposite vertical sides thereof. The U-beams 78 are preferably made of metal and are supported and secured within the rail supporting brackets 16 and retaining flanges 17 of the guard rails supports 10 a , 10 b in the same overlapping manner as described in relation to FIG. 4 . In this case, however, holes corresponding to the holes 19 of the rail supporting brackets 16 and retaining flanges 17 are pre-drilled into each U-beam. In this manner, two overlapping U-beams may be placed within the rail supporting brackets 16 and retaining flanges 17 of each guard rail support 10 and secured with suitable fasteners. Thus, in this particular embodiment, the rail supporting brackets 16 and retaining flange 17 of each guard rail support 10 are dimensioned so as to accommodate two adjacent and overlapping U-beams. It will be appreciated that the mesh-like structure 80 of FIG. 7 need not include three U-beams projecting from each side, as shown. Two projecting U-beams may provide for sufficient stability and support. In this case, a single rail supporting bracket along with the retaining flange would be used, as required.
[0033] The guard rail supports 10 , 60 of the present invention each have two rail supporting brackets 16 affixed to their upright column 12 and a single retaining flange 17 affixed to their base plate 14 for supporting upper and lower wooden rails and kick boards, respectively. Although the retaining flange 17 on each guard rail support is a necessary requirement for supporting kick boards in accordance with safety standards and regulations, it will be appreciated that the precise number of rail supporting brackets 16 affixed to the upright column 12 of a given guard rail support is not material to the invention. Those skilled in the art will appreciate that construction safety regulations in most jurisdictions require guard rail systems of the type described to have a top rail, an intermediate rail and a toe or kick board as a minimum. Thus, at least two rail supporting brackets (for supporting upper and lower wooden guard rails) and a retaining flange (for supporting the kick board) are provided in the guard rail support of the present invention in order to adhere to safety regulations. However, more than two rail supporting brackets for supporting more than two rails in addition to the kick board may be employed in alternative embodiments without departing from the scope of the invention.
[0034] In addition, it will be appreciated that safety regulations in most jurisdictions require that the top rail of a guard rail barrier be located at least 3 feet but not more than 3.5 feet above the floor or ground surface to which the guard rail barrier is to be anchored while the intermediate rail be midway between the top rail and the floor surface. Thus, in a preferred embodiment of the present invention, the rail supporting brackets 16 are spaced along the upright column 12 of the guard rail support 10 , 60 in such a manner so as to adhere to the above-prescribed safety regulations when fitted with upper and lower rails. In addition, safety regulations generally dictate that the top and intermediate rails be at least 1.5 inches by 3.5 inches in dimension and that the kick board be at least 3.5 inches in height. Advantageously, the rail supporting brackets 16 and retaining flange 17 of the guard rail support 10 , 60 of the present invention are preferably dimensioned so as to accommodate 2″×4″ wooden rails, thereby conforming to safety regulations. It will be appreciated, however, that the rail supporting brackets and retaining flange may be dimensioned in any appropriate manner that meets the minimum safety guidelines in the jurisdiction of concern.
[0035] To further comply with safety regulations, it will be appreciated that the spacing between guard rail supports of the present invention when used in the construction of a safety barrier as described should not exceed approximately 8 feet. With regard to safety line anchorage points, most safety regulations specify that the anchorage must be capable of supporting a static load on the order of 17.8 kN (or 4000 lbs) in any direction, with proper provision to accept a safety line connection. Advantageously, the safety tie-off ring 22 of the guard rail support 10 , 60 of the present invention has been tested to support a static load of 5000 lbs.
[0036] A guard rail system constructed with the guard rail support of the present invention provides for easy installation at, and removal from, sites under construction. As will be appreciated, installation may be accomplished by a single worker, if necessary. A first step in the installation procedure is to locate a plurality of supports 10 at spaced intervals up to eight feet long about the perimeter of a ground surface under construction and to attach the baseplate of each support to the ground surface using suitable fasteners or anchors. Once a series of supports according to the present invention are located and secured to the floor of a building under construction, the upper and lower safety rails may be individually placed and secured within the brackets of adjacent supports in the manner shown in FIG. 4 , so that the rails extend completely about the perimeter of a floor under construction. Thus, the assembly of a safety guard rail fence or barrier, together with kick boards may be quickly mounted in place. An advantage of the preferred embodiment is that each support may be attached to the floor of an existing building structure prior to insertion of the wooden rails or safety fences, thereby minimizing weight and bulk so that a single worker may install a guard rail assembly without assistance from another worker. Additionally, once construction is completed, the disassembly of such a guard rail assembly as well as the removal of the guard rail supports, may also be carried our in an efficient manner.
[0037] Advantageously, the guard rail support and associated guard rail assembly of the present invention reduces or eliminates the liability which may result from inadequately re-installed guard rails. Specifically, at sites under construction, workmen sometimes need to temporarily remove portions of a guard rail in order to gain access to certain regions. With prior art conventional wooden rail assemblies, the workmen typically just hammer out the appropriate section when required. Inherently lazy, however, workmen do not usually return the guard rails back to their original state, thereby compromising the integrity of the guard rail assembly and causing safety concerns. The guard rail support 10 of the present invention provides for a fast and efficient disassembling and reassembling of a portion of a guard rail assembly if need be. Furthermore, by preventing the damage of lumber which would ordinarily result from such crude hammering out, the inventive guard rail support prevents the possible reassembly of a hammered out portion of a guard rail assembly with damaged lumber. The all-steel construction of the guard rail support of the present invention also ensures durability and repeated use for many years, thereby providing a high return on investment and cost savings.
[0038] The temporary guard rail support and associated assembly of the present invention have been described in connection with the provision of a safety guard rail along the outer drop-off edge or perimeter of a concrete floor slab which defines an upper story level of a building while it is under construction; the principle purpose being to protect workmen on the floor slab from falls. It will be appreciated, however, that the guard rail support and assembly may be useful in other embodiments and a guard rail support embodying the principles of the invention may, if desired and with or without modification as required, be employed for guard rail support purposes in a wide variety of other situations or environments as, for example, in the provision of a temporary guard railing around the perimeter of a roof structure, along the sides of a bridge construction until such time as the permanent guard railings are installed, or along any drop-off edge wherever it may occur.
[0039] While preferred embodiments have been described and illustrated, it will be apparent to one skilled in the art that numerous modifications, variations and adaptations may be made without departing from the scope of the invention as defined in the claims appended hereto.
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A guard rail support and assembly is disclosed for use in providing a safe work area for workmen working at dangerous heights, particularly in the construction industry. The guard rail support assembly comprises a plurality of guard rail supports arranged in a spaced fashion and wooden guard rails extending between and attached on either end to each support. Each guard rail support comprises an attachment base having quick fastening means for quick attachment and release of the support to a ground surface of the site under construction, a plurality of rail supports having quick fastening means for quick attachment and release of the wooden guard rails and a fall-protection or tarp tie-off ring. Advantageously, a portable and lightweight guard rail assembly may be constructed with the guard rail supports in an expedient and efficient manner to provide safe, unobstructive protection against falls.
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RELATED APPLICATION
This application is a continuation-in-part of application Ser. No. 07/958,279, filed on Oct. 8, 1992, now U.S. Pat. No. 5,271,744, which is a divisional application of application Ser. No. 07/692,674, filed on Apr. 29, 1991, and which issued as U.S. Pat. No. 5,176,643 on Jan. 5, 1993.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention involves an interactive external defibrillation and drug injection system for use by a human operator for treating cardiac conditions in a patient, particularly in an out-of-hospital or pre-hospital environment. The present invention may also be used within hospitals as well, particularly where intravenous (IV) access has not been established. More specifically, this invention comprises devices capable of measuring and monitoring various physiological indicators in a patient and an expert system capable of analyzing the measured data and making recommendations to an operator for treatment of the patient using any combination of defibrillation, cardioversion, transcutaneous pacing, or intraosseous drug injection. This invention is designed to enable first responders to cardiac emergencies to provide care up to the standard of at least the beginning stages of Advanced Cardiac Life Support (ACLS).
2. Description of the Prior Art
Patients experiencing cardiac emergencies need immediate care. Survival rates for patients experiencing a cardiac emergency improve with early delivery of ACLS care. Defibrillation and the initiation of drug therapies are important components of ACLS. Unfortunately, beneficial drug therapies may be delayed by factors such as delays between the time of arrival of skilled paramedics or other advanced care providers qualified to initiate drug therapies; delays resulting from transportation of a patient to a hospital or other facility where drug therapy may be initiated; and difficulty or failure to establish IV access to a patient experiencing a cardiac emergency.
Treatment of cardiac emergencies may encompass cardiopulmonary resuscitation (CPR), cardioversion, defibrillation, transcutaneous pacing, and/or drug delivery via intraosseous injection. First responders to medical emergencies are frequently not physicians. Such first responders lack the training to make an independent evaluation regarding treatment of the patient with cardioversion, defibrillation, transcutaneous pacing, or drugs. Delays in administering such treatment can result in brain damage or death to the patient.
Prior art defibrillators include microprocessor controlled or "smart" defibrillators comprising algorithms or expert systems capable of receiving and analyzing physiological data from a patient and making a decision or recommendation as to the type of corrective action that should be administered. One type of smart defibrillator is disclosed in U.S. Pat. No. 4,619,265 to Morgan, et al. Morgan discloses an interactive portable smart defibrillator which processes physiological data from the patient and then sends messages or "prompts" to an operator, allowing the human operator to make the final decision regarding the delivery of defibrillation therapy. The device disclosed in Morgan is limited to treatment of the patient with a defibrillator. As explained above, a patient experiencing an emergency cardiac condition often requires drug delivery in addition to defibrillation or cardioversion.
Another type of smart defibrillator is the Heartstart® 3000, manufactured by Laerdal Medical Corporation of Armonk, N.Y. Use of the Heartstart® 3000 is contraindicated where the patient is conscious or breathing or where the patient has a pulse or a pacemaker. In general, consciousness, breathing, pulse, and pacemaker are contraindications precluding the use of automatic external defibrillators of the prior art. Patients in need of emergency cardiac care often exhibit one or more of these contraindications.
Another type of smart defibrillator is disclosed in U.S. Pat. No. 5,156,148 to Cohen. The system disclosed in Cohen comprises a central processing unit (CPU) that controls drug delivery devices, cardioverting apparatus, defibrillating apparatus, pacers, and heart assist pumps. However, the system disclosed in Cohen must be attached or implanted into the patient with vascular access devices in place. This presupposes that a cardiac emergency is likely. Such a system would likely be used in intensive care unit or for a very select group of very sick patients. Unfortunately, many, if not most, cardiac emergencies are unexpected and it is unlikely that such system would be in place with pre-existing vascular access for drug delivery.
A system of the type disclosed in Cohen does not require the presence of a physician for its operation, nor does it allow for human intervention in the treatment process. The system disclosed in Cohen is an automatic system where the machine or CPU makes a decision on the treatment to be administered and then administers such treatment without allowing for human input or intervention. The absence of human input or intervention from the operation of the system disclosed in Cohen raises ethical and legal concerns which may limit the application or acceptance of such a system.
There is a critical need for better and more rapid methods of vascular delivery of drugs. The development of new, life saving drugs and better knowledge of how specific drugs work has established that many drugs can prevent death or reduce morbidity if given in a timely manner. Unfortunately, most drugs need to be infused directly into the blood of the general circulation to be effective, and this is not always easily accomplished. Vascular injections and cannulations are procedures requiring professional skills and training that are usually only possessed by doctors, nurses and paramedics. Even these professionals have a significant failure rate and generate time delays for drug delivery in emergency conditions, when veins are often collapsed due to low blood pressure, and several procedures need to be accomplished as soon as possible. Many other professionals and lay personnel, such as flight attendants, police, life guards and teachers, are trained in advanced first aid and CPR, but cannot deliver drugs, due to lack of an effective method that does not require more medical training. Clearly, there is a need for a simple, better and more rapid means of drug delivery to aid both skilled professionals and para-professionals to expand the utility of life saving drugs.
It has long been known that the marrow sinuses of bones are virtual non-collapsible veins. Fluids and drugs have been shown to enter the central circulation after intraosseous (IO) infusions as rapidly or even more rapidly than peripheral vein infusions. This IO method can be used to deliver drugs via the long leg bones, the sternum, or other bones.
Many special needles and devices have been made both to sample marrow and to infuse fluids into the marrow. All of these needles require substantial training and skill for their correct and safe use and take several seconds to minutes to use them properly. Examples of such prior art devices are disclosed in U.S. Pat. Nos. 2,426,535, issued Aug. 26, 1947 to Turkel; 2,773,500, issued Jan. 26, 1955 to Young; 3,750,667, issued Aug. 7, 1973 to Pshenichny et al.; 4,969,870, issued Nov. 13, 1990 to Kramer et al., and in the following articles: Tocantins, L. M. and O'Neill, J. F., "Infusion of Blood and Other Fluids into the General Circulation Via the Bone Marrow," Surg. Gynecol. Obstet., 73, 281-287 (1941); Turkel, H. and Bethell, F. H., "A New and Simple Instrument for Administration of Fluids Through Bone Marrow," War Medicine, 5, 222-225 (1944); Glaeser, P. W. and Losek, J. D. "Intraosseous Needles: New and Improved," 38 Pediat. Emerg. Care. 4, 135-136 (1989); Sacchetti, A. D., Linkenheimer, R., Lieberman, M., Haviland, P., Kryszozak, L. B., "Intraosseous Drug Administration: Successful Resuscitation from Asystole," Pediat. Emerg. Care, 5, 97-98 (1989); Halvorsen, L., Bay, B. K., Perron, P. R., Gunther, R. A., Holcroft, J. W., Blaisdell, F. W., Kramer, G. C., "Evaluation of an Intraosseous Infusion Device for the Resuscitation of Hypovolemic Shock," J. Traum., 30, 652-659 (1990). The above references describe manually inserted needles and techniques which require skill and training for proper use and necessitate many seconds to minutes in use. An automated needle system for delivery of drugs into the marrow would have great utility.
A variety of auto-injection syringes for intramuscular or subcutaneous injections are also known in the art. Examples of such syringes are disclosed in the following U.S. Pat. Nos.: 3,396,726, issued Aug. 13, 1968 to Sarnoff; 3,712,301, issued Jan. 23, 1973 to Sarnoff; 3,882,863, issued May 13, 1975 to Sarnoff et al.; 4,031,893, issued Jun. 28, 1977 to Kaplan et al. However, these syringes are not designed, nor could they be effectively or safely used for injecting into the marrow sinuses of bones, nor do they prevent needles used in the procedures from being exposed so that there is a danger of accidental needle punctures in use of these syringes.
The present invention overcomes the drawbacks of the prior art by providing an interactive external defibrillation and vascular drug injection system comprising an expert system., thereby enabling the system to be operated by a first responder who is not a physician. The expert system of the present invention receives physiological input data from measuring devices attached to the patient, analyzes the data, and issues instructions to the operator regarding patient treatment, including defibrillation, cardioversion, and drug injection.
The present invention may also be used with a patient in need of emergency cardiac care who is conscious, breathing, or who has a pulse or a pacemaker.
SUMMARY OF THE INVENTION
The present invention provides an interactive external defibrillation and drug injection system for use by a human operator for treating cardiac conditions in a patient. The system of the present invention comprises a measuring device attachable to a patient and capable of measuring or recording a patient's electrocardiogram (ECG). The system further comprises a CPU connected to receive input signals from the measuring devices indicative of measurements taken by those devices. The CPU is capable of analyzing these measurements and is further capable of transmitting control signals. The CPU is capable of deriving the patient's heart rate and heart rhythm from the ECG. The CPU also comprises a communication system capable of communicating information and instructions in a manner perceivable by a human operator. The communication system is also capable of receiving and analyzing input from a human operator relating to the cardiological treatment and condition of a patient.
It is the intent of the present invention that the information and instructions communicated by the CPU will be consistent with updated versions of the American Heart Association's current "Guidelines for Cardiopulmonary Resuscitation and Emergency Cardiac Care Recommendations of the 1992 National Conference," as recently published in the Journal of the American Medical Association, Oct. 28, 1992, Vol. 268, No. 16, pp. 2171-2302 and periodic updates. These guidelines will hereinafter be referred to as the "AHA Guidelines for CPR/ECC." In addition to these guidelines, it is the intent of the present invention that the CPU will also communicate instructions regarding the use of intraosseous autoinjectors to inject drugs into a patient.
The system of the present invention further comprises at least two electrical leads connectable to a patient and capable of delivering a sufficient amount of electrical energy to a patient to cardiovert or defibrillate a patient's heart. The system further comprises an electrical source comprising a discharge outlet electrically connected to the electrical leads and a control signal input electrically connected to the CPU. The electrical source is capable of storing and discharging electrical energy through the leads in sufficient predetermined selectable quantities and at sufficient predetermined selectable rates to defibrillate or cardiovert a patient's heart in a manner consistent with selected control signals and instructions from the CPU.
The system of the present invention further comprises one or more intraosseous autoinjector devices, each containing a premeasured amount of a predetermined drug. Each autoinjector device also comprises one or more identifiers such that each autoinjector drug can be promptly identified by a human operator in response to an instruction from the CPU.
Through use of the autoinjector of the present invention, a device and method is provided for very rapid, automated, and safe infusion of fluid and drugs into the circulatory system, e.g., into bone marrow. The autoinjector of the present invention further provides a device and method that will automatically puncture a bone, place a needle into the marrow, and infuse fluid into the circulatory system via the marrow. The autoinjector of the present invention automatically covers the needle before and after use to prevent accidental needle punctures. This autoinjector can be used either with the sternum or the tibia. The autoinjector of the present invention reduces the anatomical variability of skin thickness by compressing the skin over the bone in use.
The autoinjector of the present invention also provides a device and method that imparts velocity to a needle and syringe component such that the momentum rapidly places the needle through the skin and bone and into the marrow. The needle of the autoinjector of the present invention is adapted for use with such an autoinjector. This needle also facilitates drug delivery into the marrow, yet prevents backflow of fluids out of the bone.
In a first aspect of the autoinjector of the present invention, the autoinjector has a main housing with a front end. There is a forward directed aperture on the front end of the main housing. A syringe body has a front end and a rear end. The syringe body is slidably positioned in the main housing. A needle has a central bore communicating with at least one opening proximate to a tip of the needle. The needle is attached to the front end of the syringe body, communicates with an interior of the syringe, and is positioned to extend through the aperture of the main housing. A drive plunger extends from the rear of the syringe body. A means on the main housing and engaging the drive plunger locks and unlocks the drive plunger in position at the rear end of the syringe body. A means is connected to the drive plunger for applying propelling force to the drive plunger to move the syringe body along the main housing in a first direction to extend the needle from the aperture when the device is pressed against a patient to expel the drug from the syringe body into the patient. A means is connected to the syringe body to move the syringe body in a second direction opposite to the first direction for withdrawing the needle into the aperture when the device is no longer pressed against a patient.
In a second aspect of the autoinjector of the present invention, a device for delivery of a drug in liquid to bone marrow comprising a main housing with a front end is provided. There is a forward directed aperture on the front end of the main housing. The syringe body of the present invention has a front end and a rear one° The syringe is slidably positioned in the main housing. A needle having a central bore communicating with at least one opening proximate to a tip of the needle is attached to the front end of the syringe body, communicates with an interior of the syringe body, and is positioned to extend through the aperture of the main housing in appropriate distance for passing through a patient's skin, penetrating a bone and entering the marrow inside the bone. A means imparts a force to the syringe body and to the needle, to extend the needle through the aperture of the main housing the appropriate distance at a sufficient velocity to pass through the patient's skin, penetrate the bone and enter the marrow. A means discharges the drug in liquid form from the autoinjector of the present invention through the needle and into the marrow.
In a third aspect of the autoinjector of the present invention, a needle for use in a device for delivery of a drug in liquid form with a taper along its length and a conical, orifice-free tip, is provided. A central bore communicates with a plurality of orifices proximate to the tip. The plurality of orifices are positioned circumferentially on the needle at different distances from the tip.
In a fourth aspect of the autoinjector of the present invention, a method for delivering a drug in liquid form to bone marrow includes positioning a syringe including a needle above a patient's skin at a location over a bone containing marrow. Sufficient velocity is imparted to the syringe so that the needle will have sufficient momentum to pass through the patient's skin, penetrate the bone and enter the marrow. The drug in liquid form is discharged from the syringe, through the needle and into the bone marrow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-section view of a first embodiment of a device for rapid vascular drug delivery of the invention.
FIGS. 2-5 are similar cross-section views of the device of FIG. 1 at different stages in its use.
FIG. 6 is an external perspective view of a second embodiment of a device for rapid vascular drug delivery of the invention.
FIG. 7 is an exploded perspective view of the device of FIG. 6.
FIGS. 8-12 are cross-section views of a portion of the device of FIGS. 6-7.
FIG. 13 is an enlarged side view of a portion of the devices of FIGS. 1-12 in use.
FIG. 14 is a block diagram of one embodiment of the present invention.
FIG. 15 is a more detailed illustration of the internal configuration of the CPU of the present invention.
FIG. 16 is a block diagram of one embodiment of the autoinjector housing of the present invention.
FIG. 17 is an isometric view of one embodiment of the present invention.
FIGS. 18A-18I, when taken together, constitute a flow chart of algorithms employed by the expert system of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Turning now to the drawings, more particularly to FIG. 1, there is shown a an intraosseous autoinjector 10 for rapid vascular drug delivery. The intraosseous autoinjector 10 incorporates a cylindrical syringe body 12, fitted with a double side-holed pencil point needle 14. The syringe body is held in a cylindrical main housing 16 having a front barrel 18 with an orifice 20 through which the needle 14 may be extended. A cylindrical actuation handle 48 fits over end 24 of the main housing 16 for sliding movement along the main housing. A syringe plunger 26 contacts drive plunger 28 and extends into the syringe body 12 to confine liquid medication 32 in the syringe body 12. A main spring 34 extends between the drive plunger 28 and partition 36 on the actuation handle 48 to bias the actuation handle 48 in its extended position along the main housing 16 as shown in FIG. 1. A needle return spring 38 extends between the front barrel 18 and a collar 40 on the syringe body 12 to bias the needle to its retracted position as shown in FIG. 1. The main spring 34 exerts a stronger biasing force when compressed than the needle return spring 38. The drive plunger 28 has an annular peripheral socket 42 for one or more lock balls 44, which engage one or more openings 45 on the main housing 16 to lock the drive plunger in position with respect to the syringe body 12. A mating annular lock ball trip pocket 46 is positioned on inside surface of the actuation handle 48 to allow the intraosseous autoinjector 10 to be fired when the lock ball(s) in socket 42 reach the pocket 46. In FIG. 1, the intraosseous autoinjector 10 is shown in its uncocked position.
In use, the intraosseous autoinjector 10 is placed with the end of the front barrel 18 on the midline of the sternum at the second or third intercostal space, and then the intraosseous autoinjector 10 is pushed against the sternum. Compression of the spring 34 behind the syringe body 12 occurs as the front barrel 18 is pushed toward the actuation handle 48 and generates a force that will be used for needle 14 advancement and drug 32 injection. When an adequate force has been stored in the spring 34, the front barrel 18 has been pushed back to a point so that the lock ball(s) 44 are able to enter the trip pocket 46, as shown in FIG. 2. This entry releases the lock ball(s) 44, so that the main spring 34 is free to drive the syringe body 12 and the needle 14 forward with a force of approximately 25 to 40 pounds until collar 40 rests against ridge 50, as shown in FIG. 3.
The needle 14 is extended from about 8 mm to about 25 mm in order to ensure that side holes in the needle are in the marrow. The main spring 34 then pushes the syringe plunger 26 forward to the position shown in FIG. 4 to deliver the drug 32 through the extended needle 14 to the marrow in the sternum. Needle placement takes about 1/10th of a second, while drug delivery usually occurs in less than a second. Operation in this manner causes the syringe body 12 to reach a sufficient velocity so that the penetration of the needle 14 into the marrow occurs in a single, rapid, uninterrupted motion due to momentum of the syringe body 12 and needle 14. Relying on momentum in this manner means that a smaller diameter needle can be used than would be required if the penetration resulted from application of penetrating force on the needle while it was at rest against the skin or bone. Upon completion of drug delivery, the operator releases the pressure against the sternum, and the needle retraction spring 38 withdraws the needle 14 into the barrel 18 of the main housing 16 to the position shown in FIG. 5.
FIGS. 6-12 show another intraosseous autoinjector 100 for the rapid delivery of a drug to the marrow. The intraosseous autoinjector 100 incorporates a locking, cylindrical protective cover 102 over front barrel 104 to ensure that needle 14 is never exposed except when the intraosseous autoinjector 100 is both pressed against the patient's body and actuated. A cover return spring 106 is positioned between the protective cover 102 and shoulder 108 on cylindrical main housing 110 of the device. The protective cover 102 has an end 112 that extends into actuation handle 114 of the intraosseous autoinjector 100. End 112 is equipped with a tab locking mechanism 116 that, once actuated, prevents the protective cover 102 from being moved from its extended position as shown in FIG. 8 to its withdrawn position, against the barrel 104, as shown in FIG. 9. The locking mechanism 116 consists of two parts: a lock 118 circumferentially positioned around the end 112 between the protective cover 102 and the actuation handle 114, and a sleeve 120 concentrically positioned over the lock 118. The lock 118 has a plurality of spring tabs 122 extending rearward of the actuation handle 114 from a cylindrical base 124. The sleeve 120 has a plurality of projections 126, which are not springs, extending rearward beyond the tabs 122 from a similar cylindrical base 128. With the parts of the intraosseous autoinjector 100 in the positions shown in FIG. 8, prior to use of the intraosseous autoinjector 100, the cylindrical base 128 of the sleeve 120 rests over the spring fingers 122 of the lock 118, holding them down. A sealing membrane 134 is provided inside the barrel 104, over orifice 136, to protect the needle 14 prior to use of the device.
In use of the intraosseous autoinjector 100, with the spring fingers 122 in their down position, the protective cover 102 is free to retract against the barrel 104 to the position shown in FIG. 9, when the protective cover 102 is pressed downward against, e.g., the sternum or the tibia. As the protective cover 102 moves toward the barrel 104, the projections 126 of the sleeve 120 engage shoulder 130 of the actuating handle 114, so that the base 128 of the sleeve 120 is pushed down over the base 124 of the lock 118, allowing the spring fingers 122 of the lock 118 to spring outward, as shown in FIG. 9. Continued downward pressure of the intraosseous autoinjector 100 on the sternum or tibia moves the protective cover 102 and the barrel 104 into the actuating handle 114, as shown in FIG. 10, until the main body 108 and the actuating handle reach the firing position, as in the FIGS. 1-5 embodiment. At that time, firing occurs, the needle 14 is extended into the sternum or tibia, and the drug is ejected into the marrow through the needle 14, as shown in FIG. 11 in the same manner as in the FIGS. 1-5 embodiment. When the intraosseous autoinjector 100 is no longer pressed against the patient, the protective cover 102 is returned to its original position by the force of spring 106, as shown in FIG. 12. Because the spring tabs 122 have sprung outward, they engage shoulder 132, on the actuating handle, to lock the protective cover 102 over the needle 14. Thus, the needle is never exposed except when the intraosseous autoinjector 100 is actually pressed against the patient, and the needle 14 cannot be re-exposed after actuation, even if the device is again pressed against the patient or any object. In addition to the main spring 34, a secondary spring 138, separated from the main spring by member 140, is provided to ensure that there is still a spring force urging the needle 14 forward when it is fully extended. Except as shown and described, the construction and operation of the FIGS. 6-10 embodiment of the invention is the same as that of the FIGS. 1-5 embodiment.
FIG. 13 shows details of the needle 14 used in the devices 10 and 100. The needle 14 has a slight taper along its length toward a conical, orifice free tip 150. The taper promotes a good seal between the needle 14 and bone 156. The tip 150 of the needle 14 is free of an orifice because orifices located there would tend to clog during penetration of the bone 156. Orifices 158 are located behind the conical tip 150 and communicate with a central bore 160 extending the length of the needle to communicate with the reservoir of drug 32 (FIG. 1). The orifices 158 are staggered around the circumference of the needle 14 and connect to slits 162 extending vertically along the side of the needle. This configuration and placement of the orifices 158 and the slits 162 allow discharge of the drug 32 from an orifice 158, even if it is partially blocked by a tissue globule 164 in the marrow 166.
Examples of drugs that can be life saving for specific medical and cardiac emergencies if administered into the circulation in a timely manner, and hence, candidates for packaging in the devices 10 and 100, are shown in the following table:
__________________________________________________________________________DRUG MEDICAL EMERGENCY__________________________________________________________________________Adenosine Symptomatic Paroxysmal Supra Ventricular Tachycardia (PSVT)Aminophylline Asthma, congestive heart failure (CHF)Amrinone CHF not associated with myocardial infarction (MI)Atropine Bradycardia, organophosphate poisoning, third degree heart block, asystoleBretylium Ventricular fibrillationBumetanide CHF, pulmonary edemaButorphanol Moderate to severe painCalcium Chloride Acute hyperkalemia, hypocalcemiaChlorpromazine (Thorazine ®) Acute psychotic episodesDexamethasone AnaphylaxisDiazepam (Valium ®) SeizuresDiazoxide (Hyperstat ®) Hypertensive emergencyDigoxin CHF, atrial flutter/fibrillationDiphenhydramine (Benadryl ®) AnaphylaxisDobutamine CHFDopamine Cardiogenic shock, hypovolemic shockEdrophonium Cardiac arrest, shock, anaphylaxis, etc.Esmolol Symptomatic supraventricular tachycardiaFurosemide CHF, pulmonary edemaGlucagon HypoglycemiaHaloperidol (Haldol ®) Acute psychotic episodesHydralazine Hypertiesive emergencyHydrocortisone Severe anaphylaxisInsulin Diabetic ketoacidosisIsoproterenol BradycardiasLabetalol Hypertensive crisisLidocaine Ventricular arrhythmias, MIMagnesium sulfate EclampsiaMannitol Acute cerebral edema, blood transfusion reactionsMeperidine (Demerol ®) Severe painMetaraminol Cardiogenic shockMethylprednisolone Severe anaphylaxisMetoprolol (Lopressor ®) Acute MIMorphine Severe pain, pulmonary edemaNalbuphine Moderate to severe painNaloxone (Narcan ®) Narcotic overdose, comaNorepinephrine (Levophed ®) Hypotension, neurogenic shockOxytocin Postpartum vaginal bleedingPhenobarbitol Seizures, acute anxietyPhenytoin (Dillantin ®) Major seizuresPhysostigmine Tricyclic overdose, belladonna or atropine overdosePralidoxime (2-PAM, Organophosphate poisoningProtopam ®)Procainamide Ventricular arrhythmiasPromethazine (Phenergan ®) Nausea and vomitingPropanolol (Inderal ®) Cardiac arrhythmiasSodium Bicarbonate Cardiac arrest, antidepressant overdoseSodium Nitroprusside Hypertensive emergencySuccinylcholine To induce paralysisThiamine (vitamin B1) Coma, alcoholism, delirium tremorsVerapamil PSVT__________________________________________________________________________
Many of the above medical emergencies are and can be life threatening. The vascular delivery of the above drugs can be life saving. Even a few seconds delay in therapy can be a matter of life or death in a medical emergency. The intraosseous autoinjector of the present invention can be used to administer these drugs into the central circulation, often in less than 1 or 2 seconds. The administration of drugs in this manner can be safely and effectively performed by a lay person with minimal training and, overall, offers a safe, effective, and extremely rapid means to treat medical emergencies.
Because momentum is used to advance the needle through the cortical bone and into the marrow, even a small gauge needle, such as a 20 to 25 gauge simple pencil-point with side holes, could be properly placed. Because the effective dose of most of the previously listed drugs could be carried in exceedingly small volumes, such as 0.1 to 0.2 ml or less, such a small gauged needle could be used for rapid drug delivery. Alternatively, a larger needle (12 to 18 gauge), either a simple pencil-point or the design previously described, could be used to administer rapidly 1.0 to 5.0 ml of fluid. The invention and these needles can be used to effectively deliver drugs into circulation in as short a time as 1 to 2 seconds or less.
While the intraosseous autoinjector of the present invention has been shown in two preferred forms, various modifications of it could be made. For example, the device could be construed so that it is cocked or loaded prior to placing it in contact with the patient, and merely fired after it is pressed against the patient with a suitable pressure. The devices 10 and 100 have been shown and described as configured for IO infusion. The same principle of an automatic syringe that is automatically spring loaded for injection by pressing against the patient could be adapted to an automatic syringe for subcutaneous or intramuscular injection as well.
The intraosseous autoinjector of the present invention punctures a bone containing marrow, places a needle into the marrow, and infuses fluid into the circulatory system via the marrow. The device covers the needle before and after use to prevent accidental needle punctures.
A block diagram of an interactive external defibrillation and drug injection system for use by a human operator for treating cardiac conditions or other medical emergencies in a patient is shown in FIG. 14. A measuring device 220 is attached to a patient 200. The measuring device is capable of measuring a patient's ECG. In a preferred embodiment, the measuring device is also capable of measuring a patient's blood pressure. A CPU 230 is connected to receive input signals from the measuring device indicative of measurements taken by the measuring device. As shown in FIG. 15, these input signals may include an ECG input 222 and a blood pressure input 224.
The CPU is capable of analyzing the measurements received from the measuring device and of transmitting control signals. In a preferred embodiment, the CPU comprises a programmable expert system 234 that is capable of analyzing measurements from the measuring devices to identify cardiac dysrhythmias, and a signal processor 233 capable of receiving an input signal indicative of a patient's ECG. The expert system is also capable of receiving ECG data from the signal processor and identifying the QRS complex and the R wave. The expert system is further capable of analyzing inputs from the measuring devices to determine heart rate and heart rhythm, or to diagnose atrial contraction, or a ventricular contraction. The signal processor is further capable of transmitting a control signal to the electrical source. The dysrhythmias and conditions that the expert system is capable of identifying include ventricular fibrillation (VF), ventricular tachycardia (VT), acute myocardial infarction (MI), bradycardia, tachycardia, pulseless electrical activity (PEA), asystole, hypotension, shock, and acute pulmonary edema (APE).
In a preferred embodiment, the expert system comprises a multiplicity of cardiological treatment and diagnostic algorithms capable of receiving input data from the measuring device and from a human operator, and further capable of Generating instructions to a human operator via the communication system 235. These algorithms are depicted in FIGS. 18A-18I. In the embodiment shown in FIG. 17, the buttons labeled "1" and "2" are intended for use by a qualified person, such as a medical director of an emergency medical services department, to program the expert system of the present invention. In a preferred embodiment the programming means is located in the back of the device in a compartment that is masked by a locked panel.
FIG. 18A is a block diagram depicting the scope of treatment and diagnostic algorithms encompassed by the expert system of the present invention. These algorithms may be modified to conform with the most current standards of CPR/ECC, as published by The American Heart Association in journals known in the art, such as the Journal of the American Medical Association. Additionally, some modifications to these algorithms may be programmed by the end user under the direction of qualified medical personnel, to reflect "standing orders" or standards of practice of CPR/ECC of an end user EMS system.
The interactive nature of this expert system is illustrated by block 300, depicting an assessment of a patient's responsiveness by a first respondence and by block 360 depicting various instructions or prompts Generated by the expert system to the first responder regarding treatment to be administered to a patient. The assessments depicted by blocks 315-345 in FIG. 18A, reflect action that a first responder would be trained to take without the assistance of an expert system. Block 350 depicts the attachment of measuring devices of the present invention such that the expert system can perform the analysis and provide the instructions depicted in block 360. The various dysrhythmias that may be diagnosed by the expert system are depicted at blocks 361-367 of FIG. 18A. Each of these dysrhythmias is shown in greater detail in FIGS. 18B-18I.
FIG. 18B depicts the general algorithm for use in treating VF and VT. The interactive nature of the present invention is illustrated by the prompts and instructions shown at blocks 410, 420, 440, and 450. These instructions encompass the use of electrical shocks, as well as the administration of drugs. It is the intent of the present invention that where instructions to administer drugs, such as those shown in blocks 440 and 450 are given, the first responder would administer such drugs using the autoinjectors of the present invention. The instruction depicted by block 445 is an instruction to perform the analysis depicted at block 360 at FIG. 18A.
The algorithm of the expert system for the treatment of PEA is shown in FIG. 18C. PEA is also known as electromechanical dissociation to those of ordinary skill in the cardiological art. Block 520 illustrates an instruction from the expert system to administer a drug using the autoinjector, as well as CPR.
The algorithm of the expert system for the treatment of asystole is illustrated in FIG. 18D. Block 620 and 630 illustrate instructions from the expert system to administer drugs to a patient using the autoinjector. Block 650 and 655 instruct the operator to perform the analysis shown in block 360 of FIG. 18A.
The algorithm of the expert system for the treatment for acute MI is illustrated in FIG. 18E. As shown in block 710, this algorithm utilizes blood pressure input 224, as also depicted in FIG. 15. Block 720 illustrates prompts from the CPU to the operator to administer drugs to a patient, using the autoinjectors of the present invention.
The algorithm of the expert system for the treatment of bradycardia is illustrated in FIG. 18F. As shown in block 800, this algorithm utilizes heart rate. In response to the prompts shown in block 810, it is the intent of the present invention that the operator would input data into the CPU using data input terminal 238 of FIG. 15. The expert system would then use this data to proceed with the algorithm, as shown in blocks 820-850.
The algorithm of the expert system for the treatment of tachycardia where the heart rate of the patient is greater than 150 beats per minute, is illustrated in FIG. 18G. As shown in block 910, this algorithm utilizes heart rate input or blood pressure input 224, as also depicted in FIG. 15. The synchronized cardioversion referred to in block 920 is performed in conjunction with the output of a control signal from signal processor 233 to electrical source 240.
The algorithm of the expert system for the treatment of tachycardia where the heart rate of the patient is less than 150 beats per minute as measured by measuring devices 200 is illustrated in FIG. 18H. In contrast to treatment for tachycardia where the heart rate of the patient is greater than 150 beats per minute, treatment for tachycardia where the heart rate of the patient is less than 150 beats per minute, initially includes drugs rather than cardioversion.
The algorithm of the expert system for the treatment of hypotension, shock, or acute pulmonary edema is illustrated by FIG. 18I. As shown in blocks 1133-1139, blood pressure input 224 is used by this algorithm to determine which drugs are to be administered by the autoinjectors.
In a preferred embodiment, the communication system of the CPU comprises a data display device 236 capable of displaying data from the measuring device and instructions generated by the algorithms of the expert system, as shown in FIGS. 15 and 17. In a preferred embodiment, the data display device comprises an LCD visual display 239 and an audio communicator 237. Input from a human operator 231 is received via a data input terminal 238.
In a preferred embodiment, the data input terminal is a keyboard, or, alternatively, one or more buttons that can be pushed by a human operator to signal an affirmative or a negative response to an inquiry or "prompt" generated by the expert system. The buttons labeled "yes" and "no," 238 in FIG. 17, may be pushed by a human operator to indicate an affirmative or negative response, respectively, to a query generated by the CPU. The audio communicator is capable of communicating data and instructions to a human operator in an audibly perceivable manner.
In a preferred embodiment, the invention comprises a data storage device 262 that stores all data received by the CPU from the measuring devices or from an operator and all instructions and control signals generated by the CPU, as shown in FIG. 14. This data is stored in a retrievable fashion such that an operator can later determine what measurements and input were received by the CPU, as well as what instructions were given by the CPU. In a preferred embodiment, the data storage device further comprises a clock capable of storing the time at which all data was received by and all instructions were generated by the CPU, in a retrievable fashion.
The invention may further comprise an audio recorder 227, capable of recording audible events occurring near the CPU. Such events would include audio commands from the communication system of the CPU and statements made to and from the operator of the invention.
In a preferred embodiment, a printer 260 may be attached to the CPU such that any retrievably stored data in the CPU can be printed out on a "hard copy." In another embodiment of the present invention, the data storage device 262 is a digital data recorder 262, which is electrically coupled to the CPU, as shown in FIG. 15. In a preferred embodiment, the digital data recorder is automatically activated whenever the CPU is turned on. The digital data recorder records all signals transmitted by measuring devices to the CPU, all input from an operator to the CPU, all instructions generated by the CPU, and the times that all data inputs, operator inputs, control signals, and instructions were received or generated by the CPU, in a retrievable fashion.
The interactive external defibrillation and drug injection system of the present invention further comprises at least two electrical leads 244 connectable to a patient 200 and capable of delivering a sufficient amount of electrical energy to a patient to cardiovert or defibrillate a patient's heart. These leads may be repositioned on the patient, or an additional lead may be used, to confirm the presence of asystole. In a preferred embodiment, the present invention comprises more than two electrical leads. Such an embodiment is particularly useful when the operator wishes to diagnose MI.
The system of the present invention further comprises an electrical source 240 comprising a discharge outlet 242 electrically connected to the electrical leads. The electrical source further comprises a control signal input 246 electrically connected to the CPU. The electrical source is capable of storing and discharging electrical energy through the discharge outlet to the leads in sufficient predetermined selectable quantities and at sufficient predetermined selectable rates to defibrillate or cardiovert a patient's heart in a manner consistent with selected control signals and instructions from the CPU.
In a preferred embodiment, the electrical source is further capable of discharging electrical energy through the discharge outlet to the leads in sufficient predetermined selectable quantities and at sufficient predetermined selectable rates to transcutaneously pace a patient's heart in a manner consistent with selective control signals and instructions from the CPU. In this embodiment, the control signal generated by the CPU to regulate the transcutaneous pacing is indicative of the P wave, the QRS complex, the R wave, atrial contraction, and/or ventricular contraction of a patient's heart.
In one embodiment of the present invention, the electrical source and CPU are housed in a portable console 245 as shown in FIG. 17. In another embodiment, the electrical source and communication system are configured in a housing like that of the Heartstart® 3000 system.
In the preferred embodiment of FIG. 17, the electrical source further comprises a rechargeable battery 241 and a multiplicity of control devices 243 operable to permit a human operator to select the magnitude and duration of electrical energy discharged by the electrical source. Alternatively, this selection can be made by the expert system, and transmitted to the electrical source. The human operator would merely push button 256 on the console to deliver an electrical shock of the magnitude and duration selected by the expert system.
A console of the type shown in FIG. 17 may contain receptacles at its rear to receive leads from the measuring devices. In a preferred embodiment, this console would comprise at least three connections for three ECG leads. In another preferred embodiment, the console shown in FIG. 17 comprises an audio recorder, located at its rear. The audio recorder would automatically be activated anytime inputs are received by the CPU or instructions are generated by the CPU.
In the preferred embodiment shown in FIG. 17, the autoinjector housing 250 comprises a multiplicity of autoinjectors, including an autoinjector containing a premeasured amount of epinephrine (EPI), an autoinjector containing a premeasured amount of atropine (ATR), an autoinjector containing a premeasured amount of morphine (MOR), an autoinjector containing a premeasured amount of tissue plasminogen activator (tPA), an autoinjector containing a premeasured amount of lidocaine (LID), and an autoinjector containing a premeasured amount of adenosine (ADE). Each of these autoinjectors is an intraosseous autoinjector. The embodiment of the invention shown in FIG. 17 shows the preferred number of autoinjectors containing each drug.
The system of the present invention further comprises at least one intraosseous autoinjector which contains a premeasured amount of a predetermined drug. Each autoinjector device comprises an identifier, such that it can be promptly identified by a human operator in response to an instruction from the CPU. In a preferred embodiment, each autoinjector is removably housed in a portable autoinjector housing 250 comprising a visual labeling system 254 such that the drug contained within each autoinjector is readily perceivable by a human operator.
It is envisioned that the present invention is particularly applicable to pre-hospital or out-of-hospital treatment of a patient experiencing a cardiac emergency. When such a patient is delivered to a hospital or to the care of a person more highly trained than a first responder, such as a paramedic or a physician, it is particularly important for the paramedic or physician to known what drugs have been administered to the patient. The autoinjector housing embodiment of the present invention provides a means for a paramedic or other professional to readily ascertain what drugs have been administered from the number and color of empty autoinjector receptacles in the housing, as well as from a printout of all data and first responder or operator inputs recorded by the CPU.
In one embodiment of the present invention, the portable autoinjector housing is electrically coupled to the CPU, as shown in FIG. 15, such that it can receive a signal from the CPU indicative of which drug to administer to a patient. In this embodiment of the present invention, an electrical light 253 is situated in close proximity to each autoinjector and electrically connected to the CPU such that each light may be selectively illuminated by the CPU pursuant to instructions from the expert system to visually indicate which drug should be administered to a patient, as shown in FIG. 17. In one embodiment, these lights may be LEDs. These lights may be electrically coupled to the CPU such that they blink to indicate that an autoinjector should be used to administer drugs to a patient and they remain illuminated to indicate that an autoinjector has already been used to administer drugs.
In another embodiment of the present: invention, each autoinjector may be a unique color indicative of the drug it contains. In this embodiment, the unique color associated with each drug is programmed into the expert system such that the expert system can issue instructions regarding drug injection that identify a particular autoinjector by its color. This embodiment is not preferred when the operator is color blind; however, color coding may be used in conjunction with other forms of autoinjector identification, such as the electrical lights, described above, in order to provide redundant means of autoinjector identification.
In yet another embodiment, the autoinjector housing comprises a multiplicity of extendable jacks 251. One extendable jack is installed in each compartment, directly adjacent an autoinjector, as shown in FIG. 16. Each jack is mechanically coupled to a transducer 257 that is electrically coupled to the CPU such that each transducer can receive an extension signal for a specific autoinjector from the CPU, and transmit the signal to a specific jack, causing it to telescopically extend, thereby extending the adjacent autoinjector to a more prominent position relative to the other auto:injectors in the autoinjector housing. This extension provides a visual signal to a human operator to remove the extended autoinjector from the housing and administer the drug contained within that autoinjector to a patient.
In this embodiment, the CPU memory records which jack was actuated, the time it was actuated and the particular drug contained within the autoinjector stored adjacent that Jack. The CPU is also capable of providing prompts from its visual display in conjunction with the operation of the jack, instructing a human operator to remove the autoinjector that has been extended by operation of the jack. In this embodiment, the CPU would send inquiries to the human operator asking him to verify whether he has administered the drug contained within the extended autoinjector to a patient. The CPU memory would be capable of retrievably storing a human operator's answer and the time of the answer to such an inquiry.
Many modifications and variations may be made in the embodiments described herein and depicted in the accompanying drawings without departing from the concept of the present invention. Accordingly, it is clearly understood that the embodiments described and illustrated herein are illustrative only and are not intended as a limitation upon the scope of the present invention.
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This invention involves an interactive external defibrillation and drug injection system for use by a human operator for treating cardiac conditions in a patient, particularly in an out-of-hospital or pre-hospital environment. The present invention may also be used within hospitals as well as where intravenous (IV) access has not been established. More specifically, this invention comprises measuring devices capable of measuring and monitoring various physiological indicators in a patient and an expert system capable of analyzing the measured data and making recommendations to an operator for treatment of the patient using any combination of defibrillation, cardioversion, transcutaneous pacing, or vascular drug delivery via intraosseous drug injection. This invention is designed to enable first responders to cardiac emergencies to provide care up to the standard of at least the beginning stages of Advanced Cardiac Life Support (ACLS).
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CROSS REFERENCE TO RELATED APPLICATIONS
This is a continuation of copending application Ser. No. 139,543, filed on Dec. 30, 1987 abandoned.
This application is related to commonly assigned, concurrently filed U.S. patent application Ser. Nos. (139,570, 139,567 and 139,566) which are concerned with the production of alcohol(s) and/or ether(s).
BACKGROUND OF THE INVENTION
This invention relates to a process for the production of ether(s) and, optionally, mixtures of alcohol(s) and ether(s) of predetermined composition. More particularly, the invention relates to a process for the conversion of a light olefin such as ethylene, propylene, butenes, pentenes, hexenes, heptenes, etc., and their mixtures, in a conversion unit employing an acidic zeolite as olefin conversion catalyst to produce a mixture of alcohol(s) and ether(s) and thereafter recovering the ether(s) containing at most only small amounts of water. If desired, the ether(s) can be recombined with co-produced alcohol(s) to provide substantially dry alcohol/ether mixtures in virtually any desired ratio. The ether(s) and their mixtures with alcohol(s) are useful, inter alia, as high octane blending stocks for gasoline.
There is a need for an efficient catalytic process for manufacturing ethers and alcohols from light olefins thereby augmenting the supply of high octane blending stocks for gasoline. Lower molecular weight ethers such as diisopropyl ether (DIPE) and alcohols such as isopropyl alcohol (IPA) are in the gasoline boiling range and are known to have a high blending octane number. In addition, by-product propylene from which DIPE and IPA can be made is usually available in a fuels refinery. The petrochemicals industry also produces mixtures of light olefin streams in the C 2 to C 7 molecular weight range and the conversion of such streams or fractions thereof to ethers and alcohols can also provide products which are useful as solvents and as blending stocks for gasoline.
The catalytic hydration of olefins to provide alcohols and ethers is a well-established art and is of significant commercial importance. Representative olefin hydration processes are disclosed in U.S. Pat. Nos. 2,162,913; 2,477,380; 2,797,247; 3,798,097; 2,805,260; 2,830,090; 2,861,045; 2,891,999; 3,006,970; 3,198,752; 3,810,849; and, 3,989,762, among others.
Olefin hydration employing zeolite catalysts is known. As disclosed in U.S. Pat. No. 4,214,107, lower olefins, in particular, propylene, are catalytically hydrated over a crystalline aluminosilicate zeolite catalyst having a silica to alumina ratio of at least 12 and a Constraint Index of from 1 to 12, e.g., HZSM-5 type zeolite, to provide the corresponding alcohol, essentially free of ether and hydrocarbon by-product.
According to U.S. Pat. No. 4,499,313, an olefin is hydrated to the corresponding alcohol in the presence of hydrogen-type mordenite or hydrogen-type zeolite Y, each having a silica-alumina molar ratio of 20 to 500. The use of such a catalyst is said to result in higher yields of alcohol than olefin hydration processes which employ conventional solid acid catalysts. Use of the catalyst is also said to offer the advantage over ion-exchange type olefin hydration catalysts of not being restricted by the hydration temperature. Reaction conditions employed in the process include a temperature of from 50°-300° C., preferably 100°-250° C., a pressure of 5 to 200 kg/cm 2 to maintain liquid phase or gas-liquid multi-phase conditions and a mole ratio of water to olefin of from 1 to 20. The reaction time can be 20 minutes to 20 hours when operating batchwise and the liquid hourly space velocity (LHSV) is usually 0.1 to 10 in the case of continuous operation.
European Patent Application 210,793 describes an olefin hydration process employing a medium pore zeolite as hydration catalyst. Specific catalysts mentioned are Theta-1, said to be preferred, ferrierite, ZSM-22, ZSM-23 and NU-10.
The reaction of light olefins with alcohols to provide ethers is also a well known type of process. According to U.S. Pat. No. 4,042,633, DIPE is prepared from isopropyl alcohol (IPA) employing montmorillonite clay catalysts, optionally in the presence of added propylene. U.S. Pat. No. 4,175,210 discloses the use of silicatungstic acid as catalyst for the reaction of olefin(s) with alcohol to provide ether(s). As disclosed in U.S. Pat. No. 4,182,914, DIPE is produced from IPA and propylene in a series of operations employing a strongly acidic cation exchange resin as catalyst. In the process for producing a gasoline blending stock described in U.S. Pat. No. 4,334,890, a mixed C 4 stream containing isobutylene is reacted with aqueous ethanol to form a mixture of ethyl tertiary butyl ether and tertiary butanol. U.S. Pat No. 4,418,219 describes the preparation of methyl tertiary-butyl ether (MTBE), a high octane blending agent for motor fuels, by reacting isobutylene and methanol in the presence of, as catalyst, boron phosphate, blue tungsten oxide or a crystalline aluminosilicate zeolite having a silica to alumina mole ratio of at least 12:1 and a Constraint Index of from 1 to about 12 as catalyst. U.S. Pat. No. 4,605,787 discloses the preparation of alkyl tert-alkyl ethers such as MTBE and methyl tert-amyl ether (MTAE) by the reaction of a primary alcohol with an olefin having a double bond on a tertiary carbon atom employing as catalyst an acidic zeolite having a constraint index of from about 1 to 12, e.g., zeolite ZSM-5, 11, 12, 23 dealuminized zeolite Y and rare earth exchanged zeolite Y. European Patent Application 55,045 describes a process for reacting an olefin and an alcohol to provide an ether, e.g., isobutene and methanol to provide MTBE, in the presence of an acidic zeolite such as zeolite Beta, zeolites ZSM-5, 8, 11, 12, 23, 35, 43 and 48 and others, as catalyst. Germany Patent No. 133,661 describes the reaction of isobutene and methanol to provide a mixture of products including MTBE, butanol and isobutene dimer in the presence of acidic zeolite Y as catalyst. According to Japan Patent No. 59-25345, a primary alcohol is reacted with a tertiary olefin in the presence of a zeolite having a silica to alumina mole ratio of at least 10 and the x-ray diffraction disclosed therein to provide a tertiary ether.
It is an object of the present invention to provide a process for converting low cost, readily available sources of light olefins to ether(s) and, optionally, mixtures of alcohol(s) and ether(s), which can be used as high octane blending stocks for gasoline.
It is another object of the invention to provide a process for catalytically converting olefin(s) in an olefin conversion unit to mixtures of alcohol(s) and ether(s) employing an acidic zeolite catalyst and thereafter recovering the ether(s) in essentially pure form.
It is a specific object of this invention to react a feed containing a substantial amount of propylene with water in an olefin conversion unit in the presence of an acidic large pore zeolite such as zeolite Beta to provide a mixture of IPA and DIPE and to recover the DIPE in pure form or to add co-produced substantially dry IPA to said DIPE in a predetermined ratio.
SUMMARY OF THE INVENTION
By way of realizing the foregoing and other objects of the invention, a process is provided for producing ether containing at most relatively minor amounts of water which comprises:
(a) contacting at least one light olefin with water in an olefin conversion unit in the presence of an acidic zeolite as catalyst to provide an aqueous mixture of alcohol and ether, the olefin conversion unit being operated under conditions which are effective to provide alcohol by the reaction of olefin and water therein and ether by the dehydration of alcohol and/or by the reaction of olefin and alcohol therein;
(b) introducing the aqueous mixture of alcohol and ether into a distillation unit supplied with at least a part of the ether layer recovered from a downstream decantation operation, said distillation unit being operated under conditions which are effective to provide an azeotropic overheads fraction comprising ether, water, oligomer and minor amounts of alcohol, and a bottoms fraction comprising a major amount of alcohol and a minor amount of ether alcohol;
(c) introducing the azeotropic overheads fraction into a decanter unit operated under conditions which are effective to provide a ether layer containing at most negligible amounts of water and an aqueous layer containing negligible amounts of alcohol; and,
(d) introducing at least part of the ether layer into the distillation unit to reduce the water content of the final ether product.
The present process offers great flexibility in providing essentially pure ethers or ethers combined with controlled quantities of alcohols.
BRIEF DESCRIPTION OF THE DRAWINGS
The annexed figure of drawing is a schematic representation of the process of the invention as applied to the production of an IPA/DIPE mixture of predetermined composition containing less than 1 weight percent water.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is applicable to the conversion of individual light olefins and mixtures of olefins of various structures, preferably within the C 2-7 range, to ethers. Accordingly, the invention is applicable to the conversion of ethylene, propylene, butenes, pentenes, hexenes and heptenes, mixtures of these and other olefins such as gas plant off-gas containing ethylene and propylene, naphtha cracker off-gas containing light olefins, fluidized catalytic cracked (FCC) light gasoline containing pentenes, hexenes and heptenes, refinery FCC propane/propylene streams, etc. For example, a typical FCC light olefin stream possesses the following composition:
______________________________________Typical Refinery FCC Light Olefin Composition Wt. % Mole %______________________________________Ethane 3.3 5.1Ethylene 0.7 1.2Propane 14.5 15.3Propylene 42.5 46.8Isobutane 12.9 10.3n-Butane 3.3 2.6Butenes 22.1 18.3Pentanes 0.7 0.4______________________________________
The process of the invention is especially applicable to the conversion of propylene and propylene-containing streams to DIPE and IPA/DIPE mixtures containing little if any water.
The conversion of the light olefin takes place in an olefin conversion unit wherein several reactions occur simultaneously to provide a mixture of alcohol and ether. Thus, olefin will react with water to produce alcohol, alcohol will react with olefin to produce ether and/or alcohol will undergo dehydration to produce ether.
The foregoing olefin conversion reactions can be carried out under liquid phase, vapor phase or mixed vapor-liquid phase conditions in batch or in a continuous manner under stirred tank reactor or fixed bed flow reactor conditions, e.g., trickle-bed, liquid-up-flow, liquid-down-flow, counter-current flow, co-current flow, etc.
In general, the useful olefin conversion catalysts embrace two categories of zeolite, namely, the intermediate pore size variety as represented, for example, by ZSM-5, which possess a Constraint Index of greater than about 2 and the large pore variety as represented, for example, by zeolites Y and Beta, which possess a Constraint Index no greater than about 2. Both varieties of zeolites will possess a framework silica-to-alumina ratio of greater than about 7, usually greater than at least about 20, preferably greater than at least about 200 and more preferably still, greater than about 500. The zeolite will be in the acid form and as such, will possess an alpha value of at least about 1, preferably at least about 10 and more preferably at least about 100. It will often be advantageous to provide the zeolite as a composite bound with catalytically active or inactive material such as alumina or silica which is stable under the olefin conversion conditions employed.
Of particular interest for use herein are the large pore acidic zeolites, e.g., zeolite Beta, X, L, Y, USY, REY, Deal Y, ZSM-3, ZSM-4, ZSM-12, ZSM-20 and ZSM-50, as disclosed in commonly assigned, concurrently filed U.S. patent application Ser. No. 139,567. In accordance with said application, these large pore zeolite catalysts are used to effect the conversion of light olefin(s) to a mixture of alcohol(s) and ether(s) by contacting the olefin(s) with water in the vapor and/or liquid phase at a temperature of from about 100° to 230° C., preferably from about 120° to about 220° C. and most preferably from about 140° to about 200° C., a total system pressure of at least about 5 atm, preferably at least about 20 atm and more preferably at least about 40 atm, a water to total olefin mole ratio of from 0.1 to less than about 1.0, preferably from about 0.2 to 0.8 and most preferably from about 0.3 to 0.7 and an LHSV of from about 0.1 to about 10 in the presence of an acidic form of the zeolite. In the specific case of acidic zeolite Beta, and as described in commonly assigned, concurrently filed U.S. patent application Serial No. 139,570, the contents of which are incorporated herein, the hydration conditions need not be so limited as those stated above for the case of large pore zeolites generally. Thus, use of acidic zeolite Beta can be accompanied by essentially any practical set of hydration conditions which provides alcohol(s) and ether(s) in appreciable amounts. As disclosed in said application, good results can generally be obtained employing a temperature ranging from ambient up to about 300° C., preferably from about 50° to about 220° C. and more preferably from about 90° to about 200° C., a total system pressure of at least about 5 atm, preferably at least about 20 atm and more preferably at least abut 40 atm, a water to total olefin mole ratio of from about 1 to about 30, preferably from about 0.2 to about 15 and most preferably from about 0.3 to about 5, and an LHSV of from about 0.1 to about 10. It may be noted that at the unusually low water:olefin mole ratios called for by the process disclosed in U.S patent application Ser. No. 139,567, the production of olefin hydration products employing zeolite Beta as catalyst shifts toward ether(s) and away from alcohol(s).
The aqueous mixture of alcohol and ether produced in the olefin conversion unit containing unconverted olefin and any inert gaseous material such as saturated hydrocarbon which may have been part of the olefin feed stream, and the small quantities of oligomer which are typically present in the reaction effluent, are then passed to a separator unit to provide a gaseous phase containing the unconverted olefin and a liquid phase containing alcohol, ether, water and oligomer. The gaseous phase is recycled to the olefin conversion unit with part of it being vented off as may be necessary to avoid build-up of any inert component(s) in the system. The aqueous phase made up of alcohol, ether and oligomer is then introduced into distillation tower to provide an azeotropic overheads fraction containing most of the ether, a minor part of the alcohol and most of the water and oligomer and a bottoms fraction containing a major part of the alcohol, a minor part of the ether and oligomer and essentially no water. Part or all of the bottoms fraction can be recycled to the olefin conversion unit to maintain a high level of alcohol therein as this has been found to shift selectivity to ether. Alternatively, part or all of the bottoms fraction can be recombined with product ether to provide a dry alcohol/ether mixture of just about any desired composition.
The distillation unit is supplied with part or all of the ether-rich upper phase recovered from a downstream decanter unit in order to reduce the water content of the final ether product even further. If all of the decanter overhead is totally recycled, the water content in the product ether will be zero. If only part of the decanter overhead is recycled, the water content in the product ether will generally be between zero and about 1 wt. %.
Following condensation of the azeotrope from the distillation tower, the liquid product is introduced into a decanter unit where phase separation takes place. The decanter overheads are recovered as essentially dry ether and the aqueous decanter bottoms containing a small amount of alcohol can, if desired, be introduced into the olefin conversion unit.
The following example is illustrative of the process of the invention.
EXAMPLE 1
The conversion of propylene contained in a propylene/propane propane refinery stream (70 mole % propylene, 30 mole % propane) is illustrated in the process scheme shown in the appended FIGURE of drawing. The conditions of the propylene conversion employing an extrudate of zeolite Beta (85 wt. %) bound with silica (15 wt %) are: 160° C., 1800 psig, 0.5 water to propylene mole ratio and 0.5 weight hourly space velocity (WHSV) based on propylene. The results in moles/hr of feeds/products are set forth in the following Table:
TABLE__________________________________________________________________________IPA/DIPE Via Propylene Conversion over Zeolite BetaFeed/Product Moles/HrStream 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Wt__________________________________________________________________________ %Propane 155.0 -- 157.9 -- 312.8 312.8 155.0 -- -- -- -- -- -- --Propylene 361.6 -- 85.8 -- 447.4 170.0 84.2 -- -- -- -- -- -- --DIPE -- -- -- 0.1 0.1 ---- 92.5 158.1 22.7 158.0 88.3 69.3 92.4 63.1IPA -- -- -- 1.4 1.4 -- -- 86.5 18.7 77.4 17.4 9.7 7.7 35.1 34.2Oligomer -- -- -- 0.0 0.0 -- -- 3.7 6.4 0.9 6.4 3.6 2.8 3.7 2.1Water -- 182.5 -- 40.8 223.3 -- -- 45.8 52.1 0.0 11.3 6.3 5.0 5.0 0.6__________________________________________________________________________
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Olefin undergoes conversion in the presence of water to a mixture of alcohol and ether which is then subjected to various downstream operations including distillation and decantation to provide an ether-rich product containing little if any water. If desired the ether can be combined in any predetermined ratio with co-produced alcohol to provide alcohol/ether mixtures of desired composition. The foregoing process is especially suitable to the conversion of propylene and propylene-containing streams to diisopropyl ether and mixtures of isopropyl alcohol and diisopropyl ether which are useful, inter alia, as octane improves for gasoline.
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FIELD OF INVENTION
The present invention relates generally to computer technology, and more specifically, to the fabrication of a semiconductor device, such as a fin field effect transistor (FinFET).
DESCRIPTION OF RELATED ART
Dopant diffusion may be used in connection with FinFET junction engineering. For example, dopant diffusion is employed for extension overlap formation. Issues may be encountered in connection with spacer doping and resultant junction gradients. It may be difficult to provide or obtain doping in a region between one or more fins and a gate (potentially in connection with a spacer or insulator). Conventionally, implants are used to achieve doping. However, implants can cause damage to the fins, which leads to an undesirable increase in terms of resistance.
BRIEF SUMMARY
Embodiments are directed to a method for fabricating a semiconductor device comprising: forming a structure comprising at least one fin, a gate, and a spacer, applying an annealing process to the structure to create a gap between the at least one fin and the spacer, and growing an epitaxial semiconductor layer in the gap between the spacer and the at least one fin.
Embodiments are directed to a semiconductor device comprising: a fin, a gate formed on the fin, a spacer formed on the gate and the fin, and an epitaxial layer formed in a gap between the fin and the spacer as a result of an application of an annealing process to the device.
Embodiments are directed to a fin field effect transistor (FinFET) comprising: a plurality of silicon fins, a gate formed over the fins, a spacer formed over the gate and at least a portion of the fins, and an epitaxy layer formed in a gap between each of the fins and the spacer, wherein the gap is formed based on an application of an annealing process to the transistor.
Additional features and advantages are realized through the techniques described herein. Other embodiments and aspects are described in detail herein. For a better understanding, refer to the description and to the drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The subject matter which is regarded as the invention is particularly pointed out and distinctly claimed in the claims at the conclusion of the specification. The foregoing and other features and advantages are apparent from the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1A is an exemplary diagram of a structure in accordance with one or more embodiments;
FIG. 1B shows a front perspective view of the structure of FIG. 1A along the line A-A′ shown in FIG. 1A ;
FIG. 1C shows a side perspective view of the structure of FIG. 1A along the line B-B′ shown in FIG. 1A ;
FIG. 2A is an exemplary diagram of the structure of FIG. 1A following annealing in accordance with one or more embodiments;
FIG. 2B shows a front perspective view of the structure of FIG. 2A along the line A-A′ shown in FIG. 2A ;
FIG. 2C shows a side perspective view of the structure of FIG. 2A along the line B-B′ shown in FIG. 2A ;
FIG. 3A is an exemplary diagram of the structure of FIG. 2A following growth/insertion of epitaxy (epi) in accordance with one or more embodiments;
FIG. 3B shows a front perspective view of the structure of FIG. 3A along the line A-A′ shown in FIG. 3A ;
FIG. 3C shows a side perspective view of the structure of FIG. 3A along the line B-B′ shown in FIG. 3A ; and
FIG. 4 is a flow chart of an exemplary method in accordance with one or more embodiments.
DETAILED DESCRIPTION
It is noted that various connections are set forth between elements in the following description and in the drawings (the contents of which are included herein by way of reference). It is noted that these connections in general and, unless specified otherwise, may be direct or indirect and that this specification is not intended to be limiting in this respect. In this regard, a coupling of entities may refer to either a direct or an indirect connection.
Turning to FIGS. 1A-1C , an exemplary embodiment of a structure 100 is shown. The structure 100 is shown as including one or more silicon (Si) fins 102 with a spacer 104 and a PC 106 . The fins 102 may be substantially parallel to one another as shown in FIG. 1A . The PC 106 may correspond to the gate of the structure 100 . The spacer 104 may protect the gate/PC 106 by providing insulation between the gate/PC 106 and a source-drain region of the structure 100 .
The fins 102 , spacer 104 , and PC 106 may be formed on, a buried oxide (BOX) 108 . The BOX layer 108 may be part of a semiconductor-on-insulator (SOI) substrate, e.g., a silicon-oxide-silicon stack-up.
Turning to FIGS. 2A-2C , the structure 100 is shown following the application of an annealing process. For example, hydrogen (H 2 ) annealing may be applied at approximately: seven-hundred fifty degrees Celsius and ten torr for five minutes. Based on the annealing, the fins 102 may undergo shrinkage, leaving a gap or space (denoted by, or in proximity to, the dashed circle 206 ) between the fins 102 and the spacer 104 as shown in FIGS. 2A-2C . The annealing process may leave the fins 102 generally in place with respect to the structure 100 (e.g., the fins might not be disturbed) and may serve as a controlled process for creating generally uniform gaps/spaces 206 . The annealing process may be contrasted with conventional processes, wherein the conventional processes: (1) tend to be manual in nature, (2) upset or move the fins, and (3) tend to lack uniformity. The annealing process described herein may be performed to facilitate a growth of an epitaxy (epi) layer as described below.
The gap/space 206 may be created to allow for growth of an epi layer on the exposed silicon surfaces of the fins 102 . For n-type devices, phosphorous-doped polysilicon may be used. For p-type devices, boron may be used. Other types of materials or dopants may be used in some embodiments.
Turning to FIGS. 3A-3C , the structure 100 is shown following the growth of epi 312 in the gap/space 206 between the spacer 104 and the fins 102 . The epi 312 may ensure proper extension overlap and a suppressed extension junction gradient. The sharper junction (less junction gradient) contributes to improved gate short channel control, and thus, less leakage current when the transistor is in an off state. Typically, the junction can be achieved with a reduced thermal budget (less dopant diffusion). But, a reduction in terms of thermal budget/lower dopant diffusion may lead to insufficient dopant activation, and thus, an increase of series resistance. Embodiments described herein can achieve a sharp extension junction without compromising the dopant activation, since a reduction in the distance that the dopants need to diffuse is provided.
Turning now to FIG. 4 , a flow chart of an exemplary method 400 in accordance with one or more embodiments is shown. The method 400 may be used to provide a controlled process for doping a FinFET structure while minimizing the movement, changes to, or damage to the fins.
In block 402 , a FinFET structure may be constructed. For example, the FinFET structure constructed in block 402 may generally correspond to the structure 100 as shown in FIGS. 1A-1C .
In block 404 , an annealing process may be applied to the structure constructed in block 402 . The annealing process may result in a space or gap being created in the structure. For example, a space or gap may be created between one or more fins (e.g., fins 102 ) and a spacer (e.g., spacer 104 ) as shown in FIGS. 2A-2C .
In block 406 , epi may be grown or inserted in the gap/space created in block 404 . In this manner, dopants may be delivered more efficiently relative to conventional solutions, and a proper extension overlap and a suppressed extension junction gradient may be obtained.
The method 400 is illustrative. In some embodiments, one or more of the blocks (or portions thereof) may be optional. In some embodiments, one or more blocks or operations not shown may be included. In some embodiments, the blocks or operations may execute in an order or sequence different from what is shown in FIG. 4 .
Embodiments of the disclosure may be used to form an extension (e.g., an epi-extension) close to a gate edge (underneath an offset spacer). One or more processes may be self-aligned in that hydrogen (H 2 ) diffusion may be limited by a geometry near a spacer to prevent a gate short to a source-drain region.
The illustrative examples described herein included references to various elements, materials, and compounds. One skilled in the art would appreciate that other elements, materials, and compounds may be substituted for those that were specifically referenced herein.
In some embodiments, various functions or acts may take place at a given location and/or in connection with the operation of one or more apparatuses or systems. In some embodiments, a portion of a given function or act may be performed at a first device or location, and the remainder of the function or act may be performed at one or more additional devices or locations.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting. As used herein, the singular forms “a”, “an” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms “comprises” and/or “comprising,” when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, element components, and/or groups thereof.
The corresponding structures, materials, acts, and equivalents of all means or step plus function elements in the claims below are intended to include any structure, material, or act for performing the function in combination with other claimed elements as specifically claimed. The present disclosure has been presented for purposes of illustration and description, but is not intended to be exhaustive or limited to the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the disclosure. The embodiments were chosen and described in order to best explain the principles of the disclosure and the practical application, and to enable others of ordinary skill in the art to understand the disclosure for various embodiments with various modifications as are suited to the particular use contemplated.
The diagrams depicted herein are illustrative. There may be many variations to the diagram or the steps (or operations) described therein without departing from the spirit of the disclosure. For instance, the steps may be performed in a differing order or steps may be added, deleted or modified. All of these variations are considered a part of the disclosure.
It will be understood that those skilled in the art, both now and in the future, may make various improvements and enhancements which fall within the scope of the claims which follow.
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Embodiments are directed to forming a structure comprising at least one fin, a gate, and a spacer, applying an annealing process to the structure to create a gap between the at least one fin and the spacer, and growing an epitaxial semiconductor layer in the gap between the spacer and the at least one fin.
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CROSS-REFERENCES TO RELATED APPLICATIONS
This application claims the priority of German Patent Application, Serial No. 103 47 936.8-14, filed Oct. 15, 2003, pursuant to 35 U.S.C. 119(a)-(d), the disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
The present invention relates, in general, to the field of multiport valves, and more particularly to a valve assembly and a method for functional differentiation of a valve assembly.
Nothing in the following discussion of the state of the art is to be construed as an admission of prior art.
Valves have various functional characteristics depending on the specific requirements, e.g. 2/2, 3/2 NO, 3/2 NC, 4/2 monostable, 4/2 bistable, 4/3 vented, 4/3 blocked, 4/3 vacuum-vented, 5/2 monostable, 5/2 bistable, 5/3 vented, 5/3 blocked, 5/3 vacuum-vented etc. With sliding valves, the various valve functions can be realized, for example, with different valve slides.
In conventional multiport valves, the adjustment of these functional characteristics requires a multitude of different components, depending on which valve function is desired. On the other hand, the structural requirements of valves are often the same with respect to their geometric dimensions since they are positioned side by side on a base plate.
German utility model no. DE 94 21 326 discloses a multiport valve in which a 5/2 multiport valve can be transformed into two 3/2 multiport valves using the two-way design of a valve rod. This transformation is, however, complicated and not all the usual valve types can be adjusted.
It would therefore be desirable and advantageous to provide an improved valve assembly and an improved method for functional differentiation of a valve assembly to obviate prior art shortcomings and to allow adjustment of the functional differentiation or the determination of the valve function in a simple manner.
SUMMARY OF THE INVENTION
According to one aspect of the present invention, a valve assembly includes at least one multiport valve for controlling operation of a fluid-operated pneumatic unit, a base plate having passageways for supply of compressed fluid to the multiport valve and drainage of compressed fluid from the multiport valve, and a grid plate disposed between the base plate and the multiport valve for functional differentiation of the valve assembly and determination of the valve assembly function.
The present invention resolves prior art problems by interposing a grate plate between the base plate and the multiport valve for determination of the particular function of the valve assembly. As a result, the base plate and the multiport valve can have a uniform structure for all valve types. The function of the valve assembly is determined by the grid plate. It is to be understood by persons skilled in the art that the term “grid plate” is used here in a generic sense and the principles described in the following description with respect to the grid plate are equally applicable to any device which generally follows the concepts outlined here and is capable of being used for functional differentiation of a valve or for determining a valve function for the application at hand.
According to another feature of the present invention, the grid plate may have pneumatic lines for connecting the passageways of the base plate and the multiport valve for functional differentiation of the valve assembly and determination of the valve assembly function. In this way a function differentiation can be achieved in a simple manner.
According to another feature of the present invention, the grid plate may have electrical lines and/or electrical devices for connection to and/or the control of the base plate, the multiport valve or a pilot valve for functional differentiation of the valve assembly and determination of the valve assembly function. In this way the functional differentiation can also easily be achieved, and further ways to control the valve are provided.
The valve assembly is adjustable by means of the grid plate, preferably to any one of the functions of the group comprising: 2/2, 3/2 NO, 3/2 NC, 3/2 monostable, 4/2 bistable, 4/3 vented, 4/3 blocked, 4/3 vacuum-vented, 5/2 monostable, 5/2 bistable, 5/3 vented, 5/3 blocked, 5/3 vacuum-vented. This means that almost all the usual valve types can easily be adjusted.
According to another feature of the present invention, the grid plate is part of a modular kit including a plurality of grid plates to allow exchange of grid plates. The term “exchange” or “exchangeable” in the context of the present invention, relates hereby in particular to the capability to modify the functional differentiation of the valve, without dismantling the valve or the multiport valve. It is thus possible to change the functional characteristics of the valve in a simple manner and to minimize downtimes and/or production losses, even when the valves have already be assembled and have been in use.
According to another feature of the present invention, the base plate and/or the multiport valve are constructed for form-fitting or aligned attachment of the grid plate.
According to another aspect of the present invention, in a method for functional adjustment of a valve assembly having a multiport valve for controlling operation of a fluid-operated pneumatic unit, and a base plate provided with passageways for supplying compressed fluid to the multiport valve and for drainage of compressed fluid from the multiport valve, a grid plate is selected from a modular kit comprised of a plurality of grid plates, and the selected grid plate is placed between the base plate and the multiport valve for realizing a particular function of the valve assembly.
BRIEF DESCRIPTION OF THE DRAWING
Other features and advantages of the present invention will be more readily apparent upon reading the following description of currently preferred exemplified embodiments of the invention with reference to the accompanying drawing, in which:
FIG. 1 is an exploded view of one embodiment of a valve assembly according to the present invention having two valve slides;
FIG. 2 a is an elevational view of another embodiment of a valve assembly according to the present invention with a different grid plate;
FIG. 2 b is a horizontal sectional view of the valve assembly of FIG. 2 a , taken along the line A-A in FIG. 2 d , modified with a different grid plate;
FIG. 2 c is a vertical sectional view of the valve assembly of FIG. 2 a , taken along the line C-C in FIG. 2 a ; and
FIG. 2 d is a vertical sectional view of the valve assembly of FIG. 2 a , taken along the line B-B in FIG. 2 a.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Throughout all the Figures, same or corresponding elements are generally indicated by same reference numerals. These depicted embodiments are to be understood as illustrative of the invention and not as limiting in any way. It should also be understood that the drawings are not necessarily to scale and that the embodiments are sometimes illustrated by graphic symbols, phantom lines, diagrammatic representations and fragmentary views. In certain instances, details which are not necessary for an understanding of the present invention or which render other details difficult to perceive may have been omitted.
Turning now to the drawing, and in particular to FIG. 1 , there is shown an exploded view of a valve assembly according to the present invention, generally designated by reference numeral 1 and including two valve slides according to a first embodiment of the present invention. The valve assembly 1 includes a base plate 10 , a multiport valve 20 , and a pilot valve 40 . The base plate 10 has two working pressure lines 70 , 80 for applying compressed air to a pneumatic unit (not shown), such as a pneumatic cylinder, a feeder pressure line 60 , a vent line 90 and a plurality of pneumatic lines 100 arranged on top of base plate 10 .
Disposed between the base plate 10 and the multiport valve 20 is a grid plate 30 for functional differentiation of both valve slides. The base plate 10 is provided with anchors 12 in the form of studs 12 for form-fitting or aligned attachment of the grid plate 30 to the base plate 10 and the at least one multiport valve 20 . As an alternative, or in addition, the studs 12 can also be formed on the multiport valve 20 . It is thus ensured that the grid plate 30 can be arranged between the base plate 10 and the multiport valve 20 in a secure and precise way.
FIGS. 2 a - d show a valve assembly adjusted as a 5/2 monostable multiport valve. Parts corresponding with those in FIG. 1 are denoted by identical reference numerals and not explained again. The description below will center on the differences between the embodiments. In the presently preferred embodiment, the grid plate 30 is structured such that it includes at least one pneumatic line 120 . As can be seen from FIGS. 2 c and 2 d , the grid plate 30 has for each valve slide 110 three pneumatic lines 120 which selectively connect some or all of the pneumatic lines 100 arranged on the base plate 10 with selected lines 130 of the multiport valve and ultimately with the valve slides 110 . Depending on the connection of the lines 100 with the lines 130 , a different functional characteristic of the valve is achieved. Thus, valves of most varied functions can be adjusted, including, but not limited to: 2/2, 3/2 NO, 3/2 NC, 4/2 monostable, 4/2 bistable, 4/3 vented, 4/3 blocked, 4/3 vacuum-vented, 5/2 monostable, 5/2 bistable, 5/3 vented, 5/3 blocked, 5/3 vacuum-vented.
The base plate 10 and the multiport valve 20 are applicable for any of the various valves, without modification. As a result, manufacture and maintenance of the valves are greatly simplified, and the number of components required for making different valves is also reduced since the function is determined by the grid plate 30 , while the other components remain the same.
The grid plate 30 can be made of any material known to the artisan in the field of valves. Currently preferred is the manufacture of the grid plate 30 from a two component part comprised of a hard plastic as a carrier, and a resilient material as a sealing material (e.g. POM/AU).
The pilot valve 40 shown in FIG. 1 is provided with lines or plugs 42 fitting into corresponding connections 44 of the base plate 10 . In another embodiment of the present invention, the grid plate 30 may additionally be provided with electrical lines and/or electrical devices (not shown in the drawing) which are interposed between the pilot valve 40 and the connections 44 for control of the pilot valve 40 . This may be advantageous in particular when it is necessary for the two valve slides of multiport valve 20 to be actuated in synchronism. This may be ensured by a corresponding circuit on the grid plate 30 . In the event, synchronous actuation of the valve slides is not required, a different connecting scheme can be used when a different grid plate is used—or the electrical lines may be simply omitted. Of course, it is also conceivable to also control the base plate 10 and/or the multiport valve 20 by electrical lines and/or devices in the grid plate 30 .
In one advantageous embodiment of the invention, the grid plate is exchangeable. This can be realized, for example, by simply allowing the grid plate 30 to be slid out to the side. By inserting a different grid plate, a valve having a different function can easily be adjusted.
In the present embodiment, the valve assembly has two valve slides. Of course, grid plates that allow only one valve slide or more than two valve slides to be functionally adjustable are also conceivable.
While the invention has been illustrated and described in connection with currently preferred embodiments shown and described in detail, 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. The embodiments were chosen and described in order to best explain the principles of the invention and practical application to thereby enable a person skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated.
What is claimed as new and desired to be protected by Letters Patent is set forth in the appended claims and includes equivalents of the elements recited therein.
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A valve assembly includes at least one multiport valve for controlling and applying pressure to a pneumatic unit and a base plate having passageways for supplying compressed fluid to a multiport valve and for draining compressed fluid from the multiport valve. Interposed between the base plate and the multiport valve is a grid plate for functional differentiation of the valve assembly and determination of the valve assembly function.
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GOVERNMENT RIGHTS
This invention was made with government support under Grant No. GM 44154 awarded by the National Institutes of Health. The U.S. government has certain rights in the invention.
CROSS-REFERENCE TO RELATED APPLICATION
This is a divisional of application Ser. No. 07/933,140, filed Dec. 18, 1992, now U.S. Pat. No. 5,358,859.
TECHNICAL FIELD
The invention relates to KDO aldolase (EC 4.1.2.23) having a broad substrate specificity with respect to its reverse reaction and to condensation reactions employing such KDO aldolase for synthesizing a broad range of 6-9 carbon 2-keto-3-deoxy-onic acids, viz. 2-keto-3-deoxy-hexulosonate, 2-keto-3-deoxy-heptulosonate, 2-keto-3-deoxy-octulosonate, and 2-keto-3-deoxy-nonulosonate. More particularly, the invention relates to Aureobacterium barkerei strain KDO-37-2 (ATCC 49977), to KDO aldolase produced by and isolated from such bacteria, to the employment of such KDO aldose with respect to the synthesis of 2-keto-3-deoxy-onic acids such as 3-deoxy-D-manno-2-octulosonic acid (D-KDO) and to the use of protected forms of such 2-keto-3-deoxy-onic acids for the production of 7 and 8 carbon aldoses by means of radical mediated decarboxylation.
BACKGROUND OF THE INVENTION
2-Keto-3-deoxy-octulosonic acid (KDO) appears as a ketosidic component of all Gram-negative bacteria for which a KDO determination has been made. More particularly, 3-deoxy-D-manno-2-octulosonic acid (D-KDO) is widely found in Gram-negative bacteria. KDO is incorporated into lipopolysaccharides and is localized, as such, within the outer membrane compartment of Gram-negative bacteria. KDO appears to be a vital component of Gram-negative bacteria. KDO can also occur as an acidic exopolysaccharide. In such instances, the KDO can serve as part of a K-antigen.
As illustrated in FIG. 7, the biosynthetic incorporation of KDO into lipopolysaccharides consists of two steps, i.e.:
1. Activation of KDO to form CMP-KDO by means of CMP-KDO synthetase (EC 2.7.7.38); and then
2. Coupling of the activated CMP-KDO to lipid A precursor to form lipid A-KDO by means of KDO transferase.
The rate-limiting step with respect to the biosynthesis of KDO containing lipopolysaccharides is the activation of the KDO moiety, i.e., the formation of CMP-KDO. Accordingly, inhibitors of CMP-KDO synthetase are potentially useful as antibacterial agents.
Several chemical and enzymatic synthetic routes have been developed for the synthesis of KDO and its analogs. One route for the chemical synthesis of KDO employs Cornforth's method. (Ghalambor, M. et al. J. Biol. Chem. 1966, 241, 3207 and Hershberger, C. et al. J. Biol. Chem. 1968, 243, 1585.) The chemical synthesis of KDO produces multiple enantiomers. In order to obtain enantiomerically pure D-KDO, a separation step must be incorporated into the chemical synthetic route.
Synthetic routes employing enzymes are more stereospecific than chemical synthetic routes. An enzymatic synthetic route employing KDO-8 phosphate synthase and KDO-8-P phosphatase as catalysts and arabinose-5-P and PEP as substrates is illustrated in FIG. 7. (Bednarski, M. et al. Tetrahedron Letters 1988, 29, 427.) An alternative enzymatic synthetic route employs sialic acid aldolase. (Aug e, C. et al. Tetrahedron 1990, 46, 201.)
An enzymatic synthetic route employing the reverse reaction of KDO aldolase for a micromolar scale synthesis of KDO is disclosed by Ghalambor. (Ghalambor, M. et al., J. Biol. Chem. 1966, 241, 3222.) The synthetic route described by Ghalambor employs KDO aldolase isolated from Aerobacter colacae. The reverse reaction of KDO aldolase is driven by employing high substrate levels, i.e. high concentrations of D-arabinose and D-pyruvate. Ghalambor discloses that there is a 41% yield with this enzyme and narrow substrate specificity.
KDO aldolase (EC 4.1.2.23) is known to be inductively produced by several bacteria, viz. Escherichia coli, strains 0111, B, and K-12, Salmonella typhimurium, Salmonella aldelaide, and Aerobacter colacae. Ghalambor discloses that all of these known KDO aldolases have comparable activities. For example, all of these KDO aldolases hydrolyze 3-deoxy-D-manno-2-octulosonic acid to form D-arabinose and pyruvate in a forward reaction. As indicated above, Ghalambor also discloses that known KDO aldolase may be employed in a reverse reaction to condense D-arabinose and pyruvate to form 3-deoxy-D-manno-2-octulosonic acid. The substrate specificity of known KDO aldolases with respect to this reverse reaction is confined to D-arabinose and has been specifically shown to lack a measurable specificity for D-ribose in connection with this reverse reaction.
What was needed was an enzymic synthetic route for the production of a wide range of 2-keto-3-deoxy-onic acids and analogs thereof potentially having activity as inhibitors of CMP-KDO synthetase.
What was also needed was a method of converting 2-keto-3-deoxy-onic acids to high-carbon 2-deoxy aldoses.
SUMMARY OF THE INVENTION
Aureobacterium barkerei strain KDO-37-2 (ATCC 49977) and KDO aldolase (EC 4.1.2.23) isolated therefrom are disclosed therein. KDO aldolase catalyzed condensation employing this enzyme has been demonstrated to be effective for the synthesis of KDO and analogs. The reactions are stereospecific with formation of a new R-stereocenter at C-3 from D-arabinose and related substrates. Decarboxylation of the aldolase products provides a new route to heptose and octose derivatives.
Unlike known KDO aldolases which have a narrow substrate specificity, the KDO aldolase isolated from this source is disclosed to have a very wide substrate specificity with respect to catalyzing its reverse reaction, i.e. the condensation of aldoses with pyruvate. In particular, 3-deoxy-D-manno-2-octulosonic acid (D-KDO) can be synthesized from D-arabinose and pyruvate in 67% yield. Furthermore, studies with respect to the substrate specificity of the enzyme using more than 20 natural and unnatural sugars indicate that this enzyme widely accepts trioses, tetroses, pentoses and hexoses as substrates, especially the ones with R configuration at 3position. The substituent of 2 position has little effect on the aldol reaction. Nine of these substrates are submitted to the aldol reaction to prepare various 2-keto-3-deoxy-onic acids, including D-KDO, 3-deoxy-D-arabino-2-heptulosonic acid (D-DAH), 2-keto-3-deoxy-L-gluconic acid (L-KDG), and 3-deoxy-L-glycero-L-galacto-nonulosonic acid (L-KDN). The attack of pyruvate appears to take place on the re face of the carbonyl group of acceptor substrates, a facial selection complementary to sialic acid aldolase (si face attack) reactions. The aldolase products can be converted to aldoses via radical-mediated decarboxylation. For example, decarboxylation of pentaacetyl KDO and hexaacetyl neuraminic acid gives penta-O-acetyl-2-deoxy-β,3-D-manno-heptose and penta-O-acetyl-4-acetamido-2,4-dideoxy-β-D-glycero-D-gala cto-octose, respectively.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 illustrates saccharides having good specificity for KDO aldolase isolated from Aureobacterium barkerei KDO-37-2.
FIG. 2 illustrates saccharides having fair specificity for KDO aldolase isolated from Aureobacterium barkerei KDO-37-2.
FIG. 3 illustrates saccharides having poor specificity for KDO aldolase isolated from Aureobacterium barkerei KDO-37-2.
FIG. 4 illustrates the stereochemistry of the aldol condensation catalyzed by KDO aldolase isolated from Aureobacterium barkerei KDO-37-2.
FIG. 5 illustrates the 1 H NMR spectrum of 6, the product from 2-deoxy-D-ribose (400 MHz), CDCl 3 .
FIG. 6 illustrates the chemical assignment of the 1 H NMR spectrum compound 6 as shown in FIG. 6.
FIG. 7 illustrates a prior art biosynthetic incorporation of KDO into lipopolysaccharides and a prior art enzymatic synthetic route employing KDO-8 phosphate synthase and KDO-8-P phosphatase as catalysts and arabinose-5-P and PEP as substrates.
FIGS. 8A-I illustrate a synthetic scheme employing an aldolase condensation reaction and an excess of pyruvate for producing KDO from a variety of starting sugars.
FIG. 8A illustrates a synthetic scheme employing KDO aldolase and D-arabinose.
FIG. 8B illustrates a synthetic scheme employing KDO aldolase and D-ribose.
FIG. 8C illustrates a synthetic scheme employing KDO aldolase and 2-deoxy-D-ribose.
FIG. 8D illustrates a synthetic scheme employing KDO aldolase and D-erythrose.
FIG. 8E illustrates a synthetic scheme employing KDO aldolase and D-glyceraldehyde.
FIG. 8F illustrates a synthetic scheme employing KDO aldolase and D-threose.
FIG. 8G illustrates a synthetic scheme employing KDO aldolase and L-glyceraldehyde.
FIG. 8H illustrates a synthetic scheme employing KDO aldolase and L-mannose.
FIG. 8I illustrates a synthetic scheme employing sialic acid aldolase and D-mannose.
FIGS. 9A and B illustrate a synthetic route employing a decarboxylation of KDO aldolase condensation products. Additionally, FIG. 9A illustrates the stabilization of a planar conformer of the radical intermediate, stabilized both by the electron-donating and withdrawing effects, thereby allowing the maximum interaction between the one-electron p orbital and the lone pair electrons on the adjacent ring oxygen.
DETAILED DESCRIPTION
A New Source of KDO Aldolase
Aureobacterium barkerei strain KDO-37-2 (ATCC 49977) was isolated from garden soil using KDO as a major carbon source. The microorganism (strain KDO-37-2) grows well on LB medium. It is aerobic, gram-positive, not motile and with colonies 1-3 millimeters in diameter on LB agar plates. The colony morphology is circular, low convex, entire edge and produces yellow pigment. Optimum growth temperature is about 30° C. Major fatty acids are anteiso-C 15:0 and anteiso-C 17:0 . The strain was identified as Aureobacterium barkerei according to Bergey's manual. A deposit of Aureobacterium barkerei strain KDO-37-2 was made Jul. 30, 1992 with the American Type Culture Collection (ATCC) 12301 Parklawn Drive, Rockville, Md., USA 20852 and was given Accession Number ATCC 49977.
The deposit with accession Number ATCC 49977 was made in compliance with the Budapest Treaty requirements that the duration of the deposits should be for 30 years from the date of deposit at the depository or for the enforceable life of a U.S. patent that matures from this application, whichever is longer. The cell line will be replenished should it become non-viable at the depository.
A preferred medium for KDO aldolase production is defined as follows: NH 4 Cl (5 grams), K 2 SO 4 (1 gram), MgSO 4 •7H 2 O (200 milligrams), CaCl 2 (20 milligrams), FeSO 4 •7H 2 O (1 milligram), yeast extract (1 gram), Na 2 HPO 4 •7H 2 O and KH 2 PO 4 (3 grams) in distilled water (1 liter) at pH 7.2. A seed culture may be made by admixing in a 100 milliliter Erlenmeyer flask 50 milliliters of the above medium together with 25 microliters of a 40% glucose solution and 100 milligrams (0.2%) of KDO. The seed culture is then inoculated with a loopful of Aureobacterium barkerei strain KDO-37-2 (ATCC 49977). The flask is then shaken at 250 r.p.m. on a gyrorotory shaker at 30° C. for 16 hours. The seed culture thus obtained may then be poured into the 1950 milliliters of the same medium containing LDO as a major carbon source. The culture was incubated for 24 hours at 30° C. with shaking. The cells may be harvested as a source of KDO aldolase enzyme.
For routine culture preservation, the culture can grow on LB medium and can be incubated overnight at 30° C. This strain of Aureobacterium barkerei is shown to be a source of KDO aldolase (EC 4.1.2.23) having a broad substrate specificity with respect to the reverse aldol condensation reaction.
A New Source of KDO Aldolase
KDO aldolase (EC 4.1.2.23) was first reported by Ghalambor and Heath in 1966 as the enzyme responsible for the KDO degradation (FIG. 7). After their preliminary investigation on the substrate specificity as well as the μmol scale synthesis of KDO, no synthetic application of this enzyme has been reported, while the related enzyme N-acetylneuraminic acid (sialic acid) aldolase has been extensively studied.
It is disclosed herein that the Gram-positive bacterium Aureobacterium barkerei strain KDO-37-2 can be induced to contain high levels of KDO aldolase. The aldolase activity from this source was assayed according to Aminoff's method (Biochem. J. 1961, 81, 384). Two liters of culture contained 10.2 U based on the degradation of KDO. This KDO activity is 4 times and 8 times higher than the corresponding KDO activity from Escherichia coli K-12 and Aerobacter colacae, respectively, as reported by Gharambor (supra).
Partially purified KDO aldolase simply obtained by ammonium sulfate precipitation (8.0 U/mL; 0.19 U/mg for degradation of KDO) was used in substrate-specificity studies reported herein. The KDO aldolase employed for the kinetic analysis reported herein, was further purified via DEAE sepharose, DEAE substituted beaded agarose, and phenyl sepharose, phenyl substituted beaded agarose, column chromatography to a specific activity of 5.7 U/mg. The K m for D-arabinose and V max are 1.2M and 0.73 U/mg, respectively. The unusually high concentration of K m in the condensation compared with that in the course of degradation (6×10 -3 M for KDO) indicates that the enzyme may accept the open form of aldoses as acceptors in the aldol condensation. The enzymatic reaction favors the cleavage of KDO, with the equilibrium constant K eq =[pyruvate][arabinose]/KDO=9×10 -2 M.
TABLE I______________________________________Relative Rates of Several Substrates for KDO Aldolasefrom Aureobacterium barkeri KDO-37-2 relative relativesubstrate rate.sup.a substrate rate.sup.a______________________________________D-arabinose 100 D-altrose 25 N.D..sup.b,c L-mannose 15D-threose 128 L-arabinose N.D.D-erythrose 93 D-xylose N.D.D-ribose 72 D-allose N.D.2-deoxy-D-ribose 71 D-glucose N.D.L-glyceraldehyde 36 D-mannose N.D.D-glyceraldehyde 23 L-fucose N.D.2-deoxy-2-fluoro- 46 N-acetyl N.D.D-arabinose D-mannosamineD-lyxose 35 N-acetyl N.D. L-mannosamine5-azido-2,5- 15 D-fructose N.D.dideoxy-D-ribose______________________________________ .sup.a) Measured at pH 7.5 with 500 mM of sugar and 10 mM of pyruvate. Fo detailed condition, see experimental. Specific activity based on Darabinose is 0.2 U/mg; 1 U = 1 μmol KDO formed per min. .sup.b) Not detectable. .sup.c) Fluoropyruvate (10 mM) was used instead of pyruvate.
Substrate Specificity
This enzyme exhibits a wide substrate specificity. Several 3-6 carbon sugars were accepted as substrates for the condensation. From the results shown in Table I and FIG. 1, the structural requirements for the sugar for this enzyme are as follows. At C-2 position, although the aldolase prefers and S configuration, the difference is not significant [examples: between L- and D-glyceraldehyde; D-threose and D-erythrose; D-arabinose, D-ribose and 2-deoxy-D-ribose]. It is noteworthy that this enzyme also accepts D-ribose as a good substrate (rel. V=72%), while that from E. coli or Aerobacter colacae poorly accepts this substrate (rel. V<5%), according to Gharambor (supra). Accordingly, the substrate specificity of KDO aldolase from Aureobacterium barkerei strain KDO-37-2 with respect to D-ribose is considered favorable since it exceeds 7% of the corresponding substrate specificity of the enzyme with respect to D-arabinose. At C-3 position, this enzyme prefers an R-configuration [examples: comparison between D-arabinose and L-arabinose, D-lyxose and D-xylose]. Hexoses are generally not as good substrates as tetroses and pentoses, even in the case of D-altrose (rel. V=25%) and L-fucose (rate not detectable), both being homoanalogs of the natural substrate D-arabinose. The reason that L-mannose is a better substrate than D-mannose is because the former has the favorable 2R,3R configurations and the latter has the unfavorable 2S,3S configurations. Finally, neither fluoropyruvate nor ketohexose was accepted by this enzyme.
The Aldol Condensation
The enzymatic synthesis of KDO on multi-mmol scales using 10 molar excess of pyruvate worked well (e.g., 1 was obtained in 67% yield). The synthetic route is illustrated in FIG. 8A. The reagents employed in this synthesis are as follows:
______________________________________Step Reagent or Enzyme______________________________________(a) KDO aldolase(b) Ac.sub.2 O/py,DMAP(c) CH.sub.2 N.sub.2.______________________________________
The yield of the enzymatic reaction is comparable to the highest one obtained by the modified Cornforth synthesis (66%). The crystalline KDO ammonium salt monohydrate was isolated in 37% yield: [α] 26 D +40.3° (c 2.06, H 2 O) [lit. according to Unger: [α] 27 D +42.3° (c, 1.7, H 2 O), authentic sample from Sigma [α] 26 D +40.2° (c 2.06, H 2 O)]. (Unger: Adv. Carbohydr. Chem. Biochem. 1981, 38, 323.) The 1 H NMR spectrum in D 2 O is identical with that of an authentic sample, although it is complicated by the fact that KDO exists as an anomeric mixture of pyranose and furanose forms, and readily cyclizes to the corresponding lactone in aqueous solution. The crystalline ammonium salt was further converted to pentaacetate methyl ester derivative 2, whose 1 H NMR spectrum was in good accordance with that reported previously and clearly shows the 5 C 2 -pyranose conformation (Table II).
TABLE II__________________________________________________________________________.sup.1 H NMR Analysis of Pyranose, Furanose and 1 → 5 LactoneForms Observedin the Products Possessing a C-5 Axial Substituent in the Pyranose Form ##STR1## ##STR2## ##STR3## ##STR4## chemical shifts (δ, ppm) coupling constants (Hz)compound H-3 H-3' J.sub.3,3' J.sub.3,4 J.sub.3',4 J.sub.3,5__________________________________________________________________________1 (KDO, in D.sub.2 O)α-pyranose form 1.863 1.951 13.0 5.5 12.0 1.0β-pyranose form 2.373 1.735 11.7 5.0 11.7 1.0furanose form 2.275 2.351 13.5 7.5 7.5 --1' (in D.sub.2 O) 2.053 2.562 14.0 3.0 7.5 --2 (in CDCl.sub.3) 2.245 2.201 13.0 6.0 12.0 --11 (in D.sub.2 O)α-pyranose form 1.90-1.98 -- -- -- --furanose form 2.301 2.384 13.4 7.0 7.0 --11' (in D.sub.2 O) 2.072 2.576 14.2 3.1 7.3 --12 (in CDCl.sub.3) 2.339 2.972 14.9 2.4 9.5 0.612' (in CDCl.sub.3) 2.10 2.80 15.0 2.5 9.0 --13 (in D.sub.2 O)α-pyranose form 1.873 1.984 13.0 5.2 11.9 --furanose form 2.284 2.341 13.1 6.4 6.4 --13' (in D.sub.2 O) 2.051 2.521 14.1 3.2 7.5 --14 (in CDCl.sub.3) 2.292 2.288 -- 7.0 10.1 0.4__________________________________________________________________________
Several substrates with good or fair relative rate are shown to be employable in the aldol condensation. The reactions with D-ribose and 2-deoxy-D-ribose are illustrated in FIGS. 8B and 8C respectively. These reactions took place smoothly to give 3 (57% after derivation to 4) and 5 (47% as 6), respectively. 1 H NMR spectra of 3, 4, 5, and 6 clearly show a 5 C 2 pyranose form in both products (Table III). The 1 H spectrum of 6 is shown in FIG. 2. It is noteworthy that in these cases, even though the relative rates are lower (72% for D-ribose and 71% for 2-deoxy-D-ribose) than that of D-arabinose, TLC analysis of the reaction products showed no starting material left, whereas a substantial amount of starting material always remains in the reaction with D-arabinose. It is suggested that formation of the pyranose form of 3 and 5, where all substituents are located in the stable orientation, further shifted the equilibrium toward condensation.
The products 7 (3-deoxy-D-arabino-2-heptulosonic acid, DAH, 39% as 8) and 9 (11% as 10) were also obtained from D-erythrose and D-glyceraldehyde, as illustrated in FIGS. 8D and 8E respectively. These yields indicate that this aldolase-catalyzed condensation is also useful for the synthesis of lower homologs of KDO. The phosphate of 7 (DAHP) plays an important role in the shikimate synthesis pathway in plants and microorganisms. The selected chemical shifts and coupling constants for the 1 H NMR spectra of products 3-10 are summarized in Table III.
TABLE III______________________________________.sup.1 H NMR Analysis of the α-Pyranose FormObserved in the Products Possessing a C-5 Equatorial Substituent ##STR5##chemical shift(δ, ppm) coupling constants (Hz)compound H-3eq H-3ax J.sub.3eq,3ax J.sub.3eq,4 J.sub.3ax,4 J.sub.3eq,5eq______________________________________3.sup.a 2.148 1.773 13.0 5.1 11.4 --4.sup.b 2.559 2.010 13.5 5.2 11.6 --5.sup.a 2.094 1.591 12.7 4.6 12.1 1.86.sup.b 2.454 1.783 13.1 4.8 11.6 1.87.sup.a 2.180 1.773 13.0 5.1 11.8 --8.sup.b 2.658 2.087 13.6 5.2 11.4 --9.sup.a 2.176 1.795 13.1 5.1 11.6 --10.sup.b 2.618 1.948 13.5 5.2 11.2 --______________________________________ .sup.a) Measured in D.sub.2 O. .sup.b) Measured in CDCl.sub.3.
FIG. 8F illustrates the aldolase catalyzed condensation reaction can be employed to produce product 11 from D-threose. Product 11 has a 1 H NMR spectrum similar to that of KDO. The reaction with L-glyceraldehyde, illustrated in FIG. 8G afforded 13 (2-Keto-3- deoxy-L-gluconic acid, KDG), an enantiomer of D-KDG, whose phosphate (KDGP) is an intermediate in the Entner-Doudoroff pathway. (Entner, N.; Doudoroff, M. J. Biol. Chem. 1952, 196, 853.) The 1 H NMR spectrum of 13 was very complicated (see experimental). To clarify the stereochemistry, preparation of derivatives was attempted; however, the products were still difficult to identify. The only isolable component from 11 was a bicyclic lactone. The structure was determined as 12 (FIG. 8F) by comparing its 1 H NMR spectrum with that of the higher homolog 12', which had been obtained from KDO and unambiguously characterized previously. (Charon, D.; Auzanneau, F.-I.; M erienne, C.; Szab o, L. Tetrahedron Lett. 1987, 23, 1393.)
In its 1 H NMR spectrum (Table II), a long range coupling between H-3 and H-5 (0.6 Hz) indicates that the pyranose form of the product exists as a twisted boat conformation, and all of the coupling constants are consistent with those observed in the case of 12'. It is interesting that in the spectra of 11, 13 and KDO, a substantial proportion of the similar signals were observed, where one of the H-3 signal appears at very low field (Table II). From these results, it is assumed that the bicyclic 1<<5 lactones 1', 11' and 13' form at nearly neutral pH. The formation of 1<<7 lactone is excluded, since those signals were observed in the case of a hexulosonate 13' without any C-7 hydroxy group. The homologs prepared here also proceed through a spontaneous 1<<5 lactone formation, as already proposed previously for KDO. (Menton, L. D., et al. Carbohydr. Res. 1980, 80, 295.) Compound 13 mainly exists as 5 C 2 pyranose form as indicated in 14.
The reaction with L-mannose illustrated in FIG. 8H gave 15 (3-deoxy-L-glycero-L-galacto-2-nonulosonic acid, L-KDN, 61% as 16), which is an enantiomer of D-KDN, a component in polysialoglycoprotein and ganglioside of rainbow trout eggs. (Lin, C.-H., et al., J. Am. Chem. Soc., in press; Nadano, D. et al. J. Biol. Chem. 1986, 261, 11550; and Song, Y., et al. J. Biol. Chem. 1991, 266, 21929). The optical rotation [[α] 25 D +26.3° (CHCl 3 )] and 1 H NMR spectrum of 16 were in good accordance with those of 16' [[α] 25 D -26.0° (CHCl 3 )], which was obtained via reaction with D-mannose catalyzed by sialic acid aldolase, as illustrated in FIG. 8I, except for the sign of rotation (Tetrahedron 1990, 46, 201). The availability of both enantiomers of KDN may develop new analogs of sialyl oligosaccharides. (Ichikawa, Y., et al. Anal. Biochem. 1992, 202, 215.)
Finally, the aldol reaction with an unnatural sugar containing a fluorine atom was conducted to give 18 (19% of 19). By comparing the 1 H NMR spectra, the proportion of the β-isomer (10.71) of 18 was ca. 1.5 times higher than that of KDO (6.9%), probably due to the absence of furanose and 1<<5 lactone forms. This result suggests that 18 might be a good substrate for CMP-KDO synthetase, since the enzyme accepts the unstable β-form of KDO as a substrate. (Kohlbrenner, W. E. and Fesik, S. W., J. Biol. Chem. 1985, 260, 14695.) We therefore synthesized 18 in a larger scale by combining the use of KDO aldolase and pyruvate decarboxylase, which made the workup procedure much easier. Preliminary study using 18 toward CMP-KDO synthetase which had recently been cloned and over-expressed in this group showed that 18 was accepted to the enzyme.
Based on these results, the stereochemical course of the aldol condensation catalyzed by this KDO aldolase is probably as follows: The attack of pyruvate always takes place on the re face of the carbonyl group of the substrates, a facial selection complementary to sialic acid aldolase reactions (si face attack). The stereochemical requirements of substrates and the stereochemical course of the aldol condensation are indicated in FIG. 3. It is concluded that in general the enzyme accepts substrates with an R-configuration at C-3. The substrates with an S configuration at C-2 is kinetically favored, while those with R configuration at C-2 are thermodynamically favored to give a better yield.
Synthesis of Decarboxylated Analogs
Decarboxylation of KDO and its analogs will yield the corresponding aldose derivatives. A synthetic route employing decarboxylation of KDO aldolase condensation products is illustrated in FIGS. 9A and 9B. The reagents employed in these synthetic routes is as follows:
______________________________________Step Reagent______________________________________(a) Ac.sub.2, DMAP/pyridine(b) CsCO.sub.3, BnBr/DMF(c) H.sub.2,Pd--C/EtOH(d) (COCl).sub.2 /toluene(e) 17, DMAP/pyridine-toluene(f) t-BuSH, hv(g) Me.sub.3 N═C═NEt (WSCI)-Cl, 17 (5 eq.) , T--CuSH, DMAP, Et.sub.3 N, MS4A/Ch.sub.2 Cl.sub.2,______________________________________ hv
The aldodeoxyheptose structure is particularly interesting since a number of heptoses are widely distributed in nature, some of which play important roles in metabolic pathways. Barton's radical-mediated decarboxylation of the penta-O-acetyl derivative 20a obtained from the corresponding benzyl ester 20b seems to be the most straightforward route to the desired heptose derivative 21. (e.g., Crich, D. and Lim, L. B. L. J. Chem. Soc. Perkin I 1991, 2209 and Auzanneau, F.-I. et al. Carbohydr. Res. 1990, 201, 337.)
There have recently been growing interests in the synthesis of physiologically active carbohydrate- and nucleic acid-related compounds via anomeric radical intermediates. It appears to us that radical-mediated reaction stabilized both electron withdrawing and donating group (capto-dative effect), e.g. Viehe, H. G. et al. Acc. Chem. Res. 1985, 18, 148.) at anomeric position [--C()(OAc)O-type] is rare (only a few related examples [eg. --C()(CO 2 Me)O-- type, --C()(CHF 2 )O-- type] are known), while examples in the case of simple anomeric radical [--C()(H or R)O-- type] and the one bearing two electron donating oxygen atom [--C()(OR))-- type] have been extensively studies. (e.g. Crich, D. and Lim, L. B. L. J. Chem. Soc. Perkin I 1991, 2205 and J. Chem. Soc. Perkin I 1991, 2209; Schmidt, R. et al. Tetrahedron Lett. 1988, 29, 3643; Myrvold, S. et al. J. Am. Chem. Soc. 1989, 111, 1861; Motherwell, W. B. et al. Synlett. 1989, 68; and Samadi, M. J. Med. Chem. 1992, 35, 63.) The radical intermediate was formed by the thermal decomposition of the thiohydroxamate 20c generated in situ from the corresponding acid chloride and 22 in the presence of azobisisobutyronitrile (AIBN). The subsequent trapping with tributyltin hydride resulted in only a disappointing (less than 2%) yield of 21. The yield was, however, dramatically improved to 68% by irradiation with white light in the presence of t-butylmercaptane.
The 1 H NMR spectrum of 21 clearly shows the exclusive β-anomer (δ 5.75, dd, J 1 ,2eq =3.0, J 1 ,2ax =10.0 Hz, H-1), indicating that the abstraction of hydrogen atom from t-butylmercaptane took place at the bottom side of the six-membered ring. The proposed mechanism for the exclusive formation of β-isomer is as follows. The stable conformer of the radical intermediate which is stabilized both by the electron-donating and withdrawing effects is supposed to be in a plane form as depicted in FIGS. 9A and 9B, which allows the maximum interaction between the one-electron p orbital and the lone pair electrons on the adjacent ring oxygen. t-Butylmercaptane is easily accessible from the bottom side, while the approach from the top side is sterically hindered by the hydrogen and acetoxy groups. This explanation in terms of kinetic control is well matched with the thermodynamic stability of the β-product.
The radical process was also applied to the synthesis of the decarboxylated analog of N-acetylneuraminic acid. It turned out, however, that all attempts for the synthesis of the acyl chloride resulted in a complex mixture, even from fully protected peracetate form 23a of sialic acid, because NHAc proton still has a substantial reactivity to chlorinating reagents. The direct formation of thiohydroxamate 23b was also found to be difficult because of the inherent steric hindrance around carbonyl group in the starting material. Through an extensive examination of the reaction conditions, it was found that the combination of ethyl (diethylamino)propylcarbodiimide hydrochloride (WSCI-Cl, 1.5 eq) and excess of 22 (5.0 eq) worked well for the in situ formation and degradation of thiohydroxamate, to give 24 (27% yield from 23a). This condition has the advantage that the reaction can be carried out in one step. The newly formed product was exclusively an α-anomer where the OAc group is located in the equatorial orientation, consistent with the result obtained in the decarboxylation of KDO derivative. (Haverkamp, J. et al. Eur. J. Biochem. 1982, 122, 305.)
PREPARATION OF EXAMPLES
General
Optical rotations were measured on Perkin-Elmer 241 spectrophotometer UV and visible spectra were recorded on a Beckmann DU-70 spectrometer. 1 H and 13 C NMR spectra were recorded at 400 and 500 MHz on Bruker AMX-400 and AMX-500 spectrometer. High-resolution mass spectra (HRMS) were recorded on a VG ZAB-ZSE mass spectrometer under fast atom bombardment (FAB) conditions. Column chromatography was carried out with silica gel of 70-230 mesh. Preparative TLC was carried out on Merck Art. 5744 (0.5 mm).
Isolation of the Microorganism
Aureobacterium barkerei containing high levels of KDO aldolases was selected with the S medium containing 0.25% of synthetic KDO mixture as carbon source (20 mL) in serum bottles (158 mL) and incubated at 37° C. for 2 days with shaking (250 r.p.m.). (McNicholas, P. A. et al. Carbohydr. Res. 1986, 146, 219 and Shirai, R.; and Ogura, H. Tetrahedron Lett. 1989, 30, 2263.) The bottles which showed turbidity were transferred to the same fresh medium. After several transfers, the cultures were plated on the S medium agar plates (1.5% agar) containing 0.25% of synthetic KDO mixture. The isolated colonies were transferred to the liquid medium as described above. To confirm the utilization of KDO, the disappearance in the medium was monitored by TLC as described in the synthesis of KDO. The cultures which showed the utilization of KDO were harvested by centrifugation and resuspended in 50 mM phosphate buffer (pH 7.0). The cell suspension was incubated with 1% (w/v) of authentic KDO (from Sigma) at 37° C. overnight to confirm the degradation of KDO by TLC. The cultures were then replated on LB agar plates to ensure the purity of the culture.
Preparation of the Enzyme
With one slight modification, the incubation was carried out according to the procedure reported by Gharambor (supra). The ingredients of the medium were as follows: NH 4 Cl (5 g), K 2 SO 4 (1 g), MgSO 4 •7H 2 O (200 mg), CaCl 2 (20 mg), FeSO 4 •7H 2 O (1 mg), yeast extract (1 g), Na 2 HPO 4 •7H 2 O (10 g), and KH 2 PO 4 (3 g) in distilled water (1 L), at pH 7.2. To a 50 mL of this medium in a 100 mL Erlenmeyer flask, were added D-glucose (40% solution in water, 25 μL) and KDO (100 mg, 0.2%), and a loopful of Aureobacterium barkerei KDO-37-2 was incolutated. The flask was shaken at 250 r.p.m. on a gyrorotary shaker at 30° C. for 16 h. The seed culture thus obtained was poured into the 1950 mL of the same incubation medium containing KDO (3.9 g). The mixture was divided and poured into two of 2.8 L Erlenmeyer flasks. The flasks were shaken at 250 r.p.m. at 30° C. for 24 h. The growth of microorganism was estimated by OD at 600 nm to be 1.90. The cells were harvested at 10,000×g for 30 min at 4° C. and washed with 50 mM potassium-sodium phosphate buffer (pH 7.5). The collected cells were then resuspended in the same buffer solution (20 mL) and disrupted by French-pressure apparatus (at 16,000 lb/in). The cell debris were removed by centrifuge at 23,000×g for 1 h at 4° C. to give the supernatant (ca. 20 mL) as the crude enzyme preparation. The enzyme activity was determined to be 1.45 U/mL for the degradation of KDO according to the method of Aminoff (Biochem. J. 1961, 81, 384). Ammonium sulfate precipitation between 45-75% saturation was collected and dialyzed in phosphate buffer (2 L; 100 mM, 1 mM of dithiothreitol, 2 L) to give partially purified enzyme (13.5 mL, 1.73 U/mL for KDO degradation), according to the method of Kim (J. Am. Chem. Soc. 1988, 110, 6481).
Kinetic Measurements
The rates for aldolase-catalyzed reactions were obtained by measuring the amount of remaining pyruvate, according the method of Kim (supra). The reactions were carried out in 0.1M phosphate buffer (pH 7.5) containing: varied concentrations of pyruvate, 2.0, 3.33, 5, and 10 mM; varied concentrations of D-arabinose, 0.2, 0.25, 0.33, and 0.50M in 0.5 mL of solution. Each solution was incubated at 37° C. Periodically, a small aliquot (25-100 μL) was withdrawn and mixed with an assay solution (1.4 mL) containing 0.1M phosphate (pH 7.5) buffer, 0.3 mM NADH, and 20-30 U of L-lactate dehydrogenase. The decrease in absorbance at 340 nm was measured and converted into the amount of the unreacted pyruvate using 6220M -1 cm -1 for the molecular absorbance of NADH. The kinetic parameters were obtained from the Lineweaver-Burk plots.
For the relative rate measurements, the concentration of pyruvate (fluoropyruvate) and sugar were fixed at 10 mM and 0.5M, respectively. Other conditions were the same as above.
Example 1
Ammonium 3-deoxy-α-D-manno-2-octulosonate monohydrate (KDO ammonium salt monohydrate, 1)
D-Arabinose (250 mg, 1.67 mmol), sodium pyruvate (1.83 g, 16.7 mmol), dithiothreitol (1.5 mg), NaN 3 (2% solution in water, 100 μL), NaHPO 4 •7H 2 O (53 mg), and KH 2 PO 4 (13 mg) were added to the KDO aldolase (5.1 U, 10 mL). The pH was adjusted to 7.5 and the mixture was stirred under N 2 at 30° C. for 3 days. The product was purified by treatment with a Dowex-1 resin column (bicarbonate form) eluted with a linear gradient from 0 to 0.25M of ammonium bicarbonate. KDO ammonium salt was further purified by Biogel P-2 column. The fraction eluted with H 2 O containing KDO was collected and its total amount was estimated to be 1.11 mmol (67%) by Aminoff's assay (supra). The residue after lyophilization was recrystallized from aqueous ethanol to give colorless plates (168 mg, 37% from D-arabinose): mp 123°-125° C. (decomposition) [lit. according to Hershberger: mp 121°-123° C., authentic sample from sigma mp 123°-125° C. (decomposition)]; [α] 26 D +40.3° (c 2.06, water) [lit. according to Hershberger: [α] 27 D +42.3° (c 1.7, water), authentic sample from Sigma [α] 26 D +40.2° (c 2.03, water)]. Its 1 H NMR spectrum in D 2 O was identical with that of an authentic sample. (Hershberger: J. Biol. Chem. 1968, 243, 1585.) A small portion was converted to pentaacetate methyl ester derivative 2: 1 H NMR (CDCl 3 ) δ 1.994 (3H, s, acetyl), 1.998 (3H, s, acetyl), 2.045 (3H, s acetyl), 2.108 (3H, s, acetyl), 2.139 (3H, s, acetyl), 2.201 (1H, dd, J 3ax ,4 =12.0, J 3ax ,3eq =13.0 Hz, H-3ax), 2.245 (1H, dd, J 3eq ,4 =6.0, J 3eq ,3ax =13.0 Hz, H-3eq), 3.810 (3H, s, COOCH 3 ), 4.113 (1H, dd, J 8' ,7 =12.5, J 8' ,8 =12.5 Hz, H-8'), 4.173 (1H, dd, J 6 ,5 =1.3, J 6 ,7 =9.5 Hz, H-6), 4.475 (1H, dd, J 8 ,7 =4.0, J 8 ,8' =12.5 Hz, H-8), 5.220 (1H, ddd, J 7 ,8 =4.0, J 7 ,6 =9.5, J 7 ,8' =12.5 Hz, H-7), 5.322 (1H, ddd, J 4 ,5 =3.0, J 4 ,3eq =6.0, J 4 ,3eq =6.0, J 4 ,3ax =12.0 Hz, H-4), 5.385 (1H, dd, J 5 ,6 =1.3, J 5 ,4 =3.0 Hz, H-5). The 1 H NMR spectrum was in good accordance with that reported previously by Unger (Adv. Carbohydr. Chem. Biochem. 1981, 38, 323).
Example 2
Methyl 2,4,5,7,8-penta-O-acetyl-3-deoxy-α-D-altro-2-octulosonate (4)
In the same manner as described for the preparation of 1, the product 3 (as ammonium salt) was prepared from D-ribose (0.33 mmol): 1 H NMR (D 2 O) δ 1.773 (1H, dd, J 3ax ,4 =11.9, J 3ax ,3eq =13.0 Hz, H-3ax), 2.148 (1H, dd, J 3eq ,4 =5.1, J 3eq ,3ax =13.0 Hz, H-3eq), 3.500 (1H, dd, J 5 ,4 =9.1, J 5 ,6 =10.0 Hz, H-5), 3.745 (1H, dd, J 8 ,7 =7.3, J 8 ,8' =12.1 Hz, H-8), 3.789 (1H, dd, J 8' ,7 =3.7, J 8' ,8 =12.1 Hz, H-8'), 3.809 (1H, dd, J 6 ,7 =2.8, J 6 ,5 =10.0 Hz, H-6), 3.901 (1H, ddd, J 4 ,3eq =5.1, J 4 ,5 =9.1, J 4 ,3ax =11.9 Ha, H-4), 4.004 (1H, dd, J 7 ,6 =2.8, J 7 ,8' =3.7, J 7 ,8 =7.3 Hz, H-7). This was converted to 4 by the successive treatment with acetic anhydride-pyridine-DMAP (see also the preparation of 20b) and etherial diazomethane solution. The product was purified with silica gel preparative TLC to afford 4 (87.7 mg, 57% from D-ribose) as an oil, [α] 25 D +70.9° (c 0.81, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 2.010 (1H, dd, J 3ax ,4 =11.6, J 3ax ,3eq =13.5 Hz, H-3ax), 2.030 (3H, s, acetyl), 2.050 (3H, s, acetyl), 2.064 (3H, s, acetyl), 2.105 (3H, s, acetyl), 2.154 (3H, s, acetyl), 2.559 (1H, dd, J 3eq ,4 =5.2, J 3eq ,3ax =13.5 Hz, H-3eq), 3.793 (3H, s, COOCH 3 ), 4.084 (1H, dd, J 6 ,7 =3.2, J 6 ,5 =10.3 Hz, H-6), 4.241 (1H, dd, J 8 ,7 =7.0, J 8 ,8' =12.0 Hz, H-8), 4.415 (1H, dd, J 8' ,7 =4.0 J 8' ,8 =12.0 Hz, H-8'), 5.110 (1H, dd, J 5 ,4 =9.3, J 5 ,6 =10.3 Hz, H-5), 5.169 (1H, ddd, J 7 ,6 =3.2, J 7 ,8' =4.0, J 7 ,8 =7.0 Hz, H-7), 5.271 (1H, ddd, J 4 ,3eq =5.2, J 4 ,5 =9.3, J 4 ,3ax =11.6 Hz, H-4); 13 C NMR (CDCl 3 ) δ 20.52, 20.56, 20.56, 20.67, 20.67, 35.47, 53.12, 61.23, 68.33, 68.96, 69.85, 71.98, 96.66, 166.21, 167.94, 169.52, 169.85, 169.89, 170.38. HRMS (M+Cs + ) calcd C 19 H 26 O 13 Cs 595.0428, found 595.0428.
Example 3
Methyl 2,4,7,8-tetra-O-acetyl-3,5-dideoxy-α-D-manno-2-octulosonate (6)
In the same manner as 3, the product 5 (as ammonium salt) was prepared from 2-deoxy-D-ribose (0.33 mmol): 1 H NMR (D 2 O) δ 1.400 (1H, ddd, J 5ax ,4 =11.9, J 5ax ,6 =11.9, J 5ax ,5eq =12.3 Hz, H-5ax), 1.591 (1H, dd, J 3ax ,4 =12.1, J 3ax ,3eq =12.7 Hz, H-3ax), 2.009 (1H, dddd, J 5eq ,3eq =1.8, J 5eq ,6 =2.2, J 5eq ,4 =4.6, J 5eq ,5ax =12.3 Hz, H-5eq), 2.094 (1H, ddd, J 3eq ,5eq =1.8, J 3eq ,4 =4.6, J 3eq ,3ax =12.7 Hz, H-3eq), 3.398 (1H, dd, J 8 ,7 =7.1, J 8 ,8' =11.8 Hz, H-8), 3.588 (1H, dd, J 8' ,7 =4.1, J 8' ,8 =11.8 Hz, H-8'), 3.786 (1H, ddd, J 7 ,8' =4.1, J 7 ,6 =4.6, J 7 ,8 =7.1 H8, H-7), 3.945 (1H, ddd, J 6 ,5eq =2.2, J 6 ,7 =4.6, J 6 ,5ax =11.9 Hz, H-6), 4.112 (1H, dddd, J 4 ,3eq =4.6, J 4 ,5eq =4.6, J 4 ,5ax =11.9, J 4 ,3ax =12.1 Hz, H-4). This was converted to 6 (62.2 mg,, 47% from 2-deoxy-D-ribose): [α] 25 D +86.0° (c 0.56, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 1.488 (1H, ddd, J 5ax ,4 =12.0, J 5ax ,6 =12.0, J 5ax ,5eq =12.7 Hz, H-5ax), 1.783 (1H, dd, J 3ax ,4 =11.6, J 3ax ,3eq =13.1 Hz, H-3ax), 2.045 (3H, s, acetyl), 2.054 (3H, s, acetyl), 2.070 (3H, s, acetyl), 2.123 (3H, s, acetyl), 2.177 (1H, dddd, J 5eq ,3eq =1.8, J 5eq ,6 =2.2, J 5eq ,4 =4.7, J 5eq ,5ax =12.7 Hz, H-5eq), 2.454 (1H, ddd, J 3eq ,5eq =1.8, J 3eq ,4 =4.8, J 3eq ,3ax =13.1 Hz, H-3eq), 3.782 (3H, s, COOCH 3 ), 4.034 (1H, ddd, J 6 ,5eq =2.2, J 6 ,7 =7.6, J 6 ,5ax =12.0 Hz, H-6), 4.169 (1H, dd, J 8 ,7 =5.1, J 8 ,8' =12.2 Hz, H-8), 4.457 (1H, dd, J 8' ,7 =2.8, J 8' ,8 =12.2 Hz, H-8'), 5.093 (1H, ddd, J 7 ,8' =2.8, J 7 ,8 =5.1, J 7 ,6 =7.6 Hz, H-7), 5.186 (1H, dddd, J 4 ,5eq =4.7, J 4 ,3eq =4.8, J 4 ,3ax =11.6, J 4 ,5ax =12.0 Hz, H-4); 13 C NMR (CDCl 3 ) δ 20.56, 20.56, 20.73, 20.96, 32.21, 36.03, 52.96, 61.82, 65.72, 69.00, 71.96, 97.61, 167.02, 167.96, 169.81, 170.06, 170.32. HRMS (M+Cs + ) calcd C 17 H 24 O 11 Cs 537.0373, found 537.0373.
Example 4
Methyl 2,4,5,7-tetra-O-acetyl-3-deoxy-α-D-arabino-2-heptulosonate (8)
7: 1 H NMR (D 2 O) δ 1.773 (1H, dd, J 3ax ,4 =11.8, J 3ax ,3eq =13.0 Hz, H-3ax), 2.180 (1H, dd, J 3eq ,4 =5.1, J 3eq ,3ax =13.0 Hz, H-3eq), 3.433 (1H, dd, J 5 ,4 =9.2, J 5 ,6 =9.5 Hz, H-5), 3.744 (1H, ddd, J 6 ,7 =3.5, J 6 ,7' =3.5, J 6 ,5 =9.5 Hz, H-6) 3.807 (1H, m, H-7), 3.812 (1H, m, H-7'), 3.930 (1H, ddd, J 4 ,3eq =5.1, J 4 ,5 =9.2, J 4 ,3a =11.8 Hz, H-4).
8: (50.0 mg, 39% from 0.33 mmol of D-erythrose): [α] 25 D +54.0° (c 0.50, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 2.034 (3H, s, acetyl), 2.053 (3H, s, acetyl), 2.087 (3H, s, acetyl), 2.087 (1H, dd, J 3ax ,4 =11.4, J 3ax ,3eq =13.6 Hz, H-3ax), 2.173 (3H, s, acetyl), 2.658 (1H, dd, J 3eq ,4 =5.2, J 3eq ,3ax =13.6 Hz, H-3eq), 3.808 (3H, s, COOCH 3 ), 4.058 (1H, dd, J 6 ,7 =2.3, J 6 ,7' =4.3, J 6 ,5 =10.2 Hz, H-6), 4.100 (1H, J 7 ,6 =2.3, J 7 ,7' =12.4 Hz, H-7), 4.355 (1H, J 7' ,6 =4.3, J 7' ,7 =12.4 Hz, H-7'); 13 C NMR (CDCl 3 ) δ 20.65, 20.76, 20.76, 20.84, 35.58, 53.31, 61.69, 68.16, 68.37, 71.51, 97.29, 166.41, 168.43, 169.61, 170.13, 170.77. HRMS (M+Cs + ) calcd C 16 H 22 O 11 Cs 523.0216, found 523.0216.
Example 5
Methyl 2,4,5-tri-O-acetyl-2-keto-3-deoxy-α-D-galactonate (10)
9: 1 H NMR (D 2 O) δ 1.795 (1H, dd, J 3ax ,4 =11.6, J 3ax ,3eq =13.1 Hz, H-3ax), 2.176 (1H, dd, J 3eq ,4 =5.1, J 3eq ,3ax =13.1 Hz, H-3eq), 3.60-3.65 (2H, m), 3.77-3.91 (2H, m).
10: (11.0 mg, 11% from 0.33 mmol of D-glyceraldehyde): [α] 25 D +31.8° (c 1.10, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 1.948 (1H, dd, J 3ax ,4 =11.2, J 3ax ,3eq =13.5 Hz, H-3ax), 2.055 (3H, s, acetyl), 2.059 (3H, s, acetyl), 2.170 (3H, s, acetyl), 2.618 (1H, dd, J 3eq ,4 =5.2, J 3eq ,3ax =13.5 Hz, H-3eq), 3.629 (1H, dd, J 6ax ,5 =10.6, J 6ax ,6eq =11.3 Hz, H-6ax), 3.809 (3H, s, COOCH 3 ), 4.149 (1H, dd, J 6eq ,5 =5.7, J 6eq ,6ax =11.3 Hz, H-6eq), 5.049 (1H, ddd, J 5 ,6eq =5.7, J 5 ,4 =9.5, J 5 ,6ax =10.6 Hz, H-5), 5.320 (1H, ddd, J 4 ,3eq =5.2, J 4 ,5 =9.5, J 4 ,3ax =11.2 Hz, H-4); 13 C NMR (CDCl 3 ) δ 20.67, 20.72, 20.89, 35.81, 53.25, 62.17, 67.66, 68.49, 96.80, 166.96, 168.50, 169.84, 170.05. HRMS (M+Cs + ) calcd C 13 H 18 O 9 Cs 451.0005, found 451.0005.
Example 6
2,4,7-Tri-O-acetyl-3-deoxy-α-D-lyxo-2-heptulosonic acid 1<<5 lactone (12)
11: 1 H NMR (D 2 O) δ 1.90-1.98 (m, H-3 of the major component); a minor pair of H-3protons: 2.072 (dd, J 3 ,4 =3.1, J 3 ,3' =14.2 Hz, H-3), 2.576 (dd, J 3' ,4 =7.3, J 3' ,3 =14.2 Hz, H-3'); another minor pair of H-3 protons: 2.301 (dd, J=7.0, 13.4 Hz), 2.384 (dd, J=7.0, 13.4 Hz); 3.60-3.95 (m), 3.95-4.20 (m), 4.48-4.52 (m).
12: (1.9 mg): 1 H NMR (CDCl 3 ) δ 2.096 (3H, s, acetyl), 2.127 (3H, s, acetyl), 2.180 (3H, s, acetyl), 2.339 (1H, ddd, J 3 ,5 =0.6, J 3 ,4 =2.4, J 3 ,3' =14.9 Hz, H-3) 2.972 (1H, dd, J 3' ,4 =9.4, J 3' ,3 =14.9 Hz, H-3'), 4.180 (1H, ABX type, J 6 ,7 =5.6, J 6 ,7' =9.9 Hz, H-6), 4.28-4.35 (2H, m, ABX type, H-7, H-7'), 4.904 (1H, d, J 5 ,4 =2.0 Hz, H-5), 5.164 (1H, ddd, J 4 ,5 =2.0, J 4 ,3 =2.4, J 4 ,3' =9.4 Hz, H-4). HRMS (M+Cs + ) calcd C 13 H 16 O 9 Cs 448.9849, found 448.9858.
Example 7
Methyl 2,4,5-tri-O-acetyl-2-keto-3-deoxy-α-L-gluconate (14)
13 (L-KDG): 1 H NMR (D 2 ) A major pair of H-3-protons: δ 1.873 (dd, J 3eq ,4 =5.2, J 3eq ,3ax =13.0 Hz, H-3eq), 1.984 (dd, J 3ax ,4 =11.9, J 3ax ,3eq =13.0 Hz, H-3ax); a minor pair of H-3 protons: 2.051 (dd, J 3 ,4 =3.2, J 3 ,3' =14.1 Hz, H-3), 2.521 (dd, J 3' ,4 =7.5, J 3' ,3 =14.1 Hz, H-3'); a minor H-3 proton ( 2 C 5 β-pyranose form is suggested): 2.167 (dd, J 3 ,4 =4.0, J 3 ,3' =13.7 Hz), in this case the H-3' proton could not be specified by overlapping of the signals; another minor pair of H-3 protons: 2.284 (dd, J=6.4, 13.1 Hz), 2.341 (dd, J=6.4, 13.1 Hz); 3.60-4.10 (m), 4.15-4.20 (m), 4.30-4.40 (m).
14: (2.0 mg): 1 H NMR (CDCl 3 ) δ 2.034 (3H, s, acetyl), 2.150 (3H, s, acetyl), 2.152 (3H, s, acetyl), 2.288 (1H, d, J 3ax ,4 =10.1 Hz, H-3ax), 2.292 (1H, dd, J 3eq ,5 =0.4 Hz, J 3eq ,4 =7.0 Hz, H-3eq), 3.830 (3H, s, COOCH 3 ), 3.999 (1H, dd, J 6eq ,5 =1.5, J 6eq ,6ax =13.2 Hz, H-6eq), 4.092 (1H, dd, J 6ax ,5 2.0, J 6ax ,6eq =13.2 Hz, H-6ax), 5.251 (1H, dddd, J 5 ,3eq =0.4, J 5 ,6eq =1.5, J 5 ,6ax =2.0, J 5 ,4 =2.7, Hz, H-5), 5.313 (1H, ddd, J 4 ,5 =2.7, J 4 ,3eq =7.0, J 4 ,3ax =10.1 Hz, H-4). HRMS (M+Na + ) calcd C 13 H 18 O 9 Na 341.0849, found 341.0849.
Example 8
Methyl 2,4,5,7,8,9-hexa-O-acetyl-3-deoxy-β-L-glycero-L-galacto-nonulosonate (16)
15 (L-KDN): 1 H NMR (D 2 O) δ 1.773 (1H, dd, J 3ax ,4 =11.8, J 3as ,3eq =12.9 Hz, H-3ax), 2.168 (1H, dd, J 3eq ,4 =5.1, J 3eq ,3ax =11.8 Hz, H-3eq), 3.579 (1H, dd, J 5 ,4 =9.3, J 5 ,6 =9.9 Hz, H-5), 3.654 (1H, dd, J 9 ,8 =6.3, J 9 ,9' =11.8 Hz, H-9), 3.766 (1H, ddd, J 8 ,9' =2.6, J 8 ,9 =6.3, J 8 ,7 =9.0 Hz, H-8), 3.831 (1H, dd, J 7 ,6 =1.1, J 7 ,8 =9.0 Hz, H-7), 3.873 (1H, dd, J 9' ,8 =2.6, J 9' ,9 =11.8 Hz, H-9'), 3.925 (1H, dd, J 6 ,7 =1.1, J 6 ,5 =9.9 Hz, H-6), 3.971 (1H, ddd, J 4 ,3eq =5.1, J 4 ,5 =9.3, J 4 ,3ax =11.8 Hz, H-4).
16 (108.3 mg, 61% from 0.33 mmol of L-mannose): [α] 25 D +26.3° (c 1.14, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 2.084 (1H, dd, J 3ax ,4 =11.6, J 3ax ,3eq =13.6 Hz, H-3ax), 2.013 (3H, s, acetyl), 2.024 (3H, s, acetyl), 2.040 (3H, s, acetyl), 2.069 (3H, s, acetyl), 2.115 (3H, s, acetyl), 2.157 (3H, s, acetyl), 2.625 (1H, dd, J 3eq ,4 =5.3, J 3eq ,3ax =13.6 Hz, H-3eq), 3.790 (3H, s, COOCH 3 ), 4.141 (1H, dd, J 9 ,8 =5.8, J 9 ,9' =12.6 Hz, H-9), 4.186 (1H, dd, J 6 ,7 =2.3, J 6 ,5 =10.3 Hz, H-6), 4.440 (1H, dd, J 9' ,8 =2.5, J 9' ,9 =12.6 Hz, H-9'), 4.975 (1H, dd, J 5 ,4 =9.6, J 5 ,6 =10.3 Hz, H-5), 5.150 (1H, ddd, J 8 ,9' =2.5, J 8 ,9 =5.8, H 8 ,7 =6.3 Hz, H-8), 5.264 (1H, ddd, J 4 ,3eq =5.3, J 4 ,5 =9.6, J 4 ,3ax =11.6 Hz, H-4), 5.396 (1H, dd, J 7 ,6 =2.3, J 7 ,8 =6.3 Hz, H-7); 13 C NMR (CDCl 3 ) δ 20.46, 20.48, 20.58, 20.58, 20.67, 35.32, 53.06, 61.67, 66.68, 67.21, 68.57, 70.00, 71.27, 97.14, 165.91, 168.03, 169.46, 169.57, 169.80, 169.96, 170.41. HRMS (M+Cs + ) calcd. C 22 H 30 O 15 Cs 667.0639, found 667.0639.
16': [α] 25 D -26.0° (c 1.00, CHCl 3 ). The 1 H NMR spectrum was identical with that of 16.
Example 9
2-Deoxy-2-fluoro-D-arabinose (17b)
To a solution of a tribenzoate 17a (available from Pfanstiehl Co., 500 mg, 1.08 mmol) in ethanol (5 mL) was added 10N NaOH aqueous solution (485 μL, 1.5 eq of each OBz group, total 4.5 eq) at room temperature. After 15 min, H 2 O (10 mL) and ethanol (5 mL) were added and the mixture was stirred and heated to 50° C. to dissolve the precipitated sodium benzoate. The mixture was further stirred for 1 h at room temperature. After ethanol was evaporated in vacuo, the residue was dissolved in H 2 O and Dowex 50W-X8 (H + form) was added to acidify the mixture. The precipitated benzoic acid was filtered off, and the filtrate was treated with Dowex 1-X8 (HCO 3 - form) and filtered, then concentrate in vacuo to give 17b as colorless syrup (153 mg, 94%); 1 H NMR (D 2 O) δ 3.60-4.20 (4H, m), 4.337 (ddd, J 2 ,1 =7.7, J 2 ,3 =9.3, J 2 ,F =51.8 Hz, H-2 of β-anomer), 4.666 (ddd, J 2 ,1 =3.7, J 2 ,3 =9.5, J 2 ,F =49.5 Hz, H-2 of α-anomer), 4.763 (dd, J 1 ,F =3.3, J 1 ,2 =7.7, H-1 of β-anomer), 5.434 (dd, J 1 ,F =1.5, J 1 ,2 =3.7 Hz, H-1 of α-anomer). This anomeric mixture was used in the next step without further purification.
Example 10
Methyl 2,4,7,8-tetra-O-acetyl-3,5-dideoxy-5-fluoro-α-D-manno-2-octulosonate (19)
18: 1 H NMR (D 2 O) δ 1.814 (dd, J 3ax ,3eq =12.4, J 3ax ,4 =12.4 Hz, H-3ax of β-anomer), 1.988 (1H, ddd, J 3eq ,5 =0.8, J 3eq ,4 =5.6, J 3eq ,3ax =12.9 Hz, H-3eq of α-anomer), 2.058 (1H, dd, J 3ax ,4 =11.8, J 3ax ,3eq =12.9 Hz, H-3ax of α-anomer), 2.461 (ddd, J 3q ,5 =0.8, J 3eq ,4 =5.3, J 3eq ,3ax =12.4 Hz, H-3eq of β-anomer), 3.663 (1H, dd, J 8 ,7 =5.4, J 8 ,8' =12.1 Hz, H-8), 3.828 (1H, dd, J 8' ,7 =2.4, J 8'8 =12.1 Hz, H-8'), 3.80-3.95 (2H, m), 4.182 (1H, dddd, J 4 ,5 =2.4, J 4 ,3eq =5.6, J 4 ,3ax =11.8, J 4 ,F =30.5 Hz, H-4), 4.957 (1H, ddd, J 5 ,3eq =0.8, J 5 ,4 =2.4, J 5 ,F =50.9 Hz, H-5).
19 (25.3 mg, 18% from 0.33 mmol of 17b): [α] 25 D +96.4° (c 2.53, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 2.043 (3H, s, acetyl), 2.067 (3H, s, acetyl), 2.131 (3H, s, acetyl), 2.137 (3H, s, acetyl), 2.271 (1H, dd, J 3ax ,4 =11.5, J 3ax ,3eq =13.3 Hz, H-3ax), 2.319 (1H, dd, J 3eq ,4 =5.9, J 3eq ,3ax =13.3 Hz, H-3eq), 3.805 (3H, s, COOCH 3 ), 4.073 (1H, dd, J 6 ,7 =9.5, J 6 ,F =27.8 Hz, H-6), 4.154 (1H, dd, J 8 ,7 =3.5, J 8 ,8' =12.5 Hz, H-8), 4.601 (1H, dd, J 8' ,7 =2.2, J 8' ,8 =12.5 Hz, H-8'), 4.827 (1H, dd, J 5 ,4 =2.1, J 5 ,F =50.9 Hz, H-5), 5.240 (1H, dddd, J 4 ,5 =2.1, J 4 ,3eq =5.9, J 4 ,3ax =11.5, J 4 ,F =21.3 Hz, H-4), 5.288 (1H, ddd, J 7 ,8' =2.2, J 7 ,8 =3.5, J 7 ,6 =9.5 Hz, H-7); 13 C NMR (CDCl 3 ) δ 20.56, 20.56, 20.71, 20.83, 30.60, 53.18, 61.46, 66.45, (d, J C ,F =17.8 Hz), 67.89 (d, J C ,F =4.1 Hz), 69.60 (d, J C ,F =18.2 Hz, 83.02 (d, J C ,F =186.2 Hz), 97.04, 166.49, 167.75, 169.14, 170.18, 170.20. HRMS (M+Cs + ) calcd C 17 H 23 O 11 FCs 555.0279, found 555.0288.
Example 11
Larger scale synthesis of 18
Fluorosugar 17b (340 mg, 2.25 mmol), sodium pyruvate (2.074 g, 28.9 mmol), dithiothreitol (1.7 mg), NaN 3 (2.3 mg), phosphate buffer (pH 7.5, 50 mM, 1.12 mL) was added to the enzyme solution (3.0 mL, 24 U). After the pH was adjusted to 7.5, the volume was made up to 10.0 mL. The mixture was stirred under N 2 at room temperature for 7 days. The pH was lowered to 2.5 by addition of Dowex 50W-X8 (H + form) and the mixture was kept at 0° C. for 1 h. The precipitate was removed by centrifugation at 23,000×g for 1 h at 4° C. Before the anion-exchange resin treatment, the excess pyruvate was removed as follows. The mixture was diluted to 80 mL and the pH was adjusted to 6.5 by the addition of 2N aqueous ammonia solution. The antifoam (Antifoam AF emulsion, Dow-Corning Nakaraitesque, 10% emulsion in water, 0.32 mL) and pyruvate decarboxylase (Sigma P 6810, 0.2 mL, 12.5 U) was added and the mixture was stirred at room temperature with bubbling of N 2 (1.5 L/min). The pH was monitored and occasionally adjusted between 6.0 and 6.5, by addition of Dowex 50W-X8 (H + form). The decarboxylase was periodically added to the mixture (each 0.2 mL) at an interval of 30 min, to avoid the denaturation which is caused by the rapid formation of acetaldehyde. The total amount of the enzyme as 3.2 mL (200 U). The reaction mixture was further stirred overnight. Then the mixture was centrifuged, and the supernatant was diluted to 100 mL and applied to a column of Dowex 1-X8 (20-50 mesh, bicarbonate form, bed volume, 100 mL). The pH of the eluent and washings was re-adjusted to 5.5 and further applied to the same column to ensure the adsorption of desired product. After washing with water, the desired product was eluted with a linear gradient from 0 to 0.3M of ammonium bicarbonate. The product was further purified by Biogel P-2 column (bed volume 20 mL) to give 192 mg (33%) of 18. The 1 H NMR spectrum was identical with the sample mentioned above.
Example 12
Benzyl 2,4,5,7,8-penta-O-acetyl-3-deoxy-α-D-manno-2-octulosonate (20b)
A suspension of KDO ammonium salt monohydrate (160 mg, 0.59 mol), acetic anhydride (3 mL), pyridine (3 mL), and 4-(N,N-dimethylamino)pyridine (DMAP, 2 mg) was stirred overnight at room temperature. Ice-cooled water was added and the mixture was stirred for 30 min. After dilution with water, the pH of the mixture was adjusted to 3.5 by addition of Dowex 50W-X8 (H + form). The resin was filtered off, and the filtrate was concentrated in vacuo. The residue was diluted with a mixture of chloroform and toluene and the solvent was evaporated. This procedure was repeated three times to remove trace of water. The residue was dissolved in anhydrous DMF. Benzyl bromide (161 mg, 0.94 mmol), Cs 2 CO 3 (390 mg, 1.20 mmol), and tetrabutylammonium iodide (33 mg) were added and the mixture was stirred for 4 h at room temperature under N 2 . The mixture was diluted with 0.5N ice-cooled hydrochloric acid and extracted twice with a mixture of diethyl ether and toluene (1:1). The organic layer was successively washed with water, saturated aqueous NaHCO 3 and brine, dried over anhydrous Na 2 SO 4 and concentrated in vacuo. The residue was chromatographed over silica gel (20 g). Elution with hexane-diethyl ether (2:1-1:1) afforded 15b, which was recrystallized from diethyl ether to give 220 mg (70%) as colorless plates, mp 102°-103° C. (lit. 26b mp 98°-99° C.); [α] 26 D +293° (c 1.0, CHCl 3 ) [lit. 26b [α] 25 D +91.9° (c 0.9, CHCl 3 ). Its 1 H NMR spectrum (CDCl 3 ) was in good accordance with that reported previously by Nakamoto (Chem. Pharm. Bull. 1987, 35, 4537). HRMS (M+Na + ) calcd 561.1584, found 561.1602.
Example 13
2,4,5,6,8-Penta-O-acetyl-3-deoxy-α-D-manno-2-octulosonic acid (20a)
A mixture of 20b (220 mg, 0.41 mmol) and Pd-C (10%, 55 mg) in ethanol (3mL) was vigorously stirred under H 2 at room temperature for 1 h. After the catalyst was filtered off, the filtrate was concentrated in vacuo. The residue was recrystallized from diethyl ether to give 20a (177 mg, 97%) as fine needles, mp 132°-133° C.; [α] 25 D +374° (c 0.88, CHCl 3 ). Its 1 H NMR spectrum (C 6 D 6 ) was identical with that reported previously by Unger et al. (Carbohydr. Res. 1980, 80, 191).
Example 14
1,3,4,6,7-Penta-O-acetyl-2-deoxy-β-D-manno-heptose (21)
To a solution of acid chloride prepared from 20a (30 mg, 0.067 mmol) in toluene was added dropwise a solution of N-hydroxythiopyridone 22 (11mg, 0.09 mmol) and DMAP (2 mg) in toluene (0.5 mL) and pyridine (0.3 mL) at room temperature under N 2 in the dark. After stirring for 10 min, t-butylmercaptane (0.5 mL) was added and the mixture was irradiated with white light (tungsten lamp, 100 W) at room temperature. After stirring for 10 min, N 2 was introduced to the mixture under a slightly reduced pressure to remove residual t-butylmercaptane for 30 min. Usual workup and purification by silica gel preparative TLC [developed with hexane-Et 2 O (1:1)] afforded 21 (18.5 mg, 68% as an oil, [α] 22 D +36.8° (c 1.85, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 2.000-2.150 (2H, m, H-2ax, H-2eq), 2.010 (6H, s, acetyl), 2.082 (3H, s, acetyl), 2.119 (3H, s, acetyl), 2.137 (3H, s, acetyl), 3.882 (1H, dd, J 5 ,4 =1.5, J 5 ,6 =10.0 Hz, H-5), 4.115 (1H, dd, J 7' ,6 =4.5, J 7' ,7 =12.5 H, H-7'), 4.437 (1H, dd, J 7 ,6 =2.5, J 7 ,7' =12.5 Hz, H-7), 5.073 (1H, ddd, J 3 ,4 =3.0, J 3 .2eq =5.0, J 3 ,2ax =12.5 Hz, H-3), 5.165 (1H, ddd, J 6 ,7 =2.5, J 6 ,7' =4.5, J 6 ,5 =10.0 Hz, H-6), 5.303 (1H, dd, J 4 ,5 =1.5, J 4 ,3 =3.0 Hz, H-4), 5.748 (1H, dd, J 1 ,2eq =3.0, J 1 ,2ax =10.0 Hz, H-1); 13 C NMR (CDCl 3 ) δ 20.59, 20.59, 20.65, 20.65, 20.84, 30.35, 62.26, 63.84, 67.32, 67.90, 71.62, 91.67, 168.60, 169.60, 169.83, 170.30, 170.54. HRMS (M+Cs + ) calcd C 17 H 24 O 11 Cs 537.0373, found 537.0359.
Example 15
4-Acetamido-1,3,6,7,8-Penta-O-acetyl-2,4-dideoxy-α-D-glycero-D-galacto-octose (24)
A 25 mL two-necked flask equipped with septum, micro-scale Dean-Stark trapp which was filled with molecular sieves 4A, and a reflux condenser, was used as the reaction vessel. A mixture of 23a (35.0 mg, 0.70 mmol), DMAP (12.3 mg, 1.5 eq), 22 (41.0 mg, 5.0 eq), triethylamine (19 μL) in CH 2 Cl 2 (1 mL) was placed in the flask as above. To this was successively added a solution of WSCI-Cl (20 mg) in CH 2 Cl 2 (1 mL) and t-butylmercaptane (0.5 mL). The mixture was stirred and irradiated with white light (tungsten lamp, 100 W) at room temperature for 5 h. The reaction was worked up in a similar manner as described above. The crude produce was purified by silica gel preparative TLC [developed with ethyl acetate-tetrahydrofuran (1:1)] to give 24 (8.7 mg, 27% from 23a) as an oil, [α] 22 D +21.3° (c 2.87, CHCl 3 ); 1 H NMR (CDCl 3 ) δ 1.908 (3H, s, N-acetyl), 1.915 (1H, ddd, J 2ax ,1 =10.3, J 2ax ,3 =11.5, J 2ax ,2eq =12.4 Hz, H-2ax), 2.043 (3H, s, O-acetyl), 2.051 (3H, s, O-acetyl), 2.102 (3H, s, O-acetyl), 2.107 (3H, s, O-acetyl), 2.134 (3H, s, O-acetyl), 2.219 (1H, ddd, J 2eq ,1 =2.1, J 2eq ,3 =4.9, J 2eq ,2ax =12.4 Hz, H-2eq), 3.764 (1H, dd, J 5 ,6 =2.4, J 5 ,4 =10.4 Hz, H-5), 4.023 (1H, dd, J 8 ,7 =5.5, J 8 ,8' =12.6 Hz, H-8), 4.062 (1H, ddd, J 4 ,NH =10.0, J 4 ,3 =10.3, J 4 ,5 =10.4 Hz, H-4), 4.389 (1H, dd, J 8'7 =2.6, J 8' ,8 =12.6 Hz, H-8'), 5.127 (1H, ddd, J 7 ,8' =2.6, J 7 ,8 =5.5, J 7 ,6 =7.3 Hz, H-7), 5.058 (1H, ddd, J 3 ,2eq =4.9, J 3 ,4 =10.3, J 3 ,2ax =11.5 Hz, H-3), 5.190 (1H, d, J NH ,4 =10.0 Hz, NH), 5.391 (1H, dd, J 6 ,7 =7.3, J 6 ,5 =2.4 Hz, H-6), 5.646 (1H, dd, J 1 ,2eq =2.1, J 1 ,2ax =10.3 Hz, H-1); 13 C NMR (CDCl 3 ) δ 20.70, 20.70, 20.75, 20.83, 20.83, 23.15, 35.09, 49.22, 61.98, 67.11, 70.23, 70.23, 73.67, 91.19, 168.75, 169.90, 170.12, 170.36, 170.59, 170.88. HRMS (M+Cs + ) calcd C 20 H 29 O 12 NCs 608.0744, found 608.0750.
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Aureobacterium barkerei strain KDO-37-2 (ATCC 49977) and KDO aldolase (EC 4.1.2.23) isolated therefrom are disclosed. The KDO aldolase is further disclosed to have a broad substrate specificity with respect to its reverse reaction, i.e. the condensation of aldoses with pyruvate to form a wide range of 2-keto-3-deoxy-onic acids, including 2-keto-3-deoxy-nonulosonic acid, 2-keto-3-deoxy-octulosonic acid, 2-keto-3-deoxy-heptulosonic acid, and 2-keto-3-deoxy-hexulosonic acid. In particular, 3-deoxy-D-manno-2-octulosonic acid (D-KDO), a vital component of lipopolysaccharides found in the bacterial outer membrane may be synthesized from D-arabinose and pyruvate in 67% yield.
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FIELD OF THE INVENTION
The present invention relates to a device for winding yarn packages at a work station of a textile machine which produces wound yarn bobbins, such as a winder, wherein each yarn package is surface driven by a friction roller driven by its own motor and wherein the motor and the friction roller are seated in a common housing for the operational units of the work station.
BACKGROUND OF THE INVENTION
The conventional options for winding bobbins are either to drive directly the empty bobbin on which the yarn package is to be wound or indirectly by surface contact of the yarn package with a friction roller. Yarn packages are driven by friction rollers in open end spinning machines and bobbin winding machines in particular. In bobbin winding machines, the friction rollers are typically embodied as grooved cylinders and are simultaneously used for yarn placement on the bobbin. The friction roller is generally driven by a motor via an interposed gear or via a belt drive, with the motor being seated in the housing of the work station by which the bobbin is wound. Such a drive is known for example from German Patent Publication DE 39 16 918 A1. A gear or a belt drive is required because of the spatial separation of the mounting locations of the friction roller and the motor.
SUMMARY OF THE INVENTION
It is accordingly an object of the present invention to simplify the design of devices for winding yarn onto bobbins and to make it easier to perform maintenance.
Briefly summarized, the present invention accomplishes this objective by providing a device for winding of yarn packages at a bobbin winding work station of a textile machine which comprises a housing, friction roller means rotatably supported by the housing to extend axially therefrom for surface driving of a bobbin during winding thereof, and a respective motor for driving the friction roller means, the motor comprising a stator directly received within the housing and the friction roller means comprising an axial bearing for the shaft disposed within the housing adjacent the motor. Preferably, the friction roller means comprises a continuous shaft and a friction roller mounted on the shaft and the motor comprises a rotor, the friction roller and the rotor being supported on the shaft.
The advantages of a continuous shaft on which the friction roller and the rotor of the drive motor are seated together rest in eliminating assembly and adjustment work conventionally necessary when connecting the drive shaft of a friction roller with the drive shaft of a motor. The reduction of the number of components also simplifies maintenance and possible replacement of the shaft. The support of the shaft is furthermore simplified in that only a radial bearing need be provided in the housing for the operational components of the work station, while the shaft is axially supported at the motor, preferably by fixing the axial bearing in a motor cover of the housing. In this manner, it is possible to remove the friction roller, together with the rotor, out of the stator windings of the motor after the housing cover has been removed and the friction roller has been freed. Since furthermore the stator windings of the motor are inserted directly into a recess in the housing of the work station, a simple replacement of the drive unit is possible. The direct installation of the stator windings into the housing and the continuous character of the motor shaft and the friction roller shaft in accordance with the invention have the advantage that the friction roller may be replaced without replacing the entire motor, in contrast to the conventional embodiment of the friction roller as an external rotor motor, such as is known, for example, from German Patent DE-PS 593 358.
In a preferred embodiment of the invention, the friction roller itself can be a grooved cylinder for traversing yarn placement on the bobbin, which is generally typical of bobbin winding machines. Advantageously, a reciprocating grooved cylinder offers the option of more uniform placement of the yarn on the bobbin end edges in order to achieve an even yarn structure at the bobbin ends. In accordance with the invention, an eccentric drive with a controllable electric motor is provided for imparting the reciprocating motion which offers the advantage that any desired reciprocating motion can be continuously set.
The axial movement during reciprocating motion of the grooved cylinder is generated in accordance with the invention in that the axial bearing of the shaft is resiliently supported on the housing cover for the drive motor, e.g., by a biasing spring, and the eccentric drive is powered by means of a controllable electric motor which is in operative connection with the axial bearing. The amount of the reciprocating motion is minimal, e.g., approximately three millimeters. The reciprocating motion can be taken, for example, from an eccentric disk driven by the motor and mechanically transmitted to the shaft of the friction roller. This arrangement offers the advantage that the generation of the reciprocating motion is divorced from the rotary movement of the shaft and, in this manner, any desired reciprocating rhythm and stroke can be set. In contrast, in a device known from French Laid-Open Application 1,436,308, the reciprocating motion of a friction roller is generated by an obliquely installed continuous ball drive. Aside from the fact that the reciprocating motion of such device depends on the rpm of the cylinder, the device is subjected to increased wear at high rpm and is therefore likely to malfunction.
If the axial support of the shaft is provided in the housing cover of the motor, it is possible to replace a rigid housing cover by a housing cover in which the axial bearing of the shaft is resiliently supported on the housing cover. In this manner, it is possible in a simple manner to convert a conventional work station into a bobbin winding station with an reciprocating friction roller by the installation of an reciprocating drive.
According to a further aspect of the invention, the drive motor of the friction roller is preferably an electronically commutated three-phase synchronous motor. Such motors are simple in construction and because of the commutation they can be exactly controlled by means of Hall sensors.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic side elevation, partially in cross-section, of an exemplary embodiment of a device for winding yarn packages in accordance with the present invention;
FIG. 2 is a cross-sectional view of a device in accordance with one embodiment of the present invention, having an reciprocating drive of the friction roller;
FIG. 3 is a plan view of the friction roller drive motor of the device of FIG. 2, taken in the direction toward the friction roller and with the housing cover removed; and
FIG. 4 is a cross-sectional view of an alternative embodiment of the present invention having a non-reciprocating friction roller, showing the axial seating of the shaft of the friction roller.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
One work station 1 of a textile winding machine for winding yarn into bobbins according to the present invention is schematically shown in FIG. 1. A yarn 2 is directed from a yarn supply, not shown, which can either be a feeding bobbin or a spinning station, through a yarn guide element 3 in the direction of the arrow 4 onto a friction roller 5 in the form of a grooved cylinder used for placement of the yarn onto a yarn package 6 of a cheese 7 resting with its circumferential surface on the grooved friction roller 5. in this manner, the yarn 2 is placed in crosswise layers 8 from the grooved cylinder 5 onto this yarn package 6. The cheese 7 is supported in a known manner in a creel 10, only partially shown. Winding of a cheese is known per se from the prior art and therefore does not need to be described in detail herein.
The friction roller 5 is fastened on a shaft 11 which is seated in radial bearings 13 in a wall of a housing 12 for the operational units of the work station 1. The end 11k of the shaft 11 is conically shaped and is received in a correspondingly shaped recess of the friction roller. The friction roller is fastened on the shaft 11 by a screw connection 11v.
The housing 12 also serves as the housing for a drive motor 15 for the friction roller 5, the motor 15 being received in a recess 14 of the housing 2. In the illustrated embodiment, the stator windings 16 of the motor 15 are received in the recess 14 of the housing while the rotor 17 of the drive motor 15 is fastened on the shaft 11.
Axial support of the shaft 11 is provided in an outward cover 18 of the housing enclosing the motor which is fastened on the housing 12 by means of screws 19, as symbolically indicated.
In the schematic drawing of FIG. 1, the housing cover 18 is formed in two parts. One part 18a, which is directly screwed to the housing 12, supports a deep groove ball bearing assembly 20 in which the shaft 11 rotates. This ball bearing assembly 20 is fastened in the cover part 18a by means of the other cover part 18b which is screwed together with the cover part 18a, as indicated by the screw symbols 21. A locking ring 22 fixes the ball bearing assembly 20 on the shaft 11. The schematic drawing of FIG. 1 shows a stationary, non-reciprocating friction roller 5.
If the friction roller 5 is removed from the shaft 11 and the housing cover 18 is lifted after the screws 19 have been removed, the shaft 11 with the rotor 17 seated thereon can be pulled out of the stator windings 16 of the drive motor 15 and the ball bearing assembly 20 remains on the shaft 11.
After removing the shaft 11, the stator windings 16 may be pulled out of the recess 14 in the housing 12. In accordance with the steps described above, it is therefore readily possible to increase the output of the motor by exchanging one rotor for another rotor made of a magnetic material of a higher order. It is also possible to replace an entire motor in a very short time. This is of advantage, for example, if a motor of higher output is to be used for larger bobbins (e.g. 10" bobbins) or for extremely high winding speeds. The installation of a new motor is thus possible without changing the dimensions of the housing.
The rotor of an electronically commutated three-phase synchronous motor, preferably employed in accordance with the present invention, is composed of permanent magnets. An increase in output can be achieved by stronger permanent magnets, for example, as well as a correspondingly adapted winding package of the stator windings.
FIG. 2 depicts a more detailed cross-section through a device in accordance with the present invention for winding yarn packages at a work station 1 of a textile bobbin winding machine. The friction roller has been omitted in this figure in order to more clearly show the design of the drive for the friction roller. As in the embodiment of FIG. 1, the conical extension 11k of the shaft is received in a correspondingly shaped conical bore in the interior of the friction roller and the friction roller is fastened on the shaft 11 by means of a screw 11v. In the area of the friction roller, the shaft 11 is displaceably supported within a tube 23 by means of a needle bearing 24 which is fastened by means of a locking ring 25 in the tube 23. The tube 23 is cantilevered from the housing 12 for the work station 1, with radial bearings 13 being located inside the tube 23 in the area of the mounted end of the housing 12 for providing further support of the shaft 11 in the housing 12.
A rotor 17, which is made of a package of permanent magnets, is mounted on the shaft 11. A rotor of permanent magnets has the advantage of being simply constructed and no electrical supply lines are required. In contrast, transfer of current between a conventional rotating rotor with windings and the stationary housing part is only possible by means of collector rings and brushes, which are prone to wear.
A compatible assembly of stator windings 16 is inserted into the recess 14 of the housing 12 as a complete, enclosed package 26 and is fixed against rotation by lateral centering projections 27 on the casing 26 of the stator package, as can be seen in the sectional view of FIG. 3. The installation and removal of the stator windings is thus made easier by not pressing the stator windings into the recess of the housing.
The drive motor 15 of the friction roller 5 is an electronically commutated DC motor with its stator windings wired as in a three-phase synchronous motor. Commutation of the motor takes place by means of a pole ring 28 and three Hall sensors 29, one of which is visible in FIG. 2, which are distributed in a defined arrangement about the circumference of the stator windings. The Hall sensors 29 scan the position of the pole ring 28 on the shaft 11 and thus the position of the rotor 17 in order to control the supply of the individual windings of the stator package on the basis of this position. The signals of the Hall sensors are transmitted to a control device 30 via a signal line 29a. The control device 30 is connected with a net 31 and controls the transmission of current to individual winding cables 32 by means of which the stator windings are supplied. Instead of being excited by their own pole ring 28, the Hall sensors can also be directly excited by the magnet of the rotor 17 for commutating the stator current.
An additional magnet wheel 33 is fastened on a knurled portion llr at the right end of the shaft 11 disposed behind the motor 15, as viewed in FIG. 2, for detecting the length of the wound yarn. Together with another Hall sensor 34 installed into the housing cover 18, the magnet wheel 33 is used for yarn length measuring and rpm detection. Because the pole ring 28 has too small a diameter and the rotor 17 too few poles, they are less suitable for exact yarn length measuring. The magnet wheel 33 and the Hall sensor 34 produce a sensor signal which is supplied for evaluation to the winding station computer 35 via a signal line 34a. In turn, the winding station computer can control the control device 30 of the friction roller motor 15 in respect to predetermined rpms by means of predetermined signals. The winding station computer 35 is connected via a signal line 35a with the control device 30 for this purpose.
The instant exemplary embodiment shows a device with a friction roller drive having a grooved cylinder making reciprocating motions in the axial direction. The reciprocating motion, indicated by the two-headed arrow 36 in FIG. 2, is achieved by means of an eccentric drive 37 which consists of a rocker-shaped lever 38 resting with a crimped end 39 against a displaceable cover assembly 18s made of several parts. The end 39 of the lever 38 rests on a cap 18sk which, in turn, rests on a ring-shaped element 18sr. The deep groove ball bearing assembly 20 is seated in this ring-shaped element 18sr and forms an axial bearing of the shaft 11. The ring-shaped element 18sr slides at its circumference in the housing cover 18a and, in the process, the ring-shaped part 18sr is supported by means of a compression spring 40 on the housing cover part 18a which is fixedly connected with the housing 12. The ring-shaped element 18sr, and thus the cap 18sk, are pressed against the crimped end 39 of the lever 38 by means of the compression spring 40. Since the ball bearing assembly 20 is fixedly connected with the displaceable ring 18sr, the shaft 11 together with the friction roller mounted thereon is pushed rightward until a stable end position is achieved. An elastic cover 41 which engages the cap 18sk and at the same time encloses the cover 18a protects the bearing assembly 20 and the displaceable ring 18sr from dirt and debris.
The rocker-shaped lever 38 is rotatably seated in a hinge 42 on the housing 12 of the work station and supports a roller 44 on its other end 43. This roller 44 peripherally engages a wheel 45 which, as shown by the line 46 representing its axis, is eccentrically mounted on a shaft 47 supported within the housing for the work station 1. The shaft 47 additionally supports a gear wheel 48 which is centered on the shaft 47 and in turn meshes with a drive pinion 49 of a motor 50. The motor 50 is mounted in the housing of the work station 1 and is connected via a signal line 50a with the winding station computer 35, which presets the rpm of the motor 50 and thus the reciprocating frequency of the shaft 11. When the pinion 49 is rotated by the driving force of the motor 50, the meshing gear wheel 48 also rotates and, as a result, the wheel 45 is also driven. From the initial position shown in FIG. 2, the axis 46 of the wheel 45 follows an eccentric circular motion about the rotational axis 51 of the shaft 47. After a rotational movement of 180°, the axis 46 of the wheel 45 is in the position 46' and the periphery of the wheel 45 then assumes the position 45' shown in broken lines and thereby displaces the roller 44 by the distance 52. While the roller 44 is displaced by this amount rightward into the position 44', the lever 38 pivots about the hinge 42 causing its upper end 39 to push in the direction of the arrow 53 against the cap 18sk which correspondingly pushes against the displaceable part of the ring 18sr. The ball bearing assembly 20 and thus the shaft 11 are correspondingly displaced leftward with the ring 18sr in the direction of the arrow 53.
When the roller 44 is shifted into the position 44', the end 39 of the rocker-shaped lever 38 is moved toward the left in the direction of the arrow 53 by a defined, predetermined amount as a result of the configuration of the lever 38. Thus, the assembled unit of the shaft 11 with the rotor 17 and the friction roller fastened thereon are moved to the left into the position shown in broken lines. In actuality the displacement is approximately 3 mm. By means of this movement, it is possible to control the placement of the yarn at the axial ends of the cheese in such a way that an even, uniform end edge construction is assured. The alternating frequency of the axial reciprocation of the shaft 11 and the friction roller can be preset through control of the rpm of the motor 50 by means of the winding station computer 35.
In the course of such alternation, care must be taken that the Hall sensors can continue to receive the signals of the magnet wheels intended for them. For this reason, the pole ring 28 and the magnet wheel 33 are embodied to be appropriately wide in order to cover the Hall sensors during their reciprocating motion.
During the subsequent one-half revolution of the wheel 45 by 180°, the wheel 45 returns into the initial position causing the roller 44 to also moves back into the position shown in full lines and the lever 38 yields rightward under the biasing force of the spring 40. The shaft 11 thus also returns into the initial position shown in full lines. During the ongoing reciprocating motion of the shaft 11, the lever 38 performs a continuous rocking motion about the hinge 42 as indicated by the two-headed arrow 54.
The difference between the reciprocating motion created in accordance with the described embodiment of the present invention and the alternating motion of a friction roller as known from French Laid-Open Application 1,436,308 is that, in the present invention, the reciprocating motion is independent from the rotating motion of the friction roller. Thus, for example, it is possible to control the reciprocating motion via the winding station computer independently of the rotating motion of the friction roller and as a function of the yarn parameters or the bobbin diameter.
FIG. 3 shows a plan view of the motor 15 in a direction toward the housing cover 18, which has been omitted in the drawing. In addition to the magnet wheel 33, the arrangement of the centering projections 27 of the casing 26 of the motor 15 as mounted into the recess 14 of the housing 12 is shown. The centering projections prevent the rotation of the stator windings in the housing. The position of the Hall sensor 34 in relation to the magnet wheel 33 is also indicated. Additionally, the position of the winding cables 32, the current supply line to the stator windings and the position of the signal lines 29a of the Hall sensors 29 are indicated.
FIG. 4 illustrates the axial mounting of a non-reciprocating shaft 11 in the housing cover 18 of the motor 15 by means of a deep groove ball bearing assembly 20. In contrast to the winding station represented in FIG. 1, the arrangement of the magnet wheel 33 for yarn length measuring and for the determination of the length of the discarded yarn during cleaning cuts is shown as affixed on the shaft 11. The winding station 1 may thus be readily converted for reciprocation of the shaft 11 according to the present invention by replacing the housing cover 18 with a housing cover as shown in FIG. 2.
It will therefore be readily understood by those persons skilled in the art that the present invention is susceptible of a broad utility and application. Many embodiments and adaptations of the present invention other than those herein described, as well as many variations, modifications and equivalent arrangements will be apparent from or reasonably suggested by the present invention and the foregoing description thereof, without departing from the substance or scope of the present invention. Accordingly, while the present invention has been described herein in detail in relation to its preferred embodiment, it is to be understood that this disclosure is only illustrative and exemplary of the present invention and is made merely for purposes of providing a full and enabling disclosure of the invention. The foregoing disclosure is not intended or to be construed to limit the present invention or otherwise to exclude any such other embodiments, adaptations, variations, modifications and equivalent arrangements, the present invention being limited only by the claims appended hereto and the equivalents thereof.
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At each work station of a textile machine producing wound bobbins, the yarn package on which yarn is wound is driven by a friction roller. In contrast to the conventional driving of the roller by a gear motor flanged to the housing of the work station, which has the disadvantage of requiring space and difficulty in removing and replacing the friction roller for maintenance, the present invention simplifies the friction roller drive by configuring the housing of the work station for the direct reception of the stator windings of the drive motor for the friction roller and mounting the friction roller and the rotor of the drive motor together on a continuous shaft.
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[0001] This is a U.S. national stage application of International Application No. PCT/JP2009/004650, filed on 16 Sep. 2009. Priority under 35 U.S.C. §119(a) and 35 U.S.C. §365(b) is claimed from Japanese Application No. JP2008-269188, filed 17 Oct. 2008, the disclosure of which is also incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to an optical element and a light emitting device.
[0004] 2. Description of Related Art
[0005] In these years, LED lighting devices are coming into practical use in accordance with the development of high power LEDs (Light Emitting Diodes) and high efficiency LEDs as alternatives to incandescent light-bulbs and fluorescent lamps. Being compared with an incandescent light-bulb and a fluorescent lamp, an LED is small in its size and high in the luminous density. Furthermore, while the incandescent light-bulb and fluorescent lamp emit light all the directions, the LED is provided with a feature of having a narrow directivity. Moreover, recently power LEDs with their capacity of 3 W and 10 W have been also coming into practical use.
[0006] As a light emitting device using such an LED for a light source, a light emitting device described next is proposed. In the light emitting device, light emitted from an LED goes through a translucent member, and is reflected by a reflecting mirror and the like. The reflected light is reflected by a reflecting mirror so as to be launched from a second surface located at a place opposite to a first surface of a disk-shaped member (Refer to Patent Document 1).
PRIOR ART DOCUMENT
Patent Document
[0000]
Patent Document 1: JP 2004-87630 A
SUMMARY OF THE INVENTION
[0008] Unfortunately, in the case of such a light emitting device described in Patent Document 1, light emitted from an LED is introduced into a tight area located at a side part of the LED so as to be launched from the side part, and then the light is launched to one side of a disk-shaped member. Therefore, when a flat surface side of the disk-shaped member is used as a light source, a central section of the flat surface may sometimes become excessively bright, or contrarily too dark. In other words, if light linearly emitted toward an upper part of the LED passes through there, the central section of the flat surface has a high luminous density so as to result in a high brightness (glare) there. Meanwhile, if light at the central section is interrupted by a reflecting mirror, there appears a dark circle at the central section of the flat surface. Thus, the light emitting device described in Patent Document 1 is hardly appropriate as a surface light source.
[0009] Moreover, in the case of the light emitting device described in Patent Document 1; light launched from the side part of the LED is refracted at the side part, if the side part does not intersect at a right angle with the launched light; so that it becomes hardly possible to radiate the light to the reflecting mirror at a predetermined angle. Furthermore, if the side part of the LED is rough with unevenness, a launching direction of the light from the LED diffuses in a relatively wide angular range and then it becomes hardly possible to control the launched light in a certain direction. Thus, if there exists any light that do not progress to the reflecting mirror with a designed angle, a part of launched light may not be radiated to the reflecting mirror, or a part of the launched light may be reflected in directions other than a predetermined direction. As a result, the light emitting device has a high percentage of light of radiation loss.
[0010] Thus, it is an object of the present invention to provide an optical element and a light emitting device that suppress the appearance of glare parts and dark sections, furthermore having a high optical efficiency so as to be suitable for surface luminescence.
[0011] To achieve the object described above, an optical element according to the present invention includes: a light incoming section through which light enters; a first light guiding section for guiding the light incident on the light incoming section; a reflecting surface, placed to be opposite to a light entry side of the first light guiding section, for totally-reflecting a linearly-traveling part of the incident light; and a second light guiding section for guiding the reflected light; wherein the first light guiding section contains light scattering particles for multiply-scattering light and generating light which passes through the reflecting surface and is emitted externally; and the second light guiding section launches at least a part of the incident light in a direction of the same surface side as the light passing through the reflecting surface travel out.
[0012] It is preferable that the second light guiding section includes a prism section at a position, opposite to a side of the reflecting surface; the prism section having its sawtooth-like section for changing traveling directions of the guided light in the direction of the same side as the reflecting surface.
[0013] It is preferable that a reflecting part is formed at an edge positioned within the second light guiding section, being distant from the first light guiding section; the reflecting part reflecting the guided light toward the same side as the reflecting surface.
[0014] It is preferable that; with regard to the light scattering particles, where a scattering parameter and a thickness of the first light guiding section are expressed as “τ” and “T”, respectively, the product of “τ” and “T” with respect to the light scattering particles is within a range of 0.1 to 50.
[0015] To achieve the object described above, a light emitting device according to the present invention includes: a translucent member, and a light emitting component; the translucent member including: a light incoming section through which light enters, a first light guiding section for guiding the light incident on the light incoming section, a reflecting surface, placed to be opposite to a light entry side of the first light guiding section, for totally-reflecting a linearly-traveling part of the incident light, and a second light guiding section for guiding the reflected light; and the light emitting component emitting light into the light incoming section; wherein the first light guiding section contains light scattering particles for multiply-scattering light and generating light which passes through the reflecting surface and is emitted externally; and the second light guiding section launches at least a part of the incident light in a direction of the same surface side as the light passing through the reflecting surface travel out.
[0016] It is preferable that the second light guiding section is formed to be plate-like; and the first light guiding section is placed at a center of the plate-like second light guiding section.
[0017] It is preferable that the translucent member is made of a translucent resin material, and the light scattering particles are silicon particles having their particle diameter within a range from 1 to 10 μm; and the light scattering particles are also included in the second light guiding section.
[0018] According to the present invention, provided can be an optical element and a light emitting device that suppress the appearance of a glare zone and a dark section, furthermore having a high optical efficiency so as to be suitable for surface luminescence.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 is a plan view drawing to show a structure of a translucent member as an optical element according to an embodiment of the present invention.
[0020] FIG. 2 is a front elevation view of the translucent member shown in FIG. 1 .
[0021] FIG. 3 is a bottom plan view of the translucent member shown in FIG. 1 .
[0022] FIG. 4 is a cross-sectional view taken from the line A-A of the plan view of FIG. 1 .
[0023] FIG. 5 is an enlarged view showing details of a part of a reflecting surface of the translucent member shown in the cross-sectional view of FIG. 4 .
[0024] FIG. 6 is a graph showing an angle distribution (A, Θ) of a scattered light intensity by a single spherical particle.
[0025] FIG. 7 is an enlarged general view showing a main part of a second light guiding section of the translucent member shown in the cross-sectional view of FIG. 4 .
[0026] FIG. 8 shows a structure of a light emitting device according to the embodiment of the present invention.
[0027] FIG. 9 shows paths through which rays of light emitted from an LED enter the translucent member, and then the rays are reflected at the reflecting surface so as to be guided to the second light guiding section, in the light emitting device according to the embodiment of the present invention.
[0028] FIG. 10 shows a brightness distribution in a light emitting device of a first modification with respect to the light emitting device according to the embodiment of the present invention.
[0029] FIG. 11 shows a brightness distribution in a light emitting device of a second modification with respect to the light emitting device according to the embodiment of the present invention.
[0030] FIG. 12 shows a brightness distribution in the light emitting device according to the embodiment of the present invention.
[0031] FIG. 13 shows a brightness distribution in a light emitting device of a third modification with respect to the light emitting device according to the embodiment of the present invention.
[0032] FIG. 14 is a graph showing a relationship between a light divergence angle and a light transmission factor as a density of light scattering particles varies; wherein the light scattering particles, used for the light emitting device according to the embodiment of the present invention, being contained in an acrylic resin plate with a thickness of 10 mm.
[0033] FIG. 15 is a plan view drawing to show a first modification of the translucent member according to the embodiment of the present invention.
[0034] FIG. 16 is a drawing to show an example of using a light emitting device applying the translucent member shown in FIG. 15 as a street lamp, the drawing showing a view from a road side.
[0035] FIG. 17 is a drawing to show the example of using the light emitting device applying the translucent member shown in FIG. 15 as the street lamp, the drawing showing a view in a traveling direction.
[0036] FIG. 18 is a plan view drawing to show a second modification of the translucent member according to the embodiment of the present invention.
[0037] FIG. 19 is a side elevation view of the translucent member of the second modification shown in FIG. 18 , the side elevation view showing a view taken from a direction of a large arrow “C” in FIG. 18 .
[0038] FIG. 20 is a side elevation view of the translucent member of the second modification shown in FIG. 18 , the side elevation view showing a view taken from a direction of a large arrow “B” in FIG. 18 .
[0039] FIG. 21 is a schematic cross-sectional view of a sign applying a light emitting device using the translucent member of the second modification, as a light source.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0040] Structures and functions of an optical element and a light emitting device according to an embodiment of the present invention are described below with reference to the accompanied drawings.
[0041] (Structure of Optical Element)
[0042] FIG. 1 is a plan view drawing to shows a structure of a translucent member 1 as an optical element according to an embodiment of the present invention, and in the meantime, FIG. 2 and FIG. 3 are a front elevation view and a bottom plan view of the translucent member, respectively.
[0043] As shown in FIGS. 1 to 3 , having its circular contour, the translucent member 1 is a transparent poly-methyl methacrylate (hereinafter abbreviated to “PMMA”) resin compact that contains spherical and translucent silicone particles (not illustrated) with their particle diameter of several micro-meters, as light scattering particles. The translucent member 1 includes a first light guiding section 2 positioned at a central area, and being flat and circular-shaped; and a second light guiding section 3 positioned around the first light guiding section 2 , and being torus or doughnut-shaped. The first light guiding section 2 includes a light incoming section 11 through which light enters the first light guiding section 2 (Refer to FIG. 3 and FIG. 4 ), and a reflecting surface 12 that reflects the incident light on the light incoming section 11 , and is located at a surface opposite to the light incoming section 11 .
[0044] Positioned at a center of the reflecting surface 12 is a center point 13 , which is a center of the translucent member 1 , and a center of the first light guiding section 2 , as well as a center of the second light guiding section 3 . In the translucent member 1 , the incident light on the light incoming section 11 is guided to the reflecting surface 12 , and then the light reflected by the reflecting surface 12 is guided to the second light guiding section 3 . The first light guiding section 2 and the second light guiding section 3 are integrated into a whole in such a manner that the translucent member 1 is so made as to look like just a wholly-integrated single component. In the following explanation, an upper side and a lower side in FIG. 2 are called a topside and a bottom side of the translucent member 1 , respectively.
[0045] The first light guiding section 2 shown in FIG. 1 has its outer radius (R 1 ) of 11 mm, meanwhile the second light guiding section 3 has its outer radius (R 2 ) of 80 mm. Therefore, in the translucent member 1 , an area that the first light guiding section 2 occupies is calculated from a formula (πR 12 /πR 22 ) to be approximately 1.89%.
[0046] As shown in FIG. 2 , a topside surface of the second light guiding section 3 of the translucent member 1 is a flat surface, meanwhile a bottom side surface of the second light guiding section 3 is so formed as to slope from an edge 15 of the translucent member 1 toward the first light guiding section 2 positioned at the center of the translucent member 1 to gradually increase the thickness of the second light guiding section 3 . Then, at a lower side of the edge 15 of the translucent member 1 , there is formed a ring-shaped reflecting part 16 that fully reflects upward the light guided into the second light guiding section 3 . The reflecting part 16 is placed in a concentric pattern having its center at the center point 13 . In the meantime, the first light guiding section 2 has an LED holder 17 , shaped to be cylindrical, at its bottom side.
[0047] As shown in FIG. 3 , the circular first light guiding section 2 is located at a central area of the translucent member 1 ; and the LED holder 17 , being ring-shaped, is located at a bottom side of the first light guiding section 2 . In the meantime, the reflecting part 16 , being ring-shaped, is formed with a uniform shape at each location along an entire circumference at a bottom side of the edge 15 of the second light guiding section 3 .
[0048] FIG. 4 is a cross-sectional view taken from the line A-A of the plan view of FIG. 1 . The LED holder 17 is shaped to be cylindrical, being protruded toward a bottom side. Though constituting a part of the first light guiding section 2 , the LED holder 17 may be placed at a bottom side of the second light guiding section 3 , being formed as a part of the second light guiding section 3 . An inner-circumferential surface 17 a of the LED holder 17 stretches to a bottom side, being perpendicular to a flat surface of the light incoming section 11 . In the meantime, an outer-circumferential surface 17 b of the LED holder 17 is so formed as to make an acute angle “α” with respect to the inner-circumferential surface 17 a . When light coming from a light source to be described later enters the LED holder 17 , the outer-circumferential surface 17 b reflects incident light and guides the light toward the first light guiding section 2 and the second light guiding section 3 .
[0049] FIG. 5 is an enlarged view showing details of a surrounding part of the reflecting surface 12 of the translucent member 1 shown in the cross-sectional view of FIG. 4 . A most concave part in the reflecting surface 12 has the center point 13 . Incidentally, the translucent member 1 shown in FIG. 5 contains light scattering particles 21 . The light scattering particles 21 are silicone particles with their particle diameter of 1 to 10 μm, and are contained with a higher density in the first light guiding section 2 than in the second light guiding section 3 . More specifically, a content rate of the light scattering particles 21 in the first light guiding section 2 is 0.1 weight percent, meanwhile that in the second light guiding section 3 is 0.06 weight percent. Incidentally, where a scattering parameter and a thickness of the first light guiding section 2 are expressed as “τ” and “T”, respectively, the product of “τ” and “T” with respect to the light scattering particles 21 contained in the first light guiding section 2 is within a range of 0.1 to 50.
[0050] In the present embodiment, the LED holder 17 also contains the light scattering particles 21 , and a content rate of the light scattering particles 21 there is the same as that in the first light guiding section 2 . However, it is also possible for the LED holder 17 to contain no light scattering particles 21 or to have the same content rate of the light scattering particles 21 as that in the second light guiding section 3 . FIG. 5 shows that the light scattering particles 21 are placed in a dispersed state.
[0051] The light scattering particles 21 are further described next. The light scattering particles 21 are light guiding elements provided with a uniform scattering power within their volume-wise extent, and they include a number of spherical particles as scattering fine particles. When light enters an internal area of the first light guiding section 2 or the second light guiding section 3 , the light is scattered by the scattering fine particles.
[0052] The Mie scattering theory that provides the theoretical fundamentals of the light scattering particles 21 is explained next. Calculated in the Mie scattering theory is a solution for Maxwell's equations of electromagnetism in the case where spherical particles (scattering fine particles) exist in a ground substance (matrix) having a uniform refractive index, wherein the spherical particles having a refractive index that is different from the refractive index of the matrix. A formula (1) described below expresses a light intensity distribution I (A, Θ) dependent on scatting angles of light scattered by scattering fine particles that correspond to the light scattering particles 21 . “A” is a size parameter representing an optical size of the scattering fine particles, and the parameter shows an amount corresponding to a radius “r” of the spherical particles (the scattering fine particles) standardized with a wavelength “λ” of light in the matrix. Meanwhile, an angle “Θ” represents a scattering angle, wherein a direction identical to a traveling direction of incident light corresponds to “Θ=180 deg.”
[0053] “i1” and “i2” in the formula (1) are expressed with formulas (4). Then, “a” and “b” subscripted with “v” in formulas (2) to (4) are expressed with formulas (5). P(cos Θ) superscripted with “1” and subscripted with “v” is a Legendre polynomial; meanwhile “a” and “b” subscripted with “v” are composed of a first kind Recatti-Bessel function Ψ V , a second kind Recatti-Bessel function ζ v , and their derivatives. “m” is a relative refractive index of the scattering fine particles with reference to the matrix, namely “m=n-scatter/n-matrix.”
[0000]
[
Expression
1
]
I
(
A
,
Θ
)
=
λ
2
8
π
2
(
i
1
+
i
2
)
(
1
)
K
(
A
)
=
(
2
α
2
)
∑
v
=
1
∞
(
2
v
+
1
)
(
a
v
2
+
b
v
2
)
(
2
)
A
=
2
π
r
/
λ
(
3
)
i
1
=
∑
v
=
1
∞
2
v
+
1
v
(
v
+
1
)
{
a
v
P
v
1
(
cos
Θ
)
sin
Θ
+
b
v
P
v
1
(
cos
Θ
)
Θ
}
i
2
=
∑
v
=
1
∞
2
v
+
1
v
(
v
+
1
)
{
b
v
P
v
1
(
cos
Θ
)
sin
Θ
+
a
v
P
v
1
(
cos
Θ
)
Θ
}
(
4
)
a
v
=
Ψ
v
′
(
m
A
)
Ψ
v
(
A
)
-
m
Ψ
v
(
m
A
)
Ψ
v
′
(
A
)
Ψ
v
′
(
m
A
)
ζ
v
(
A
)
-
m
Ψ
v
(
m
A
)
ζ
v
′
(
A
)
b
v
=
m
Ψ
v
′
(
m
A
)
Ψ
v
(
A
)
-
Ψ
v
(
m
A
)
Ψ
v
′
(
A
)
m
Ψ
v
′
(
m
A
)
ζ
v
(
A
)
-
Ψ
v
(
m
A
)
ζ
v
′
(
A
)
(
5
)
[0054] FIG. 6 is a graph showing a light intensity distribution I (A, Θ) by a single spherical particle on the basis of the above formulas (1) to (5). Namely, FIG. 6 shows an angular distribution of scattered light intensity I (A, Θ) in the case of incident light coming in from a lower side, wherein a spherical particle as a scattering fine particle exists at a position of an origin “G.” In the figure, a distance from the origin “G” to each of curves S 1 to S 3 represents the scattered light intensity in a corresponding angular direction of the scattered light. Each curve of S 1 , S 2 , and S 3 shows the scattered light intensity when the size parameter “A” is 1.7, 11.5, and 69.2, respectively. In FIG. 6 , the scattered light intensity is expressed in a logarithmic scale. Therefore, even a slight difference of intensity that appears in FIG. 6 is a significantly large difference in fact.
[0055] As shown FIG. 6 , it is understood that; the greater the size parameter “A” is (the larger the particle diameter is, at a certain wavelength “λ”), the more intensively the light is scattered in an upward direction (a frontward direction in the direction of radiation) with high directivity. In reality, the angular distribution of scattered light intensity I (A, Θ) can be controlled by using the radius “r” of the scattering element and the relative refractive index “m” between the matrix and the scattering fine particles as parameters, while the wavelength “λ” of incident light is set to be constant.
[0056] Thus, when incident light enters a scatter light guiding element that contains N (in number) single spherical particles, the incident light is scattered by a spherical particle. Moving forward through the scatter light guiding element, the scattered light is then scattered again by another spherical particle. In the case where particles are added with a certain volume concentration or higher, such scattering operation sequentially repeats several times and then the light is launched out of the scatter light guiding element. A phenomenon, in which such a scattered light is further scattered, is called a multiple scatter phenomenon. Though it is not easy to analyze such a phenomenon of multiple scattering in a translucent polymer substance by means of a ray tracing method, the behavior of a ray can be traced by Monte Carlo method for analysis of its characteristics. According to the analysis, in the case of incident light having no polarization, a cumulative distribution function of scattering angle “F(Θ)” is expressed with a formula (6) described next.
[0000]
[
Expression
2
]
F
(
Θ
)
=
∫
0
Θ
I
(
Θ
)
sin
Θ
Θ
∫
0
π
I
(
Θ
)
sin
Θ
Θ
(
6
)
[0057] “I(Θ)” in the formula (6) means the scattered light intensity of the spherical particle of the size parameter “A” expressed in the formula (1). When light having an intensity “I 0 ” enters the scatter light guiding element, and transmits for a distance “y” so as to be attenuated into “I” through the scattering, a formula (7) described below represents a relationship of the phenomenon.
[0000]
[
Expression
3
]
I
I
0
=
exp
(
-
τ
y
)
(
7
)
[0058] “τ” in the formula (7) is called the turbidity (having the same meaning as the “scattering parameter” mentioned previously); and it corresponds to a scattering coefficient of the matrix, and being proportional to the number of particles “N”, as a formula (8) indicates below. In the formula (8), “σ s ” represents a scattering cross-section area.
[0059] [Expression 4]
[0000] τ=σ s N (8)
[0060] According to the formula (7), the probability “p t (L)” of transmission passing through the scatter light guiding element having its length “L” without any scattering is expressed by a formula (9) described below.
[0000]
[
Expression
5
]
p
t
(
L
)
=
I
I
0
=
exp
(
-
σ
s
NL
)
(
9
)
[0061] On the contrary, the probability “p s (L)” of having any scattering within the optical path length “L” is expressed by a formula (10) described below.
[0062] [Expression 6]
[0000] p s ( L )=1 −p s ( L )=1−exp(−σ s NL ) (10)
[0063] It is understood according to the formulas described above that adjusting the turbidity “τ” makes it possible to control a degree of multiple scattering in the scatter light guiding element.
[0064] As the formulas indicate above, by using at least one of the size parameter “A” and the turbidity “τ” with respect to the scattering fine particles as a parameter, it becomes possible to control multiple scattering in the scatter light guiding element, and also to suitably set the launching light intensity and the scattering angle at a launching surface.
[0065] FIG. 7 is an enlarged general view showing mainly a part of the second light guiding section 3 of the translucent member 1 shown in the cross-sectional view of FIG. 4 . The second light guiding section 3 has a prism section 22 at its bottom side, the prism section 22 having its sawtooth-like section and being placed on a circle concentric with the center point 13 . In the present embodiment, a total of 225 saw teeth 23 are formed in the prism section 22 . Incidentally, only 25 in total of the saw teeth 23 are shown in FIG. 7 for the purpose of simple indication. The prism section 22 changes a course of light guided to a bottom side of the second light guiding section 3 to a topside. Meanwhile, a protrusion angle θ of a saw tooth 23 located at a position closer to the center point 13 is acuter than a protrusion angle θ of another saw tooth 23 located at a position further from the center point 13 .
[0066] Protrusion angles θ of the saw teeth 23 are specifically explained below. A protrusion angles θ of 25 saw teeth 23 existing within a width of 5 mm being closest to the center point 13 is 50 degrees. A protrusion angles θ of 25 saw teeth 23 existing within a width of 5 mm being next closer to the center point 13 is 55 degrees. A protrusion angles θ of 25 saw teeth 23 existing within a width of 5 mm being next closer to the center point 13 is 60 degrees. A protrusion angles θ of 25 saw teeth 23 existing within a width of 5 mm being next closer to the center point 13 is 65 degrees. A protrusion angles θ of 50 saw teeth 23 existing within a width of 10 mm being next closer to the center point 13 is 70 degrees. A protrusion angles θ of 75 saw teeth 23 existing within a width of 15 mm being furthest from the center point 13 is 75 degrees. Thus, the prism section 22 includes 6 divided groups of saw teeth 23 . Incidentally, the greater gradually the protrusion angle θ of the saw tooth 23 may be made, the further from the center point 13 the saw tooth 23 is located. In the meantime, a distance “H” between neighboring two saw teeth 23 is 0.2 mm, and the saw teeth 23 are placed to be symmetrical with respect to the center point 13 .
[0067] In FIG. 7 , a crossing angle β formed by a line “L” connecting protrusion peaks of the saw teeth 23 in a radial direction and the topside surface of the second light guiding section 3 is 6.5 degrees. Though an angle γ formed by a surface, at a closer side to the center point 13 , of each of the saw teeth 23 and the line “L” is 90 degrees, the angle γ may be set to be greater than 90 degrees. If the angle γ is set to be greater, the translucent member 1 can more easily be removed from a mold after the translucent member 1 is formed with the mold. Incidentally, at the lower side of the edge 15 adjacent to a saw tooth 23 located at the furthest position from the center point 13 , there is placed the reflecting part 16 . An angle θ 1 formed by a surface of the reflecting part 16 and the topside surface of the second light guiding section 3 is 30 degrees.
[0068] (Structure of Light Emitting Device)
[0069] FIG. 8 shows a structure of a light emitting device 40 according to the embodiment of the present invention, the light emitting device 40 having a chip-shaped LED 30 functioning as a light emitting component placed in the translucent member 1 shown in FIG. 4 . The LED 30 is placed in a section surrounded by the light incoming section 11 and the LED holder 17 of the translucent member 1 . A bottom part 31 of the LED 30 is shaped like a disc so that its circumferential surface 32 faces the inner-circumferential surface 17 a of the LED holder 17 . The circumferential surface 32 of the bottom part 31 and the inner-circumferential surface 17 a of the LED holder 17 are fixed to each other with a fixing member that is not illustrated. By means of fixing that part, the LED 30 is fixed to the LED holder 17 . In the meantime, the LED 30 is located at a position facing the center point 13 .
[0070] (Condition of Light Reflection at Reflecting Surface 12 )
[0071] FIG. 9 shows light paths, with dotted lines, through which rays of light emitted from the LED 30 enter the light incoming section 11 to get into the translucent member 1 , and then the light is reflected at the reflecting surface 12 so as to be guided to the second light guiding section 3 . When the light emitted from the LED 30 enters the first light guiding section 2 through the light incoming section 11 , the light is refracted somewhat in a direction toward the center point 13 , and then arrives at the reflecting surface 12 . Incidentally, an interface between PMMA as a substance of the translucent member 1 and the atmosphere is formed at the reflecting surface 12 . When light is radiated to the reflecting surface 12 with an incident angle θ 2 with respect to the interface (namely, the reflecting surface 12 ) while the incident angle being greater than a total reflection critical angle (41.84 degrees); the light, traveling from a medium having a higher optical refractive index (PMMA) to another medium having a lower optical refractive index (the atmosphere), does not pass through the interface, but is totally reflected there. On this occasion, the incident angle θ 2 is an angle formed between a normal line at a point, where incident light arrives at the reflecting surface 12 , and the incident light. The reflecting surface 12 is so formed as to satisfy the condition for such a total reflection, and furthermore to make the reflected light travel in parallel with the topside surface of the second light guiding section 3 . Therefore, most of light emitted from the LED 30 is totally reflected at the reflecting surface 12 so as to become parallel light, and is guided to the second light guiding section 3 .
[0072] In the meantime, on a profile curve of the reflecting surface 12 shown in FIG. 9 , a point corresponding to the center point 13 has a surface where a sum of an incident angle and a reflection angle becomes 90 degrees for light emitted straight upward from the LED 30 as a light source. In other words, an incident angle θ 2 for the point corresponding to the center point 13 is 45 degrees (an angle θ t1 as a sum of the incident angle and reflection angle there is equal to 90 degrees); and a tangential line on the reflecting surface 12 at the reflection point there intersects the topside surface of the second light guiding section 3 with an angle of 45 degrees. On the other hand, at a point where the profile curve of the reflecting surface 12 meets a plane of the topside surface of the second light guiding section 3 , an angle θ t2 as a sum of the incident angle and reflection angle there is described as “θ t2 =90 degrees+θ c ” (wherein the angle θ c is the total reflection critical angle; i.e., 41.84 degrees). A curve F(x) connecting these two points described above is a parabolic curve, as a kind of aspheric curve; and its derivative F′(x) is expressed as “tan(90−θt/2).”
[0073] Incidentally, the translucent member 1 contains the light scattering particles 21 . Therefore, in a course from emission out of the LED 30 through entering the first light guiding section 2 to reaching the reflecting surface 12 , and another course from reflection at the reflecting surface 12 to being guided into the second light guiding section 3 , the light is scattered. Since the light scattering particles 21 multiply-scatter most of the light within the translucent member 1 without attenuation, a part of the incident light passes through the reflecting surface 12 of the first light guiding section 2 to exit upward. In the meantime, the size of the light scattering particles 21 is adjusted according to the Mie scattering theory so as to increase the proportion of scattering in a traveling direction of the incident light, and therefore most of the light travels through almost the same path as they do without the light scattering particles 21 . In other words, most of the light that enters the light incoming section 11 travels along the dotted lines with an arrow shown in FIG. 9 from the first light guiding section 2 toward the second light guiding section 3 as almost parallel light.
[0074] In the operation described above, the light scattering particles 21 make a part of the light emitted from the LED 30 pass through the reflecting surface 12 , and generate light that exits outside. Namely, a past of the light emitted from the LED 30 exits upward from the first light guiding section 2 .
[0075] (Condition of Light Refraction and Reflection in the Second Light Guiding Section 3 )
[0076] As described above, the light guided into the second light guiding section 3 changes their traveling directions toward the topside surface of the second light guiding section 3 by the prism section 22 and the reflecting part 16 . The line “L” (Refer to FIG. 7 ) connecting the protrusion peaks of the saw teeth 23 of the prism section 22 is so formed as to make the crossing angle β by intersecting the optical paths of rays of the light guided into the second light guiding section 3 . Therefore, the guided parallel light is radiated to the prism section 22 .
[0077] The light radiated to the prism section 22 changes the traveling direction toward the topside surface of the second light guiding section 3 . With regard to the changed traveling direction, an output angle θ 3 at an outer circumferential position becomes smaller, because a protrusion angle θ at the outer circumferential position is greater in the translucent member 1 . That is to say; when being applied as a light source, the translucent member 1 works as a light source without directivity for illuminating a wide-angled area (Refer to FIG. 7 ). Since the light traveling through the second light guiding section 3 is partly scattered by the light scattering particles 21 , a part of the light radiated to the prism section 22 may pass through a saw tooth 23 that the light collides with at first, but most of the light that has passed through there at first is radiated to a neighboring saw tooth 23 so as to change its traveling direction toward the topside surface of the second light guiding section 3 by the saw tooth 23 . Incidentally, the dotted lines with an arrow shown in FIG. 7 indicate optical paths of rays of the light that change their traveling directions when no light scattering particles 21 exist, or when the light does not collide with the light scattering particles 21 .
[0078] As described above, the protrusion angle θ of a saw tooth 23 is greater, as the saw tooth 23 is located to be further from a side of the LED 30 toward the edge 15 of the second light guiding section 3 within an area of the second light guiding section 3 . Due to the arrangement, as described above, the light that changes its traveling direction is emitted from the topside surface of the second light guiding section 3 with a smaller output angle θ 3 , as the emitting position is located to be further from the side of the LED 30 .
[0079] Furthermore, the light guided to the reflecting part 16 is reflected by the reflecting part 16 , and then guided toward the topside surface of the second light guiding section 3 , and eventually emitted from the topside. The LED 30 has a strong optical directivity. Then, light traveling in a direction toward the center point 13 is strong, and light traveling in a direction away from the center point 13 is weak. Therefore, in FIG. 7 , quantity of light is lager for light guided from a lower area of the reflecting surface 12 (an area close to the center point 13 ) and an intermediate area of the reflecting surface 12 (an area somewhat away from the center point 13 ), and in the meantime quantity of light is smaller for light guided from an upper area of the reflecting surface 12 (an area close to the second light guiding section 3 ) as the area is located to be higher. Thus, the prism section 22 for mainly changing traveling direction of light guided to the lower area and the intermediate area of the reflecting surface 12 changes traveling direction of most of light radiated from the LED 30 , and the reflecting part 16 changes traveling direction of residual light. By means of the operation described above, eventually most of the light traveling through the second light guiding section 3 are emitted from the topside.
[0080] Incidentally, the second light guiding section 3 also contains the light scattering particles 21 . Therefore, in a traveling process of the light entering the second light guiding section 3 from the reflecting surface 12 and traveling further, and also in a traveling process of the light radiated from the prism section 22 toward the topside of the second light guiding section 3 , the light is scattered in a complex manner. Then, the light scattering particles 21 multiply-scatter most of the light within the second light guiding section 3 in the same direction as the incident direction. Therefore, most of the light has the same traveling direction so that the light is radiated along the dotted lines shown in FIG. 7 . In the meantime, a part of the scattered light follows other path, being different from the dotted lines of FIG. 7 , and is emitted from the topside. Specifically, the second light guiding section 3 contains the light scattering particles 21 in a high dense state. Therefore, light from the topside surface of the translucent member 1 is radiated in a fading-bright condition, being different from light coming out of an LED, a naked light bulb, and the like. Furthermore, light emitted from the LED 30 , working almost like a point light source, is transformed into those of a surface light source by the first light guiding section 2 and the second light guiding section 3 , and therefore the quantity of light radiation per unit area becomes less.
[0081] (Advantageous Effect Achieved by the Embodiment of the Present Invention)
[0082] The translucent member 1 and the light emitting device 40 have the first light guiding section 2 equipped with the reflecting surface 12 . Therefore, while most of the light that enters the light incoming section 11 travels along the dotted lines with an arrow shown in FIG. 9 from the first light guiding section 2 toward the second light guiding section 3 as almost parallel light, the light is suitably scattered in other directions. Accordingly, the translucent member 1 and the light emitting device 40 that are suitable for surface luminescence can be provided, suppressing the appearance of glare parts and dark sections.
[0083] More specifically, it can be said that the translucent member 1 and the light emitting device 40 do not allow most of light, emitted upward linearly from the LED 30 , to pass through but totally-reflect it; and furthermore no mirror reflector intercepts light of a central area. Moreover, some of the strong light emitted from the LED 30 is so scattered as to pass through the reflecting surface 12 , and therefore the reflecting surface 12 itself works as a part of a light source. In addition, the second light guiding section 3 emits most of incident light in the same direction as the light passing through the reflecting surface 12 . Accordingly, the translucent member 1 and the light emitting device 40 are suitable for surface luminescence, and are also able to suppress any appearance of an excessively glaring part. Furthermore, being able to emit most of the incident light to the topside, the translucent member 1 and the light emitting device 40 are provided with good light efficiency.
[0084] A part of light that enters the first light guiding section 2 pass through the reflecting surface 12 to form a surface light source from the first light guiding section 2 ; and the other part of residual light, as almost parallel light, enter the second light guiding section 3 , and afterwards emit from the topside of the second light guiding section 3 so as to form a surface light source from the second light guiding section 3 . Therefore, light radiation loss of the light emitting device 40 can be restrained. Meanwhile, even if a part of light, which does not become almost-parallel light and enters the second light guiding section 3 , is radiated to the topside of the second light guiding section 3 , this light is totally reflected there and not scattered. Therefore, light radiation loss of the light emitting device 40 can further be restrained. Moreover, the light totally-reflected at the topside of the second light guiding section 3 is afterwards reflected at the prism section 22 in a direction according to design intent of the light emitting device 40 so that light radiation loss of the light emitting device 40 can still further be restrained.
[0085] Meanwhile, since a content rate of the light scattering particles 21 in the first light guiding section 2 is higher than in the second light guiding section 3 , the light that enters the first light guiding section 2 is likely to pass through the reflecting surface 12 , and accordingly a light radiation distribution of an entire part of the translucent member 1 can be almost homogenized. Since a degree of multiple scattering can be controlled by adjusting the scattering parameter “τ”, an adjustment can be made suitably so as to conform the brightness of the light passing through the reflecting surface 12 to the brightness of the light emitted from the topside of the second light guiding section 3 . FIGS. 10 to 13 show brightness distributions in the light emitting device 40 under conditions where the content rate of the light scattering particles 21 in the second light guiding section 3 is kept constant (0.06 wt. %), and meanwhile the content rate of the light scattering particles 21 in the first light guiding section 2 is changed. As a method for making the content rates of the light scattering particles 21 in the first light guiding section 2 and the second light guiding section 3 different from each other, the first light guiding section 2 and the second light guiding section 3 are formed in advance, while each having a different content rate of the light scattering particles 21 , and then afterwards the two light guiding sections are assembled together through integrating into a whole.
[0086] FIG. 10 shows a brightness distribution in the light emitting device 40 (the light emitting device 40 of a first modification) in which the first light guiding section 2 contains none of the light scattering particles 21 (Content rate=0 wt. %). According to FIG. 10 , it is understood that the second light guiding section 3 is brighter than the first light guiding section 2 . A reason why some brightness can also be observed in the first light guiding section 2 is that the LED 30 as the light source is not a point light source, and therefore the light is not necessarily totally-reflected and some of the light is allowed to pass through the reflecting surface 12 . Incidentally, each horizontal axis in FIGS. 10 to 13 represents distances from the center point 13 , where a position of the center point 13 is related to “0.” Diameters of the first light guiding section 2 and the second light guiding section 3 are 22 mm and 160 mm, respectively.
[0087] FIG. 11 shows a brightness distribution in the light emitting device 40 (the light emitting device 40 of a second modification) in which the first light guiding section 2 contains 0.03 wt. % concentration of the light scattering particles 21 , namely the concentration is a half of the content rate (0.06 wt. %) of the light scattering particles 21 in the second light guiding section 3 . It is understood that the second light guiding section 3 is a little bit brighter than the first light guiding section 2 . It is because the quantity of light passing through the light scattering particles 21 increases as a result of scattering by the light scattering particles 21 to increase the brightness of the first light guiding section 2 , and consequently the quantity of light that enters the second light guiding section 3 decreases.
[0088] FIG. 12 shows a brightness distribution in the light emitting device 40 in which the first light guiding section 2 contains 0.1 wt. % concentration of the light scattering particles 21 , namely the concentration is a slightly higher than the content rate (0.06 wt. %) of the light scattering particles 21 in the second light guiding section 3 . The brightness distribution shown is that of the light emitting device 40 according to the embodiment of the present invention. It is understood that the first light guiding section 2 and the second light guiding section 3 have roughly equalized brightness. It is because the quantity of light passing through the reflecting surface 12 further increases as a result of the light scattering particles 21 increased more in the first light guiding section 2 , and meanwhile the quantity of light that enters the second light guiding section 3 decreases further.
[0089] FIG. 13 shows a brightness distribution in the light emitting device 40 (the light emitting device 40 of a third modification) in which the first light guiding section 2 contains 0.3 wt. % concentration of the light scattering particles 21 , namely the concentration is 5 times higher than the content rate (0.06 wt. %) of the light scattering particles 21 in the second light guiding section 3 . It is understood that the first light guiding section 2 is brighter than the second light guiding section 3 .
[0090] FIG. 14 shows a relationship between a light divergence angle and a light transmission factor as a density of the light scattering particles 21 varies; wherein a PMMA plate with a thickness of 10 mm contains the light scattering particles 21 with a particle diameter of 7.3 μm. In this situation, the light divergence angle is an angle spread in a 360-degree indication at which scattered and spread light has a half of the brightness at the center. As shown in FIG. 14 , when the content rate of the light scattering particles 21 is 0.06 wt. %, almost no divergence happens and the light transmission factor is around 98%. By making use of FIG. 14 , the brightness of the translucent member 1 and the launching direction of light ray can be set in various ways.
[0091] Where a scattering parameter is expressed as “τ” (“1/τ” is a mean free path, to be expressed in “cm”), and a thickness of the first light guiding section 2 is expressed as “T” (expressed in “cm”), the product of “τ” and “T” with respect to the light scattering particles 21 is within a range of 0.1 to 50. If the product of “τ” and “T” is 0.1 or less, the mean free path of light rays becomes long and the amount of light rays scattered within a distance of the thickness “T” becomes less so that an adequate amount of light rays cannot be emitted externally from the reflecting surface 12 of the first light guiding section 2 . Meanwhile, if the product of “τ” and “T” is 50 or greater, the mean free path of light rays becomes short and the amount of light rays multiply-scattered within the distance of the thickness “T” becomes great so that the backscatter becomes great and a frontward light transmission factor decreases, as shown in FIG. 14 . In other words, the light efficiency of light rays, which enter the light incoming section 11 and travel along the dotted lines with an arrow shown in FIG. 9 from the first light guiding section 2 toward the second light guiding section 3 , becomes less.
[0092] In the prism section 22 , the protrusion angle θ of a saw tooth 23 positioned closer to the center point 13 is smaller than that of a saw tooth 23 positioned further from the center point 13 . Therefore, at a position further from the center point 13 , light can be radiated in a direction for traveling further away from the LED 30 so that light can be radiated in a wide-angle spread. As a result, the light emitting device 40 becomes appropriate for an application of lighting equipment that can illuminate a wide extent. Furthermore, owing to radiation in a wide-angle spread, the light emitting device 40 can be made to be thin. Moreover, when the light emitting device 40 is modularized so as to be placed in a multiple arrangement, the number of modules can be reduced because of radiation in a wide-angle spread, and consequently it can lead to cost reduction.
[0093] As shown in FIGS. 10 , 11 , 12 , and 13 , even a position being distant from the translucent member 1 is illuminated, and therefore it is obvious that the light emitting device 40 can radiate in a wide-angle spread.
[0094] Since the protrusion angle θ can be modified arbitrarily, the way of illumination can be changed in accordance with an application of the light emitting device 40 . The way of illumination can be made for radiating in a wide-angle spread, as described above, and contrarily it is also possible to radiate in a narrow-angle spread as a downlight does. In the case where the crossing angle β formed by the line “L” connecting protrusion peaks of the saw teeth 23 in a radial direction and the topside surface of the second light guiding section 3 is within a range of 2 to 10 degrees, preferably the protrusion angle θ should be set in a range of 45 to 75 degrees.
[0095] Furthermore, at the lower side of the edge 15 , in the second light guiding section 3 , being distant from the LED 30 , there is formed the reflecting part 16 for reflecting guided light toward the topside. Therefore, even if there remain any light, which the prism section 22 alone cannot change traveling directions of, it is still possible to change the traveling direction of such light toward the topside.
[0096] (Other Modifications)
[0097] Besides the above explanation with regard to the translucent member 1 and the light emitting device 40 according to the embodiment of the present invention, various other modifications may be made without changing the concept of the present invention.
[0098] The optical element (the translucent member 1 ) according to the embodiment of the present invention includes: the light incoming section 11 through which light enters; the first light guiding section 2 for guiding the light incident on the light incoming section 11 ; the reflecting surface 12 , placed to be opposite to a light beam entry side of the first light guiding section 2 , for totally-reflecting a linearly-traveling part of the incident light; and the second light guiding section 3 for guiding the reflected light; wherein the first light guiding section 2 contains the light scattering particles 21 for multiply-scattering light and generating light which passes through the reflecting surface 12 and is emitted externally; and the second light guiding section 3 launches at least a part of the incident light in a direction of the same surface side as the light passing through the reflecting surface 12 travel out. Alternatively, the second light guiding section 3 may also contain the light scattering particles 21 . Furthermore, the light incoming section 11 includes the bottom side of the first light guiding section 2 and the LED holder 17 , and the bottom side of the first light guiding section 2 may include an entire section or a part of the bottom side. Moreover, the light, which the second light guiding section 3 launches, goes out in the direction of the same surface side as the light beams passing through the reflecting surface 12 travel out; and in this situation, a part of the light or the entire light may be launched from the bottom side of the second light guiding section 3 , or launched to an outer circumference side of the edge 15 .
[0099] The optical element (the translucent member 1 ) according to the embodiment of the present invention has the prism section 22 at a position, opposite to a side of the reflecting surface 12 , in the second light guiding section 3 , the prism section 22 having its sawtooth-like section for changing traveling directions of the guided light in the direction of the same side as the reflecting surface 12 . Alternatively, the prism section 22 may be omitted since it is not an essential element. Furthermore, the prism section 22 may be placed at an upper side of the second light guiding section 3 . Alternatively moreover, not having its sawtooth-like section, the prism section 22 may be formed as a straight line as the line “L” is, or as a curved line. Still further, though the saw teeth 23 include 6 divided groups, the grouping is not necessary. For example, the greater gradually the protrusion angle θ of each saw tooth 23 may be made while every saw tooth having a different protrusion angle θ, the further from the center point 13 toward the edge 15 the saw tooth 23 is located.
[0100] Preferably, the optical element (the translucent member 1 ) according to the embodiment of the present invention should include the reflecting part 16 for reflecting the guided light toward the same side as the reflecting surface 12 , at the edge 15 positioned within the second light guiding section 3 , being distant from the first light guiding section 2 . Alternatively, the reflecting part 16 may be omitted since it is not an essential element. Furthermore alternatively, the prism section 22 may be extended up to the edge 15 .
[0101] The optical element (the translucent member 1 ) according to the embodiment of the present invention contains the light scattering particles 21 in the second light guiding section 3 , and the content rate of the light scattering particles 21 in the first light guiding section 2 is higher than that in the second light guiding section 3 . Alternatively, the content rate of the light scattering particles 21 in the first light guiding section 2 may be lower than that in the second light guiding section 3 , or the content rate in both the sections may be the same. Furthermore, the second light guiding section 3 may not contain the light scattering particles 21 .
[0102] With regard to the light scattering particles 21 in the optical element (the translucent member 1 ) according to the embodiment of the present invention; wherein a scattering parameter and a thickness of the first light guiding section 2 are expressed as “τ” and “T”, respectively, the product of “τ” and “T” with respect to the light scattering particles 21 is within a range of 0.1 to 50. Alternatively, the product of “τ” and “T” may be outside the range, being such as 0.01, 0.05, 60, 70, 80 and the like.
[0103] The light emitting device 40 according to the embodiment of the present invention includes: the translucent member 1 and the light emitting component (the LED 30 ); the translucent member 1 having: the light incoming section 11 through which light enters; the first light guiding section 2 for guiding the incident light on the light incoming section 11 ; the reflecting surface 12 , placed to be opposite to a light beam entry side of the first light guiding section 2 , for totally-reflecting a linearly-traveling part of the incident light; and the second light guiding section 3 for guiding the reflected light; and the light emitting component (the LED 30 ) emitting light into the light incoming section 11 ; wherein the first light guiding section 2 contains the light scattering particles 21 for multiply-scattering light and generating light which passes through the reflecting surface 12 and is emitted externally; and the second light guiding section 3 launches at least a part of the incident light in a direction of the same surface side as the light passing through the reflecting surface 12 travel out. Alternatively, the second light guiding section 3 may also contain the light scattering particles 21 . Furthermore, as the light emitting component, one of a light guiding member for guiding light from a light source and a light reflecting member for reflecting light from a light source may be used instead of a light source for emitting light directly into the light incoming section 11 .
[0104] In the light emitting device 40 according to the embodiment of the present invention, the second light guiding section 3 is formed to be plate-like; and placed at a center of the plate-like second light guiding section 3 is the first light guiding section 2 that is circular in its plane. Alternatively, the second light guiding section 3 may have its contour of a polygonal shape, such as a triangular contour, a quadrilateral contour, etc.; and furthermore it may also have an oval-figured contour as well. By the same token, the first light guiding section 2 may also have its contour in its plane, such as any polygonal contour, an oval-figured contour, and the like.
[0105] In the light emitting device 40 according to the embodiment of the present invention, the translucent member 1 is made of a translucent resin material, and the light scattering particles 21 are translucent silicon particles having their particle diameter within a range from 1 to 10 μm; wherein the light scattering particles 21 are also included in the second light guiding section. Alternatively, any other kinds of light scattering particles may be used as the light scattering particles 21 , regardless of their material, shape, particle diameter, and the like, as long as they multiple-scatter light in the translucent member 1 . In this regard, the light scattering particles 21 should preferably be translucent silicon particles with their diameter in a range from 1 to 10 μm, from the viewpoint that, while traveling along the optical paths shown in FIG. 9 (the dotted lines with an arrow), the light should suitably be scattered in other directions. To describe more in detail, using silicon particles with their diameter of 1 μm or greater makes it possible to suppress the spread of the angular distribution, and lessen an element of the backscatter. Then, it becomes possible to prevent the frontward light intensity from being lessened, and to prevent the quantity of light guided into the second light guiding section 3 from decreasing excessively, so that it becomes easy to restrain the quantity of light passing through the reflecting surface 12 of the first light guiding section 2 from becoming excessively great. In the meantime, using silicon particles with their diameter of 10 μm or smaller makes it possible to refrain the angular distribution from becoming excessively narrow, so that it becomes possible to obtain the enough quantity of light passing through the reflecting surface 12 of the first light guiding section 2 .
[0106] Used as the translucent member 1 is a component made of PMMA. Alternatively, for the member, it is also possible to use any other translucent resin material such as acrylic resin material, polystyrene, polycarbonate, and the like that are other kinds of polymer materials of acrylic acid ester, or methacrylate ester, and are amorphous synthetic resin materials having high transparency, as well as glass material and so on. Though the first light guiding section 2 and the second light guiding section 3 are assembled together through integrating later into a whole, alternatively the translucent member 1 may be obtained by forming a wholly-integrated single component including the first light guiding section 2 and the second light guiding section 3 from the very beginning.
[0107] Though the light incoming section 11 is a part of the first light guiding section 2 , and flat-surfaced; alternatively the light incoming section 11 may be formed to be convex, curved, aspheric, etc. When the light incoming section 11 is formed to be spherical or aspheric, the curvature may be modified arbitrarily. Furthermore, the light incoming section 11 may be also prepared separately from the first light guiding section 2 .
[0108] The light emitting component is not limited to the LED 30 , and alternatively other light emitting elements such as organic electro-luminescence (OEL), inorganic electro-luminescence (IEL), laser luminescence, and the like may be used. Furthermore, a chip-shaped component is used as the LED 30 , and alternatively an LED component equipped with a lens may be used.
[0109] Having its circular contour, the translucent member 1 includes; the reflecting surface 12 which is circular- and concave-shaped, and located at the center of the translucent member 1 ; and the second light guiding section 3 for guiding light, which is circular-shaped, and located around the reflecting surface 12 . Alternatively, the contour of the translucent member 1 , the shape of the reflecting surface 12 in its plane, the shape of the second light guiding section 3 , and the like may be modified. For example, when the second light guiding section 3 has its quadrilateral contour as described above, the translucent member 1 can also have its quadrilateral contour. Thus, an advantage of the translucent member 1 having its quadrilateral contour is that the translucent member 1 enables placement of light-emitting faces of a plurality of light emitting devices 40 with no gap among them. In the case of placement of the light-emitting faces in this way for their use, it becomes easy for the light-emitting faces to emit light uniformly.
[0110] The reflecting surface 12 of the translucent member 1 has a curved surface in such a way that a differentiation result of a function corresponding to its profile curve is given as a formula of “tan(90−θt/2)”, as shown in FIG. 9 . Alternatively, the profile curve may be structured with another curve according to any other conditions as far as the curve enables totally-reflection of light from the LED 30 deemed as a point light source. Furthermore, being different from a structure with a profile curve such as an aspheric surface curve, the reflecting surface 12 may have another kind of section with an angular shape, namely a series of straight lines connected. Namely in this case, light reflected by the angular-shaped section may not need to form light paths being almost parallel in the second light guiding section 3 .
[0111] The second light guiding section 3 of the translucent member 1 includes the prism section 22 composed of 225 saw teeth 23 which are placed on concentric circles centered at the center point 13 , and formed on the bottom surface in FIG. 7 . Then, in the saw teeth 23 , a protrusion angle θ of a position closer to the center point 13 is smaller than that of a position further from the center point 13 . Alternatively, a location and a shape of the prism section 22 , the number of saw teeth, and a protrusion angle θ of each saw tooth may be modified. For example, while the saw teeth 23 being placed on concentric circles centered at the position of the LED 30 , the translucent member 1 may have a quadrilateral contour through cutting out the edge 15 of the second light guiding section 3 .
[0112] Though the prism section 22 is formed through placement of the saw teeth 23 on the concentric circles centered at the center point 13 , alternatively the saw teeth 23 may be placed on a straight line. For example, when a contour of the translucent member 1 is quadrilateral, the saw teeth 23 may be formed along straight lines of the quadrilateral contour. Furthermore, the reflecting part 16 is placed for totally-reflecting the guided light, and the part may be prepared through printing treatment by using white ink, or may be so made as to have a mirror-like surface through mirror-coating, etc., by using aluminum, silver, and the like. It is preferable that the reflecting part 16 is so structured as to totally-reflect the guided light since structuring in this way eliminates any further preparation, such as printing treatment and so on in the manufacturing step.
[0113] Though, in the present embodiment, the distance “H” between neighboring two saw teeth 23 is 0.2 mm, alternatively the distance “H” may be modified so as to be set with, e.g., 0.1 mm, 0.3 mm, and so on. Furthermore, it is also possible to set the distance “H” with varying distance values. Namely, there may exist some different distance values in the translucent member 1 .
[0114] The saw teeth 23 are placed on the concentric circles, and one end of the prism section 22 is a part of the prism section 22 at a side closer to the center of the concentric circles, while another end of the prism section 22 is a part of the prism section 22 at a side further from the concentric circles. Alternatively, a location and a shape of the prism section 22 may be changed. For example, the prism section 22 may be formed to have polygonal shapes, such as quadrilateral forms and the like, as saw teeth 23 a of a translucent member 1 a of a first modification of the translucent member 1 shown in FIG. 15 , being different from concentric circles; the quadrilateral forms having one center common to them.
[0115] FIGS. 16 and 17 are drawings to show an example of using a light emitting device 40 applying the translucent member 1 a shown in FIG. 15 , as a street lamp. One end of a support post 50 is connected to a light emitting side of the light emitting device 40 , meanwhile the other end of the support post 50 is buried into the ground, and the light emitting device 40 illuminates an area W 1 to be illuminated on the ground from an elevated position. In the area W 1 to be illuminated, light from the light emitting device 40 is spread radially and uniformly along a road 51 .
[0116] An area W 2 to be illuminated by the light emitting device 40 in a widthwise direction of the road 51 extends radially in such a way as to cover an entire area of a width Y of the road 51 . The way of extending is to cover a wide area at a side of the road 51 and a narrow area at an outside of the road 51 , as shown in FIG. 17 . This way of illumination is achieved by changing protrusion angles θ of the saw teeth 23 a placed in the translucent member 1 a shown in FIG. 15 according to their positions. In other words, a protrusion angle θ of saw teeth 23 a 1 positioned at an upper side in FIG. 15 is set to be smaller than that of saw teeth 23 a 2 positioned at a lower side. When protrusion angles are set in this way, an area to be illuminated can be controlled arbitrarily, such as making an area to be illuminated wider at the side of the road, for example, in the case of installing a street lamp applying the light emitting device 40 at a boundary between a road and a forest.
[0117] Sometimes it may be preferable that the support post 50 is so connected as to cover a section corresponding to the first light guiding section 2 in the light emitting side of the light emitting device 40 . For example, when the light emitting device 40 has a relatively non-uniform brightness distribution as shown in FIG. 10 and FIG. 11 , a relatively dark area corresponding to the first light guiding section 2 is covered by the support post 50 so as to enable uniforming the illuminating condition. Furthermore, as a translucent member for illuminating a right-side area and a left-side area equally in a certain direction while illuminating a right-side area and a left-side area unequally in a direction perpendicular to the above-mentioned direction as shown in FIG. 16 and FIG. 17 , even the translucent member 1 with a circular form as shown in FIG. 1 may be applied, being different from the translucent member 1 a with a quadrilateral form as shown in FIG. 15 .
[0118] Shown in FIG. 18 as a second modification of the translucent member 1 is a bottom plan view of a translucent member 1 b prepared by placing the saw teeth 23 positioned on concentric circles centered at a location of the LED 30 , and cutting out the edge 15 of the second light guiding section 3 , in order to make a contour of the translucent member 1 quadrilateral (square). Each component having the same shape and the same function as its corresponding one existing in the translucent member 1 is provided with the same reference numeral that the corresponding one has in FIG. 3 , and an explanation on the component is omitted. A square contour section of the translucent member 1 b has an edge 15 a constituting each side part and an edge 15 b constituting each corner point. Each reflecting part 16 b corresponding to the reflecting part 16 of the translucent member 1 includes 4 oval-lined part, each of which is formed by swelling toward the center point 13 in a direction connecting neighboring reflecting parts 16 along each edge 15 a.
[0119] FIG. 19 is a side elevation view of the translucent member 1 b shown in FIG. 18 , taken from a direction of a large arrow “B” in the drawing. FIG. 20 is a side elevation view of the translucent member 1 b shown in FIG. 18 , taken from a direction of a large arrow “C” in the drawing. Also with respect to FIG. 19 and FIG. 20 , each component having the same shape and the same function as its corresponding one existing in the translucent member 1 is provided with the same reference numeral that the corresponding one has in FIG. 3 , and an explanation on the component is omitted. An angle formed by a surface of the reflecting part 16 b and the top surface of the second light guiding section 3 is 30 degrees, as the angle θ is. As shown in FIG. 20 , no reflecting part 16 b exists at a position of edge 15 b.
[0120] FIG. 21 is a schematic cross-sectional view of a sign 60 including 3 light emitting devices 42 , each of which is a second modification of the light emitting device 40 using the translucent member 1 b , as light sources. On a front surface 61 b of the sign 60 , there are illustrated some characters and images, or there is placed a poster and the like. Each of the light emitting devices 42 can illuminate a wide area, and practically illuminates an area W 3 . In other words, as shown in FIG. 21 , the light emitting devices 42 illuminate in such a way that an area to be illuminated by one of the light emitting devices 42 overlaps a part of that (an edge part) of a neighboring one of the light emitting devices 42 . Therefore, the sign 60 is observed as if an entire area of the sign 60 emits light in its illuminating direction. This illumination status can be achieved even when each of the light emitting devices 42 is placed, while having a clearance W 4 from its neighboring light emitting device, in the sign 60 . Accordingly, in the case of the sign 60 , the number of light sources can be reduced dramatically, being compared with another case where conventionally a number of LEDs are placed and used as light sources for a sign. As a result, the sign 60 exerts its effects of reduction in power consumption, reduction in the number of constituent components, and so on.
[0121] FIG. 21 shows a case where 3 light emitting devices 42 are placed in a vertical direction. Alternatively, 3 lines of light emitting devices in both vertical and horizontal directions so as to have 9 light emitting devices 42 in total may be placed for making up a sign 60 having a square surface 61 , and furthermore 3 lines by 5 lines of 15 light emitting devices 42 in total may be placed for making up another rectangular sign 60 . Any number of devices in vertical and horizontal directions may be adopted arbitrarily.
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Provided is an optical element which suppresses generation of glare and a dark section and is applicable to planar light emission having improved light efficiency. A light emitting device is also provided. A light emitting device is provided with: a light transmitting member having a light inputting section having light inputted thereto, a first light guide section which guides light inputted to the inputting section to a reflecting surface, the reflecting surface which is arranged on the first light guide section on the side opposite to the light inputting side and totally reflects light which forms one linear path among inputted light, and a second light guide section which guides reflected light; and a light emitting member which inputs light to the inputting section. The first light guide section contains light scattering particles, which multiply scatter light and generate light that passes through the reflecting surface and is outputted to the external, and the second light guide section partially or entirely outputs inputted light to the same surface to which light passed through the reflecting surface is outputted.
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TECHNICAL FIELD
The technical field of this invention is an occupant weight detection system for a vehicle seat with a foam seat cushion.
BACKGROUND OF THE INVENTION
Vehicle occupant restraint device controls are now being designed to distinguish seat occupants by weight and use this information in determining, in the case of a crash, whether or not to deploy a restraint and, if so, with what force. One type of vehicle seat occupant weight detecting system uses a force or pressure sensor under a foam seat cushion on which an occupant sits; and a particular type of force or pressure sensing apparatus is a non-compressible fluid filled bladder comprising an array of cells in fluid communication with each other and a pressure sensor connected to the interior of the bladder to measure the fluid pressure therein.
Systems of this type have had to be refined to accurately distinguish between two or more classes of vehicle occupants defined in certain governmental regulations; and this refinement involves, among other things, compensation for certain mechanical and/or environmental effects inherent in the apparatus that tend to distort the output pressure signal from that indicating the true weight of the occupant. It has been discovered that one of these effects is relative humidity within the foam material of the seat cushion, which affects the force/pressure transmitting properties of the foam and thus the relationship between the weight of a seat occupant and the pressure exerted on pressure sensing apparatus under the seat cushion. Although the prior art includes references to correcting the output of occupant weight sensors for humidity of the air, such references deal with systems having sensors, such as open capacitive sensors or ultrasound reflective sensors, in which the sensor itself is sensitive to humidity. It has not been known in the prior art that it would be necessary or advantageous to correct for humidity in the seat foam when the sensor was itself not significantly affected by humidity.
Testing has shown that there can be a significant time delay between a change in relative humidity of the air adjacent the foam and a change in the humidity level within the foam. The foam material includes a large number of very small air pockets, only a small proportion of which are close to the outer surface of the foam cushion. In addition, the seat foam is usually covered with a material that further impedes air flow in and out of the foam. Exchanges in air flow between the seat foam and the atmosphere are propelled by “foam activity”: that is, compression of the foam to expel a portion of the air within, followed by release of the compression to allow the foam to expand and pull in external air. In the absence of “foam activity” it can take a very tong, time for the average humidity within the foam to adjust to that outside the foam; but in the presence of such activity, the response can be significantly faster.
Furthermore, some foam seat cushions tend to exhibit a cross-correlation effect between relative humidity and temperature, most probably due to the facts that (1) the humidity effect on a foam seat cushion appears to vary with the absolute amount of water in the foam and (2) the relationship between the measured relative humidity and the absolute humidity in air can vary in a strongly non-linear manner with changes in temperature. In some cases, the cross-correlation effect can be as great as the effect of humidity alone.
SUMMARY OF THE INVENTION
The invention described and claimed herein provides a humidity compensated vehicle seat occupant classification system with pressure responsive apparatus adapted for engagement with an underside of a foam seat cushion so as to respond to a weight of an occupant on an upper side of the foam seat cushion and generate a pressure signal therefrom. In the system, a humidity sensor is adapted to respond to relative humidity of air adjacent the pressure responsive apparatus to generate a humidity signal. The humidity signal is used to compensate at least one of the following: the pressure signal, a stored reference pressure value and/or a stored threshold value. The occupant classification is determined at least partly in response to the compensated one of the pressure signal, the stored reference pressure value and the stored threshold value. In a preferred embodiment, a stored reference pressure value representing an empty seat pressure is compensated; and in another preferred embodiment, the stored threshold value is also compensated.
Preferably, the system includes a time delay between the reading of a humidity value and the full use of that humidity value in compensation, and the time delay is preferably variable according to an activity factor of the foam seat cushion derived from dynamic variations in the pressure signal associated with a pumping action on the foam tending to increase the rate of exchange of air between the foam and the atmosphere outside the foam. In a preferred embodiment, the activity factor is derived by counting consecutive, alternating excursions of signal magnitude above a first predetermined level and below a second predetermined level lower than the first predetermined level.
Preferably, the temperature adjacent the foam seat cushion or the pressure sensor is further used with the humidity signal to generate a cross-correlation value for further compensating whichever of the pressure signal, the stored reference pressure value and the stored threshold value is humidity compensated. This cross-correlation value may be derived from a product of tile humidity and temperature signals and may further be derived from a product of the humidity signal and the square of the temperature signal.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a block diagram of an occupant weight detection system for a vehicle seat with a foam seat cushion providing compensation for humidity within the seat cushion foam.
FIG. 2 shows a seat with pressure sensing apparatus under the seat cushion.
FIGS. 3A, 3 B and 4 show a computer flow chart for a humidity compensation algorithm for use in the system of FIGS. 1 and 2.
FIG. 5 is a circuit diagram of a humidity sensor for use in the system of FIGS. 1 and 2.
FIG. 6 is a graph showing a typical functional relationship between occupant weight and pressure sensor output voltage in the system of FIGS. 1 and 2.
FIG. 7 is a computer flow chart of an occupant classification algorithm for use in the system of FIGS. 1 and 2.
FIG. 8 is an alternate embodiment of a humidity compensation algorithm for use in the system of FIGS. 1 and 2 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
A vehicle passive restraint control system comprises an airbag control module (ACM) 10 that receives signals from crash sensors, not shown, and provides deploy signals as required to airbags, not shown. The crash sensors and airbags may be any such articles known in the art for use in vehicle restraint systems. A vehicle seat 14 is provided with a seat cushion member 16 , generally comprising a shaped block of foamed material providing a comfortable seating support, usually covered in a fabric for protection, desired surface qualities and appearance. A bladder 18 packaged with seat cushion member 16 is typically located under seat cushion member 16 but above a seat pan member 19 , as shown in FIG. 2, and is filled with a non-compressible fluid so as to generate a pressure in the fluid in response to the weight of a seat occupant on the seat cushion member. The pressure in the fluid is sensed by a pressure sensor 20 in a sensor module 24 that, together with bladder 18 , forms a seat characteristic sensor apparatus providing an output signal of the weight born by seat cushion member 16 . An example of pressure sensing apparatus such as bladder 18 and pressure sensor 20 is shown in U.S. Pat. No. 5,987,370, issued Nov. 16, 1999. A relative humidity sensor 22 , which produces an output humidity signal, is also provided, preferably and conveniently along with pressure sensor 20 within sensor module 24 . The output signals of both pressure sensor 20 and humidity sensor 22 are provided to an occupant detection system module 12 , which includes a controller such as a programmed digital microcomputer, not shown. Occupant detection system module 12 may also receive signals from other sensors such as a seat belt tension sensor 26 or a seat belt latch sensor 28 , and it communicates with airbag module 10 over a bus 11 . A temperature sensor 29 may provide a temperature signal to module 12 ; and a preferred location for sensor 29 is in the sensor module 24 , although it is not so shown in FIG. 1, due to lack of space.
FIGS. 3A and 3B show a computer flow chart illustrating the operation, relative to the invention, of a microcomputer in occupant detection system module 12 in a routine HUMIDITY COMPENSATION. The microcomputer, in a low power sleep mode, looks for a time-based wakeup signal at step 40 and repeats the step until the wakeup signal is received. As the computer wakes up to full operation, it receives a sample pressure reading from pressure sensor 20 at step 42 and updates an activity factor at step 44 . The activity factor is a measure of the rate at which the foam in seat cushion 16 is compressed and released, and thus of the rate at which the air within seat cushion 16 is replaced by atmospheric air. Most air pockets within the foam are comparatively distant from the external surface, through tortuous paths so that the exchange rate of air with the external atmosphere is very slow in the absence of an occupant sitting on the seat and generating a pumping action thereon by movements, whether active or passive (due to road bumps, etc.). The process described herein monitors changes in pressure in the bladder under seat cushion 16 to determine the activity thereof and determines a count indicative of the activity rate as described with reference to the subroutine CALC ACTIVITY FACTOR of FIG. 4 .
The basic operation of the CALC ACTIVITY FACTOR subroutine is to monitor the pressure signal and determine excursions between predetermined low and high values, incrementing a count with each complete excursion. Thus, after the pressure level falls below the predetermined low value, a count is incremented when it next exceeds the predetermined high level; and after this excursion higher than the high level, the count is incremented an when the level once again falls below the low level. Thus, the more seat activity that causes the bladder pressure to swing up to the high level and down to the low level, the higher will be the activity factor. A higher value of the activity factor indicates a more rapid replacement of air within the foam and thus a smaller time delay between the sensing of a humidity value outside the foam by humidity sensor 22 and the achievement of the same humidity value within seat cushion 16 ; a low value indicates the opposite.
Referring to FIG. 4, the subroutine begins at step 70 by determining if the pressure value is greater than or equal to a predetermined reference value HIREF. If it is, the subroutine then checks a direction flag at step 72 to determine whether the relevant direction is up or down: that is, whether the subroutine was looking for the high reference value HIREF (direction=up) or a predetermined low reference value LOREF (direction=down). The two predetermined reference values determine the pressure range defining an activity count, and the direction flag prevents the count from being incremented before full travel between the reference values has occurred. If the direction flag indicates down, program flow returns to the main program. But if the direction flag indicates up, the subroutine increments ACTIVITY COUNT at step 74 and sets the direction flag at step 76 to indicate DOWN before returning to the main program.
From step 70 , if the pressure is not greater than or equal to HIREF, the subroutine determines at step 78 if it is less than or equal to the predetermined reference value LOREF, which is lower in value than HIREF. If it is not, program flow returns to the main program. If it is less than or equal to LOREF, the subroutine determines at step 80 if the direction flag indicates DOWN: that is, if it is looking for the LOREF value. If the answer is no, program flow returns to the main routine; but if the answer is yes, the subroutine increments ACTIVITY COUNT at step 82 and sets the direction flag to indicate UP before program flow is returned to the main routine. The value of ACTIVITY COUNT is available at any time in memory to be used as the activity factor by the main routine in compensation calculations.
In a variation of the routine described above, an extra step or subroutine is inserted at the beginning, prior to step 70 . This extra step updates an average value of the pressure signal and determines or modifies the values of HIREF and LOREF to bracket the updated average value. Thus, when the seat has an occupant for a continuous period of time who provides small magnitude vertical force inputs to the seat foam due to road inputs through the suspension or clue to shifting position in the seat, the pressure values will be optimally aligned to cross both of references HIREF and LOREF. When the average value drops toward zero after the occupant leaves the seat, the values of HIREF and LOREF may revert to predetermined values greater than zero.
Returning to the main routine in FIG. 3A, the routine determines at step 46 if it is time to sample the humidity sensor. This is done at specified time intervals which are typically significantly greater than the intervals between pressure readings since humidity changes significantly affecting the foam in seat cushion 16 do not generally occur very quickly. A typical time interval might be 15 minutes. The choice of the time interval is a choice in a specific case: more frequent sampling might provide faster response to humidity changes under some conditions; but it might also generally produces a greater accumulated round-off error and will generally increase current draw from the vehicle battery and thus increase chances of draining the battery when the vehicle is not used for a long period. If Such a time interval has not passed since the last humidity reading, the routine exits. If it has passed, the humidity sensor signal is sampled at step 48 and the value of the reading is added to a temporarily stored value HUMIDITY SUM.
The routine then determines at step 52 if it is time to calculate an average humidity value HUMIDITY AVG. In this embodiment the average is calculated every hour: that is, after every four consecutive samples (at 15 minute intervals) of the humidity sensor. If it is not time to calculate the average value, the routine is exited; but if the time has come, the routine determines and stores the average value at step 54 (FIG. 3 B). The average value is calculated by dividing the value of HUMIDITY SUM, which is the temporarily stored sum of the last four consecutively sampled values of the humidity sensor output signal, by the number four (or whatever other number of samples have been summed). The resulting value of HUMIDITY AVG is stored in memory as the latest in an ordered array of previously calculated average humidity values. The temporarily stored value of HUMIDITY SUM is then cleared to zero at step 56 . In addition, the routine next, at step 58 , determines the ACTIVITY FACTOR for the previous hour by storing the value of ACTIVITY COUNT accumulated over the hour and then clearing, the ACTIVITY COUNT to zero.
The routine next begins the calculation of the compensation gains, which is done every hour, but using data going back over a 48 hour period. First, at step 60 , the routine determines average humidity values and activity factors for each of 6 consecutive, previous eight hour periods. The average humidity value for the previous eight hour period is calculated as follows:
T 0 to − 7=(Σ T 0 H+T −1 H+ . . . +T −7 H )/8
Wherein the summed terms are the values of HUMIDITY AVG for each of the previous eight hours. Similar average values are calculated for each of the eight hour periods T −8 to −15 , T −16 to −23 , T −24 to −31 , T −32 to −39 and T −10 to −47 . The total activity factor for each of the eight periods is also determined as the sum of the stored activity factors for all one hour periods within the eight hour period.
With average humidity values and total activity factors for each of the six eight hour periods calculated, the routine can now determine the compensation gains at step 60 using a weighting factor for each eight hour period. An empty seat humidity compensation gain EHG is calculated as follows:
EHG=T 0 to −7 *A 0 to −7 *KEHG 1 + T −8 to −15 *A −8 to −15 *KEHG 2 + . . . + T −40 to −47 *A −40 to −7 *KEHG 8
wherein KEHG 1 , KEHG 2 , . . . KEHG 8 are predetermined weighting factors, which are preferably greater, generally, for more recent samples. Likewise, a threshold humidity compensation gain THG is calculated as follows:
THG=T 0 to −7 *A 0 to −7 *KTHG 1 + T −8 to −15 *A −8 to −15 *KTHG 2 + . . . + T −40 to −47 *A −40 to −7 *KTHG 8
wherein KTHG 1 , KTHG 2 , . . . KTHG 8 are predetermined weighting factors, which are preferably greater, generally, for more recent samples.
The two humidity compensation factors EHG and THG are the outputs of routine HUMIDITY COMPENSATION and are used to modify values in an occupant status determination algorithm, the basic portion of which is shown in FIG. 7 . Routine DETERMINE OCCUPANT STATUS begins at step 90 by calculating an empty seat pressure value compensated for humidity as follows:
Comp Empty Seat Pressure=Calibrated Empty Seat Pressure* EHG,
wherein the Calibrated Empty Seat Pressure is a stored calibration value that was determined by reading the pressure sensor output in an installed occupant weight determination system under controlled environmental conditions (temperature, humidity), typically at the point of seat or vehicle assembly.
Next, at step 92 , the routine determines a threshold reference value compensated for humidity as follows:
Comp Threshold=Stored Threshold* THG,
wherein the Stored Threshold is based on predetermined criteria defining the conditions under which the relevant airbag or similar restraint is to be deployed or not deployed in a detected vehicle crash event and is preferably determined by a test which may involve the dropping of an object having predetermined weight and shale onto a scat cushion in a predetermined manner and recording the pressure sensor reading, again under controlled environmental (temperature, humidity) conditions. Stored threshold values may be based on predetermined data such as that shown in FIG. 6 relating the pressure sensor output signal to the weight of a seat occupant and stored in a table for lookup on the basis of the pressure sensor output signal, filtered and/or processed as desired.
The Relative Pressure is then determined at step 94 as follows:
Relative Pressure=Pressure Sensor Output−Comp Empty Seat Pressure,
wherein Pressure Sensor Output is the current output signal of the bladder pressure sensor, filtered as desired.
Finally, the Relative Pressure value is compared at step 96 to the compensated threshold value Comp Threshold. A first occupant status is declared at step 98 if Relative Pressure is greater than Comp Threshold; otherwise a second occupant status is declared at step 99 . The first occupant status may be, for example, that an occupant is present in the seat; and the second occupant status may be, for example, that there is no occupant in the seat. The first occupant status would call for deployment of an airbag in a sensed crashed event, while the second occupant status would suppress deployment. Another example would identify the first occupant status with the presence of a heavy occupant such as an adult male, whereas the second occupant status would signify a light occupant such as a child or a fifth percentile female. In this case, the first occupant status would still provide for deployment of the airbag; but the second occupant status would either suppress deployment or deploy at a lower level. In any case, the accuracy of the weight calculation, and therefore of the occupant classification and deployment decision, would be improved by the compensation of the bladder pressure sensor output signal for moisture in the seat foam by means of humidity detection.
An example humidity sensor is described with reference to FIG. 5 . The sensing element includes a commercially available capacitor chip C S that is designed to be highly responsive to relative humidity of the air around it and is mounted exposed to that air. It is electrically connected in an oscillator circuit built around a standard 555 timer chip 30 . A PIC12C671 microprocessor chip 32 is programmed to repeatedly activate the oscillator for short periods by providing power to the 555 timer chip through diode CR 1 and to receive a voltage signal from pin 3 (Vout) of the timer chip that oscillates at a variable frequency controlled by capacitor C S . Microprocessor chip 32 measures the frequency (with reference to its own internal clock) and determines the relative humidity through a stored mathematical model or look-up table and stores the values thereof. When module 12 signals microprocessor chip 32 , the latter communicates selected stored values of the relative humidity to module 12 . But there is nothing about this circuit that is critical to the operation of the invention; and it could be easily replaced by many other relative humidity measuring circuits known in the art. The pin connections for the 555 timer chip are +Power ( 4 , 8 ), Time C ( 2 , 6 ), GND ( 1 ) and Vout ( 3 ). The pin connections for the microprocessor chip 32 are +Power ( 1 ), GND ( 8 ) at all times, data in/out ( 2 - 7 ) in data communication mode and power Out to oscillator ( 6 ) and oscillator voltage signal in ( 5 ) in oscillator activation mode (with pins 2 - 5 available for signalling from module 12 ).
Some seats employing foam seat cushions appear to exhibit a cross-correlation between humidity and temperature, due at least partly to the fact that the effect of moisture in the load transmission of a seat cushion foam varies with the absolute amount of water in the air trapped within the foam but the humidity parameter that is actually measured is relative humidity. The absolute volume of water in a given volume of air at a given value of relative humidity varies substantially with the temperature of the air; and this contributes significantly to the cross-correlation. For a seat wherein this humidity/temperature cross-correlation is sufficiently large, it may be compensated by substituting, for the measured relative humidity, a parameter Δ defined as follows:
Δ= A*RH+B*T*RH+C*T 2 *RH+K
wherein A, B, C are weighting constants, RH is the measured relative humidity, K is a constant and T is the measured temperature of the atmosphere in the vicinity of the pressure sensor and foam seat cushion. In this expression, the first term (A*RH) is the contribution of relative humidity; and the second and third terms together (B*T*RH+C*T 2 *RH) comprise the cross-correlation contribution, with the T 2 term included due to the strongly non-linear variation in the relationship between relative humidity and absolute humidity through the temperature range. In practice the temperature could be measured each time the humidity is measured, and the value of Δ could be stored and used in place of the values of relative humidity in the method and apparatus of FIGS. 1-5 to provide the compensation factors for the method of FIGS. 6-7. Alternatively, the temperature and relative humidity values could be stored in linked memory locations with the value of Δ calculated as needed later in performing the remaining calculations. In either case, the value of Δ could alternatively be read from a three dimensional look-up table on the basis of relative humidity and temperature inputs.
An alternative embodiment of the invention is described with reference to FIG. 8, which is a top level block diagram of an algorithm, which can be performed by a programmed digital computer. Inputs to this cross-correlation algorithm include a temperature reading and a relative humidity reading. A non-linear correction function 100 contains terms including at least, but not limited to, a coefficient times temperature, a coefficient times humidity and a coefficient times the cross-product of humidity and temperature. In general, higher order polynomials in temperature and humidity may be included in an embodiment of this invention. In addition, cross-product terms with other system variables are envisioned. Such additional cross-product terms may include: pressure (related to weight), totalized (integrated, summed, etc.) weight, time and others. In this embodiment, the correction function 100 may be expressed His follows.
Δ=A*T+B*RH+C*T*RH+D*T
2
*RH+K
wherein T is air temperature near the seat cushion, RH is the relative humidity of air near the seat cushion, K is a constant, and A, B, C and D are weighting coefficients, usually constants. The third term—C*T*RH—is the basic term for the cross-correlation between temperature and relative humidity. The fourth term—D*T 2 *RH—is a higher order cross-correlation term suggested by the strong non-linear curves relating relative humidity, absolute humidity and temperature. The determination of whether the last term is used in a particular case will depend on the degree of accuracy required and the calculating resources and time available.
The consecutive values of Δ are provided to a circular buffer 102 , from which they are selected as required for use in the calculations to determine occupant classification as shown in the flow chart of FIG. 7 . The buffer is used to introduce a controllable time delay into the process. The buffer has two pointers: a write (input) pointer and a read (output) pointer. New values of Δ are stored in the buffer as the write pointer advances regularly from one memory location to the next; but values are read out of the buffer according to the read pointer, which can be moved relative to the write pointer to provide a controlled, variable time delay between input and output values. The circular buffer is large enough to accommodate the longest allowable time delay without writing over required data.
The output pointer of circular buffer 102 is controlled according to a delay function 104 , provided to account for time delay effects in the system, which are dominated by the delay of air exchange between the atmosphere and the foam seat cushion. This delay is important because the measured temperature and humidity are characteristics of the atmospheric air outside the foam while the load transmitting effects are produced by moisture within the foam. The delay is affected by many factors, including characteristics of the foam itself, the nature of the seat cushion covering and the timing and amount of seat activity—that is, the alternate compression and expansion of the foam that can greatly increase the rate of air exchange over that occurring due to diffusion with an unmoved cushion. An example of a delay function is given by the following: Γ = ( E * ∫ P + F * P ) σ P
wherein Γ is the delay value, P is the pressure signal, ∫P is the time integral of the pressure signal, and σP is a variance value. E and F are weighting factors and are typically constants. The time integral of the pressure signal ∫P is derived in an integration function 106 , which receives the pressure signal P and a time signal as inputs and integrates the pressure signal in a known manner. The variance signal σP is derived in a variance function 108 , which receives the pressure signal P and may, as an example, be the same as or similar to the derivation of the activity factor described with respect to FIG. 4 . The calculated delay factor Γ is applied to the circular buffer to control the read (output pointer), with higher values of Γ tending to increase the lag of the read pointer relative to the steadily moving write pointer by moving the former away from the latter and lower values of Γ tending to decrease the lag by moving the read pointer close to the write pointer.
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A vehicle seat occupant classification system uses a pressure responsive, fluid filled bladder and pressure sensor adapted for engagement with an underside of a foam seat cushion so as to generate a pressure signal corresponding to the weight of an occupant on an upper side of the foam seat cushion. A humidity sensor responds to relative humidity of air adjacent the pressure sensor and/or foam seat cushion to generate a humidity signal that is used to compensate at least one of the pressure signal, a stored reference pressure value and a stored threshold value, from which at least in part; an occupant classification is determined. The system preferably includes a time delay between the reading of a humidity value and the full use of that humidity value in compensation; and the time delay may be responsive to an activity factor derived from dynamic variations in the pressure signal associated with a pumping action on the foam tending to increase the rate of exchange of air between the foam and the atmosphere outside the foam. Preferably, the temperature adjacent the pressure sensor and/or foam seat cushion is also determined and used in conjunction with the humidity signal to provide au additional cross-correlation compensation.
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This application is a continuation of International Application No. PCT/AT2006/000175, filed Apr. 28, 2006.
BACKGROUND OF THE INVENTION
The invention concerns a furniture item with a furniture body and a movable furniture part located in or on the furniture body, and an ejection device which has an ejection element to move the movable furniture part out of a closed position into a first open position, and a latchable actuator for the ejection element. Furthermore, a process for opening and closing the new type of furniture item will be proposed.
Furniture items of this type are known already in the state of the art in which typical ejection devices are designated as so-called “touch-latch” mechanisms. These require pressure (a touch) to be applied, for example, to the movable furniture part, a switch, button or something of that nature to unlatch the ejection device, which has the effect of moving the movable furniture part by means of the ejection element from its closed position into a first open position. If the actuator comprises a manually loaded energy accumulator, the loading of the latter is usually effected when the furniture item is closed. It has been found that an unsatisfactory aspect of this state of the art is that the user has only part of the closure path immediately by the closed position to load the energy accumulator.
The invention sets out, therefore, to propose an improved version of the furniture item in question which will avoid the drawbacks recognized in the state of the art. The proposal will include a process for opening and closing the new type of furniture item.
The invention resolves this task by providing a means of moving one or more ejection elements beyond of the first open position.
In the case of actuators generally comprising a manually loaded energy accumulator, preferably a tension spring, to preload the energy accumulator, the ejection element on which the accumulator acts over a part of the closure path is in contact with either the movable furniture part or with the furniture body, depending on whether the ejection device is arranged on the furniture body or on the movable furniture part. In those ejection devices known up to the present time, this contact action occurs in the section of the opening or closing path of the movable furniture part located between the closed end position and the first open position of the movable furniture part whereby the first open position of the movable furniture part corresponds to the position of the ejection element after the end of the ejection process. This means that the user, when closing the movable furniture part, may just move it slightly to reach the first open position before having to apply additional pressure in the last section of the closing path to load the energy accumulator.
SUMMARY OF THE INVENTION
In contrast, in the furniture item according to the invention, an arrangement is proposed whereby, once the ejection process has ended, the ejection element is moved beyond the first open position of the furniture part, and the partial section of the closing path in which the ejection element is in contact with the movable furniture part, or furniture body as the case may be, to load the energy accumulator, is displaced in the direction of the opened end position. This means that, immediately after or simultaneous with the start of the closing motion of the movable furniture part, the user begins to load the energy accumulator of the actuator and, at the end of the loading process, has then to apply a small force to move the movable furniture part into its closed end position. This will give the user the impression that the closure of the movable furniture part is a completely smooth closing motion.
According to a first design example of the invention, the means directly or indirectly contacting or contactable with the ejection element provided to move at least one ejection element through the first open position are arranged on the movable furniture part regardless of whether the movable furniture part is in the form of a door, lid or drawer.
This lends itself to a simple design whereby the means include at least a first part arranged on the movable furniture part and at least a second part arranged on the ejection element such that they exert a magnetic attractive force on one another. Other solutions are possible, naturally. Thus, it is possible, for example, that the first part could be formed as a hinged rod arranged on the movable furniture part and the second part of the means could be arranged, for example, in the form of a longitudinal guide on the ejection element.
According to another design example of the invention, the means directly or indirectly contacting or contactable with the ejection element provided to move at least one ejection element beyond the first open position are arranged on the furniture body and/or in or on the ejection device. A preferred design example according to the invention provides that the actuator in addition to the ejection device has at least one additional auxiliary actuator which constitutes the means for moving the ejection element during the opening of the movable furniture part beyond the first open position.
A simple but nevertheless sturdy solution for this is if the auxiliary actuator is an energy accumulator, preferably manually loaded and preferably a pressure spring.
Although it would also be conceivable to configure the movement of the ejection element beyond the first open position to be independent of the movement of the movable furniture part, a technically simple solution is achieved if the one (or more) ejection element in the ejection device stays in contact or follows the movable furniture part in at least one part section of the opening or closing path of the movable furniture part situated between the first open position and the closed end position. Beneficially, the one (or more) ejection element in the ejection device is in contact with the movable furniture part during 50%, or preferably 80%, of the opening or closing path of the movable furniture part.
According to an alternative design version of the invention, it is arranged that the means for moving the ejection element during the opening of the movable furniture part through the first open position which is directly or indirectly linked with the ejection element is fitted to the furniture body and/or to the ejection device.
Regardless of whether the ejection element is arranged on the furniture body or on the movable furniture part so that it moves linearly or rotates, a further design example of the invention provides that the furniture part is located translationally movable in or on the furniture body, for example in the form of a drawer. According to another design example of the invention, the movable furniture part can, however, be located rotationally movable in or on the furniture body, again regardless of whether the ejection element is arranged on the furniture body or on the movable furniture part so that it moves linearly or rotates.
This means that the invention is suitable for all conceivable combinations of a movable furniture part with an ejection element, as long as it is ensured that the location of the ejection element changes in relation to its starting position with a latched ejection device in the first open position, i.e., after completion of the ejection process and at the start of the loading process. In other words, the distance between the contact point of the ejection element in the starting position and the contact point in its position after the end of the ejection process on the one hand, and the distance between the contact point of the ejection element in the starting position and the contact point in its position after the end of the opening process on the other hand must be different.
A preferred design example is characterised by a rotatable ejection element whereby there is a difference between the opening angle of the ejection element in its position after the end of the ejection process in the first open position of the movable furniture part on the one hand, and the opening angle of the ejection element in its position after the end of the opening process in the opened end position of the movable furniture part on the other.
In the case where the movable furniture part is pivotably supported, the maximum opening angle of the ejection element is favorably approximately equal (as close as possible) to the maximum opening angle of the movable furniture part, whereby the ejection element can follow the movable furniture part substantially during the entire opening path of the movable furniture part.
According to a further preferred design version of the invention, the ejection device is formed to at least partly load the energy accumulator of the actuator for the ejection element during a closing movement of the movable furniture part in a part section of the opening or closing path of the movable furniture part located between the opened end position and the first open position. Thus, the closing of the movable furniture part is quiet and smooth if the ejection device is constructed to start the loading process of the energy accumulator in general with each closing movement of the movable furniture part, preferably regardless of the position of the movable furniture part.
If, in this alternative design, the ejection element is pivoted, it can be further arranged that there is a difference between the opening angle of the ejection element at the end of the ejection process in the first open position of the movable furniture part on the one hand, and the angle at the start of the loading process of the energy accumulator on the other, or, respectively, the distance between the contact point of the ejection element in the home position and the contact point at the end of the ejection process on the one hand, and the distance between the contact point of the ejection element in the home position and the contact point at the start of the loading process of the energy accumulator, on the other.
According to a preferred example of the invention, the ejection device has a pivoted ejection element and a latchable actuator, preferably a coil tension spring, which interact with a transmission device, preferably a gear train. A simple means can be arranged whereby the ejection element is linked to the actuator through a link element and has a section with gear teeth that is formed to engage with a driving pinion secured to a bearing element which can rotate. This method can save space if at least the ejection element, the bearing element for the driving pinion and the link element are arranged coaxially.
Latching of the ejection device can be arranged, for example, by using a detent or a catch guided in a heart-shaped slide track, as provided for in a further design example according to the invention, via an elbow lever and/or a dead point mechanism.
The free running needed between the driving pinion and the link element to move the ejection element beyond the first open position is arranged in a further design example according to the invention, in which one arm of the elbow lever is pivoted at its free end with the link element. The dead point mechanism has a lever which is pivoted at one end with the elbow of the elbow lever and at the other end pivoted with a curved coupling element, whereby the curved coupling element is secured, preferably coaxially with the link element, so that it will rotate.
It is necessary in loading the energy accumulator to eliminate free movement between the coupling element and the pinion to be able to transfer the force acting on the ejection element to the link element. According to a design example of the invention, this is achieved by connecting the driving pinion, so that it will not turn, to a coaxial brake disk whereby the brake disk is shaped so that it is in contact at its perimeter with the curved coupling element. This means that, immediately following or at the start of the closing process of the movable furniture part, the brake disk is brought into contact at its perimeter with the curved coupling element, thus blocking the rotation of the pinion, and the force of the movable furniture part, which is closing, acting on the ejection element is transferred to the link element, a process which loads the energy accumulator.
A simple configuration of the ejection device is provided according to a preferred design example if the ejection device is arranged in a housing with an outlet aperture at least for the ejection element. The housing can then be fitted simply in a suitable location either on the movable furniture part or on the furniture body.
To ensure that the movable furniture part always reaches the same first open position at the end of the closing process, it is necessary to define the opening angle of the ejection element in the first open position. The opening angle is achieved by a preferred design example in which at least one stop for the bearing element of the actuating pinion is arranged in the housing, whereby the bearing element rests on the stop in the first open position of the movable furniture part.
A further design example of the invention provides that the means to move the ejection element beyond the first open position is in the form of a preferably curved leaf spring whose first leg engages with the ejection element and whose second leg engages with the link element. In this case, the movable furniture part must be held against the force of the preferably curved leaf spring in its closed end position which can be achieved by a retracting device or a hinge.
According to another example, the means to move the ejection element beyond the first open position is in the form of a spiral spring whose first leg engages with the ejection element and whose second leg, preferably rotatable and held in position, engages with the housing. With an appropriate arrangement of the spiral spring, a form of snap mechanism can be produced such that the spiral or torsion spring holds the ejection element in the exit position but trips when unlatching the energy accumulator and forces the ejection element in the opening direction of the movable furniture part.
According to a further design example of the invention, the ejection device also has a release mechanism with a release element to unlatch the actuator. A preferred design example in this case provides that the release mechanism is configured for the release element to rest in direct contact on the movable furniture part or the furniture body in the closed position of the movable furniture part, in order to precisely define the release path.
Furthermore, it is intended to propose a process for opening and, as the case may be, closing a movable furniture part located in or on a furniture body of a furniture item using an ejection device which has an ejection element which is contacted, or can be contacted, by a latchable actuator, preferably a manually loaded energy accumulator. The latchable actuator is loaded during the closing movement of the movable furniture part by an ejection element which is characterised according to the invention in that the loading process of the energy accumulator is started, after the movable furniture part had been opened, beyond a first open position during a closing movement of the movable furniture part in a part section of the opening, or closing, path of the movable furniture part between the first open position and the closed end position.
In contrast to the state of the art, therefore, the loading process of the energy accumulator is begun right at the start of the closing movement of the movable furniture part whereby, according to a preferred design example of the invention, the loading process for the energy accumulator is started in general with each closing movement of the movable furniture part, preferably independent of the open position of the movable furniture part. In other words, the loading of the energy accumulator occurs based on the ratchet principle, i.e., after the end of the ejection process, the ejection element is free to move in relation to the energy accumulator during the further opening path while, in the reverse direction, it is in constant contact, in every position, with the energy accumulator.
BRIEF DESCRIPTION OF THE DRAWINGS
Other benefits and details of the invention are explained in more detail in the following description of the figures, referring to the design examples illustrated in the drawings, in which:
FIG. 1 show a first design example of a furniture item according to the invention with a movable hinged furniture part,
FIG. 2 a - 2 d show in each case, the movable furniture part and the ejection element in different positions,
FIG. 3 a - 3 c are diagrammatic representations of different positions of the movable furniture part,
FIG. 4 a - 4 c are diagrammatic representations of different positions of the ejection element,
FIG. 5 a is an exploded view of a preferred example of an ejection device according to the invention,
FIG. 5 b is a rear view of the upper part of the ejection element from FIG. 5 a,
FIG. 6 a - 15 show different positions of the movable furniture part and the ejection device from FIG. 5 a during opening and closing the movable furniture part,
FIG. 16 a is an exploded view of a second example of an ejection device according to the invention,
FIG. 16 b is a rear view of the upper part of the ejection element from FIG. 16 a and
FIG. 17-28 show different positions of the movable furniture part and the ejection device from FIG. 16 a during opening and closing the movable furniture part.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a perspective view of the entire furniture item 1 according to the invention in which a movable furniture part 3 is arranged on a furniture body 2 so that it can rotate by means of two hinges 28 . The ejection device 4 is arranged on the furniture body 2 inside, generally level with the front edge of the furniture body 2 such that the pivoted ejection element 5 can move the movable furniture part 3 in the opening direction.
FIG. 2 a shows a plan view of a detail of the furniture item 1 shown in FIG. 1 whereby the movable furniture part 3 is in its closed end position. The gap remaining between the furniture part 3 and the furniture body 2 is needed to allow the movable furniture part 3 to move from its closed end position to, as seen from the closing direction viewpoint, a released position after it whereby the latch on the actuator for the ejection element has been released. After the actuator is unlatched, the ejection element 5 forces the movable furniture part 3 to a first open position ( FIG. 2 b ). At this point, the energy accumulator for the actuator has now completely discharged and the ejection element 5 had ended the ejection process. The reference symbol 26 indicates the release element of the ejection device, more of which will be explained later. Up to this point shown in FIG. 2 b , the invention has followed the touch-latch operation principle known already in the state of the art.
The invention now takes over where the movable furniture part 3 is positioned as shown in FIG. 2 c . As also happens with a conventional touch-latch mechanism, the opening of the movable furniture part 3 has to be done by the user beyond the open position shown in FIG. 2 b since the ejection element 5 has already completed the ejection process. However, in the state of the art, the ejection element 5 does not change its location as the furniture part 3 moves beyond the first open position. The ejection device according to the invention has the means to move the ejection element 5 beyond the first open position shown in FIG. 2 b.
FIG. 2 d shows both the movable furniture part 3 as well as the ejection element 5 in the completely open position whereby the condition where the ejection element 5 is no longer in contact with the movable furniture part 3 in the fully open position is simply a simplification of the design of the ejection device. Naturally it is also possible, however, to locate the ejection element 5 in the ejection device such that the ejection element 5 rests on the movable furniture part 3 in the fully open position.
Different positions of the movable furniture part 3 are illustrated in FIGS. 3 a - 3 c . Here, the movable furniture part 3 is shown in FIG. 3 a in closed position S in which the movable furniture part 3 is aligned essentially parallel to the front of the furniture body 2 . In FIG. 3 b , the movable furniture part 3 is located in its first open position O corresponding to the position of the movable furniture part 3 after the end of the ejection process. The opening angle is designated by 13 which represents the change in position of the movable furniture part 3 from its closed position S to its first open position O. At the end of the ejection process, the movable furniture part 3 is moved by the user beyond the first open position O to its opened end position E. The opening angle β′ extends in this case between the closed position S to the opened end position E of the movable furniture part 3 .
It should be pointed out that the opened end position E does not necessarily have to be the completely open position of the movable furniture part 3 —as shown in FIG. 3 c —that is, the opening angle β′ must simply be greater than the opening angle β in the closed position S of the movable furniture part 3 and smaller or equal to the maximum opening angle when the movable furniture part 3 is in its fully open position.
Similarly, FIGS. 4 a - 4 c show different positions of the ejection element 5 which is pivoted in the ejection device 4 in the design example shown. FIG. 4 a shows the ejection element 5 is the home position S′ corresponding to the position of the ejection element 5 with a latched ejection device 4 and the movable furniture part 3 in the closed end position. FIG. 4 b shows the position O′ of the ejection element 5 after the end of the ejection process. The opening angle α here extends between the position O′ of the ejection element 5 and the position of the ejection element 5 in the exit position S′. d is used to designate the distance between the contact point of the ejection element 5 in the closed position S′ and the contact point of the ejection element 5 after the end of the ejection process, while d′ denotes the distance between the contact point of the ejection element 5 in the closed position S′ and the contact point of the ejection element 5 after the end of the opening process of the movable furniture part.
If FIGS. 4 b and 4 c , which show the position E′ of the ejection element 5 after the end of the opening process of the movable furniture part 3 , are compared, it can be seen that the distances d, d′, or, respectively, the opening angles α, α′ are different in both positions.
A basic idea of the invention consists of sending the ejection element 5 , after the end of the ejection process, to, viewed in the opening direction, a position E′ located beyond position O′ which represents the position of the ejection element 5 after the end of the opening process of the movable furniture part 3 . This is done by linking the movable furniture part 3 right at the start or immediately after the start of the closing process with the ejection element 5 , whereby, with an appropriate linking of the ejection element 5 with the ejection device, the loading process for the energy accumulator can begin as early as the first section of the closing path, during which the loading of the energy accumulator can be completed using known devices in the part section of the closing path of the movable furniture part 3 immediately before the closed position.
This means that, essentially, the whole of the path traveled by the movable furniture part as it closes can now be used to load the energy accumulator. This is due to the invention and the construction of the ejection device using the ratchet principle such that the ejection element, at the end of the ejection process, is free to move in relation to the energy accumulator of the actuator during the further opening path, during which it is in constant contact, i.e., in every position, with the energy accumulator in the opposite direction. Thus, on the one hand, the path traveled by the movable furniture part as the energy accumulator is being loaded can be made greater than the path traveled by the movable furniture part during the ejection process, so that a user requires less force to load the energy accumulator due to the lengthened path.
A second possibility is to make the length of the path traveled by the movable furniture part during the charging and ejection processes essentially the same but to move this section to the immediate vicinity of the opened end position of the opening and closing path of the movable furniture part. The result of this is that the user will apply a force to load the energy accumulator right at the start of the closing process, giving the user the feeling of a smooth process when closing the movable furniture part.
Using two of the design examples presented in FIGS. 6 a - 15 and FIGS. 16 a - 28 , the functioning sequence of a furniture item according to the invention during the opening and closing processes will be described below.
FIG. 5 a shows an exploded view of a first example of an ejection device 4 according to the invention. All parts of the inventive ejection device 4 are arranged in an enclosed housing 20 , whereby the housing cover is not shown to allow a clear overall view. The rotatable ejection element 5 arranged in the housing 20 is in the form of a single-arm lever and has an upper part 27 and a lower part 27 ′. A rotatable roller 29 is arranged on its end furthest from the pivot point, whereby the axes of rotation of the roller 29 and the ejection element 5 are essentially parallel. This roller 29 provides the means of linking the ejection element 5 with the movable furniture part.
A bearing element 13 , a coupling element 16 and a link element 14 are also rotatable and arranged coaxially with the ejection element 5 between the lower part 27 ′ and the upper part 27 . A pinion 12 and a brake disk 19 , connected together and unable to rotate relative to each other, are anchored and can rotate about an axis which is essentially parallel to the rotation axis of the ejection element 5 or, respectively, that of the bearing element 13 . The pinion 12 is constructed so that it engages with a toothed section Z ( FIG. 5 b ) on the upper part 27 of the ejection element 5 , while the brake disk 19 is constructed to engage with a toothed section Z′ arranged on the coupling element 16 . Furthermore, a guide element 30 is arranged between the coupling element 16 and the brake disk 19 , and the guide element 30 serves to provide a secure engagement with the teeth in the toothed section Z′ of the coupling element 16 arranged around the perimeter of the brake disk 19 (i.e., this prevents a tooth tip on the brake disk 19 from coming into contact with a tooth tip on the toothed section Z′ on the coupling element 16 when the brake disk 19 engages with the coupling element 16 ).
In the example shown, the means to move the ejection element 5 through a first open position comprise two auxiliary actuators 23 , 23 ′ whereby the first auxiliary actuator 23 ′ in the form of a spiral spring bears on the bearing element 13 in the opening direction, whose movement is restricted by a stop 22 arranged in the housing, which allows the required freedom of movement for the ejection element 5 between the brake disk 19 and the coupling element 16 . The second auxiliary actuator 23 ′ is in the form of a torsion spring whose first leg 24 engages with the upper part 27 of the ejection element 5 while the second leg 24 ′ is rotatable but fixed in position to the housing 20 of the ejection device 4 .
Furthermore, the actuator 6 for the ejection element 5 is arranged in the ejection device 4 , where the actuator 6 has a manually loaded energy accumulator 8 in the form of a tension spring, a retainer 7 for the energy accumulator 8 and an adjusting element 9 to adjust the energy accumulator 8 . The adjusting element 9 is arranged in the housing 20 such that it is accessible externally to make adjustment of the energy accumulator 8 simple and uncomplicated. At its open end, the energy accumulator 8 constructed as a tension spring for the actuator 6 is hooked over a projection 10 on the link element 14 , so that, as the energy accumulator 8 discharges, the link element 14 is moved in the direction of the actuator 6 .
The actuator 6 is latched, in the design example shown, by an elbow lever 17 and a dead point mechanism. In this system, the first arm 18 of the elbow lever 17 is pivoted at its free end with the link element 14 , while the second arm 18 ′ is pivoted to the housing 20 of the ejection device 4 . The dead point mechanism comprises a pivoted lever 15 and is connected at one end to the elbow of the elbow lever 17 and at the other end, also pivoted, to the coupling element 16 . The actuator 6 is latched, when charging the energy accumulator 8 by the ejection element 5 , when the link element, due to its engagement with the brake disk 19 and with the coupling element 16 of the link element 14 is moved so far to the right until the energy accumulator 8 is fully loaded and the lever 15 crosses the dead point of the elbow lever 17 , which latches the elbow lever 17 , and, therefore, the link element 14 .
The actuator 6 is unlatched by a release mechanism 25 which comprises a release element 26 , an eccentric rotating element 33 , a restoring spring 32 for the rotating element 33 , a wedge-shaped adjusting element 34 , a release lever 35 , a damping element 36 and a restoring element 37 , contacted by the damping element 36 , to restore the rotating element 33 . The release mechanism 25 is linked to the lever 15 of the dead point mechanism by a connecting part 38 , preferably in the form of a lever, which can rotate at one end with the release lever 35 and at the opposite end with the lever 15 of the dead point mechanism, or, respectively, the coupling element 16 .
FIG. 6 a shows the ejection device 4 with the energy accumulator 8 in the latched condition. The movable furniture part 3 is in the closed position whereby the release element 26 of the release mechanism 25 rests directly on to the movable furniture part 3 . More will be explained later about the direct contact of the release element 26 with the movable furniture part 3 which is essentially accomplished by means of the wedge-shaped adjusting element 34 which is contacted by the restoring element 37 .
The view of the device is clarified by omitting the cover of the housing 20 and the upper part 27 of the ejection element 5 from the drawing. In the situation shown, the energy accumulator 8 for the actuator 6 is loaded. This means that the tension spring which constitutes the energy accumulator 8 is anchored in the retainer 7 and tensioned by the link element 14 . On its front side facing the movable furniture part 3 , the housing 20 has an exit aperture 21 for the ejection element 5 and the release element 26 . All of the remaining components of the ejection device 4 are contained inside the enclosed housing 20 except the adjusting element 9 for the energy accumulator 8 .
The energy accumulator 8 is latched by means of an elbow lever 17 acting on the link element 14 where the lever 17 is latched in the position shown by a lever 15 in a dead point mechanism. The ejection element 5 is latched in its home position S′ by the auxiliary actuator 23 constructed as a torsion spring. In this, the auxiliary actuator 23 is arranged such that the one leg 24 ′ of the spring is arranged in a bearing point 40 in the housing and the second leg 24 of the auxiliary actuator 23 is arranged in a bearing point 39 on the lower part 27 ′ of the ejection element 5 so that they swivel.
By locating the bearing point 39 , with the ejection element 5 in the home position, on the right side of the connecting line V of the pivot point of the ejection element 5 and the bearing point 40 ( FIG. 6 b ), this ensures that the auxiliary actuator 23 locks the ejection element 5 in its home position. Due to the rotational motion of the ejection element 5 during the ejection process this bearing point 39 moves to the left until it crosses the connecting line V, so that the auxiliary actuator 23 pushes the ejection element 5 in the opening direction. This means that the auxiliary actuator 23 constructed as a torsion spring is latched, similar to the actuator 6 , by means of a dead point mechanism.
In the position shown, therefore, the link element 14 , the coupling element 16 and the ejection element 5 are not free to move due to the latched elbow lever 17 or, respectively, the position of the auxiliary actuator 23 , while the bearing element 13 and, thus, the pinion 12 and the brake disk 19 can rotate. In this, the bearing element 13 is contacted by an auxiliary actuator 23 ′ formed as a curved spring which forces the bearing element in the opening direction of the movable furniture part whereby the teeth on the pinion 12 engage with the tooth-shaped section Z of the upper part 27 of the ejection element 5 .
By having the bearing element 13 forced away from the coupling element 16 by the auxiliary actuator 23 ′, the required freedom of movement can be obtained between the coupling element 16 and the brake disk 19 during the opening process. If this brake disk 19 were to engage with the tooth-shaped section Z′ of the coupling element 16 during the opening process, this would block the pinion 12 and, thus, the ejection element 5 as a result, that is, the ejection of the movable furniture part 3 by the ejection element 5 would not have been possible in this type of configuration.
FIG. 6 b differs from FIG. 6 a in that it shows the upper part 27 of the ejection element 5 , on which a catch 41 is formed.
FIG. 7 shows the movable furniture part 3 in the release position A which, viewed in the closing direction SR, is located beyond the home position S of the movable furniture part 3 , whereby the movable furniture part 3 , in the design example shown, is being moved by the user who is pressing the movable furniture part from the home position S to the release position A. The motion of the movable furniture part 3 pushes the release element 26 back into the housing 20 and the release lever 35 moves leftwards over the wedge-shaped adjusting element 34 . The release element 26 , the wedge-shaped adjusting element 34 and the release lever 35 are thus constructed and arranged as components in a rolling contact joint. The L-shaped lever 35 and the lever-type link 38 also move the lever 15 in the dead point mechanism to the left which releases the catch on the elbow lever and, thus, the latching of the energy accumulator 8 .
Even though the illustrated release mechanism represents a preferred design example, the invention is not to be seen as restricted to the design example shown. To this end, instead of using the movable furniture part 3 to release the ejection device, it is completely possible and conceivable to do this by means of a switch, a button or by direct pressure on the release element 26 itself.
In FIG. 8 , the ejection process has ended and the movable furniture part 3 has reached its first open position O. With the release of the energy accumulator 8 , the link element 14 was moved to the left which moved the ejection element 5 out of the housing 20 in the opening direction OR. The link between the ejection element 5 and the movable furniture part 3 is made by means of the idler roller 29 , which allows the movable furniture part 3 to slide smoothly on the ejection element 5 . The coupling element 16 was also moved in the opening direction OR by the lever 15 which is connected at one of its ends to the elbow of the kinked elbow lever 17 , the movement continuing until a gap appears between the brake disk 19 and the toothed section Z′ of the coupling element 16 , or, respectively, the guide 30 , so that the pinion 12 which is still engaging with the toothed section Z on the upper part 27 of the ejection element 5 (not shown) is allowed to turn.
The bearing element 13 , still being forced by the auxiliary actuator 23 ′ in the opening direction OR, is prevented from moving further outwards by the stop 22 ( FIG. 5 a ) arranged in the housing 20 .
It is further evident from FIG. 8 that the bearing element 39 for the leg 24 of the auxiliary actuator 23 formed as a torsion spring, lies between the pivot point of the ejection element and the bearing point 40 of the auxiliary actuator 23 so that the auxiliary actuator 23 ′ is still forcing the ejection element 5 in the opening direction OR. This requires the force exerted by the auxiliary actuator 23 to be arranged such that it can just move the ejection element 5 out, but is not enough for the ejection element 5 to open the movable furniture part 3 further, which is still in contact with the ejection element 5 .
It is, of course, also possible to make the acting force of the auxiliary actuator 23 so large that the auxiliary actuator 23 would not only be able to move the ejection element 5 but also the movable furniture part 3 beyond the first open position O to an opened end position E. A construction of this type would lead to the situation where the user, in closing the movable furniture part 3 , would have to apply, additional to the force to load the energy accumulator 8 , the relatively large force to load the auxiliary actuator which would give the user the impression of a movable furniture part which is stiff to move. Nevertheless, if the level of the acting force by the auxiliary actuator 23 is appropriate, a furniture item 1 with a movable furniture part 3 and an ejection device 4 can be produced where the user, in moving the movable furniture part 3 from a closed position to an opened end position, simply has to release the ejection device 4 by, for instance, applying pressure to the movable furniture part whereby the movable furniture part 3 would then be moved in a first section by the ejection element 5 and in a further section by the auxiliary actuator 23 to its opened end position without requiring any further action on the part of the user.
By contrast, in the example shown, the force exerted by the auxiliary actuator 23 is just enough for the ejection element 5 to stay in contact with the movable furniture part 3 such that the user is scarcely aware, when closing the movable furniture part, of the force applied to load the auxiliary actuator 23 .
An opened end position E of the movable furniture part 3 is illustrated in FIG. 9 . It is evident that, compared with FIG. 8 , the position of the movable furniture part 3 , the ejection element 5 and the auxiliary actuator 23 has changed. The discharging of the auxiliary actuator 23 and the movement of the movable furniture part 3 by the user to an opened end position E has enabled the ejection element 5 to follow the movement of the movable furniture part 3 . Similarly, the position of the pinion 12 has changed relative to the toothed section Z arranged on the upper part 27 of the ejection element 5 . In other words, the pinion 12 on this toothed section Z is now engaged with a point on the toothed section Z furthest from the idler roller 29 .
If the movable furniture part 3 is now moved from its opened end position E in the closing direction SR, the brake disk 19 is brought into engagement with the toothed section Z′ of the coupling element 16 , as shown in FIG. 10 . This will block the rotation of the pinion 12 along the toothed section Z on the ejection element 5 and the coupling element 16 will be forced back in the closing direction into the housing 20 by the movement of the ejection element 5 . The link element 14 is moved so far to the right by the coupling element 16 and the elbow lever 17 linked to it until the energy accumulator 8 of the actuator 6 is fully loaded. At the same time, this movement also loads the auxiliary actuators 23 , 23 ′ ( FIG. 11 a ).
As shown in FIG. 10 , the action of the guide 30 ensures that the brake disk 19 and the toothed section Z′ of the coupling element 16 engage with each other such that each tooth tip of the brake disk 19 engages with each tooth root on the toothed section Z′ of the coupling element 16 which is able to prevent any jerky movements of the ejection element 5 and, thus, of the movable furniture part 3 .
FIG. 11 b differs from FIG. 11 a in that the lever 15 of the dead point mechanism has now passed beyond the dead point of the elbow lever 17 so that the energy accumulator 8 of the actuator 6 is latched. Thus, the loading process for the energy accumulator 8 is concluded before the movable furniture part 3 has reached its first open position O. After the energy accumulator 8 has been loaded, the release element 26 of the release mechanism 25 remains in contact, with no play, with the movable furniture part 3 during the remaining section of its closing path.
Moreover, as can be seen in FIG. 11 b , the upper part 27 of the ejection element 5 has a catch 41 which is formed to engage with an eccentric rotating element 33 of the release mechanism 25 . The rotating element 33 is forced in the closing direction SR of the ejection element 5 by a restoring spring 32 to ensure that the catch 41 engages with the rotating element 33 as the ejection element 5 retracts into the housing 20 .
In FIG. 12 , the catch 41 is now engaged with the eccentric rotating element 33 , and carries it along with it in the closing direction SR of the ejection element 5 . As the ejection element 5 retracts, the locking elements of the ejection device 4 remain unchanged for the energy accumulator 8 , thus keeping the actuator latched.
In FIG. 13 , the bearing point 39 of the auxiliary actuator 23 has now passed beyond the connecting line V between the pivot point of the ejection element 5 and the bearing point 40 of the auxiliary actuator 23 on the housing 20 , whereby the auxiliary actuator 23 continues to press on the ejection element 5 in the opposite direction, that is, the ejection element 5 is now pushed back into its home position by the auxiliary actuator 23 where it is latched. The catch 41 on the ejection element 5 has restored the rotating element 33 to an end position which has tensioned the restoring element 37 completely. The eccentric rotating element 33 is connected via a toothed section (not shown) to the pinion of a damper 36 to dampen the return movement of the rotating element 33 when tensioning the restoring element 37 in the form of a tension spring, as well as avoiding noise which might arise as the rotating element 33 returns to its other end position. By locating the wedge-shaped adjusting element 34 in a ball socket arranged on the eccentric rotating element 33 by means of a ball head, the wedge-shaped adjusting element 34 is moved in conjunction with the eccentric rotating element 33 .
In FIG. 14 , the movable furniture part 3 is now back in its closed position S, in which, for example, it can be retained by the hinge 28 . The catch 41 on the ejection element 5 now snaps past the eccentric rotating element 33 which is moved to the left by the restoring element 37 . The rotating element 33 moves the wedge-shaped adjusting element 34 to the left also. Due to the rolling contact joint formed between the wedge-shaped adjusting element 34 and the release element 26 , the release element 26 is moved out of the housing 20 towards the movable furniture part 3 and just far enough so that the release element 26 rests on the movable furniture part 3 with no play between them ( FIG. 15 ).
The configuration shown in FIG. 15 corresponds to that shown in FIG. 6 b , that is, the ejection element 5 is in the home position, with the actuator 6 latched, the movable furniture part 3 is in the closed position and the release element 26 rests on the movable furniture part 3 with no play between them.
FIG. 16 a , as in FIG. 5 a , shows an exploded view of a second example of an inventive ejection device 4 . The same parts have the same identification symbols, so a repeat description of these parts will be dispensed with.
The second example shown in FIGS. 16 a - 28 differ from the first design example shown in FIGS. 5 a - 15 mainly in the design of the release mechanism 25 and its linking with the coupling element 16 via the lever-type link 38 .
As in the first example, the release mechanism 25 has a release element 26 , an eccentric rotating element 33 and a damper 36 , whereby the damper 36 comprises a bearing 42 , a rotary damper 43 and a pinion 44 . Differing from the first design example, the release element 26 in the second design example is connected directly to the eccentric rotating element 33 via a rolling contact joint. The release mechanism 25 is connected to the coupling element 16 via a lever-type link 38 which, however, is pivoted at one of its ends to the bearing 42 on the damper 36 . This means that the bearing 42 , or rotating damper 43 respectively, in the second design example assumes the function of the release lever 35 , or restoring element 37 respectively, in the first design example.
The lever-type link 38 is no longer pivoted at its opposite end with the coupling element 16 . Instead, a notched end 45 is arranged at the free end of the lever-type link 38 which is formed to engage with a projection 46 formed on the coupling element 16 . The coupling element 16 , for its part, is pivoted with the lever 15 of the dead point mechanism for the elbow lever 17 .
In contrast to the first example, the second design example has just one auxiliary actuator 23 , formed as a curved spring and acting between the link element 14 and the ejection element 5 . The difference extends to the construction of the peripheral surface of the brake disk 19 and the corresponding section Z′ on the coupling element 16 .
Whereas in the first example engagement between the brake disk 19 and the coupling element 16 was positive due to the toothed design, in the second example the brake disk 19 and the coupling element 16 form a friction contact with one another.
FIG. 17 shows the ejection device 4 with the energy accumulator 8 latched. The movable furniture part 3 is in the closed position S whereby the release element 26 of the release mechanism 25 rests on the movable furniture part 3 with no play between them. In the position shown, the energy accumulator 8 is loaded and the actuator 6 latched. The latch action is brought about by the action of an elbow lever 17 on the link element 14 , where the lever 17 is locked by a lever 15 in a dead point mechanism in the position illustrated.
The ejection element 5 is locked in its home position S by the hinge 28 . The link element 14 , the coupling element 16 and the ejection element 5 are not free to move due to the locked elbow lever 17 and the movable furniture part 3 held in its closed position by the hinge 28 , while the bearing element 13 and, thus, the pinion 12 as well as the brake disk 19 can rotate. The freedom of movement required for free motion between the coupling element 16 and the brake disk 19 is provided by simply having a stop 22 ′ for the bearing element 13 in the housing 20 .
In this example, it must be ensured that the retention force of the hinge is greater than the force exerted by the auxiliary actuator 23 which maintains the ejection element 5 in permanent contact in the opening direction OR with the movable furniture part 3 .
FIGS. 18 and 18 b differ only in that the upper part 27 of the ejection element 5 is shown transparently (dotted line). Otherwise, pressure is being exerted in FIG. 18 on the movable furniture part 3 , denoted by the changed position of the release lever 15 .
FIG. 19 shows the movable furniture part 3 in the release position A which, viewed in the closing direction SR, is located behind the closed position S of the movable furniture part 3 , whereby the user is applying pressure to move the movable furniture part 3 from the closed position S to the release position A. The movable furniture part 3 pushes the release element 26 further back into the housing 20 whereby, via the rolling contact joint, the eccentric rotating element 33 and, with it, the bearing 42 , are moved to the left. Simultaneously, the coupling element 16 and, therefore, the lever 15 in the dead point mechanism are also moved to the left by the notched end 45 ( FIG. 16 a ) arranged on the lever-type link 38 , unlatching the elbow lever 17 and so unlatching the energy accumulator 8 .
In FIG. 20 , the ejection process has ended and the movable furniture part 3 has reached its first open position O. With the release of the energy accumulator 8 , the link element 14 was moved to the left which moved the ejection element 5 out of the housing 20 in the opening direction OR. The link between the ejection element 5 and the movable furniture part 3 is made by means of the idler roller 29 , which allows the movable furniture part 3 to slide smoothly on the ejection element 5 . The bearing element 13 is prevented from moving further outwards by the stop 22 ( FIG. 16 a ) arranged in the housing.
In order to allow the eccentric rotating element 33 which, during the opening process is moved to the left by the catch 41 on the ejection element 5 , to return to a position once the catch 41 has passed, in which the catch 41 can again engage with the eccentric rotating element 33 when closing the movable furniture part 3 , a restoring spring 32 in the form of a compression spring is arranged between the housing 20 and the eccentric rotating element 33 .
An opened end position E of the movable furniture part 3 is illustrated in FIG. 21 a . It is evident that, compared with FIG. 21 a , the position of the movable furniture part 3 , the ejection element 5 and the auxiliary actuator 23 has changed. The movement of the movable furniture part 3 by the user to an opened end position E has enabled the auxiliary actuator 23 to discharge and the ejection element 5 to follow the movement of the movable furniture part 3 . Similarly, the position of the pinion 12 has changed relative to the toothed section Z arranged on the upper part 27 of the ejection element 5 . In other words, the pinion 12 on this toothed section Z is now engaged with a point on the toothed section Z furthest from the idler roller 29 .
FIG. 21 b relates to the position of the ejection device 4 shown in FIG. 21 a and differs only in that the peripheral surface of the brake disk 19 and the corresponding section Z′ of the coupling element 16 are toothed as in the first design example. Again, to avoid a jerky engagement of the brake disk 19 with the coupling element 16 , a guide 30 is arranged on the coupling element 16 .
If the movable furniture part 3 is now moved from its opened end position in the closing direction SR, the brake disk 19 is brought into engagement with the toothed section Z′ of the coupling element 16 , as shown in FIGS. 22 a and 23 . This will block the rotation of the pinion 12 along the toothed section Z on the ejection element 5 and the coupling element 16 will be forced back in the closing direction SR into the housing 20 by the movement of the ejection element 5 . The link element 14 is moved so far to the right by the coupling element 16 and the elbow lever 17 linked to it until the energy accumulator 8 of the actuator 6 is fully loaded. At the same time, this movement also loads the auxiliary actuator 23 .
FIG. 22 b again shows an alternative in which the peripheral surface of the brake disk 19 and the corresponding section Z′ of the coupling element 16 are toothed. It can be seen that the action of the guide 30 ensures that the brake disk 19 and the toothed section Z′ of the coupling element 16 engage with each other such that each tooth tip of the brake disk 19 engages with each tooth root on the toothed section Z′ of the coupling element 16 which is able to prevent any jerky movements of the ejection element 5 and, thus, of the movable furniture part 3 .
FIG. 24 differs from FIG. 23 in that the lever 15 of the dead point mechanism has now passed beyond the dead point of the elbow lever 17 so that the energy accumulator 8 of the actuator 6 is latched. Thus, the loading process for the energy accumulator 8 is concluded before the movable furniture part 3 has reached is first open position O. After the energy accumulator 8 has been loaded, the release element 26 of the release mechanism 25 remains in contact, with no play, with the movable furniture part 3 during the remaining section of its closing path.
Moreover, as can be seen in FIG. 25 , the upper part 27 of the ejection element 5 has a catch 41 which is formed to engage with an eccentric rotating element 33 of the release mechanism 25 . This rotating element 33 , as already mentioned, is acted on by a restoring spring 32 to ensure that the catch 41 engages with the rotating element 33 as the ejection element 5 retracts into the housing 20 .
In FIG. 25 , the catch 41 is now engaged with the eccentric rotating element 33 , and carries it along with it in the closing direction SR of the ejection element 5 . As the ejection element 5 retracts, the locking elements of the ejection device 4 remain unchanged for the energy accumulator 8 , thus keeping the actuator latched.
In FIG. 26 , the catch 41 on the ejection element 5 has restored the eccentric rotating element 33 to its one end position. The eccentric rotating element 33 is connected via a toothed section (not shown) to the pinion 44 and the rotary damper 43 of the damper 36 to dampen the return movement of the rotating element 33 .
In FIG. 27 , the movable furniture part 3 is now back in its closed position S, in which it can be retained by the hinge 28 . The catch 41 on the ejection element 5 now snaps past the eccentric rotating element 33 which is moved to the left by the damper element 36 . Due to the rolling contact joint formed between the eccentric rotating element 33 and the release element 26 , the release element 26 is moved out of the housing 20 towards the movable furniture part 3 and just far enough so that the release element 26 rests on the movable furniture part 3 with no play between them ( FIG. 28 ).
The configuration shown in FIG. 28 corresponds to that shown in FIG. 17 , that is, the ejection element 5 is in the home position, with the actuator 6 latched, the movable furniture part 3 is in the closed position S and the release element 26 rests on the movable furniture part 3 with no play between them.
The design examples shown should not, of course, be regarded as limiting but rather simply as individual samples of innumerable possibilities for inventive concepts for producing a movable furniture part with an ejection element by means of which the movable furniture part is moved further in the opening direction after the end of the ejection process.
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The invention relates to an item of furniture including a furniture body, a furniture part which is displaceably received in or on the furniture body, and an ejection device having at least one ejection element for displacing the moveable furniture part from a closed position into a first open position. At least one lockable drive device is provided for driving the at least one ejection element. The invention is characterized by means for displacing the at least one ejection element beyond the first open position.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a means and method for sealing roofs, walls, driveway cracks and areas where water-proofing is needed. More particularly, the present invention relates to an asphaltic composition in a form which facilitates spot application of bituminous adhesive to roof flashing around perimeters, protrusions and roof membrane laps; side wall cracks, driveway cracks and numerous other applications where asphalt might be used for caulking or water-proofing.
2. Description of the Prior Art
In the covering of roofs of buildings, a sheetlike roof-covering material is normally used. Numerous types of such sheets are known (see, for example, U.S. Pat. Nos. 4,617,221, 4,565,724, and 4,374,687).
Generally such a roofing material contains a bituminous layer which serves as an adhesive layer for securing the sheeting onto the roof. Also, it is conventional to overlap these sheets with one another in order to provide a seal. Methods for effecting such sealing are shown in U.S. Pat. No. 2,036,123.
However, because the roofing material is generally in the form of rolled sheets, it is difficult to seal off those areas of a roof which abut at sharp angles so that a tight sealing overlap can be obtained. The sheeting material itself, while flexible, is relatively rigid and does not adapt itself to contoured surfaces, particularly when the contours are defined by sharp changes of direction.
Also, numerous protrusions exist on a roof, such as, drains, vents, air-conditioning units, expansion joint covers, and the like.
Conventional methods for attempting these difficult-to-cover points of overlap or non-overlap include the use of asphaltic flashing cement. However, where roofing material containing modified bitumen is used, the roofer takes a portion of the roofing material, makes it into a roll shape, and heats the end of the roll attempting to melt whatever modified bitumen is there onto a spot location which is to be sealed. However, this method is inefficient for a number of reasons. Firstly, since the sheet is a laminate of several different materials, the bitumen or asphaltic layer makes up only a small portion of the roof sheeting and even with melting or softening the bitumen portion, one does not obtain a significant amount of melted bitumen. In addition, the rolled-up sheeting is difficult to handle and does not adapt itself easily for spot placement of molten or softened bitumen. Moreover, if it is desired merely to soften the bitumen and rub it onto a particular area, only an insufficient amount of bitumen can actually be smeared onto the area to be coated since the bitumen layer is not entirely at the surface of the sheeting.
As a result, such relatively crude attempts to spot-coat those areas which are difficult to seal with conventional roof sheeting are time consuming and inefficient. Moreover, because of the poor delivery of molten or softened bitumen to the desired area, such seals are very often incomplete. The same problems exist when it is desired to seal cracks in driveways., walls and the like, where the area is relatively small or difficult to reach.
SUMMARY OF THE INVENTION
We have discovered a device and method for its use which provides a highly facile and efficient means for sealing those difficult-to-reach or -coat areas of a roof or other surfaces, e.g., a driveway, wall, etc. More particularly, the present invention comprises a device which can be used for the spot application of molten asphaltic composition to such surfaces which is composed of solid, modified bitumen in the shape of an elongated rod. The rod may have an approximately square, triangular or cylindrical cross section and is sufficiently small to be held in the hand. The end of the rod can then be heated to melt or soften the bitumen at the very end and deliver the molten or softened bitumen to the selected spot location.
As a result of the present invention, it becomes very easy for the worker to seal those joints and severely contoured areas merely by melting the bitumen at the end of the rod and applying it to a very selective area desired to be coated and sealed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 (a) and 1 (b) show flashing sticks in accordance with the present invention.
FIG. 2 shows a holder in accordance with the present invention.
FIGS. 3(a) and 3(b) depict the method for applying bitumen to a roof utilizing the device and holders in accordance with of the present invention.
FIGS. 4 and 5 depict cross-section embodiments of molds for preparing the rod of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The asphaltic rod of the present invention is generally composed of asphalt modified by polymer additives, such as, polyolefins or styrene-butadiene, butyl rubber; styrene-ethylene-butylene-styrene block polymer (SEBS), styrene-butadiene polymer (SBR), or styrene-butadiene-styrene block copolymer. The rod can be produced by either molding or extrusion.
Typical compositions for flashing rods in accordance with the present invention include the following:
Composition No. 1
approx. 0-8% Isotactic polypropylene
0-20% Atactic polypropylene
0-20% Ethylene propylene copolymer
0-20% Filler
remainder Asphalt
Composition No. 2
approx. 3-20% Styrene butadiene block polymer (SBS)
0-60% Filler
remainder Asphalt
Particularly preferred is the following composition which exhibits improved weatherability:
Composition No. 3
approx. 3-20% Styrene-ethylene-butylene-styrene block
copolymer (SEBS)
approx. 0-60% Filler
remainder Asphalt
(All percents are by weight based on the weight of the total composition)
Preferably, the asphalt used meets the requirements specified for A.S.T.M. standard AC-5. Typically, asphalts, e.g., Indiana Farm Bureau AC-5 asphalts having a softening point (S.P.) from about 80° to 180° F. and a penetration at 25° C. of from 60 to 200 dmm are suitable. The S.P. is determined by A.S.T.M. D36 and the penetration by A.S.T.M. D5. The asphalts can have a viscosity of from 1,200 to 2,000 cps at 210° F. as determined by A.S.T.M. D4402.
The preferable filler used is limestone. However, other conventional fillers, e.g., stone dust, sawdust, mica, talc, pearlite, vermiculite, clay and the like may be used.
In addition, the composition may contain additives, such as, antioxidants, e.g., high molecular weight hindered phenolics (an example is the product Irganox 1010 produced by Ciba-Geigy); ultra-violet stabilizers, e.g., hindered amine light stabilizers (Spinuvex A-36 produced by Borg-Warner Chemicals, Inc.); carbon black, and zinc oxide; and ultraviolet screens, e.g., titanium dioxide.
The composition is molded into an elongated rod having the desired cross-sectional shape, e.g., square, rectangular, triangular or circular, of a size which can be easily handled by a roofer or other operator.
In addition, a variety of different types of holding devices may be used for holding the rod while it is being heated. FIG. 2 shows an appropriate application or holding device composed of a handle "10", a protector shield "12", and an elongated pin "14". As shown in FIG. 3(a), the pin is inserted longitudinally through the flashing rod so as to engage it on the pin "14".
An alternative type holder is shown in FIG. 3(b) which comprises a handle "16" and a spring-clamp tong "18" which has tong portions "20" which engage the rod to hold it firmly in place. In addition, a so-called "hot-melt" gun can be used, e.g., Model No. 240, manufactured by Hardman, Inc.
In use, as shown in FIGS. 3(a) and 3(b), the roofer or operator merely holds the handle of the application tool while heating, as with the torch, the exposed end of the flashing. This end of the rod is held close to that area of the roof which it is intended to seal or coat. The molten bitumen may then be allowed to drip directly onto the area to be coated. Alternately, the bitumen can be merely softened and smeared onto the desired spot location.
The rod of the present invention can be formed by extrusion. However, a particularly advantageous method for producing the inventive rod is to prepare the composition and melt it, usually at temperatures of about 340° to 390° F. The molten material is then poured into the molds and cooled. The inventors have discovered a very desirable method wherein the molds are made of a disposable material, such as, cardboard and the like. The interior surface of the mold, i.e., that surface which contacts the molten material, is treated or coated in a manner so as to impart release properties to it. Such treatments and/or release coatings are well known and conventional in the art.
Such cardboard molds are relatively inexpensive and disposable. As a result, the mold can serve a two-fold purpose, namely, as a means for preparing the rods and as a packaging or protective cover for the rod during storage prior to use. Also, the use of such a disposable mold allows a large number of rods to be manufactured at a single time and, upon cooling, the rods in the cardboard covering can be separated into any given number and sold as a unit. Thus, it may be most desirable for the purchaser to buy the rods in units of 3, 4 or 5 at a time. The cardboard covering (mold) can be designed such that each individual rod is easily separated while in the cardboard from the next adjacent mold, as by having perforations in the cardboard.
Typical molds are depicted in FIGS. 4 and 5. The mold in FIG. 4 allows for the preparation of rectangular or square shaped rods. Thus, the bituminous melt is poured into the chamber 40 of the cardboard mold. The chambers 42 are rectangular or square, being separated by partition sections depicted as 44. Moreover, partitions 44 may have perforations or a breakable score-line running longitudinally, i.e., parallel to the axis of the rod, so that each container section 40 may be easily separated from those adjacent to it. In FIG. 5, another embodiment of the cardboard or disposable mold is shown which produces rods having a triangular cross-section. In this case, the perforations or breakable score-lines would be along the top intersection indicated as 52. This particular embodiment has an additional advantage in that the mold itself is easily foldable, i.e., in an accordion-like fashion so that it can be stored in a minimal space. Also, because it has less score-lines, it is easier to manufacture.
In both of the embodiments shown in FIG. 4 and FIG. 5, it is possible to break the rods into units of 3, 4, 5, etc., which might be more preferable from the standpoint of sales to the end user. Individual rods can then be removed merely by breaking along the score-lines represented by numerals 44 in FIG. 4 or 52 in FIG. 5.
Since the flashing rod does have a somewhat tacky surface, it can be coated with a thin polymeric sheet, such as, a polyolefin sheeting, to keep it from sticking prior to use. Such a polyolefin film would melt during application and would present no interference with the actual application of the molten or softened bitumen Of course, if the rod is produced in the disposable mold as discussed hereinabove, the mold material, e.g., cardboard layer, can serve as the protective layer.
As a result of the present invention, it is possible with such an asphaltic flashing rod, used either in conjunction with or without an appropriate application tool, to apply molten or softened bitumen to very small, selected, spot locations on a roof or other surface so as to quickly and efficiently effect sealing and coating of difficult-to-reach and/or highly contoured areas, e.g., corners and the like, or small cracks in driveways, walls and the like. As a result, the rod of the present invention is particularly suited for use by home owners doing repairs by themselves.
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A device for the spot application of molten asphaltic composition to spot locations comprising a rod of solid, modified bitumen adapted for heating and end thereof. The softened or molten composition at the end can easily and conveniently be delivered to spot locations.
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FIELD OF THE DISCLOSURE
[0001] The present subject matter generally relates to clinical care plan for patients. More particularly, but not exclusively, the present disclosure discloses a method and a system for determining plausibility of a clinical care plan.
BACKGROUND
[0002] Clinical care plans or treatment plans is designed to help in managing treatments, hospital resources and financial aspects of patients. In such a plan, some of the actions may overlap, some actions may have dependencies on other past actions and some of them may be contraindicating with respect to the given patient.
[0003] Most of these tasks of identifying dependencies, overlapping and contra indicators in the actions are done manually by medical staff, which depends on his/her skills and knowledge. Further, once the plan is devised it is important to adapt the clinical care plans to each individual. Thus, once the clinical care plan is devised it is important to do plausibility check on the actions present in it. Doing this manually is time consuming and leads to ineffective plans.
[0004] The conventional techniques checks for plausibility for each action in the clinical care plans but treats each of the action independently. And also does not associate the actions with the previous action in the plan. Hence, they fail to check for plausibility considering the effect of previous actions that were taken in the care plans before the current action. The effect of the previous action is necessary in analyzing how they would affect the next actions in the plan. Also, in some of the conventional techniques the clinical care plans of a previous patient are used to derive a clinical care plan for a current patient for the similar action. However, the effects the clinical care plan differ from patient to patient and hence those clinical care plans are not effective.
SUMMARY
[0005] Disclosed herein is a method and system for determining plausibility of a clinical care plan. The clinical care plans are retrieved from a care plan document. The clinical care plan comprises of plurality of clinical actions. Each clinical action is associated with quantitative factors and quantitative values which would affect the clinical action and which get affected due to the execution of the clinical action. The quantitative factors and the quantitative values are extracted from health care documents. The quantitative factors and the quantitative values which affect a current clinical action are compared with quantitative factors and the quantitative values which were affected due to the execution of a previous clinical action. Based on the comparison, each clinical action is checked for plausibility and thereafter overall plausibility of the clinical care plan is determined.
[0006] Embodiments of the present disclosure disclose a method for determining plausibility of a clinical care plan. The method comprising retrieving, by a care plan indication system, a relevant health care document from a plurality of health care documents and a relevant care plan document from a plurality of care plan documents based on user details, wherein the plurality of care plan documents comprises one or more clinical actions. The method also comprises extracting one or more first quantitative factors affecting each of the one or more clinical actions and corresponding first quantified values and one or more second quantitative factors affected from execution of each of the one or more clinical actions and corresponding second quantified values. Upon retrieving the relevant health care document and the relevant care plan document, each of the one or more first quantitative factors of a current clinical action is compared with each of the one or more second quantitative factors of a previous clinical action. Also, first quantified value corresponding to each of the one or more first quantitative factors of the current clinical action is compared with the second quantified value corresponding to each of the one or more second quantitative factors of the previous clinical action. Further a value from a predefined value is modified when there is match in at least one of the first quantitative factors of the current clinical action and at least one of the second quantitative factors of the previous clinical action and mismatch in the first quantified value and the second quantified value of the matched at least one the first quantitative factors and the second quantitative factors. Upon modifying the value, the plausibility of the current clinical action is detected when a total value is equal to the predefined value, thereby determining the plausibility of the clinical care plan.
[0007] Embodiments of the present disclosure disclose a system for determining plausibility of a clinical care plan. The system comprises a processor and memory communicatively coupled to the processor, wherein the memory stores the processor-executable instructions, which, on execution, causes the processor to retrieve a relevant health care document from a plurality of health care documents and a relevant care plan document from a plurality of care plan documents based on user details, wherein the plurality of care plan documents comprises one or more clinical actions. The instructions also causes the processor to extract one or more first quantitative factors affecting each of the one or more clinical actions and corresponding first quantified values and one or more second quantitative factors affected from execution of each of the one or more clinical actions and corresponding second quantified values. Upon retrieving the relevant health care document and the relevant care plan document, the processor compares the one or more first quantitative factors of a current clinical action with each of the one or more second quantitative factors of a previous clinical action. The processor also compares first quantified value corresponding to each of the one or more first quantitative factors of the current clinical action with the second quantified value corresponding to each of the one or more second quantitative factors of the previous clinical action. Thereafter, the processor modifies a value from a predefined value when there is match in at least one of the first quantitative factor of the current clinical action and at least one of the second quantitative factor of the previous clinical action and mismatch in the first quantitative value and the second quantitative value of the matched at least one the first quantitative factor and the second quantitative factor. Further, the processor detects plausibility of the current clinical action when a total value is equal to the predefined value, thereby determining the plausibility of the clinical care plan.
[0008] The foregoing summary is illustrative only and is not intended to be in any way limiting. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features will become apparent by reference to the drawings and the following detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate exemplary embodiments and, together with the description, serve to explain the disclosed principles. In the figures, the left-most digit(s) of a reference number identifies the figure in which the reference number first appears. The same numbers are used throughout the figures to reference like features and components. Some embodiments of system and/or methods in accordance with embodiments of the present subject matter are now described, by way of example only, and with reference to the accompanying figures, in which:
[0010] FIGS. 1 a -1 b illustrates exemplary environment for determining plausibility of clinical care plans in accordance with some embodiments of the present disclosure;
[0011] FIG. 1 c shows exemplary representation of sequence of clinical actions of a clinical care plan in accordance with some embodiments of the present disclosure;
[0012] FIG. 2 shows detailed block diagram of a care plan indication system in accordance with some embodiments of the present disclosure;
[0013] FIGS. 3 a -3 b shows exemplary representation of a segment in the clinical care plan and its associated quantitative factors and quantified values in accordance with some embodiments of the present disclosure;
[0014] FIG. 4 shows a flowchart illustrating a method for determining plausibility of a clinical care plan in accordance with some embodiments of the present disclosure;
[0015] FIG. 5 shows a flowchart illustrating a method for determining availability of alternate clinical actions in accordance with some embodiments of the present disclosure; and
[0016] FIG. 6 shows a flowchart illustrating a method for validating the clinical care plan suggested by healthcare professionals in accordance with some embodiments of the present disclosure.
[0017] It should be appreciated by those skilled in the art that any block diagrams herein represent conceptual views of illustrative systems embodying the principles of the present subject matter. 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 executed by a computer or processor, whether or not such computer or processor is explicitly shown.
DETAILED DESCRIPTION
[0018] In the present document, the word “exemplary” is used herein to mean “serving as an example, instance, or illustration.” Any embodiment or implementation of the present subject matter described herein as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments.
[0019] While the disclosure is susceptible to various modifications and alternative forms, specific embodiment thereof has been shown by way of example in the drawings and will be described in detail below. It should be understood, however that it is not intended to limit the disclosure to the particular forms disclosed, but on the contrary, the disclosure is to cover all modifications, equivalents, and alternative falling within the scope of the disclosure.
[0020] The terms “comprises”, “comprising”, or any other variations thereof, are intended to cover a non-exclusive inclusion, such that a setup, device or method that comprises a list of components or steps does not include only those components or steps but may include other components or steps not expressly listed or inherent to such setup or device or method. In other words, one or more elements in a system or apparatus proceeded by “comprises . . . a” does not, without more constraints, preclude the existence of other elements or additional elements in the system or apparatus.
[0021] In the following detailed description of the embodiments of the disclosure, reference is made to the accompanying drawings that form a part hereof, and in which are shown by way of illustration specific embodiments in which the disclosure may be practiced. These embodiments are described in sufficient detail to enable those skilled in the art to practice the disclosure, and it is to be understood that other embodiments may be utilized and that changes may be made without departing from the scope of the present disclosure. The following description is, therefore, not to be taken in a limiting sense.
[0022] As used herein, the term “plausibility” or “plausible” refers to worth of being accepted or believable, the term “clinical care plan” refers to a treatment plan indicated or suggested by any health care unit/health care personnel such as hospitals, clinics, doctors etc., the term “clinical actions” refers to sequence of actions or operations to be performed during the treatment, the term “quantitative factors” either first quantitative factor or second quantitative factor refers to those which quantifies validity of the clinical actions in the clinical care plan for example medical vital status, blood components, effect on body parts (Ex: tumor swelling), hormonal fluids, Enzyme secretions, physiological factors etc.
[0023] FIGS. 1 a -1 b illustrates exemplary environment for determining plausibility of clinical care plans in accordance with some exemplary embodiments of the present disclosure. The environment 100 comprises one or more patient data sources, patient data source 1 101 1 to patient data source N 101 n (collectively referred as patient data sources 101 ), a communication network 103 , one or more databases for example database 1 105 1 and database 2 105 2 (collectively referred as database/databases 105 ) and a care plan indication system 107 . In an embodiment, the care plan indication system 107 may be configured as a module which may be used by hospitals, clinics or any health care units/health care personnel for determining the plausibility of the clinical care plans. In other embodiment, the care plan indication system 107 may be configured as a separate entity for example as a server and the hospitals or the clinics may be interfaced to avail the services of the care plan indication system 107 . The care plan indication system 107 receives user/patient details from the one or more patient data sources 101 . The user details comprise personal information and medical information of the user. As an example, the personal details may include, but not limited to name, demography information, contact information, care takers information etc. As an example, the medical information may include allergies of the user, current medical symptoms of the user, previous health history of the user and physiology of the user. The one or more patient data sources 101 may include but not limited to a hospital, a clinic, a health care unit and a communication device associated with the user wherein the user may directly provide the information to the care plan indication system 107 . The communication network 103 may be a wired or wireless network.
[0024] The care plan indication system 107 is associated with the one or more databases 105 . In an exemplary embodiment, the database 1 105 1 stores plurality of health care documents and the database 2 105 2 stores plurality of care plan documents as shown in the FIG. 1 a . In an embodiment, there may be a single database 105 for storing both the health care documents and the care plan documents. The databases 105 may be hosted in a cloud environment as shown in FIG. 1 a or may be hosted in the care plan indication system 107 itself as shown in FIG. 1 b.
[0025] The health care documents may include, but not limited to, information related to one or more diseases, related symptoms, corresponding treatments, list of diseases identified and summary of treatment, administrative and billing data, patient demographics, progress notes, vital signs, medical histories, diagnoses, medications, immunization dates, allergies, radiology images, lab and test results. The health care documents also comprise information related to quantitative factors and quantified values associated with each clinical action. The quantitative factors are those which quantify the validity of the clinical action. The care plan documents may comprise information related to one or more clinical care plans suggested/recommended by the health care units/health care personnel. The clinical care plan is a sequence of operation to be performed for treatment of the disease. As an example, the patient may be suffering from a chest pain. The doctor may have suggested a clinical care plan to cure the chest pain. The clinical care plan may comprise one or more actions/operations. The one or more actions in the given clinical care plan may be as shown in FIG. 1 c . Each circle in the clinical care plan indicates an action or an operation to be performed.
[0026] FIG. 2 shows a detailed block diagram of a care plan indication system in accordance with some embodiments of the present disclosure.
[0027] The care plan indication system 107 comprises an Input/output (I/O) interface 109 , a memory 111 and a processor 113 . The I/O interface 109 is configured to provide an interface with the one or more databases 105 and the plurality of patient data sources 101 . Through the I/O interface 109 , the care plan indication system 107 receives the user data, the health care documents and the care plan documents. In one embodiment, the care plan indication system 107 may retrieve only relevant health care documents and the care plan documents based on the user details i.e only those documents are retrieved which are applicable to the given user based on the details of the user. As an example, the user may be suffering from a chest pain and in the user details, the symptoms of chest pain would have been indicated. In this scenario, the health care document comprising information related to the qualitative factors such as blood sugar, body temperature and its corresponding quantified values would only be extracted. Similarly, the care plan document which comprises a care plan related to the treatment of the disease chest pain would only be retrieved. In another embodiment, all the documents may be retrieved from the databases 105 and later extract only those documents which are relevant for the given user based on the user details. In some other embodiments, the relevant health care documents and the care plan documents may also be provided to the care plan indication system 107 from the health care personnel such as doctors. The retrieved relevant health care document and the care plan documents are stored in the memory 111 . The received user details are also stored in the memory 111 . The processor 113 determines plausibility of the clinical care plan by determining plausibility of each clinical action in the clinical care plan.
[0028] In one implementation, the care plan indication system 107 receives the user data from the one or more patient data sources 101 and receives the health care documents and the care plan documents from the one or more databases 105 . In one embodiment, data 203 stored in the memory 111 comprises the patient/user data 205 , health care documents 207 , care plan documents 209 , quantitative factors data 211 , quantified values data 215 and other data 219 . In the illustrated FIG. 2 , modules 221 are described here in detail.
[0029] In one embodiment, the data 203 may be stored in the memory 111 in the form of various data structures. Additionally, the aforementioned data can be organized using data models, such as relational or hierarchical data models. The other data 219 may store data, including temporary data and temporary files, generated by modules 221 for performing the various functions of the care plan indication system 107 .
[0030] In an embodiment, the user data 205 comprises information related to personal details of the user and the medical details of the user. As an example, the personal details may include, but not limited to name, demography information, contact information, care takers information etc. As an example, the medical information may include allergies of the user, current medical records of the user, previous health history of the user and physiology of the user.
[0031] In an embodiment, the health care documents 207 , may include but not limited to, information related to one or more diseases, symptoms, corresponding treatments list of diseases identified and treated summary of treatment, administrative and billing data, patient demographics, progress notes, vital signs, medical histories, diagnoses, medications, immunization dates, allergies, radiology images, lab and test results. The health care documents 207 also comprise information related to quantitative factors which affect the clinical action and gets affected during execution of the clinical action. The quantitative factors quantify the validity of the clinical actions. The health care documents 207 also comprise information related to quantified values corresponding to each quantitative factor. The quantified values may be one of normal, increased or decreased.
[0032] In an embodiment, the care plan documents 209 comprise information related to one or more clinical care plans suggested by the doctors for a particular disease. The clinical care plan may comprise one or more actions/operations.
[0033] In an embodiment, the quantitative factors data 211 comprises information of quantitative factors associated with each clinical action in the clinical care plan. The quantitative factors are categorized into first quantitative factors and the second quantitative factors. The first quantitative factors are those which affect the execution of the action and the second quantitative factors are those which get affected due to execution of the clinical action.
[0034] In an embodiment, the quantified values data 215 comprises values corresponding to each quantitative factor associated with the clinical action. The quantified values are one of normal, increased and decreased. The normal value is the predefined value which is defined in the health care document and which may vary from one user to another user. The increased and the decreased values are identified with respect to the normal as the base value.
[0035] In an embodiment, the data stored in the memory 111 is processed by the modules 221 of the care plan indication system 107 . The modules 221 may be stored within the memory 111 . In an example, the modules 221 , communicatively coupled to the processor 113 configured in the care plan indication system 107 , may also be present outside the memory 111 as shown in FIG. 2 and implemented as hardware. As used herein, the term module refers to an application specific integrated circuit (ASIC), an electronic circuit, a processor (shared, dedicated, or group) and memory that execute one or more software or firmware programs, a combinational logic circuit, and/or other suitable components that provide the described functionality.
[0036] In an embodiment, the modules 221 may include, for example retrieving module 222 , extracting module 223 , detecting module 225 and other modules 235 . The other modules 235 may be used to perform various miscellaneous functionalities of the care plan indication system 107 . It will be appreciated that such aforementioned modules 221 may be represented as a single module or a combination of different modules 221 .
[0037] In an embodiment, the retrieving module 222 retrieves a relevant care plan document from a plurality of care plan documents and a relevant health care document from the plurality of health care documents based on the user details. The relevant care plan document comprises one or more clinical actions.
[0038] In an embodiment, the extracting module 223 extracts one or more first quantitative factors affecting each of the one or more clinical actions and corresponding first quantified values and one or more second quantitative factors affected from execution of each of the one or more clinical actions and corresponding second quantified values from the relevant health care document. As an example, the quantitative factors and the corresponding quantified values may be extracted using NLP techniques such as numerical attribute extraction.
[0039] In an embodiment, the detecting module 225 detects the plausibility of each clinical action in the clinical care plan. The process of detecting the plausibility of each clinical action is described with the help of an example as illustrated below.
Exemplary Embodiment
[0040] Consider an example of a patient visiting the hospital with symptoms of chest pain. One of the clinical care plans (hypothetical) for the treatment of chest pain is as shown in FIG. 1 c . Each circle in the clinical care plan represents an action/operation.
[0041] Consider a segment, segment 1 of the clinical care plan as shown in FIG. 3 a which contains two actions namely “open heart surgery” 301 and “barbiturates for sleep” 303 . The action “barbiturates for sleep” 303 is a current clinical action and the action “Open Heart surgery” 301 is a previous clinical action.
[0042] The extracting module 223 extracts the first quantitative factors and the corresponding first quantitative values for the action “open heart surgery” 301 as shown in the below Table 1. The first quantitative factors are the factors which affect the execution of the action “open heart surgery” 301 i.e these factors have to be monitored or should be under control for performing the action “open heart surgery” 301 . As an example the first quantitative factors are “blood sugar”, body temperature” and blood culture value”.
[0000]
TABLE 1
First Quantitative Factor
First Quantified value
Blood Sugar
Normal
Body Temperature
Normal
Blood Culture
Normal
[0043] Similarly, the extracting module 223 extracts the first quantitative factors and the corresponding first quantified values for the action “Barbiturates for sleep” 303 as shown in the below Table 2. As an example, the first quantitative factors are “blood sugar”, “body temperature” and “blood culture.
[0000]
TABLE 2
First Quantitative Factor
First Quantified value
Blood Pressure
Normal
Blood Culture
Normal
Body temperature
Normal
[0044] Further, the extracting module 223 extracts the second quantitative factors and corresponding second quantified values which would get affected by the execution of the action “open heart surgery” 301 i.e these factors may get affected when the open heart surgery is performed. For example, the blood sugar level of the patient may increase or the patient may experience a chest pain or muscle pain etc. Those second quantitative factors and the corresponding second quantified values are as shown in the below Table 3.
[0000]
TABLE 3
Second Quantitative Factor
Second Quantified value
Blood Sugar
Increased
Chest pain
Increased
Muscle pain
Increased
[0045] Similarly, the extracting module 223 extracts the second quantitative factors which would get affected by the execution of the action “Barbiturates for sleep” 303 . Those second quantitative factors and the corresponding second quantified values are as shown in below Table 4.
[0000]
TABLE 4
Second Quantitative Factor
Second Quantified value
Muscle pain
Reduced
Body Temperature
Reduced
Breathing
Reduced
[0046] FIG. 3 b shows an exemplary representation of the segment 1 with the list of first quantitative factors and the corresponding first quantified values 305 and 307 associated with the action “open heart surgery” 301 and “barbiturates sleep” respectively and the list of second quantitative factors and the corresponding second quantified values 309 and 311 associated with the action “open heart surgery” 301 and “barbiturates sleep” respectively.
[0047] In an embodiment the detecting module 225 compares each of the one or more first quantitative factors of the current clinical action with each of the one or more second quantitative factors of the previous clinical action i.e the detecting module 225 compares each of the one or more first quantitative factors of the current clinical action “Barbiturates for sleep” 303 with each of the one or more second quantitative factors of the previous clinical action “Open heart surgery” 301 .
[0048] The detecting module 225 also compares the first quantified value corresponding to each of the one or more first quantitative factors of the current clinical action i.e “Barbiturates for sleep” 303 with the second quantified value corresponding to each of the one or more second quantitative factors of the previous clinical action i.e “open heart surgery” 301 .
[0049] Based on comparison the detecting module 225 modifies a value from a predefined value when there is match in at least one of the first quantitative factors of the current clinical action and at least one of the second quantitative factors of the previous clinical action and mismatch in the first quantified value and the second quantified value of the matched at least one the first quantitative factors and the second quantitative factors. The detecting module 225 may implement matching techniques/algorithms which includes, but not limited to, NLP or semantic analysis, for matching the quantitative factors. It should be understood by those skilled in the art that any other matching technique may be used in the present invention to match the quantitative factors based on which the plausibility of the clinical action would be detected. As an example, the first quantitative factors of the current clinical action may be “blood sugar” “body temperature” and “blood culture” and the second quantitative factors of the previous clinical action may be “blood sugar”, “muscle pain” and “chest pain”. One of the first quantitative factors of the current clinical action i.e “blood sugar” is same as one of the second quantitative factors of the previous clinical action i.e “blood sugar”. Since these factors are same there is a match between these factors. In a similar way, when the quantified values are same then there is a match between the quantified values as well. Further, the term “mismatch” is used when the factors are not same or when the quantified values are not same.
[0050] The predefined value may vary from one user to another user. The predefined value as an example may be zero. In a non-limiting embodiment, the predefined value may be any positive integer or a negative integer as well. In each comparison, the value is modified.
[0051] In an embodiment, modifying the value comprises one of decrementing or incrementing the value from the predefined value when there is match in at least one of the first quantitative factors of the current clinical action and at least one of the second quantitative factors of the previous clinical action and mismatch in the first quantified value and the second quantified value of the matched at least one the first quantitative factors and the second quantitative factors.
[0052] In an embodiment, the predefined value is retained when there is mismatch in at least one of the first quantitative factors of the current clinical action and at least one of the second quantitative factors of the previous clinical action.
[0053] In an embodiment, the predefined value is retained when there is match in at least one of the first quantitative factors of the current clinical action and at least one of the second quantitative factors of the previous clinical action and match in the first quantified value and the second quantified value of the matched at least one the first quantitative factors and the second quantitative factors.
[0054] The Table 5 below shows the process of comparison of the quantitative factors and the quantified values involved in the segment 1 .
[0000]
Value (predefined Value is
Step
Comparison
zero)
1
Increased blood sugar with Normal
Value = −1
Blood sugar
Contraindication found
(increased != Normal)
hence Value is decreased
2
Increased blood sugar with Normal
Value = −1 (No change)
Body Temperature
(No match in quantitative
factors)
(Blood sugar != Body
temperature)
3
Increased blood sugar with Normal
Value = −1 (No change)
Blood culture
(No match in quantitative
factors)
(Blood sugar != Blood
culture)
4
Increased Chest pain with Normal
Value = −1 (No change)
Blood sugar
(No match in quantitative
factors)
5
Increased Chest pain with Normal
Value = −1 (No change)
Body Temperature
(No match in quantitative
factors)
6
Increased Chest pain with Normal
Value = −1 (No change)
blood culture
(No match in quantitative
factors)
7
Increased Muscle Pain with Normal
Value = −1 (No change)
Blood sugar
(No match in quantitative
factors)
8
Increased Muscle Pain with Normal
Value = −1 (No change)
Body Temperature
(No match in quantitative
factors)
9
Increased Muscle Pain with Normal
Value = −1 (No change)
blood culture
(No match in quantitative
factors)
[0055] In the “Step 1”, there is match in the quantitative factors but there is mismatch in the quantified values and hence the value is modified. The value may either be incremented or decremented from the predefined value and accordingly the plausibility of the clinical care plan is determined. As an example, in this scenario the value is decremented from the predefined value. The reduced value is “−1”.
[0056] In the “Step 2” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0057] In the “Step 3” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0058] In the “Step 4” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0059] In the “Step 5” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0060] In the “Step 6” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0061] In the “Step 7” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0062] In the “Step 8” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0063] In the “Step 9” there is mismatch in the quantitative factors and hence the value is modified. The value is decremented from the predefined value. The reduced value is “−1”.
[0064] In an embodiment, the detecting module 225 detects plausibility of the current clinical action when a total value is equal to the predefined value. In an embodiment, the total value is determined based on sum of the value identified in each comparison i.e each step. The non-plausibility of the current clinical action is detected when the total value is less than the predefined value or more than the predefined value. In this scenario, the total value is a negative integer. Since the total value is a negative integer, the action “Barbiturates for sleep” is detected as a non-plausible action.
[0065] The detecting module 225 detects plausibility of the clinical care plan upon detecting plausibility or non-plausibility of each clinical action in the clinical care plan. If there is even one clinical action which is non-plausible, then the clinical care plan would be determined as non-plausible.
[0066] In an embodiment, upon detecting plausibility of the clinical actions, the detecting module 225 checks for availability of alternate clinical actions. If the alternate clinical action is available, the extracting module 223 extracts the alternate clinical action and replaces with the non-plausible clinical action. Thereafter, the detecting module 225 determines plausibility of the alternate clinical action. The process of determining the alternate clinical action and checking for plausibility of the alternate clinical action continues until all the clinical actions in the clinical care plan is plausible so that the clinical care plan is plausible for treating the patient.
[0067] FIG. 4 shows a flowchart illustrating a method for determining plausibility of a clinical care plan in accordance with some embodiments of the present disclosure.
[0068] As illustrated in FIG. 4 , the method 400 comprises one or more blocks illustrating a method for determining plausibility of a clinical care plan. The method 400 may be described in the general context of computer executable instructions. Generally, computer executable instructions can include routines, programs, objects, components, data structures, procedures, modules, and functions, which perform particular functions or implement particular abstract data types.
[0069] The order in which the method 400 is described is not intended to be construed as a limitation, and any number of the described method blocks can be combined in any order to implement the method. Additionally, individual blocks may be deleted from the methods without departing from the spirit and scope of the subject matter described herein. Furthermore, the method can be implemented in any suitable hardware, software, firmware, or combination thereof.
[0070] At block 401 , the care plan indication system 107 receives user details. The user details comprise personal information and medical information of the user. The user details are received from one or more patient data sources 101 . As an example, the patient data source 101 may be a hospital or any health care unit which would provide details of the user for example medical records of the user, previous health details of the user, user name, user address and contact details of the user, information related to care takers of the user etc. The user may also provide the details through a computing device associated with the user such as a mobile phone or a tablet.
[0071] At block 403 , the care plan indication system 107 retrieves a relevant health care document 207 and a relevant care plan document 209 based on the user details. The care plan document 209 comprises information related to one or more clinical care plans. Each clinical care plan comprises one or more clinical actions. The clinical care plan is basically a treatment plan for treating the user based on the disease identified. The one or more clinical actions are the sequence of actions to be performed for treatment of the disease.
[0072] At block 405 , the care plan indication system 107 identifies a clinical care plan from the one or more clinical care plans which are best suited for the user.
[0073] At block 407 , the care plan indication system 107 extracts first quantitative factors and corresponding first quantified values and second quantitative factors and corresponding second quantified values from the relevant health care document 207 for each clinical action in the clinical care plan. The first quantitative factors are those which affect the execution of the clinical action and the second quantitative factors are those which would get affected due to execution of the clinical action. These factors are considered to check the effect of the same on the action and also check the after effects upon execution of the action. Based on this analysis, the doctors may consider changing the actions in the clinical care plan.
[0074] At block 409 , the care plan indication system 107 determines plausibility of each clinical action in the clinical care plan. The care plan indication system 107 compares each of the one or more first quantitative factors of the current clinical action with each of the one or more second quantitative factors of the previous clinical action. Further, the care plan indication system 107 also compares the first quantified value corresponding to each of the one or more first quantitative factors of the current clinical action with the second quantified value corresponding to each of the one or more second quantitative factors of the previous clinical action.
[0075] Based on the comparison, the care plan indication system 107 modifies a value from a predefined value when there is match in at least one of the first quantitative factors of the current clinical action and at least one of the second quantitative factors of the previous clinical action and mismatch in the first quantified value and the second quantified value of the matched at least one the first quantitative factors and the second quantitative factors. Further, the care plan indication system 107 detects plausibility of the current clinical action when a total value is equal to the predefined value. In an embodiment, if the total value is less than the predefined value or more than the predefined value then the clinical action is detected as non-plausible.
[0076] At block 411 , the care plan indication system 107 determines plausibility of the clinical plan based on plausibility of the clinical actions in the clinical care plan. If all the clinical actions in the clinical care plan are plausible then the clinical care plan is determined as plausible.
[0077] FIG. 5 shows a flowchart illustrating a method for determining availability of alternate clinical actions in accordance with some embodiments of the present disclosure.
[0078] As illustrated in FIG. 5 , the method 500 comprises one or more blocks illustrating a method for determining availability of alternate clinical actions. The method 500 may be described in the general context of computer executable instructions. Generally, computer executable instructions can include routines, programs, objects, components, data structures, procedures, modules, and functions, which perform particular functions or implement particular abstract data types.
[0079] The order in which the method 500 is described is not intended to be construed as a limitation, and any number of the described method blocks can be combined in any order to implement the method. Additionally, individual blocks may be deleted from the methods without departing from the spirit and scope of the subject matter described herein. Furthermore, the method can be implemented in any suitable hardware, software, firmware, or combination thereof.
[0080] At block 501 , the care plan indication system 107 determines plausibility of each clinical action in the clinical care plan.
[0081] At block 503 , the care plan indication system 107 detects plausibility of the clinical action and if the clinical action is plausible, then the method proceeds to block 505 . If the clinical action is not plausible, then the method proceeds to block 507 .
[0082] At block 505 , the care plan indication system 107 updates its dashboard/display interface which displays list of clinical actions which are plausible. The care plan indication system 107 also generates a report comprising information of the clinical actions which are plausible.
[0083] At block 507 , the care plan indication system 107 identifies availability of one or more alternate clinical actions from the care plan document.
[0084] At block 509 , the non-plausible actions are replaced with the available alternate clinical actions.
[0085] At block 511 , the care plan indication system 107 determines plausibility of the available one or more clinical actions. The plausibility is checked based on the process explained in FIG. 4 .
[0086] At block 513 , the care plan indication system 107 updates the dashboard with the plausible clinical actions if the alternative clinical actions are plausible. If not, then the process of detecting the availability of alternative clinical actions and determining plausibility of the same continues till all the clinical actions in the clinical care plan are plausible.
[0087] FIG. 6 shows a flowchart illustrating a method for validating the clinical care plan suggested by healthcare professionals in accordance with some embodiments of the present disclosure.
[0088] As illustrated in FIG. 6 , the method 600 comprises one or more blocks illustrating a method for validating the clinical care plan suggested by healthcare professionals.
[0089] At block 601 , the health care professional may select kind of cases through the I/O interface 109 .
[0090] At block 603 , the care plan indication system 107 provides one or more exemplary and imaginary case studies based on the type of the case. In an embodiment, the imaginary case studies may be pre-stored in the memory 111 or may be generated dynamically. For example, if the healthcare professional has selected the case related to cancer, then the care plan indication system 107 may provide an exemplary case study of a patient being suffered by severe head ache whose final diagnosis is brain cancer.
[0091] At block 605 , the care plan indication system 107 receives the clinical care plan suggested by the health care professional which comprises of one or more clinical actions.
[0092] At block 607 , the care plan indication system 107 detects plausibility of the clinical care plan suggested by the health care professional based on the method illustrated in FIG. 4 .
[0093] At block 609 , the care plan indication system 107 generates a report indicating the one or more actions which are non-plausible and provides the report to the health care professional based on which the health care professional may analyze the error made in suggesting the clinical care plan.
Advantages of Present Disclosure
[0094] Embodiments of the present disclosure provide a method and system for automating the process of determining plausibility of a clinical care plan. Therefore, significantly reduces time.
[0095] Embodiments of the present disclosure provide a system for determining the plausibility of the clinical care plan thereby avoiding manual errors.
[0096] Embodiments of the present disclosure consider effect of a previous clinical action on the current clinical action in order to check for plausibility of the current clinical action. This way, the plausibility determined for the overall clinical action is more efficient and reliable.
[0097] The described operations may be implemented as a method, system or article of manufacture using standard programming and/or engineering techniques to produce software, firmware, hardware, or any combination thereof. The described operations may be implemented as code maintained in a “non-transitory computer readable medium”, where a processor may read and execute the code from the computer readable medium. The processor is at least one of a microprocessor and a processor capable of processing and executing the queries. A non-transitory computer readable medium may comprise media such as magnetic storage medium (e.g., hard disk drives, floppy disks, tape, etc.), optical storage (CD-ROMs, DVDs, optical disks, etc.), volatile and non-volatile memory devices (e.g., EEPROMs, ROMs, PROMs, RAMs, DRAMs, SRAMs, Flash Memory, firmware, programmable logic, etc.), etc. Further, non-transitory computer-readable media comprise all computer-readable media except for a transitory. The code implementing the described operations may further be implemented in hardware logic (e.g., an integrated circuit chip, Programmable Gate Array (PGA), Application Specific Integrated Circuit (ASIC), etc.).
[0098] Still further, the code implementing the described operations may be implemented in “transmission signals”, where transmission signals may propagate through space or through a transmission media, such as an optical fiber, copper wire, etc. The transmission signals in which the code or logic is encoded may further comprise a wireless signal, satellite transmission, radio waves, infrared signals, Bluetooth, etc. The transmission signals in which the code or logic is encoded is capable of being transmitted by a transmitting station and received by a receiving station, where the code or logic encoded in the transmission signal may be decoded and stored in hardware or a non-transitory computer readable medium at the receiving and transmitting stations or devices. An “article of manufacture” comprises non-transitory computer readable medium, hardware logic, and/or transmission signals in which code may be implemented. A device in which the code implementing the described embodiments of operations is encoded may comprise a computer readable medium or hardware logic. Of course, those skilled in the art will recognize that many modifications may be made to this configuration without departing from the scope of the invention, and that the article of manufacture may comprise suitable information bearing medium known in the art.
[0099] The terms “an embodiment”, “embodiment”, “embodiments”, “the embodiment”, “the embodiments”, “one or more embodiments”, “some embodiments”, and “one embodiment” mean “one or more (but not all) embodiments of the invention(s)” unless expressly specified otherwise.
[0100] The terms “including”, “comprising”, “having” and variations thereof mean “including but not limited to”, unless expressly specified otherwise.
[0101] The enumerated listing of items does not imply that any or all of the items are mutually exclusive, unless expressly specified otherwise.
[0102] The terms “a”, “an” and “the” mean “one or more”, unless expressly specified otherwise.
[0103] A description of an embodiment with several components in communication with each other does not imply that all such components are required. On the contrary a variety of optional components are described to illustrate the wide variety of possible embodiments of the invention.
[0104] When a single device or article is described herein, it will be readily apparent that more than one device/article (whether or not they cooperate) may be used in place of a single device/article. Similarly, where more than one device or article is described herein (whether or not they cooperate), it will be readily apparent that a single device/article may be used in place of the more than one device or article or a different number of devices/articles may be used instead of the shown number of devices or programs. The functionality and/or the features of a device may be alternatively embodied by one or more other devices which are not explicitly described as having such functionality/features. Thus, other embodiments of the invention need not include the device itself.
[0105] Finally, the language used in the specification has been principally selected for readability and instructional purposes, and it may not have been selected to delineate or circumscribe the inventive subject matter. It is therefore intended that the scope of the invention be limited not by this detailed description, but rather by any claims that issue on an application based here on. Accordingly, the disclosure of the embodiments 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.
[0106] While various aspects and embodiments have been disclosed herein, other aspects and embodiments will be apparent to those skilled in the art. The various aspects and embodiments disclosed herein are for purposes of illustration and are not intended to be limiting, with the true scope and spirit being indicated by the following claims.
REFERRAL NUMERALS
[0107]
[0000]
Reference
Number
Description
100
Environment
101
Patient data source
103
Communication network
105
Database
107
Care plan indication system
109
I/O interface
111
Memory
113
Processor
205
Patient data
207
Health care documents
209
Care plan documents
211
Quantitative factors data
215
Quantified values data
219
Other data
222
Retrieving Module
223
Extracting Module
225
Detecting Module
235
Other Module
301
Action—open heart surgery
303
Action—Barbiturates Sleep
305
First Quantitative factors and first
quantified values for action “Open heart
surgery”
307
First Quantitative factors and first
quantified values for action
“Barbiturates Sleep”
309
Second Quantitative factors and second
quantified values for action “Open heart
surgery”
311
Second Quantitative factors and second
quantified values for action
“Barbiturates Sleep”
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The present disclosure relates to the field of clinical care plan for patients. More particularly, the present disclosure relates to a method and system for determining plausibility of clinical care plan. The present disclosure checks for plausibility of the clinical care plan determining plausibility of each clinical action in the action plan. The plausibility of a current clinical action is determined by comparing the quantitative factors and its corresponding quantitative values associated with the current clinical action with the quantitative factors and the corresponding quantitative values of the previous clinical action. In the present disclosure, the effects of previous clinical actions are considered for determining plausibility of the current clinical action and hence provide an effective mechanism for determining plausibility of the overall clinical care plan. The present invention substantially reduces the time for determining plausibility of clinical care plan since it is an automated process.
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FIELD OF THE INVENTION
This invention relates, in general, to microchannel plates (MCPs) for use in image intensifier tubes, and in particular, to a microchannel plate having curved channels.
BACKGROUND OF THE INVENTION
Image intensifier tubes are used in night/low light vision applications to amplify ambient light into a useful image. A typical image intensifier tube is a vacuum device, roughly cylindrical in shape, and generally includes a body, photocathode and faceplate, microchannel plate (MCP), and output optic and phosphor screen. Incoming photons are focused on the glass faceplate by external optics, and strike the photocathode that is bonded to the inside surface of the faceplate. The photocathode converts the photons to electrons, which are accelerated toward the MCP by an electric field. The MCP has many microchannels, each of which functions as an independent electron amplifier, and roughly corresponds to a pixel of a CRT. The amplified electron stream, emanating from the MCP, excites the phosphor screen and a resulting visible image is passed through output optics to any additional external optics. The body holds these components in precise alignment, provides electrical connections, and also forms a vacuum envelope.
In general, fabrication of a microchannel plate starts with a fiber drawing process, as disclosed in U.S. Pat. No. 4,912,314, issued Mar. 27, 1990 to Ronald Sink, which is incorporated herein by reference in its entirety. For convenience, FIGS. 1-4, disclosed in U.S. Pat. No. 4,912,314 are included herein and discussed below.
In FIG. 1 , there is shown a starting fiber 10 for the microchannel plate. Fiber 10 includes glass core 12 and glass cladding 14 surrounding the core. Core 12 is made of glass material that is etchable in an appropriate etching solution. Glass cladding 14 is made from glass material which has a softening temperature substantially the same as the glass core. The glass material of cladding 14 is different from that of core 12 , however, in that it has a higher lead content, which renders the cladding non-etchable under the same conditions used for etching the core material. Thus, cladding 14 remains after the etching of the glass core. A suitable cladding glass is a lead-type glass, such as Corning Glass 8161.
The optical fibers are formed in the following manner: An etchable glass rod and a cladding tube coaxially surrounding the rod are suspended vertically in a draw machine which incorporates a zone furnace. The temperature of the furnace is elevated to the softening temperature of the glass. The rod and tube fuse together and are drawn into a single fiber 10 . Fiber 10 is fed into a traction mechanism in which the speed is adjusted until the desired fiber diameter is achieved. Fiber 10 is then cut into shorter lengths of approximately 18 inches.
Several thousands of the cut lengths of single fiber 10 are then stacked into a mold and heated at a softening temperature of the glass to form hexagonal array 16 , as shown in FIG. 2 . The cut lengths of fiber 10 together form a hexagonal configuration. The hexagonal configuration provides a better stacking arrangement.
The hexagonal array, which is also known as a multi assembly or a bundle, includes several thousand single fibers 10 , each having core 12 and cladding 14 . Bundle 16 is suspended vertically in a draw machine and drawn to again decrease the fiber diameter, while still maintaining the hexagonal configuration of the individual fibers. Bundle 16 is then cut into shorter lengths of approximately 6 inches.
Several hundred of the cut bundles 16 are packed into a precision inner diameter bore glass tube 22 , as shown in FIG. 3 . The glass tube has a high lead content and is made of a glass material similar to glass cladding 14 and is, thus, non-etchable by the etching process used to etch glass core 12 . The lead glass tube 22 eventually becomes a solid rim border of the microchannel plate.
In order to protect fibers 10 of each bundle 16 , during processing to form the microchannel plate, a plurality of support structures are positioned in glass tube 22 to replace those bundles 16 which form the outer layer of the assembly. The support structures may take the form of hexagonal rods of any material having the necessary strength and the capability to fuse with the glass fibers. Each support structure may be a single optical glass fiber 24 having a hexagonal shape and a cross-sectional area approximately as large as that of one of the bundles 16 . The single optical glass fiber, however, has a core and a cladding which are both non-etchable. The optical fibers 24 , or support rods 24 , are illustrated in FIG. 3 , as being disposed at the periphery of assembly 30 and surrounding the plurality of bundles 16 . The support rods are also known as filler fibers.
The support rods may be formed from one optical fiber or any number of fibers up to several hundred. The final geometric configuration and outside diameter of one support rod 24 is substantially the same as one bundle 16 . The multiple fiber support rods may be formed in a manner similar to that of forming bundle 16 .
The assembly formed when all support rods 24 have been placed around the ends of bundles 16 is called a boule, and is generally designated as 30 in FIGS. 3 and 5 .
Boule 30 is fused together in a heating process to produce a solid boule of rim glass and fiber optics. The fused boule is then sliced, or diced, into thin cross-sectional plates. The planar end surfaces of the sliced fused boule are ground and polished.
In order to form the microchannels, cores 12 of optical fibers 10 are removed, by etching with dilute hydrochloric acid. After etching the thin plates, the high lead content glass claddings 14 remains to form microchannels 32 , as illustrated in FIG. 4 . Also, support rods 24 remain solid and provide a good transition from the solid rim of tube 22 to microchannels 32 . After the plates are etched to remove the core rods, the channels in the plate are metalized and activated.
The current method of manufacturing an MCP also includes dicing the boule at an angle into thin wafers to produce a bias angle. The wafers are then etched, hydrogen fired to form a conduction layer, and metalized to provide electrical contact. After the boule is sliced into wafers, each wafer is handled individually. A typical size of the wafer is approximately 1 inch diameter.
The microchannels of an MCP each form a generally straight bore extending from input to output surfaces of the MCP. As shown schematically in FIG. 11 , MCP 110 includes input surface 111 and output surface 112 . The microchannels, designated as 113 , are inclined at a bias angle with respect to the opposing input output surfaces. However, each microchannel forms a bore that is substantially centered about a straight axial line extending between the input and output surfaces.
Curved microchannels have been considered as a way of increasing gain of an MCP. Such curved channels have been very tricky and expensive to produce. No known MCP is produced with curved channels, although curved channel electron multipliers have been produced for testing purposes. Two methods are known for making a curved channel MCP. Both methods are described below with respect to FIGS. 6 and 7 .
The first method for making a curved channel MCP is shown in FIG. 6 . As shown, MCP 63 is heated and placed between two horizontally sliding plates, top plate 61 and bottom plate 62 . Each plate is notched to receive approximately one-half of the height of MCP 63 . The top and bottom plates are brought together to completely nestle the MCP. Next, the top plate is slid horizontally with respect to the lower plate. This causes shearing of one end surface of the MCP with respect to the other end surface of the MCP, thereby providing curves to the microchannels. This method requires exceptional temperature control, very accurate movement of the shearing plates, and probably does not produce adequate uniformity for an imaging application.
The second method of making a curved MCP is shown in FIG. 7 . As shown, MCP 73 is sandwiched between two heated plates 71 and 72 . The two closed plates are spun in a counter-clockwise direction (for example). The spinning of the plates produces a centripetal force which pushes the center of the MCP outward. With the exterior surfaces of the MCP fixed by the notches in plates 71 and 72 , it is believed that the result is curved channels in the MCP. Like the first method, this method requires accurate temperature control. This method also substitutes the difficulty of high-speed rotary motion for the problem of high accuracy linear motion. It will be understood, however, that the goal of each of these methods is higher gain, and not reduced light transmission.
SUMMARY OF THE INVENTION
To meet this and other needs, and in view of its purposes, the present invention provides a microchannel plate (MCP) formed from a boule. The MCP includes a plate having opposing end surfaces formed of acid resistant glass and acid etchable glass, and multiple channels extending longitudinally between the opposing end surfaces. The multiple channels are formed by circumferential walls of the acid resistant glass that surround the acid etchable glass. A respective circumferential wall forms a curved surface extending longitudinally between the opposing end surfaces. The curved surface is configured to reduce light from passing from one end surface to the other end surface. The acid resistant glass has a lower softening temperature than the acid etchable glass.
Another embodiment of the present invention includes a boule for forming multiple MCPs. The boule includes core rods formed of acid etchable glass, and cladding glass, surrounding the core rods, formed of acid resistant glass. The core rods and the cladding glass extend longitudinally between ends of the boule, and the core rods are smoothly curved between the ends of the boule. The core rods have a lower softening temperature than the cladding glass. The softening temperature of the core rods is at least 25 degree Centigrade lower than the softening temperature of the cladding glass. As an example, the softening temperature of the core rods is approximately 550 degrees Centigrade and the softening temperature of the cladding glass is approximately 580 degrees Centigrade. The core rods are substantially parallel to each other between the ends of the boule. A core rod forms a portion of a circle intersecting a chord, and the chord is approximately 8 inches in length and the furthest distance from the chord to the circle is approximately 0.4 inches.
Yet another embodiment of the present invention is a mold for bending a boule for making multiple MCPs. The mode includes a structure having a longitudinal direction and a transverse direction, and a notch formed in the structure, extending in the longitudinal direction between ends of the structure. The notch forms a U-shape, oriented in the transverse direction. The U-shape includes a portion of a first circle configured to receive and cradle a boule. The notch forms a portion of a second circle, oriented in the longitudinal direction, configured to impart a bend in the boule having a curved surface similar to the second circle. The structure is configured to receive the boule in a heated state having a first temperature effective in softening cladding glass in the boule, and having a temperature lower than a second temperature effective in softening core rods in the boule.
Still another embodiment of the present invention is a method for curving a boule having core rods and cladding glass surrounding the core rods. The method includes the steps of: heating the boule to a first temperature, wherein the first temperature is effective in softening the cladding glass; and bending the boule and, in turn, bending the core rods. The method also includes the steps of: placing the boule on a mold having a curved surface; and bending the boule after heating to the first temperature, so that the boule conforms to the curved surface. Another step includes dicing the boule to obtain multiple MCPs.
It is understood that the foregoing general description and the following detailed description are exemplary, but are not restrictive, of the invention.
BRIEF DESCRIPTION OF THE FIGURES
The invention may be understood from the following detailed description when read in connection with the following figures:
FIG. 1 is a partial view of a fiber used in fabricating microchannel plates.
FIG. 2 is a partial view of a bundle of fibers shown in FIG. 1 for use in fabricating microchannel plates.
FIG. 3 is a cross-sectional view of a packed boule.
FIG. 4 is a partial cut-away view of a microchannel plate.
FIG. 5 is a perspective view of a boule.
FIG. 6 is a cross-sectional view of an MCP sandwiched between two plates, used for forming a shearing force to bend the channels of the MCP.
FIG. 7 is another cross-sectional view of an MCP sandwiched between two plates, used for forming a centripetal force to bend the channels of the MCP.
FIG. 8 is a functional block diagram of an image intensifier system, in accordance with an embodiment of the present invention.
FIGS. 9A , 9 B and 9 C are different views of a mold used for providing a curvature to the boule shown in FIG. 5 , in accordance with an embodiment of the present invention.
FIG. 10A is a partial cross-sectional view of a boule, before the microchannel etchable rods are subjected to being curved.
FIG. 10B is a partial cross-sectional view of the boule of FIG. 10A , after the microchannel etchable rods are subjected to being curved, in accordance with an embodiment of the present invention.
FIG. 11 is a pictorial of an MCP having straight bores.
FIG. 12 is a pictorial of an MCP having curved bores, in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
An image intensifier includes an MCP disposed between a photocathode and an image sensing device. For example, as schematically shown in FIG. 8 , image intensifier tube 80 includes MCP 91 disposed in vacuum housing 83 between photocathode 90 and image sensing device 92 .
As shown, light energy 82 reflected from object 81 impinges upon photocathode 90 . Photocathode 90 receives the incident energy on input surface 94 and outputs the energy, as emitted electrons, on output surface 95 . The output electrons, designated as 85 , from photocathode 90 , are provided as an input to an electron gain device, such as MCP 91 . The MCP includes input surface 86 and output surface 87 . As electrons bombard input surface 86 , secondary electrons are generated within microchannels 88 of MCP 91 . The MCP generates several hundred electrons for each electron entering input surface 86 .
Although not shown, it will be understood that MCP 91 is subjected to a difference in voltage potential between input surface 86 and output surface 87 , typically over a thousand volts. This potential difference enables electron multiplication. Electrons 89 , outputted from MCP 91 , impinge upon solid state electron sensing device 92 . Electron sensing device 92 may be a CMOS imager, for example, and includes input surface 93 and output surface 96 , as shown in FIG. 8 .
In general, electron sensing device 92 includes a phosphor screen on input surface 93 . The output signals from electron sensing device 92 may be provided to image display 84 by way of a bus, or may be stored in a memory (not shown).
For reasons explained below, in an embodiment of the invention, MCP 91 includes curved microchannels 88 .
Conventional microchannels of an MCP each form a generally straight bore extending from its input surface to its output surface. As shown schematically in FIG. 11 , MCP 110 includes input surface 111 and output surface 112 . The microchannels, designated as 113 , are inclined at a bias angle with respect to the opposing input and output surfaces. Furthermore, each microchannel forms a bore that is substantially centered about a straight axial line extending between input and output surfaces 111 and 112 .
The inventor has discovered that as a result of the straight microchannels, light 114 shown in FIG. 11 is reflected from or generated by a phosphor screen (not shown), re-enters microchannels 113 , and exits the microchannels. Because light 114 propagates as photons from surface 112 to the other surface 111 without reflecting off the channel walls, light 114 is substantially unattenuated at the output surface of microchannels 112 .
The photons, after exiting surface 111 , impinge upon a photocathode (not shown) and are converted into electrons that emanate from the photocathode surface. These electrons are again amplified by the MCP. The phosphor screen converts the amplified electrons from the MCP into light. The phosphor screen is covered with an aluminum reflector layer, but this tends to have a multitude of small holes, and bleeds a small amount of light back towards the MCP. The MCP permits a small amount of light to pass through, and thus some screen light is able to re-activate the photocathode. This represents spatially-disconnected noise, and degrades the tube image.
Due to the intricacies of the screen process, the aluminum reflector layer is difficult to produce without holes. Additionally, there are known tradeoffs to the aluminum reflector thickness and its method of deposition, so reducing light leakage through changes in the screen process is likely to degrade phosphor efficiency, MTF and/or SNR.
In order to reduce light transmission through MCP 91 , the inventor has discovered that curved microchannels, as shown in FIGS. 8 and 12 , reduce the light transmission. Because light 124 ( FIG. 12 ) propagates from surface 87 to surface 86 by reflecting off the walls of microchannels 88 , light 124 is attenuated at surface 86 . The light must make multiple reflections off the channel walls, thereby losing intensity after each reflection. Although light 124 may be re-activated by photocathode 90 into electrons 85 ( FIG. 8 ) and may again be amplified by MCP 91 , the resulting re-activated electrons are substantially reduced. Thus, curved microchannels 88 are effective in reducing re-activated electrons and in reducing spatially-disconnected noise.
The inventor considered different approaches to curving the channels of an MCP. One possible approach is heating and bending a boule, such as heating and bending boule 30 ( FIG. 5 ). Simply heating and bending a boule, however, may not be desirable. The fibers disposed adjacent to the outer circumferential edge of the boule may be more stretched than the fibers disposed adjacent to the inner portion of the boule. If the outer edge fibers stretch more than the inner portion of fibers, the outer edge channels would likely be reduced in diameter. Since channel gain of an MCP is a function of channel aspect ratio, for a fixed MCP thickness, the stretched channels would cause shading in an image tube.
The inventor discovered that a preferred approach to forming curved channels in an MCP is to bend a boule that is fabricated from two types of glass. In addition, one type of glass should have a higher forming temperature than the second type of glass. For example, the core rod (core 12 in FIG. 1 ) should have a higher forming temperature than the clad glass (cladding 14 in FIG. 1 ). For example, the softening temperature for the core rod may be approximately 580° C. and the softening temperature for the clad glass may be approximately 550° C.
The inventor discovered that the above 30° C. difference in the forming temperature is adequate to induce a curve in the boule and maintain the fibers in a rigid state without stretching the edge fibers. Thus, bending of boule 30 may be accomplished by heating the boule to the softening temperature of the clad glass and then bending the boule. Because the clad glass softens and shears, the boule is bent. The core rod, however, has a higher forming temperature and remains rigid at the lower softening temperature of the clad glass. As a result, the core rod resists stretching.
As shown in FIGS. 10A and 10B , the core rods, designated as 100 (clad glass not shown), do not stretch after bending. The square ends 102 a and 102 b of boule 30 remain parallel after bending. Since the core rods do not stretch, the diameters of the resulting microchannels (after dicing and etching) are not reduced in diameter. The present invention thus reduces light transmission through the MCP without producing visible shading or FPN due to bending (or curving).
Fundamental to this process is the difference in softening temperature between the two types of glass used in fabricating the boule. The core rod must have a higher softening temperature so that it resists stretching while the clad shears. As an analogy, a bundle of uncooked spaghetti may be bent, even though the individual pieces cannot be stretched. The bending of the uncooked spaghetti occurs as the individual pieces slide relative to each other.
It will be appreciated that the present invention attempts to reduce light transmission through the microchannels of an MCP. This may be achieved by preventing light from passing through the MCP without also reflecting off the walls of the microchannels. Furthermore, the bending (or curving) of the microchannels may be slight. For example, simply offsetting the centers of the microchannels by one channel diameter results in at least two reflections of light off the channel walls. The at least two reflections produce light attenuation, which is a desired goal. Thus, the amount of curvature of the microchannels may be quite small.
Inherent in the present invention is a variation in sliced MCP bias angle, since the slicing angle is usually fixed with respect to the boule. This angular variation may be reduced by slicing the MCP at 900 to the bending axis, but this adds bias direction variation.
An exemplary structure for bending, or curving the boule is shown in FIGS. 9A , 9 B and 9 C. As shown mold 200 includes a structure having a longitudinal direction and a transverse direction. A notch is formed in the structure, extending in the longitudinal direction between ends of the structure. The notch forms a U-shape, oriented in the transverse direction. The U-shape has a portion of a first circle configured to receive and cradle a boule. The notch forms a portion of a second circle, oriented in the longitudinal direction and configured to impart a bend in the boule having a curved surface similar to the second circle.
The mold 200 is configured to receive the boule in a heated state having a first temperature effective in softening cladding glass in the boule, but having a temperature lower than a second temperature effective in softening core rods in the boule.
As an example of dimensions, mold 200 may have a length (L) of 8 inches, a height (H) of 1.25 inches, and a width (W) of 1.75 inches. The diameter of the notch (D) may be 1.125 inches and the curvature of the notch may form a minimum dimension C of 0.4 inches for a length (L) of 8 inches.
Although the invention is illustrated and described herein with reference to specific embodiments, the invention is not intended to be limited to the details shown. Rather, various modifications may be made in the details within the scope and range of equivalents of the claims and without departing from the invention.
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A microchannel plate (MCP) is formed from a boule. The MCP includes a plate having opposing end surfaces formed of acid resistant glass and acid etchable glass, and multiple channels extending longitudinally between the opposing end surfaces. The multiple channels are formed by circumferential walls of the acid resistant glass that surround the acid etchable glass. A respective circumferential wall forms a curved surface extending longitudinally between the opposing end surfaces. The curved surface is configured to reduce light from passing from one end surface to the other end surface. The acid resistant glass has a lower softening temperature than the acid etchable glass. As a result, the acid etchable glass may be subjected to a bending process, without reducing the diameter size of the microchannels that are formed after the bending process.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to an ejector apparatus for moving a lift core which extends through a core constituting a component of a resin molding mold to form an undercut portion in a molded piece and which is installed so as to be capable of moving obliquely with respect to the core surface and in the longitudinal direction.
[0003] 2. Description of the Related Art
[0004] An apparatus for moving a lift core which extends obliquely through a core constituting a component of a resin molding mold to form an undercut portion in a molded piece and which is movable in the longitudinal direction, is called an ejector apparatus, an example of which is disclosed, for example, in JP 10-95019 A.
[0005] FIG. 1 schematically shows the construction of the ejector apparatus as disclosed in JP 10-95019 A.
[0006] FIG. 1 shows a conventional ejector apparatus 20 , which was created by the present inventor. In the apparatus shown, a slide base 33 is arranged in a slide path 32 formed in a vertically movable ejector plate 26 , and the slide base 33 is forced to slide as the ejector plate 26 moves up and down, whereby an appropriate axial operating force is imparted to a lift core 28 .
[0007] FIG. 2 shows the overall configuration of a resin molding mold A equipped with this ejector apparatus 20 . The general construction of this mold is as follows: a core 21 b is arranged under a mold main body 21 a , with the mold main body 21 a and the core 21 b defining a resin molding space 22 ( FIG. 1 ).
[0008] Below the core 21 b , there is arranged a base plate 23 , and, between the core 21 and the base plate 23 , there is arranged a spacer 24 on either side, thus defining a chamber 25 between the spacers 24 under the core 21 b . In this chamber 25 , the ejector plate 26 is arranged so as to be vertically movable. Note that FIG. 1 is a partial sectional view, taken along the line I-I, of the resin molding mold A shown in FIG. 2 .
[0009] In this resin molding mold A, there is provided a lift core 28 which is passed through an angle setting hole 27 (inclined by an angle K) of the core 21 b constituting the resin molding mold A to form an undercut portion in a molded piece formed in the above-mentioned resin molding space 22 and which extends obliquely and is longitudinally movable.
[0010] The upper end portion of this lift core 28 functions as a mold portion 28 a which cooperates with the core 21 b to form a molded piece, and, by the side of this upper portion, there is formed a protrusion 28 b for integrally forming an L-shaped flange portion (which also constitutes a part of the undercut portion) in the molded piece.
[0011] This lift core 28 is passed through a guide hole 31 a formed obliquely in a guide plate 31 which is fitted into a recess 29 formed in the lower surface of the core 21 b and which is fastened to the core 21 b by bolts 30 , with the lift core 28 extending downwardly from the core 21 b.
[0012] This guide plate 31 , which allows smooth longitudinal sliding of the lift core 28 due to the guide hole 31 a formed in the guide plate 31 at a predetermined angle K, functions as a bearing. Since the inclination angle K is determined by the angle setting hole 27 formed in the core 21 b , the guide hole 31 a may be a loose fit or clearance hole.
[0013] This lift core 28 is caused to slide vertically in the angle setting hole 27 of the core 21 b by the ejector apparatus 20 . The ejector apparatus 20 used for this purpose includes an ejector plate 26 composed of two plates 26 a and 26 b superimposed one upon the other.
[0014] Formed in the lower plate 26 b of the ejector plate 26 is the slide path 32 , which extends in the direction in which the lower end of the lift core 28 makes relative horizontal movement when it ascends and descends. The slide base 33 is slidably arranged in this slide path 32 , and the lower end portion 28 d of the lift core 28 is retained by one end portion of the slide base 33 with respect to the sliding direction of the lift core 28 .
[0015] Further, the ejector apparatus 20 , which raises and lowers the lift core, is equipped with an angular guide rod (hereinafter simply referred to as the guide rod) 38 which is adjacent to the lift core 28 and which is parallel thereto. At either end of this guide rod 38 , there is formed a V-shaped cutout 39 . The upper end portion of the guide rod 38 is supported by engaging one cutout 39 thereof with a pin 40 mounted across a through hole 31 b formed in the guide plate 31 .
[0016] Incidentally, FIG. 3 is an overall view of the slide base 33 slidably provided in the ejector plate 26 . This slide base 33 includes a base main body 34 having at its ends with respect to the sliding direction thereof forked portions 34 a and 34 b that are U-shaped in plan view. In one forked portion 34 a of this base main body 34 , there is arranged a shaft coupling 35 , and, in the other forked portion 34 b , there is arranged a guide bush 36 .
[0017] The shaft coupling 35 arranged in the forked portion 34 a is rotatably mounted to opposed wall surfaces by means of pins or the like. FIG. 4 is an enlarged view of the forked portion 34 a of the base main body 34 where the shaft coupling 35 is mounted.
[0018] As is apparent from FIGS. 1 through 4 , formed at the upper end of the shaft coupling 35 is a recess or seat 35 a for receiving the lower end portion of the lift core 28 . Further, the shaft coupling 35 is equipped with a through-hole 35 b having a central axis perpendicular to the rotation axis of the shaft coupling 35 and matched with the center line of the recess 35 a mentioned above.
[0019] The lower end portion of the lift core 28 is fitted into the recess 35 a at the upper end of the shaft coupling 35 rotatably mounted to one forked portion 34 a of the base main body 34 , and the end portion of a bolt 37 inserted into the through-hole 35 b from the lower end of the shaft coupling 35 as shown in FIG. 1 is threadedly engaged with a tapped hole formed in the lower end surface of the lift core 28 , whereby the lower end portion of the lift core 28 is firmly secured to the coupling 35 .
[0020] The guide bush 36 mounted to the other forked portion 34 b of the base main body 34 has a passing hole 36 a extending along an axis perpendicular to the rotation axis of the guide bush 36 , and the above-mentioned guide rod 38 is slidably passed through this passing hole 36 a.
[0021] The guide rod 38 , which is supported at its upper end by the guide plate 31 and which is passed through the passing hole 36 a of the guide bush 36 of the slide base 33 , extends toward the base plate 23 through a clearance hole 41 formed in the lower plate 26 b , and the cutout 39 at its lower end is engaged with a pin 43 of a holder bush 42 mounted to the base plate 23 , whereby the lower end of the guide rod is supported and secured.
[0022] This holder bush 42 is inserted into an opening 44 formed in the base plate 23 and is secured in position by bolts 45 . As described above, the guide rod 38 is arranged so as to be parallel to the lift core 28 , that is, inclined by the same angle as the lift core 28 . As is apparent from FIG. 1 , the distance between the core 21 b and the base plate 23 (that is, the height of the spacers 24 ) is fixed, so that the setting of the angle of the guide rod 38 depends upon the horizontal positional relationship, that is, the distance, between the pin 40 provided in the guide plate 31 and the pin 43 provided in the holder bush 42 .
[0023] In this conventional ejector apparatus 20 , when the ejector plate 26 ascends, the slide base 33 arranged in the slide path 32 formed in the ejector plate 26 also ascends, and a vertical moving force is imparted to the lift core 28 , whose lower end is connected to the slide base 33 .
[0024] In this process, as a result of its ascent, the slide base 33 receives a horizontal component of a moving force biasing it to move along the guide rod 38 , which is mounted at the same inclination angle as the lift core 28 . As a result, a moving force to push up the lift core 28 in the longitudinal and axial directions is imparted to the lift core 28 . Descent of the ejector plate 26 results in an operation contrary to the above, and the lift core 28 is pulled down in the longitudinal direction thereof through the slide base 33 .
[0025] Incidentally, the inclination angle K (See FIG. 5A ) of the lift core 28 in this ejector apparatus is changeable to an arbitrary angle according to the molded piece 22 to be obtained, and the inclination angle K of this lift core 28 is determined by the user who is going to produce the molded piece 22 by using this ejector apparatus 20 Thus, as for the longitudinal length of the lift core 28 , additional setting is required on the part of the user who has purchased the ejector apparatus 20 .
[0026] In view of this, in the conventional ejector apparatus, when fixing the lower end portion 28 d of the lift core 28 to the slide base 33 , (1) the lift core 28 , prepared in a relatively large length, is temporarily incorporated, and (2) the amount á by which the protrusion 28 b of the lift core 28 protrudes on the molded piece side (See FIG. 5B ) is measured, determining the corrected set value of the rod length of the lift core 28 from this measurement value á. And, the lift core 28 has to be pulled out for additional machining to adjust the rod length thereof before incorporating it again.
[0027] Further, in the operation of assembling the ejector apparatus, when effecting threaded engagement of the slide base 33 through the lower end surface of the lift core 28 and the shaft coupling 35 , the base plate 23 is removed as shown in FIG. 1 or a hexagonal wrench hole is formed in the base plate 23 , thus making the lift core 28 detachable. Further, since the lift core 28 is vertically movable, and the slide base 33 is horizontally slidable, the assembly operation is rather difficult to perform. Furthermore, in addition to the corrected core rod length set value determined, it is necessary, depending upon the assembly system, to take into consideration the thermal expansion amount due to the temperature rise during molding operation of the rod of the lift core 28 . In this way, the additional setting of the lift core 28 in the longitudinal direction by the user is not only a bother but also involves extreme difficulty in achieving a predetermined machining accuracy.
[0028] The following problems are to be taken into account: (1) when the additional setting of the lift core lower end surface results in an excessive length, the lift core 28 sticks out on the resin molded piece side, resulting in fluctuation due to molding pressure and a damaged product appearance; and (2) when the additional setting results in too small a length, the ejector plate 26 is raised together with the slide base 33 connected to the lift core 28 , and due to displacement of all the components installed in this plate, the design consistency suffers, or the mounting screw 37 may be broken.
[0029] That is, in setting the length of the lift core, problems are involved whether the lift core is too long or too short, and, to determine the setting range, a very severe and difficult operation, which is contingent on the limited clearance between the slide base 33 and the slide path 32 , has to be performed while taking into account the thermal expansion of the lift core 28 .
[0030] Thus, there is a demand for an improvement in terms of the operational efficiency in assembling these components, i.e., the slide base 33 and the lift core 28 .
SUMMARY OF THE INVENTION
[0031] The present invention has been made with a view toward solving the above problems in the prior art. It is an object of the present invention to provide an ejector apparatus for use in a resin molding mold, in which, in mounting the lift core, which is to be installed in an inclined state, to the slide base, there is no need for the user to perform any machining operation, making it possible to easily mount the lift core to the slide base regardless of the inclination angle of the lift core.
[0032] The present invention relates to an ejector apparatus and has the following structures in order to solve the above-described technical objects.
[0033] That is, according to the present invention, there is provided an ejector apparatus for forming an undercut portion in a molded piece, characterized by including: a lift core extending through a core that constitutes a resin molding mold and installed so as to be movable in a longitudinal direction of the lift core with respect to a surface of the core; an ejector plate arranged between the core and a base plate so as to be capable of moving up and down, the base plate being arranged below the core while being spaced apart from the core; and an adjustment coupling constructed such that a lower end portion of the lift core is supported so as to be capable of expanding and contracting in a longitudinal direction of the lift core with respect to the ejector plate.
[0034] In this construction, the assembly setting for the rod of the lift core manufactured based on the design value can be effected after assembly within the adjustment range for the adjustment coupling without performing any machining to diminish its length. Further, it is possible to absorb the thermal expansion of the rod of the lift core.
[0035] Also, in the ejector apparatus according to the present invention, the adjustment coupling is provided on an ejector plate side and is equipped with: a support member which has an insertion hole allowing insertion of the lower end portion of the lift core, the insertion hole having a threaded portion, the lower end portion of the lift core inserted from one end of the insertion hole being supported on the ejector plate side; an adjusting screw formed as a hollow cylinder having a threaded portion on its outer peripheral surface and adapted to be threadedly inserted from the other end of the insertion hole of the support member to abut the lower end portion of the lift core; a lock nut serving as a locking means; and a bolt member for fastening together the adjusting screw and the lower end portion of the lift core.
[0036] In this construction, the setting of the thermal expansion amount can be effected based on the reversing amount of the adjusting screw.
[0037] Further, according to the present invention, there is provided an ejector apparatus for forming an undercut portion in a molded piece, characterized by including: a lift core extending through a core constituting a resin molding mold, the lift core being installed so as to be movable obliquely with respect to a surface of the core and in a longitudinal direction of the lift core; an ejector plate arranged between the core and a base plate so as to be capable of moving up and down, the base plate being arranged below the core while being spaced apart from the core; a slide path formed in the ejector plate so as to extend in a direction in which a lower end of the lift core makes relative horizontal movement at a time of ascent and descent of the lift core; a slide base movably arranged in the slide path; a guide bush supported on the slide base so as to be pivotable in an inclining direction of the lift core; and a guide rod that serves to force the slide base to slide horizontally by sliding along the guide bush at a time of ascent and descent of the ejector plate, the ejector apparatus being characterized in that the slide base is equipped with: a slide base main body; and an adjustment coupling constructed such that a lower end portion of the lift core is supported so as to be capable of expanding and contracting in a longitudinal direction of the lift core with respect to the sliding base main body.
[0038] In this construction, the assembly setting for the rod of the lift core manufactured based on the design value can be effected after assembly within the adjustment range for the adjustment coupling without performing any machining to diminish its length. Further, no sliding of the slide base due to the guide rod (release guide) occurs, thus facilitating the assembly.
[0039] Further, in the ejector apparatus according to the present invention, the adjustment coupling is constructed such that the lower end portion of the lift core is supported so as to be pivotable in an inclining direction of the lift core with respect to the sliding base main body in such a way that an inclination angle of the guide rod is the same as an inclination angle of the lift core.
[0040] In this construction, the base main body is equipped with the guide bush pivotable in the inclining direction of the lift core and the adjustment coupling pivotable in the inclining direction, whereby it is possible to forcibly move the ejector plate up and down and forcibly move the slide base in the horizontal direction while maintaining the same inclination angle for the axes of the guide rod and the lift core (i.e., keeping them parallel to each other). That is, the slide base simultaneously receives a horizontal moving force and an upward or downward moving force, and a force which would cause rotation in the slide path is exerted. However, in the present invention, as long as the slide base has been assembled so as to be parallel to the longitudinal direction of the slide path, even if a force that would cause the slide base to rotate within the slide path is exerted, it is possible to keep the slide base parallel to the slide path. Thus, the slide base can always remain parallel to the slide surface of the slide path. As a result, in the present invention, it is possible to completely avoid, with a simple structure, hindrance to sliding, without performing any additional machining on the lift core and the slide base, thus realizing smooth sliding movement.
[0041] Further, according to the present invention, there is provided an ejector apparatus for forming an undercut portion in a molded piece, characterized by including: a lift core extending through a core constituting a resin molding mold, the lift core being installed so as to be movable obliquely with respect to a surface of the core and in a longitudinal direction of the lift core; an ejector plate arranged between the core and a base plate so as to be capable of moving up and down, the base plate being arranged below the core while being spaced apart from the core; a slide path formed in the ejector plate so as to extend in a direction in which a lower end of the lift core makes relative horizontal movement at the time of ascent and descent of the lift core; a slide base movably arranged in the slide path; an adjustment coupling constructed such that a lower end portion of the lift core is supported so as to be capable of expanding and contracting in a longitudinal direction of the lift core and rotatable in an inclining direction of the lift core with respect to the sliding base main body; a guide bush supported on the slide base so as to be pivotable in an inclining direction of the lift core; and a guide rod that serves to force the slide base to slide horizontally by sliding along the guide bush at the time of ascent and descent of the ejector plate, the being characterized in that the adjustment coupling is endowed with an alignment function by which an intersection point where the guide rod and the core cross each other, an intersection point where the guide rod and the guide bush cross each other, an intersection point where the lift core and the core cross each other, and an intersection point where the lift core and the adjustment coupling cross each other, are capable of forming a parallelogram.
[0042] In this construction, it is possible to forcibly move the ejector plate up and down and forcibly move the slide base in the horizontal direction while maintaining the same inclination angle for the intersection points for the guide rod and the lift core (i.e., keeping them parallel to each other). That is, even if the slide base simultaneously receives a horizontal moving force and an upward or downward moving force, it is possible to keep the slide base parallel to the slide path due to the alignment function by which the four intersection points are capable of forming a parallelogram.
[0043] Further, in the above-mentioned ejector apparatus according to the present invention, the adjustment coupling is provided on a slide base side, and is equipped with: a support member which has an insertion hole allowing insertion of the lower end portion of the lift core, the insertion hole having a threaded portion, the lower end portion of the lift core inserted from one end of the insertion hole being supported on the slide base; an adjusting screw formed as a hollow cylinder having a threaded portion on its outer peripheral surface and adapted to be threadedly inserted from the other end of the insertion hole of the support member to abut the lower end portion of the lift core; a lock nut serving as a locking means; and a bolt member for fastening together the adjusting screw and the lower end portion of the lift core.
[0044] In this construction, the setting of the thermal expansion amount can be effected based on the reversing amount of the adjusting screw.
[0045] Further, according to the present invention, there is provided an ejector apparatus, characterized in that the adjusting screw and/or the lock nut has an inner hexagonal wrench hole.
[0046] In this construction, a minimum hole allows insertion of the hexagonal wrench and provides rotation space, thus allowing space saving in terms of the area occupied inside the ejector apparatus itself. Further,a minimum hole allows insertion of a hollow wrench (hexagonal sleeve wrench) and provides rotation space, thus making it possible to achieve a reduction in the size of the ejector apparatus itself.
[0047] Further, the hexagonal wrench, which always undergoes integral threaded insertion in assembling the adjusting screw, is inserted into the hollow of the hollow wrench, thus allowing assembly of two coaxial components (i.e., the adjusting screw and the lock nut). Further, a hexagonal wrench is inserted into the hollow wrench (the hexagonal sleeve wrench), which undergoes integral threaded insertion in assembling the lock nut, thus allowing assembly of two coaxial components.
[0048] Further, according to the present invention, there is provided an ejector apparatus characterized in that respective screws of the adjusting screw and the lock nut exhibit a screw fit length allowing locking without involving any stress relaxation due to fastening pre-tension.
[0049] Further, according to the present invention, there is provided an ejector apparatus characterized in that the adjusting screw and the lock nut each have a hexagonal wrench hole structure for a hollow hexagonal wrench with a round hole for fastening the lock nut and for a hexagonal wrench to be inserted into a hollow of the hollow hexagonal wrench with a round hole to fasten the adjusting screw, and that the base plate and the ejector plate each have a space portion in which the hexagonal wrenches are turned around an axis of the hexagonal wrench hole structure.
[0050] Further, according to the present invention, there is provided an ejector characterized in that the adjustment coupling is equipped with a clearance setting portion that serves to set a predetermined clearance in an axial length of the lift core through reversal of the adjusting screw by an amount corresponding to an angle that can be known from the pitch of the screw portion after abutting the adjusting screw against the lower end portion of the lift core.
[0051] As described above, in the ejector apparatus for a resin molding mold of the present invention, the rod of the lift core prepared based on the design value allows assembly setting within the adjusting range for the adjustment coupling after the assembly, without having to perform any machining to diminish the length thereof. Further, it is possible to absorb the thermal expansion of the rod of the lift core.
BRIEF DESCRIPTION OF THE DRAWINGS
[0052] In the accompanying drawings:
[0053] FIG. 1 is a sectional view of a conventional ejector apparatus for a resin molding mold;
[0054] FIG. 2 is an overall perspective view of a resin molding mold equipped with the ejector apparatus as shown in FIG. 1 ;
[0055] FIG. 3 is an overall perspective view of a slide base constituting the ejector apparatus shown in FIG. 1 ;
[0056] FIG. 4 is an enlarged perspective view of one forked portion of a slide base main body constituting the slide base shown in FIG. 3 , in which a shaft coupling is mounted;
[0057] FIGS. 5A and 5B are explanatory views illustrating the assembling of a lift core of an ejector apparatus;
[0058] FIGS. 6A and 6B are explanatory views illustrating the assembling of the lift core of an ejector apparatus, of which FIG. 6A shows a slide base when a shaft coupling is used, and FIG. 6B shows a slide base when no shaft coupling is used;
[0059] FIG. 7 is a sectional view of an ejector apparatus for a resin molding mold according to a first embodiment of the present invention;
[0060] FIG. 8 is a longitudinal sectional view of an adjustment coupling;
[0061] FIGS. 9A through 9D are diagrams illustrating assembly procedures for an adjustment coupling;
[0062] FIGS. 10A through 10D are diagrams illustrating assembly procedures for an adjustment coupling;
[0063] FIGS. 11A through 11C are diagrams illustrating assembly procedures for an adjustment coupling;
[0064] FIGS. 12A through 12 c are diagrams illustrating assembly procedures for an adjustment coupling;
[0065] FIGS. 13A through 13E are diagrams illustrating assembly procedures for an adjustment coupling;
[0066] FIG. 14 is a longitudinal sectional view of a slide base and an adjustment coupling;
[0067] FIG. 15 is an explanatory view of an ejector apparatus according to a second embodiment of the present invention, showing an adjustment coupling when no slide base is used;
[0068] FIG. 16 is a longitudinal sectional view of an adjustment coupling according to the second embodiment;
[0069] FIGS. 17A through 17F are diagrams illustrating assembly procedures for the adjustment coupling of the second embodiment;
[0070] FIGS. 18A through 18D are diagrams illustrating assembly procedures for the adjustment coupling of the second embodiment;
[0071] FIGS. 19A through 19D are diagrams illustrating assembly procedures for the adjustment coupling of the second embodiment;
[0072] FIGS. 20A through 20E are diagrams illustrating assembly procedures for the adjustment coupling of the second embodiment; and
[0073] FIG. 21 is a perspective view of an adjustment coupling according to another embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0074] Embodiments of an ejector apparatus for a resin molding mold of the present invention will now be described in detail.
[heading-0075] [First Embodiment]
[0076] FIG. 7 shows an ejector apparatus 100 for a resin molding mold according to a first embodiment of the present invention.
[0077] First, a resin molding mold A equipped with this ejector apparatus 100 will be described. As shown in FIG. 2 , the general construction of this mold is as follows: a core 21 b is arranged under a mold main body 21 a , with the mold main body 21 a and the core 21 b defining a resin molding space 11 ( FIG. 7 ).
[0078] Below the core 21 b , there is arranged a base plate 23 , and, between the core 21 b and the base plate 23 , there is arranged a spacer 24 on either side, thus defining a chamber 25 between the spacers 24 under the core 21 b . In this chamber 25 , an ejector plate 1 is arranged so as to be vertically movable. Note that FIG. 7 is a partial sectional view, taken along the line I-I, of the resin molding mold A shown in FIG. 2 .
[0079] In this resin molding mold A, there is provided a lift core 5 which is passed through an angle setting hole 12 (inclined by an angle K) of the core 21 b constituting the resin molding mold A to form an undercut portion in a molded piece formed in the above-mentioned resin molding space 11 and which extends obliquely and is longitudinally movable.
[0080] The upper end portion of this lift core 5 functions as a mold portion 5 a which cooperates with the core 21 b to form a molded piece, and, by the side of this upper portion, there is formed a protrusion 5 b for integrally forming an L-shaped flange portion (which also constitutes a part of the undercut portion) in the molded piece. This lift core 5 is passed through a guide hole formed obliquely in the core 21 b , extending downwardly from the core 21 b.
[0081] This lift core 5 is caused to slide vertically in the angle setting hole 12 of the core 21 b by the ejector apparatus 100 . The ejector apparatus 100 used for this purpose includes the ejector plate 1 composed of two plates 1 a and 1 b that are superimposed one upon the other.
[0082] Formed in the lower plate 1 b of the ejector plate 1 is a slide path 32 , which extends in the direction in which the lower end of the lift core 5 makes relative horizontal movement when it ascends and descends. A slide base 33 is slidably arranged in this slide path 32 , and the lower end portion 5 d of the lift core 5 is retained by one end portion of the slide base 33 with respect to the sliding direction thereof.
[0083] Further, the ejector apparatus 100 , which raises and lowers the lift core 5 , is equipped with an angular guide rod (hereinafter simply referred to as the guide rod) 8 which is adjacent to the lift core 5 and which is parallel thereto. At either end of this guide rod 8 , there is formed a V-shaped cutout 39 . The upper end portion of the guide rod 8 is supported by engaging one cutout 39 thereof with a pin 40 .
[0084] Incidentally, FIG. 14 is an overall view of the slide base 33 slidably provided in the above-mentioned ejector plate 1 .
[heading-0085] [Slide Base 33 ]
[0086] This slide base 33 includes a base main body 34 having at its ends with respect to the sliding direction of the slide base 33 forked portions 34 a and 34 b that are U-shaped in plan view. In one forked portion 34 a of this base main body 34 , there is arranged a shaft coupling 36 , and in the other forked portion 34 b , there is arranged a guide bush 36 .
[0087] The lower end portion 5 d of the lift core 5 is supported by an adjustment coupling 110 so as to be extendable in the longitudinal direction and rotatable in the inclining direction with respect to the base main body 34 .
[heading-0088] [Guide Rod 38 ]
[0089] Further, the guide bush 36 rotatably mounted to the other forked portion 34 b of the base main body 34 has a passing hole 36 a extending along an axis perpendicular to the rotation axis of the guide bush 36 , and the above-mentioned guide rod 38 is slidably passed through this passing hole 36 a.
[0090] The guide rod 38 , which is supported at its upper end by a guide holder 39 and which is passed through the passing hole 36 a of the guide bush 36 of the slide base 33 , extends toward the base plate 23 through a clearance hole 41 formed in the lower plate 26 b , and the cutout 39 at its lower end is engaged with a pin 43 of a holder bush 42 mounted to the base plate 23 , whereby the lower end of the guide rod is supported and secured.
[0091] This holder bush 42 is inserted into an opening 44 formed in the base plate 23 and is secured in position by bolts 45 . As described above, the guide rod 38 is arranged so as to be parallel to the lift core 5 , that is, inclined by the same angle as the lift core 5 . As is apparent from FIG. 7 , the distance between the core 21 b and the base plate 23 (that is, the height of the spacers 24 (See FIG. 2 )) is fixed, so that the setting of the angle of the guide rod 38 depends upon the horizontal positional relationship, that is, the distance, between the pin 40 provided in the guide holder 39 and the pin 43 provided in the holder bush 42 . In FIG. 7 , the intersection points (axial center points) 39 c and 4 c of the guide rod 38 and the intersection points (axial center points) 5 c and 6 c of the lift core 5 form a parallelogram.
[0092] By thus forming a parallelogram, it is possible to force the ejector plate 1 to move vertically and to force the slide base 33 to move horizontally, with the axial center points 39 c , 4 c , 5 c , and 6 c of the guide rod 38 and the lift core 5 maintaining the same inclination angle (that is, keeping these components parallel to each other). That is, even when the slide base 33 simultaneously receive horizontal and vertical moving forces and a force to rotate the slide base 33 within the slide path 32 is exerted, the slide base 33 can be kept parallel to the slide path due to the self-alignment function which enables the four axial center points to form a parallelogram.
[heading-0093] [Adjustment Coupling 110 ]
[0094] Next, the adjustment coupling 110 will be described with reference to FIGS. 7, 8 , and 14 .
[0095] The adjustment coupling 110 is composed of the shaft coupling 6 which is a support member supporting the lower end portion 5 d of the lift core 5 on the base main body 34 and rotatable in the inclining direction, an adjusting screw 53 abutting the lower end portion 5 d of the lift core 5 , a bolt member (also referred to as cap bolt) 51 and a washer (spacer collar) 52 for fastening the adjusting screw 53 and the lower end portion 5 d of the lift core 5 to each other, and a lock nut 55 to be threadedly engaged with the outer peripheral surface of the adjusting screw 53 until it abuts the other end portion of the shaft coupling 6 .
[0096] The shaft coupling 6 arranged in the forked portion 34 a is rotatably mounted to opposing wall surfaces by means of pins or the like. Further, the shaft coupling 6 is equipped with a through-hole 6 b in alignment with the center axis thereof which is perpendicular to the rotation axis thereof. A threaded portion is formed in the inner peripheral surface of the through-hole 6 b.
[0097] As shown in FIG. 8 , the adjusting screw 53 is formed as a hollow cylinder having a threaded portion 53 a on its outer peripheral surface. Further, the adjusting screw 53 , which is formed as a hollow cylinder, has an inner hexagonal wrench hole 54 in the inner peripheral surface at one end thereof. The adjusting screw 53 is threadedly passed through the through-hole 6 b of the shaft coupling 6 and abuts the lower end portion 5 d of the lift core 5 .
[0098] The adjusting screw 53 and the lower end portion 5 d of the lift core 5 are fastened together by the cap bolt 51 after completion of fine adjustment of the axial length of the lift core 5 (See FIGS. 13B and 13C ). When fastening with the cap bolt 51 , the spacer collar 52 is inserted between the cap bolt 51 and the adjusting screw 53 . This is done for the purpose of preventing the hexagonal hole of the adjusting screw 53 from being crushed.
[0099] The locknut 55 is formed as a hollow cylinder having a threaded portion 56 a in an inner peripheral surface thereof. Further, the lock nut 55 , which is formed as a hollow cylinder, has an inner hexagonal wrench hole 56 in the inner peripheral surface at one end thereof.
[0100] Next, the assembly procedures for the adjustment coupling 110 will be described with reference to FIGS. 9 through 14 .
[0101] As shown in FIG. 9A , the lock nut 55 is threadedly engaged with an outer peripheral surface of the adjusting screw 53 beforehand. That is, the adjusting screw 53 is screwed into the lock nut 55 from one end thereof until the forward end of the adjusting screw 53 appears at the other end of the lock nut 55 (See FIG. 9B ). While the lock nut 55 and the adjusting screw 53 provide a sufficient slackness restraining force with normal fastening, when a still firmer fastening is required, the forward screw thread of the adjusting screw 53 is previously saturated with several drops of locking agent.
[0102] As shown in FIG. 9D , when threadedly passing the adjusting screw 53 through the through-hole 6 b of the shaft coupling 6 , the forward end of a hexagonal wrench 70 is thereadedly engaged with the inner hexagonal wrench hole 54 from below the ejector apparatus 100 , thus threadely engaging the adjusting screw 53 with the shaft coupling 6 .
[0103] Next, as shown in FIG. 10A , the hexagonal wrench 70 is temporarily pulled out, and the lift core 5 is inserted into the shaft coupling 6 .
[0104] The hexagonal wrench 70 is brought into a state in which it is inserted into a hollow hexagonal wrench (hexagonal sleeve wrench) 71 (See FIG. 10B ), and the forward end portion of the hexagonal wrench 70 is engaged with the inner hexagonal wrench hole 54 of the adjusting screw 53 . Next, the adjusting screw 53 is treadedly passed through the shaft coupling 6 again through turning with the hexagonal wrench 70 (See FIG. 10C ).
[0105] Next, the apex portion of the lift core 5 is pressed axially downwards, and further, the adjusting screw 53 is threadedly passed through the shaft coupling 6 again through turning with the hexagonal wrench 70 . Then, the lower end portion of the lift core 5 abuts the adjusting screw 53 , and when the adjusting screw 53 is further advanced, a “stop” state can be observed in which the slide base 33 abuts the bottom surface of the slide path 2 the clearance of which has been set beforehand (See FIG. 10D ).
[0106] As shown in FIG. 11A , while keeping the forward end of the hexagonal wrench 70 inserted into the inner hexagonal wrench hole 54 , the adjusting screw 53 is fixed so that it may not turn with the locknut 55 . Next, the forward end of the hexagonal sleeve wrench 71 is engaged with the inner hexagonal wrench hole 56 of the lock nut 55 and fastened manually. Through this manual fastening, the end surface of the shaft coupling 6 is engaged with the lock nut 55 .
[0107] Next, through reversal and retraction of the adjusting screw 53 by an amount corresponding to an angle that can be known from the screw thread pitch of the adjusting screw 53 (See FIG. 11B ), it is possible to perform fine adjustment of thermal expansion absorption for the axial length of the lift core 5 . Thus, regarding the axial length of the lift core 5 , its value is determined at the design stage, and fine adjustment thereof is performed by the above-mentioned angle to be known, whereby there is no need to perform gauging at the time of assembly.
[0108] Next, the forward end portion of the hexagonal wrench 70 is inserted into the inner hexagonal wrench hole 54 , and, as shown in FIG. 12A , the adjusting screw 53 is fixed so as not to turn with the lock nut 55 , and the forward end portion of the hexagonal sleeve wrench 71 is engaged with the inner hexagonal wrench hole 56 of the lock nut 55 to be fastened manually. Next, the hexagonal wrench 70 is drawn out (See FIG. 12B ), and the hexagonal wrench 70 is passed through the side hole at the end of the hexagonal sleeve wrench 71 to turn the hexagonal sleeve wrench 71 , and the adjusting screw 53 and the lock nut 55 are retightened, with the lock nut 55 being engaged with the end surface of the shaft coupling 6 (See FIG. 12C ). In this way, the lock nut 55 serves as a so-called W-nut, functioning to effect locking for the adjusting screw 53 . After the completion of the retightening, the hexagonal sleeve wrench 71 and the hexagonal wrench 70 are removed (See FIG. 13A ).
[0109] Next, after the completion of the fine adjustment of the axial length of the lift core 5 , the adjusting screw 53 and the lower end portion 5 d of the lift core 5 are fastened together by the cap bolt 51 (See FIGS. 13B and 13C ). When fastening them with the cap bolt 51 , the spacer collar 52 is inserted between the cap bolt 51 and the adjusting screw 53 . This is done for the purpose of preventing the hexagonal hole of the adjusting screw 53 from being crushed. After the fastening of the adjusting screw 53 and the lift core 5 , the hexagonal wrench 70 is removed to complete the assembly of the adjustment coupling 110 .
[0110] Next, the operation of the ejector apparatus 100 for the resin molding mold A of the first embodiment will be described.
[0111] After forming a molded piece by using the mold A, the ejector plate 1 is raised. When the ejector plate 1 is raised, a vertical raising force is applied to the lower end portion of the lift core 5 through the slide base 33 arranged in the slide path 32 of the upper and lower plates 1 a and 1 b.
[0112] However, in this slide base 33 , the guide rod 38 is slidably passed through the guide bush 36 mounted to the base main body 34 , so that, simultaneously with the rise of the slide base 33 , it is forced to move horizontally along the guide rod 38 . The inclination angle of this guide rod 38 is the same as that of the lift core 5 .
[0113] As a result, the slide base 33 simultaneously receive upward and horizontal moving forces and is forced to move along the guide rod 38 . Thus, a longitudinal moving force is imparted to the lift core 5 whose lower end portion 5 d is firmly attached to the shaft coupling 6 of the slide base 33 , and neither a bending force nor a moment that would generate friction is imparted to the angle setting hole 12 of the core 21 b.
[0114] Conversely, when the ejector plate 1 descends, the slide base 33 is forced to move along the guide rod 38 , whereby a longitudinal pull-down force is imparted to the lift core 5 . As a result, also at the time of descent of the ejector plate 1 , neither a bending force nor a moment for the lift core 5 is generated, so that it is possible to completely avoid friction with the angle setting hole 12 .
[0115] According to the first embodiment, the rod of the lift core 5 produced based on the design value allows assembly setting within the adjustment range for the adjustment coupling 110 without having to perform machining for a reduction in length after assembly. Further, due to the guide rod (release guide) 38 , there occurs no sliding of the slide base 33 , thereby facilitating the assembly.
[0116] Further, according to the first embodiment, the rod of the lift core produced based on the design value allows assembly setting within the adjustment range of the adjustment coupling without having to perform machining for a reduction in length after assembly. Further, thermal expansion of the rod of the lift core can be absorbed.
[0117] Further, according to the first embodiment, the rod of the lift core produced based on the design value allows assembly setting within the adjustment range of the adjustment coupling without having to perform machining for a reduction in length after assembly. Further, due to the guide rod (release guide), there occurs no sliding of the slide base, thereby facilitating the assembly
[0118] Furthermore, according the first embodiment, the setting of thermal expansion amount can be determined by the reversal amount of the adjusting screw.
[0119] Furthermore, according to the first embodiment, a minimum hole allows insertion of the hexagonal wrench and provides rotation space, making it possible to achieve space saving in terms of the area it occupies within the ejector apparatus itself. Further, a minimum hole allows insertion of the hollow wrench (hexagonal sleeve wrench) and provides rotation space, making it possible to achieve a reduction in the size of the ejector apparatus itself.
[0120] Further, in assembling the adjusting screw, the hexagonal wrench is always inserted into the hollow wrench (hexagonal sleeve wrench) for the lock nut for integral threaded insertion, thus allowing assembly of the two coaxial components (i.e., the adjusting screw and the lock nut).
[0121] Furthermore, in the ejector apparatus of the present invention, the adjusting screw and the lock nut are always fitted integrally, so that both have a hexagonal wrench hole structure, coaxially providing a wrench area of minimum rotation space. The hexagonal wrench for the adjusting screw allows fastening through insertion into the hollow hexagonal wrench with a round hole (hexagonal sleeve wrench) for the lock nut, thus needing no socket as in the case of an outer hexagonal screw nor rotation space for a spanner wrench.
[0122] Furthermore, according to the first embodiment, the adjusting screw is once brought into contact with the lower end portion of the lift core and is then reversed by an amount corresponding to an angle that can be known from the screw thread pitch, whereby it is possible to set the requisite clearance (absorption of thermal expansion coefficient) in the lift core length.
[0123] Note that, in the above-described first embodiment the adjustment coupling 110 is designed such that the lower end portion of the lift core 5 is supported on the base main body 34 so as to be pivotable in the inclining direction thereof so that the inclination angle of the guide rod 38 may be the same as that of the lift core 5 . However, the present invention is not restricted to the construction in which the adjustment coupling 110 is supported so as to be pivotable in the inclining direction.
[0124] For example, the present invention also covers a structure as shown in FIG. 21 , which shows a slide base 33 A having a support member 33 B that is not supported so as to be pivotable in the inclining direction of the lift core 5 , the slide base simply having an insertion hole allowing insertion of the lower end portion of the lift core 5 , with the insertion hole having a threaded portion.
[heading-0125] [Second Embodiment]
[0126] While in the above-described first embodiment the slide path allowing sliding of the slide base is provided in the ejector plate, and there is provided the guide rod that serves to force the slide base to slide horizontally, the present invention also covers a case where there is provided no slide path or guide rod.
[0127] Next, a second embodiment of the present invention, in which there is no slide path or guide rod, will be described with reference to FIGS. 15 through 20 .
[0128] Unlike the first embodiment, the second embodiment adopts a construction in which a core rod standing vertically on an ejector plate (which corresponds to the lift core of the first embodiment) is caused to move up and down without using any guide rod or slide path (slide base). Therefore, here, a construction in which, unlike the first embodiment, the core rod is caused to move up and down by the ejector plate will be described in detail, and a description of any other construction will be omitted.
[0129] FIG. 15 shows an ejector apparatus 200 for a resin molding mold according to a second embodiment of the present invention.
[0130] As shown in FIG. 2 , the general construction of a resin molding mold A equipped with this ejector apparatus 200 is as follows: a core 221 b is arranged under a mold main body 221 a , with the mold main body 21 a and the core 221 b defining a resin molding space 211 ( FIG. 15 ).
[0131] In this resin molding mold A, there is provided a core rod 205 which is passed through the core 221 b constituting the resin molding mold A to form a molded piece formed in the above-mentioned resin molding space 211 and which is longitudinally movable.
[0132] The upper end portion of this core rod 205 functions as a mold portion 205 a which cooperates with the core 221 b to form a molded piece. This core rod 205 is passed through a guide hole 221 c formed in the core 221 b , extending downwardly from the core 221 b.
[0133] This core rod 205 is caused to slide vertically in an guide hole 221 c of the core 221 b by the ejector apparatus 200 . The ejector apparatus 200 used for this purpose includes an ejector plate 201 composed of two plates 201 a and 201 b that are superimposed one upon the other. The lower end portion 205 d of the core rod 205 is held between the plates 201 a and 201 b through the intermediation of a retainer collar 250 . An adjustment coupling 210 according to the present invention is used in this joint portion.
[0134] As shown in FIG. 16 , the upper plate 201 a constituting the ejector plate 201 is equipped with a hole 202 a for the core rod 205 . Further, there are provided stepped holes 202 b and 202 c , which are coaxial with the hole 202 a . Of the stepped holes 202 b and 202 c , the large diameter hole 202 c is a hole into which the retainer collar 250 is to be inserted. The small diameter hole 202 b serves as a clearance hole for an adjusting screw 253 .
[heading-0135] [Adjustment Coupling 210 ]
[0136] Next, an adjustment coupling 210 will be described with reference to FIGS. 16 to 20 .
[0137] As shown in FIG. 16 , the adjustment coupling 210 is composed of an adjusting screw 253 abutting the lower end portion 205 d of the core rod 205 , a bolt member (also referred to as cap bolt) 251 and a washer (spacer collar) 252 for fastening the adjusting screw 253 and the lower end portion 205 d of the core rod 205 to each other, and a lock nut 255 to be threadedly engaged with the outer peripheral surface of the adjusting screw 253 until it abuts the other end portion of the retainer collar 250 .
[0138] As shown in FIG. 17A , the retainer collar 250 is formed as a cylinder the side surface of which exhibits two flat faces formed by cutting. Due to this two-face cutting, the retainer collar 250 makes no axial rotation with in the large diameter hole 202 c . Further, the retainer collar 250 is equipped with a through-hole in alignment with the center axis. A threaded portion 250 a is formed in the inner peripheral surface of the through-hole.
[0139] The adjusting screw 253 is formed as a hollow cylinder having a threaded portion 253 a on its outer peripheral surface. Further, the adjusting screw 253 , which is formed as a hollow cylinder, has an inner hexagonal wrench hole 254 in the inner peripheral surface at one end thereof. The adjusting screw 253 is threadedly passed through the through-hole of the retainer collar 250 and abuts the lower end portion 205 d of the core rod 205 (See FIG. 16 ).
[0140] The adjusting screw 253 and the lower end portion 205 d of the core rod 205 are fastened together by the cap bolt 251 after completion of fine adjustment of the axial length of the core rod 205 (See FIGS. 20B and 20C ). When fastening with the cap bolt 251 , the spacer collar 252 is inserted between the cap bolt 251 and the adjusting screw 253 .
[0141] The locknut 255 is formed as a hollow cylinder having a threaded portion 256 a in the inner peripheral surface thereof. Further, the lock nut 255 , which is formed as a hollow cylinder, has an inner hexagonal wrench hole 256 in the inner peripheral surface at one end thereof.
[0142] Next, the assembly procedures for the adjustment coupling 210 will be described with reference to FIGS. 17 through 20 .
[0143] As shown in FIG. 17B , the lock nut 255 is threadedly engaged with the outer peripheral surface of the adjusting screw 253 beforehand. That is, the adjusting screw 253 is screwed into the locknut 255 from one end thereof until the forward end of the adjusting screw 253 appears at the other end of the lock nut 255 (See FIG. 17C ). While the lock nut 255 and the adjusting screw 253 provide a sufficient slackness restraining force with normal fastening, when a still firmer fastening is required, the forward screw thread of the adjusting screw 253 is previously saturated with several drops of locking agent.
[0144] As shown in FIG. 17E , when threadedly passing the adjusting screw 253 through the through-hole of the retainer collar 250 , the forward end of a hexagonal wrench 70 is thereadedly engaged with the inner hexagonal wrench hole 254 from below the ejector apparatus 200 , thus threadely engaging the adjusting screw 253 with the retainer collar 250 .
[0145] Next, as shown in FIG. 17F , the hexagonal wrench 70 is temporarily pulled out, and the core rod 205 is inserted into the retainer collar 250 .
[0146] The hexagonal wrench 70 is brought into a state in which it is inserted into a hollow hexagonal wrench (hexagonal sleeve wrench) 71 (See FIG. 18A ), and the forward end portion of the hexagonal wrench 70 is engaged with the inner hexagonal wrench hole 254 of the adjusting screw 253 . Next, the adjusting screw 253 is treadedly passed through the retainer collar 250 again through turning with the hexagonal wrench. 70 (See FIG. 18B ).
[0147] Next, the apex portion of the core rod 205 is pressed axially downwards, and, further, the adjusting screw 253 is threadedly passed through the shaft coupling 6 again through turning with the hexagonal wrench 70 . Then, the lower end portion of the core rod 205 abuts the adjusting screw 253 , and, when the adjusting screw 253 is further advanced, a “stop” state is to be observed in which the retainer collar 250 abuts the bottom surface of the plate 201 the clearance of which has been set beforehand (See FIG. 18C ).
[0148] As shown in FIG. 18D , while keeping the forward end of the hexagonal wrench 70 inserted into the inner hexagonal wrench hole 254 , the adjusting screw 253 is fixed so that it may not turn with the lock nut 255 . Next, the forward end of the hexagonal sleeve wrench 71 is engaged with the inner hexagonal wrench hole 56 of the lock nut 255 and fastened manually. Through this manual fastening, the end surface of the retainer collar 250 is engaged with the lock nut 255 .
[0149] Next, through reversal and retraction of the adjusting screw 253 by an amount corresponding to an angle that can be known from the screw thread pitch of the adjusting screw 253 (See FIG. 1C ) it is possible to perform fine adjustment of thermal expansion absorption for the axial length of the core rod 205 . Thus, regarding the axial length of the core rod 205 , its value is determined at the design stage, and fine adjustment thereof is performed by the above-mentioned angle to be known, whereby there is no need to perform gauging at the time of assembly.
[0150] Next, the forward end portion of the hexagonal wrench 70 is inserted into the inner hexagonal wrench hole 54 , and, as shown in FIG. 19B , the adjusting screw 253 is fixed so as not to turn with the lock nut 255 , and the forward end portion of the hexagonal sleeve wrench 271 is engaged with the inner hexagonal wrench hole 256 of the lock nut 255 to be fastened manually. Next, the hexagonal wrench 70 is drawn out (See FIG. 19C ), and the hexagonal wrench 70 is passed through the side hole at the end of the hexagonal sleeve wrench 71 to turn the hexagonal sleeve wrench 71 , and the adjusting screw 53 and the lock nut 55 are retightened, with the lock nut 255 being engaged with the end surface of the retainer collar 250 (See FIG. 19D ). In this way, the lock nut 55 serves as a so-called W-nut, functioning to effect locking for the adjusting screw 253 . After the completion of the retightening, the hexagonal sleeve wrench 71 and the hexagonal wrench 70 are removed (See FIG. 20A ).
[0151] Next, after the completion of the fine adjustment of the axial length of the core rod 205 , the adjusting screw 253 and the lower end portion 205 d of the core rod 205 are fastened together by the cap bolt 251 (See FIGS. 20B and 20C ). When fastening them with the cap bolt 251 , the spacer collar 252 is inserted between the cap bolt 251 and the adjusting screw 253 . This is done for the purpose of preventing the hexagonal hole of the adjusting screw 253 from being crushed. After the fastening of the adjusting screw 253 and the core rod 205 , the hexagonal wrench 70 is removed to complete the assembly of the adjustment coupling 210 (See FIGS. 20D and 20E )
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An ejector apparatus wherein, in mounting a lift core to a slide base, and in mounting an ejector core to an ejector plate, it is easy to mount the lift and ejector cores to the slide base and the ejector plate, and simultaneously perform adjustment that allows for thermal expansion of the cores. The ejector apparatus includes a lift core extending through a core constituting a mold and movably installed in a longitudinal direction of the lift core with respect to a surface of the core; an ejector plate arranged between the core and a base plate, and being capable of moving up and down, the base plate being arranged below and spaced from the core; and an adjustment coupling constructed such that a lower end portion of the lift core is supported to expand and contract in a longitudinal direction of the lift core relative to the ejector plate.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to an engine control system for controlling an ignition timing and an air-fuel ratio to prevent spark knock of an engine.
2. Description of the Prior Art
In the engine control system disclosed in Japanese Unexamined Patent Publication No. 59(1984)-200042, the air-fuel ratio is controlled by feedback control in a feedback control zone and is controlled by open loop control in an enrich zone. In the enrich zone, the ignition timing is retarded when spark knock occurs. However, when the ignition timing is retarded to prevent spark knock, there arise problems that the engine output power is lowered to adversely affect fuel economy and the exhaust gas temperature is raised. Accordingly, in the engine control system, after the ignition timing is once retarded to eliminate the spark knock, the air-fuel ratio is controlled to advance the ignition timing without occurrence of spark knock. As is well known, engine output power is generally increased for a given operating condition of the engine as the ignition timing is advanced, and spark knock becomes less apt to occur, i.e., a critical ignition timing earlier than that at which spark knock will occur is moved toward the advance side, as the air-fuel ratio becomes richer. That is, in the engine control system, the ignition timing is retarded by a certain crank-angle when spark knock occurs and then is controlled by feedback control to an earliest timing within a range in which knock cannot occur, and then the air-fuel ratio is controlled so that the ignition timing can be approximated to a predetermined optimal value on the basis of comparison of the earliest timing determined by the feedback control and the predetermined optimal value. The predetermined optimal value is generally determined taking into account fuel economy, engine output power, exhaust gas temperature and the like. However, the engine control system disclosed in the patent publication identified above is disadvantageous in that since the predetermined optimal value is fixed irrespective of the fuel octane value, the ignition timing cannot be controlled to an optimal value following change of the fuel octane value. That is, the critical ignition timing, earlier than which spark knock will occur, changes with the air-fuel ratio, and the critical ignition timing for a given air-fuel ratio depends upon the fuel octane value and is moved toward the advance side as the octane number of the fuel increases. Accordingly, for example, if said predetermined optimal value is determined for regular gasoline, and if high octane gasoline is supplied, the ignition timing and the air-fuel ratio will be controlled to values deviated from the optimal values for high octane gasoline. That is, on the knocking limit line (the line obtained by plotting the critical ignition timing against the air-fuel ratio) for regular gasoline, the air-fuel ratio corresponding to a given ignition timing is leaner than that on the knocking limit line for high octane gasoline and accordingly, if the ignition timing is controlled, along the knocking limit line, to the optimal value for regular gasoline, the air-fuel ratio will be inevitably controlled to a value leaner than the optimal value for high octane gasoline at which the exhaust gas temperature is on the higher limit, whereby the exhaust gas temperature is adversely raised. As is well known, the exhaust gas temperature substantially depends upon the air-fuel ratio and the ignition timing.
Though the problem described above may be overcome by changing the predetermined optimal value according the fuel octane value in light of the teaching in Japanese Unexamined Patent Publication Nos. 58(1983)-57072 and 58(1983)-143169. However, this approach is disadvantageous in that the octane number of gasoline is difficult to detect, it is almost impossible to prepare the optimal values for intermediate octane numbers obtained by mixing the regular gasoline and the high octane gasoline in various proportions, and the relation between the octane number and the knocking limit changes with time.
SUMMARY OF THE INVENTION
In view of the foregoing observations and description, the primary object of the present invention is to provide an engine control system in which spark knock of the engine can be quickly eliminated by retarding the ignition timing and at the same time, the retarded ignition timing can be converged on an optimal point after the spark knock is eliminated irrespective of the fuel octane value and/or the change with time of the knocking characteristics of the engine, and which is simple in structure.
The engine control system in accordance with the present invention comprises a knock detecting means for detecting knock of an engine, an ignition timing correcting means which receives the output of the knock detecting means and retards the ignition timing when knock occurs and advances the ignition timing when knock does not occur, a setting means which sets an optimal ignition timing on which the ignition timing is to be converged to a latest ignition timing to which the ignition time can be retarded without raising the exhaust gas temperature higher than a predetermined value at the actual air-fuel ratio at that time, a comparator means which compares the actual ignition timing corrected by the ignition timing correcting means with the optimal ignition timing set by the setting means, and an air-fuel ratio control means which receives the output of the comparator means, and corrects the air-fuel ratio toward the lean side when the actual ignition timing is on the advance side of the optimal ignition timing and toward the rich side when the former is on the retard side of the latter.
The feature and the basic operation of the engine control system of the present invention will be described in detail referring to FIGS. 1 and 2, hereinbelow.
In an engine 1, the air-fuel ratio is controlled by controlling the fuel injection pulse to fuel injectors 3 and the ignition timing is controlled by controlling the ignition signal to spark plugs 4. Spark knock of the engine 1 is detected by a knock sensor 5 which detects knock of the engine by way of vibration of the engine 1. When spark knock is detected, the knock sensor 5 delivers a knock signal to an ignition timing correcting means 6.
The ignition timing correcting means 6 delays the ignition timing, i.e., the time the ignition signal to each spark plug 4 is output, when knock occurs, and advances the same when knock does not occur. That is, as the ignition timing is advanced, the engine output power is increased and spark knock is more apt to occur, and accordingly, the ignition timing correcting means 6 advances the ignition timing to a point where knock does not occur.
The ignition timing correcting means 6 delivers an ignition timing signal representing the corrected ignition timing to a comparator means 7. The comparator means 7 compares the corrected ignition timing with an optimal ignition timing on which the ignition timing is to be converged and which is set by a setting means 8. The setting means sets the optimal ignition timing to a latest ignition timing to which the ignition time can be retarded without raising the exhaust gas temperature higher than a predetermined value at the actual air-fuel ratio at that time.
The output signal of the comparator means 7 is delivered to an air-fuel ratio control means 9 which controls the air-fuel ratio by controlling the fuel injection pulse to be input into the fuel injector 3. The air-fuel ratio control means 9 controls the air-fuel ratio so that the ignition timing is moved toward the optimal ignition timing, and the output signal of the air-fuel ratio control means 9 is input into the comparator means 7 as a signal representing the actual air-fuel ratio which is used for setting the optimal ignition timing in the setting means 8.
In FIG. 2, line I represents the knocking limit line for regular gasoline and line II represents the knocking limit line for high octane gasoline. Line III represents the exhaust gas temperature limit line. When the ignition timing is advanced over the knocking limit line I when the engine 1 is charged with regular gasoline, the knock intensity will exceed an acceptable limit. Similarly, when the ignition timing is advanced over the knocking limit line II when the engine 1 is charged with high octane gasoline, the knock intensity will exceed the acceptable limit. Further, when the ignition timing is retarded over the exhaust gas temperature limited line III, the exhaust gas temperature will exceed an acceptable limit. In order to maintain reliability, the engine 1 must be operated on the retard side of the knocking limit line I or II and on the advance side of the exhaust gas temperature limit line III. Taking into account these conditions together with the fuel economy and the like, the setting means 8 sets the optimal ignition timing to a latest ignition timing to which the ignition time can be retarded without raising the exhaust gas temperature higher than the predetermined value (i.e., the acceptable limit) at the actual air-fuel ratio at that time. Though the latest ignition timing is theoretically on the exhaust gas temperature limit line III, actually the optimal ignition timing is set to a value corresponding to a point on line IV depending on the air-fuel ratio at that time. The line IV is substantially parallel to the exhaust gas temperature line III and is on the advance side of the line III in view of the safety factor. The ignition timing correcting means 6 advances the ignition timing when spark knock does not occur and retards the same when spark knock occurs, and the air-fuel ratio is corrected to return the corrected ignition timing to the original timing. Separately from the knock control effected in this manner, the ignition timing and the air-fuel ratio are controlled to optimal values represented by the intersection of the line IV and the corresponding knocking limit line. For example, in the case that the engine 1 is charged with regular gasoline, the ignition timing and the air-fuel ratio are finally controlled to the values represented by point A, and in the case that the engine 1 is charged with high octane gasoline, the ignition timing and the air-fuel ratio are finally controlled to the values represented by point B. The point representing the optimal ignition timing and air-fuel ratio will be sometimes referred to as "optimal operation point", hereinbelow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic view showing the general arrangement of the engine control system in accordance with the present invention,
FIG. 2 is a graph for illustrating the principle of operation of the engine control system of the present invention,
FIG. 3 is a schematic fragmentary cross-sectional view of an engine provided with an engine control system in accordance with an embodiment of the present invention,
FIG. 4 is a block diagram for illustrating the structure of the control unit employed in the engine control system of FIG. 3, and
FIGS. 5A and 5B are two flow charts for illustrating the operation of the control unit.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 3, the intake passage 2 for feeding intake air to combustion chambers 11 of the engine 1 is provided with a throttle valve 12, a pressure sensor 13 for detecting intake vacuum, and fuel injectors 3 for the respective combustion chambers 11.
The spark plugs 4 are connected to a distributor 14. A knock sensor 15 for detecting knock of the engine 1, and a crank-angle sensor 17 for detecting the engine speed through the rpm of the crankshaft 16 are provided.
The amount of fuel to be injected from the injector 3 and the ignition timing of the spark plugs 4 are controlled by a control unit 18 which may be a micro computer for example. Into the control unit 18 are input detecting signals of the pressure sensor 13, the knock sensor 15 and the crank-angle sensor 17.
The control unit 18 has functions of the ignition timing correcting means 6, the comparator means 7, the setting means 6 and the air-fuel ratio control means 9 described above in conjunction with FIG. 1, and restrains knock of the engine when knock occurs and controls the ignition timing and the air-fuel ratio to the optimal point in the manner described above.
As shown in FIG. 4 showing the internal arrangement of the control unit 18, the control unit 18 comprises a CPU 20, ROM 21 and RAM 22. Into the CPU are input an intake vacuum signal from the pressure sensor 13 and a knock signal from the knock sensor 15 by way of an input circuit 23, a multiplexer 24 and an A/D converter 25. Further, a signal from the crank-angle sensor 17 is input into the CPU 20 by way of an input circuit 26 as an interrupt signal, and a signal from a free running counter 27 is input into the CPU 20. The control unit 18 delivers a fuel injection control signal to the injector 3 by way of a timer 28 and a drive circuit 29, and an ignition signal to the spark plugs 4 by way of a timer 30 and an igniter 31.
The operation of the control unit 18 will be described with reference to the flow chart shown in FIG. 5, hereinbelow. In the main routine shown in FIG. 5(A), step S1 is an initializing step. In step S2, the intake vacuum from the pressure sensor 13 is read, and in step S3, a basic advancing angle of the ignition timing and a basic fuel injection amount are calculated on the basis of the engine speed and the intake vacuum. Then in step S4, it is determined whether the engine operating condition is in a knock zone in which the engine speed is lower than a preset value and the intake vacuum is smaller than a preset value (a high load range).
In the interrupt routine shown in FIG. 5(B), the engine speed is calculated through the interrupt period in step S5. The value of the engine speed calculated in the step S5 is used in the steps S3 and S4 in the main routine. In step S6, the basic advancing angle of the ignition timing So and the basic fuel injection amount To are read. In step S7, it is determined whether a shift-to-high-octane flag F (to be described later) has been set. When it is determined that the shift-to-high-octane flag F has not been set, the control unit 18 proceeds to step S15 and determines whether the engine operating condition is in the knock zone. When it is determined that the engine operating condition is not in the knock zone, the ignition timing is set to the basic advancing angle So in step S36, and the amount of fuel to be injected is set to the basic fuel injection amount To in step S37.
When it is determined that the engine operating condition is in the knock zone in step S15, the knock signal from the knock sensor 15 is read in step S16, and it is determined whether spark knock occurs at present by way of whether the knock signal exists in step S17. When it is determined that knock does not occur at present in the step S17, a predetermined value θ 1 is subtracted from retarding angle θ in order to advance the ignition timing in Step S18.
When it is determined that knock occurs at present in the step S17, a knock counter C is increased in step S19 and the sum SUM of the retarding angles θ during knocking is calculated in step S20. Then in step S21, a predetermined value θ 2 is added to the retarding angle θ in order to restrain the knock. In step S22, it is determined whether the knock counter C has reached a predetermined number of times n, and when it is determined that the knock counter C has reached the predetermined number of times n, the average retarding angle θo during the knocking is calculated in step S23, and the knock counter C and the register for the sum SUM of the retarding angles θ are cleared in step S24.
Then in step S25, it is determined whether the average retarding angle θo is in a target range for high octane gasoline the lower and upper limits of which are θ 3 and θ 4 . When it is determined that the average retarding angle θo is not between the values θ 3 and θ 4 , the average retarding angle θo is compared with a value θ 5 for resetting the shift-to-high-octane flag F in step S26. When it is determined that the former is larger than the latter, the shift-to-high-octane flag F and a shift-to-high-octane-end flag G are reset in step S27.
The shift-to-high-octane flag F is set in step S32 when the average retarding angle θo during knock control enters the target range for high octane gasoline (between θ 3 and θ 4 ) as the octane number of the fuel is increased and it is determined that the average retarding angle θo is between θ 3 and θ 4 in the step S25. When the shift-to-high-octane flag F is set, the air-fuel ratio is changed to the value suitable for pure high octane gasoline in order to promote convergence to the optimal operation point in steps S7 to S14. When the octane number is reduced so that the average retarding angle θo goes outside the target range for high octane to exceed the value θ 5 , the shift-to-high-octane flag F is reset in the step S27. In step S33, it is determined whether the shift-to-high-octane-end flag G is set. The shift-to-high-octane-end flag G is set to permit change of the air-fuel ratio to a value suitable for pure high octane gasoline only once after the ignition timing (the average retarding angle θo) enters the target range for high octane gasoline in response to increase in the octane number of the fuel. Thus, the engine operating condition can be converged on the optimal operating point even when the engine is charged with fuel having an octane number approximate to pure high octane gasoline. That is, the air-fuel ratio is changed to the value suitable for pure high octane gasoline only when the shift-to-high-octane flag F is set and at the same time the shift-to-high-octane-end flag G is reset.
When the air-fuel ratio is not to be changed to a value suitable for pure high octane gasoline, a target retarding angle θt is calculated according to a current air-fuel ratio correction coefficient H in step S28. The target retarding angle θt is calculated on the basis of the relation between the air-fuel ratio and the ignition timing represented by the line IV in FIG. 2. In step S29, it is determined whether the average retarding angle θo is larger than the target retarding angle θt. When the former is larger than the latter, the ignition timing is on the retard side of the line IV. In this case, it is considered that the engine is charged with fuel having an octane number smaller than a value corresponding to the current air-fuel ratio, and a predetermined value ho is subtracted from the air-fuel ratio correction coefficient H to correct the air-fuel ratio toward the rich side in step S30. When the former is smaller than the latter, the ignition timing is on the advance side of the line IV. In this case, it is considered that the engine is charged with fuel having an octane number larger than a value corresponding to the current air-fuel ratio, and a predetermined value ho is added to the air-fuel ratio correction coefficient H to correct the air-fuel ratio toward the lean side in step S31.
Thereafter, a final ignition timing So is determined in step S34 on the basis of the retarding angle θ thus determined, and a final fuel injection amount To is determined in step S35 on the basis of the air-fuel ratio correction coefficient H thus determined. Then the ignition timing is set to the final ignition timing So in step S36 and the amount of fuel to be injected is set to the final fuel injection amount To in step S37.
When it is determined that the average retarding angle θo enters the target range for pure high octane gasoline in the step S25 and the shift-to-high-octane flag F is set in the step S32, it is determined that the shift-to-high-octane flag F is set in the step S7 and the control unit 18 proceeds to the step S8. In the step S8, it is determined whether the shift-to-high-octane-end flag G is reset. Since the shift-to-high-octane-end flag G is reset when the air-fuel ratio is changed to the value suitable for pure high octane gasoline for the first time, it is determined in the step S8 that the shift-to-high-octane-end flag G is reset. Accordingly, the control unit 18 proceeds to the step S9 and a shift constant hp is added to the air-fuel ratio correction coefficient H in the step S9 so that the air-fuel ratio approximates the optimal value for pure high octane gasoline. Further, in the step S10, a predetermined value θp is added to the retarding angle θ to move the ignition timing toward the retard side. After the knock counter C and the sum SUM of the retarding angles θ are cleared in the step S11, it is determined in the step S12 whether the air-fuel ratio correction coefficient H reaches a target correction value ht.
That is, to add the shift constant hp in the step S9 is for gradually shifting the air-fuel ratio to prevent torque shock, and in order to prevent occurrence of spark knock due to the shift of the air-fuel ratio, the ignition timing is retarded in the step S10. When the air-fuel ratio reaches the optimal value, it is determined in the step S12 that the air-fuel ratio correction coefficient H reaches the target correction value ht and the air-fuel ratio correction coefficient H is set to the target correction value ht in the step S13. Then the shift-to-high-octane-end flag G is set in the step S14 and once the air-fuel ratio is changed to a value suitable for pure high octane gasoline, the flag G is kept set until fuel having a lower octane number is charged to the engine.
When the engine is charged with fuel having a lower octane number, it is determined in the step S25 that the average retarding angle θo is not in the target range for pure high octane gasoline and it is determined in the step S26 that the average retarding angle θo is larger than the value θ 5 for resetting the shift-to-high-octane flag F. Accordingly, the shift-to-high-octane flag F and the shift-to-high-octane-end flag G are reset in the step S27. Separately from the correction of the ignition timing and the air-fuel ratio for restraining spark knock, a target retarding angle θt corresponding to the current air-fuel ratio correction coefficient H is calculated in the step S28, and the air-fuel ratio is corrected according to the difference between the average retarding angle θo and the target retarding angle θt in the step S30 or S31, whereby the engine operating condition is approximated to the optimal operating point corresponding to the octane number of the fuel.
When the knocking limit line is moved toward the advance side or the retard side due to change in the octane number of the fuel charged to the engine, change with time of the engine characteristics or the like, the operating point of the engine, that is, the relation between the air-fuel ratio and the ignition timing, is deviated from the line IV. In the engine control system of this embodiment, when the operating point of the engine is deviated from the line IV, the air-fuel ratio and the ignition timing is changed along the moved knocking limit line toward the line IV so that the operating point is finally converged on a point on the line IV, that is, the intersection of the moved knocking limit line and the line IV. The average ignition timing may be calculated by averaging the ignition timings when knock occurs, or by averaging the ignition timings when the ignition timing is most retarded, or in various other ways. In any case, since occurrence of spark knock is a phenomenon of probability, the average ignition timing during the knock control for controlling the engine operating condition near the knocking limit fluctuates each time it is calculated. When the optimal operating point enters the range of errors, the speed at which the engine operating condition is converged on the optimal operating point is lowered. However, by converging the engine operating condition to the optimal point when the average ignition timing enters a predetermined range, the converging speed can be increased.
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An ignition timing correcting circuit which retards ignition timing when knock occurs and advances ignition timing when knock does not occur. An optimal ignition timing on which the ignition timing is to be converged is set to a latest ignition timing to which the ignition time can be retarded without raising the exhaust gas temperature higher than a predetermined value at the actual air-fuel ratio at that time. The actual ignition timing corrected by the ignition timing correcting circuit is compared with the optimal ignition timing. An air-fuel ratio control circuit corrects the air-fuel ratio toward the lean side when the actual ignition timing is on the advance side of the optimal ignition timing and toward the rich side when the former is on the retard side of the latter.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the priority of Provisional Application No. 61/784,017, filed on Mar. 14, 2013, which is herewith incorporated by reference in its entirety.
FIELD OF THE INVENTION
This invention relates to a testing device for a motor vehicle and in particular to a pressure tester for fuel systems adapted for motorcycles.
BACKGROUND OF THE INVENTION
In maintenance and diagnostic procedures, certain tests are performed for fuel systems to determine if elements of the system are operating properly. Modern large motorcycles feature a fuel sending unit disposed inside the fuel tank of the motorcycle. The sending unit typically includes an electric fuel pump along with a pickup tube, filter screen, and a fuel level sensor. The sending unit is powered by the vehicle electrical bus and pressurizes the fuel and supplies it to a fuel line, which leads to the induction system of the vehicle engine, typically a fuel injection unit, although some older motorcycles use carburetors.
Maintenance professionals use a variety of diagnostic tools in tracking down vehicle maintenance and breakdown issues. A fast and accurate testing system is desired, which enables the fuel pressure generated by the fuel sending unit to be measured. It is preferred that the use of such a diagnostic tool can be done quickly and with a minimal number of steps required of the maintenance technician. The tool should also be usable without causing unnecessary spillage of highly flammable gasoline in the symbol to operate.
In addition to a fuel system pressure test in a static or idle condition; namely, a condition in which the vehicle's engine is not demanding a maximum of fuel flow rate, there is further a need to measure fuel pressure in an operating condition which is equivalent to a full load condition. Ideally, such a fuel system test may be carried out without requiring that the engine being operated at full power, either on the road or on a chassis dynamometer. Both of these requirements are labor and equipment intensive and pose certain risks. Moreover, some fuel system faults cannot be resolved without performing a load test. For example, a clogged or partially clogged fuel pickup screen may be capable of enabling a normal no-load pressure to be generated, while such a fault would not permit pressure to be maintained in a fuel flow condition equivalent to a high-power operating condition of the engine.
SUMMARY OF THE INVENTION
The fuel system pressure tester in accordance with this invention is adapted to be quickly connected in-line with a conventional motorcycle fuel system. The system of the present invention enables tests to be carried out quickly, without special tools, and can provide both static and load testing evaluations.
According to one aspect of the invention, a fuel system pressure tester for motorcycles is adapted to be connected in-line with a fuel tank female fitting and a fuel line male fitting. The pressure tester includes a fitting body, a male fitting affixed to the fitting body adapted for connection with the fuel tank female fitting, a female fitting affixed to the fitting body adapted for connection with the fuel line male fitting, a pressure gauge affixed to the fitting body, a manually operated valve affixed to the fitting body having a valve actuating element and a connection for a fuel hose, and an internal passageway in the fitting body connecting the male fitting, the female fitting, the pressure gauge, and the manually operated valve.
According to another aspect of the invention, the valve actuating element may be a plunger element and the manually operated valve is normally in a closed condition and opens when the plunger element is actuated.
According to a further aspect of the invention, the female fitting has an internal normally closed valve with a valve member and a valve seat, and the fuel system pressure tester may further include a venting tool with a post having a sufficient length to remove the valve member of the female fitting from the valve seat and to open the manually operated valve. The venting tool may be attached to the fitting body with a flexible strap.
According to yet another aspect of the invention, a method of testing a fuel system of a motorcycle having a fuel tank with a female fitting, a fuel line with a male fitting, and an in-tank fuel sending unit, includes the steps of providing a pressure tester having a fitting body, a male tester fitting affixed to the fitting body adapted for connection with the fuel tank female fitting, a female tester fitting affixed to the fitting body adapted for connection with the fuel line male fitting, a pressure gauge affixed to the fitting body, a valve affixed to the fitting body having a valve actuating element and a connection for a fuel hose, the fitting body having an internal passageway connecting the male tester fitting, the female tester fitting, the pressure gauge, and the manually operated valve, connecting the pressure tester to the fuel tank by connecting the male tester fitting with the fuel tank female fitting, and connecting the female tester fitting with the fuel line male fitting, energizing the in-tank fuel sending unit, and reading pressure within the tester indicated by the pressure gauge.
According to another aspect of the invention, the method may further include the step of relieving pressure in the pressure tester after reading the pressure by activating the valve actuating element.
According to a further aspect of the invention, the method may further include the step of conducting a fuel pressure load test by inserting the fuel hose into a receptacle and reading the pressure step occurring while the valve actuating element is operated and causes a fuel flow through the pressure tester simulating a full-load operating condition of the motorcycle engine. The receptacle may be the fuel tank of the motorcycle, and the fuel hose may be inserted through a filler opening of the fuel tank.
After completion of the tests, the method may further include the steps of deenergizing the in-tank fuel sending unit, inserting the fuel hose into a receptacle, operating the valve actuating element, and releasing fuel through the fuel hose until atmospheric pressure prevails inside the fitting body. Afterwards, the pressure tester may be disconnected from the fuel tank by disconnecting the male tester fitting from the fuel tank female fitting, and by disconnecting the female tester fitting from the fuel line male fitting. A post of a venting tool may be inserted into the female fitting for opening an internal valve while the fuel hose is or remains inserted in the receptacle. Operating the valve actuating element will then allow the fuel to drain from the fitting body through the fuel hose by gravitational force.
Further details and benefits will become apparent by the following description of the accompanying drawings.
BRIEF SUMMARY OF THE DRAWINGS
In the drawings,
FIG. 1 shows a fuel system pressure tester in accordance with this invention;
FIG. 2 shows the fuel system pressure tester of FIG. 1 coupled with a motorcycle fuel tank and fuel line and conducting a static pressure test or a load fuel system pressure test;
FIG. 3 shows a detail of the fuel system pressure tester of FIG. 1 in a cross-section along the line A-A; and
FIGS. 4 a and 4 b show further alternative details of the fuel system pressure tester of FIG. 1 in a cross-section along the image plane.
DETAILED DESCRIPTION OF THE INVENTION
The drawing figures are included for purely illustrative purposes and are not intended to limit the scope of the invention. The drawings, in particular FIGS. 4 a and 4 b , are not necessarily to scale, unless specified.
The fuel system pressure tester in accordance with this invention is shown in FIGS. 1 and 2 and is generally designated by reference number 10 . Pressure tester 10 is particularly adapted for use with heavyweight Harley-Davidson motorcycles, such as model types Dyna, Softail, or Touring, to name a few, which are very numerous in the United States and around the world. Pressure tester 10 could be adapted for use with other motorcycle models and brands with provisions of suitable fuel system connections.
As shown in FIG. 2 , the associated motorcycle has fuel tank 12 having an extending female quick connect fitting 14 . Fitting 14 is normally connected with fuel line 16 which has a complementary male fitting 18 . To provide ease of installation on the vehicle and servicing, fittings 14 and 18 are easily connected and disconnected. Female fuel connection fitting 14 includes an axially moving movable outer sleeve 20 which can be pushed up when it is desired to insert and connect male fitting 18 or when it is desired to release male fitting 18 . Accordingly, in the normal use condition, male fitting 18 and fuel line 16 would be connected to the fuel tank 12 through the connection formed by fittings 14 and 18 . Female fuel tank fitting 14 includes an internal plunger type valve (not shown in FIG. 2 ), which is closed when male fitting 18 is disconnected to prevent uncontrolled fuel leakage. Connection of male fitting 18 to fitting 14 acts on the internal valve element to open the flow path when the two fittings are connected.
Fuel system pressure tester 10 , which is shown as a separate device in FIG. 1 and connected to the motorcycle in FIG. 2 , includes fitting body 22 having an internal hollow passageway communicating with the number of flow paths as will be described. Fitting body 22 forms male fitting 24 , which is identically dimensioned as is male fitting 18 , enabling male fitting 24 to be connected to fuel tank 12 in a manner equivalent to the connection with fuel line fitting 18 . Fitting body 22 further forms a female fitting 26 identical in construction with fuel tank fitting 14 also having an axially movable sleeve 28 . Male fitting 24 and female fitting 26 are shown in greater detail in FIG. 3 . Each of the female and male fittings 26 and 24 contains a valve 50 , which is held open when the fittings 26 and 24 are coupled with the male and female connectors 18 and 20 of the motorcycle, thereby allowing fuel to flow through the fitting body 22 . When the fittings 26 and 24 are disconnected, a spring 52 in each of the valves 50 closes the valve 50 by allowing a valve member 54 to seal against an annular seat 56 formed by an O-ring, thereby stopping the flow of fuel through the fitting.
Fitting body 22 further features a drilled and tapped pressure gauge port 30 (not shown in detail) which receives pressure gauge 32 . Valve 34 is also a threaded into an associated threaded valve port 36 (not shown in detail) and includes an internal plunger type valve 38 , which is normally closed. Internal components of plunger valve 38 may be similar to or identical with Schrader type inflation valves found in vehicle tires. When plunger end 40 is depressed, a fuel flow path opens through valve fitting 36 and into nipple 42 having relief and gas flow hose 44 attached thereto. The internal cavity of fitting body 22 communicates with internal passageway 25 of each of fittings 24 and 26 , as well as ports 30 and 36 .
FIGS. 4 a and 4 b show two embodiments of valves 38 ′ and 38 ″ that may form manually operated valve 38 . Valve 38 ′ of FIG. 4 a is a spring-loaded seat valve operated by a ramp 62 that is moved by the plunger end 40 of plunger 60 ′. The plunger 60 ′ is biased outward by a spring 64 so that valve 38 is normally closed. Upon pressing plunger end 40 , the ramp 62 acts on valve member 64 against a valve spring and removes the valve member 64 from its valve seat. Seat valves have the advantage that elastic components can compensate for manufacturing tolerances so that productions costs are low.
While not shown, a seat valve may alternatively be arranged coaxially with the plunger 60 ′, for instance a valve similar to the one in the female fitting, where the valve member is biased toward the plunger end 40 and rests on a valve seat between the valve member and the plunger. The valve member may be arranged in the fitting body between the nipple 42 on one side and the male and female fittings on the other side. This arrangement would have the advantage that the pressure inside the fitting body 22 acts on the valve in the valve closing direction.
FIG. 4 b shows a machined sliding valve 38 ″. Plunger 60 ″ has an internal channel extending from its distal axial face to a radial opening 66 that normally has no overlap with a radial bore 68 through nipple 42 . Upon pressing plunger end 40 , the radial opening 66 is aligned with the radial bore 68 , thus establishing a fluid communication of male and female fittings 24 and 26 with bore 68 . A sliding valve has the advantage that the pressure inside the fitting body 22 acts on the plunger in the valve closing direction so that the valve 38 ″ cannot be opened by a high internal pressure.
Use and operation of pressure tester 10 will now be described with reference to FIG. 2 . As mentioned previously, in the normal operating condition of the motorcycle, fuel line 16 is connected with fuel tank 12 through quick connect fittings 14 and 18 . When it is desired to conduct a static, idle, or part-load pressure test, pressure tester 10 is inserted in-line with fuel line 16 , as shown in FIG. 2 . Pressure tester 10 does not interfere with the flow of fuel from the fuel tank 12 to the associated engine, enabling it to be operated during the testing process. Some motorcycles are designed such that its electric fuel pump will not operate without the engine running as a safety feature to prevent a dangerous fuel spillage condition from occurring. When pressure tester 10 is installed as shown in FIG. 2 , the associated motorcycle engine may be operated, for example in an idle condition. Such operation will cause the internal fuel sending unit within the tank 12 to be activated, supplying pressurized fuel through pressure tester 10 and into fuel line 16 . Pressure gauge 32 reads the pressure of the fuel within the fuel line. This can be used as a diagnostic tool to determine if the measured pressure is within predetermined limits for a partial load condition. In this operating condition, plunger valve 38 is not operated.
For motorcycles that allow the fuel pump to operate to provide a fuel pressure without operating the engine, a static fuel pressure test can be performed by starting the fuel pump, but not the engine, so that no fuel flow occurs through the fuel line 16 .
If it is only desired to conduct a static or partial load pressure test, after reading pressure from pressure gauge 32 , pressure tester 10 may be removed after shutting off the motorcycle engine. Since pressurized fuel remains within the fuel system after the sending unit is deactivated, it is desirable to provide a pressure relief feature. This is provided by plunger valve 38 and its connection with hose 44 . The distal end of hose 44 can be placed into fuel tank 12 's fuel filler opening (not shown), and the plunger end 40 may be depressed, which will squirt a small quantity of fuel into the tank. This relieves pressure in the tester 10 and the associated fuel delivery system components of the motorcycle, and enables the tester to be disconnected without a spray of fuel at the connections.
Pressure tester 10 may also be used to provide a fuel system load pressure test in which fuel system pressure is measured while the fuel system is delivering fuel at a high flow rate, for example, equivalent to a maximum-load, full-throttle condition of the engine, but without requiring the motorcycle engine to be operated at the full-throttle condition. This can be done by depressing plunger end 40 while the vehicle is engine is running at idle, and placing the distal end of hose 44 into the tank fuel filler opening. In this case a small flow of fuel is flowing through fuel line 16 to the engine, which is operating at an idle condition. However, a significant flow rate of fuel occurs through valve 34 and hose 44 and, therefore, the fuel system components in fuel tank 12 are delivering fuel at a high rate simulating a full-throttle, full-load operating condition. To this end, the path to and through the valve 34 may be provided with a calibrated orifice dimensioned for a fuel flow that corresponds to the difference between the fuel consumption of the idling engine and the fuel consumption of the engine run at full throttle to that the sum of the fuel flow through the fuel line 16 and through the hose 44 properly simulates the fuel flow through the fuel line 16 when the engine runs at full throttle. Instead of a calibrated orifice, the pressure tester 10 may in its entirety inherently have an overall maximum flow capacity through hose 44 that corresponds to the difference to the difference between the fuel consumption of the idling engine and the fuel consumption of the engine run at full throttle.
In analogy, the above-described test may be likewise performed by only operating the fuel pump with battery power without starting the engine, where possible. The fuel flow through hose 44 simulates an operating engine. The fuel consumption of an idling engine is very low compared with a full-throttle condition so that the lack of fuel flow to an idling engine may be insignificant for measuring purposes. It is, however, conceivable to provide for a variety of insertable orifices (not shown) that are dimensioned for simulating various operating conditions with or without a running engine.
Pressure as measured by pressure gauge 32 is recorded to determine if it meets manufacturer specifications for such operating conditions. After either the static (partial load) or a load test, the engine is stopped and pressure tensor tester 10 is disconnected after relieving any residual pressure in the system by a depressing plunger valve end 40 .
A venting tool with a post 46 is provided which is attached to pressure sensor 10 by a flexible strap 48 . Venting post 46 is provided to be inserted into female fitting 26 to depress its internal valve member 54 to permit drainage of fuel in tester 10 after it is disconnected from fuel tank 12 . When simultaneously the plunger end 40 is depressed, the drainage occurs by the force of gravity through hose 44 .
While the above description constitutes the preferred embodiment of the present invention, it will be appreciated that the invention is susceptible to modification, variation and change without departing from the proper scope and fair meaning of the accompanying claims.
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A fuel system pressure tester for motorcycles adapted to be connected in-line with a fuel tank female fitting and a fuel line male fitting, has a fitting body, a first fitting for connection with the fuel tank fitting with an internal, normally closed valve, a second fitting for connection with the fuel line fitting, a pressure gauge, and a manually operated valve with a valve actuating element and a connection for a fuel hose. The fitting body has an internal passageway connecting the first fitting, the second fitting, the pressure gauge, and the manually operated valve. A method of testing a fuel system of the motorcycle involves connecting the pressure tester to the fuel tank by connecting the male tester fitting with the fuel tank female fitting, and connecting the female tester fitting with the fuel line male fitting, energizing the in-tank fuel sending unit, and reading pressure within the tester indicated by the pressure gauge.
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This application claims benefit of provisional patent application Ser. No. 60/360,919, filed Feb. 28, 2002.
TECHNICAL FIELD
The present invention relates to document handling, in particular to feeding of envelopes and other flat articles, of intermixed size and thickness, to a slitting device or other document processor.
BACKGROUND
Organizations which receive a lot of mail have automated and semi-automated labor-saving devices to handle and open the mail, by orienting and slitting the envelopes and extracting the contents for processing. There are various types of commercial machines that are well suited to handling envelopes that are of nearly the same size, such as for instance standard envelopes bearing payments for a utility company. In essence, such machines must first singulate envelopes, that is, select and feed one envelope after another from a stack, so they can be slit or otherwise processed one by one.
However, when the envelopes within a lot being processed vary in shape and especially thickness from piece to piece, then many prior art machines are less effective at singulating. Thick envelopes will jam at the singulator nip if the machine is configured for thin envelopes. Mis-feeding, of multiples of thinner envelopes, occurs when the machine is configured for the thicker envelopes. Thicker envelopes tend to have somewhat variable and indefinite wedge shape edges. Larger and thicker flat envelopes present special problems because they resist aligning against a downstream hopper surface in orderly fashion, and may even be shingled in the direction opposite of the direction of feeding. Whether or not thickness varies greatly, intermixed large and small shape envelopes present handling problems.
Another problem that attends many commercial envelope handling machines is the tendency for roller or belt surfaces to become fouled by debris picked up from the surfaces of the envelopes or other articles. When that occurs, frictional engagement with the articles diminishes, and any singulating or feeding action becomes impaired. To restore functionality, the machine has to be stopped so the rollers or belts can be cleaned or replaced.
The weight of a stack can create high inter-envelope friction among the bottommost envelopes, impeding singulating. On the other hand, when there are hardly any envelopes in the hopper, poor feeding and singulating can take place because of low friction in the system. Thus, there tends to be a need for continuing operator intervention, to correct deviations, or to maintain the hopper stack within some maximum and minimum range. Still another problem with prior art machines is that when envelopes, particularly ones which vary in size and shape, are put in a hopper for feeding to a singulator or document handling device, there is a tendency for them to “hang up”, or to lightly wedge in the hopper, and to cease dropping down as each bottommost envelope is fed away. A machine will then cease processing of items until the operator intervenes to aid the downward feeding manually.
Thus, even though there has been a lot of past development, and there have been many designs of machines for handling envelopes and other flat objects, there continues to be a need for improvements in the ways that have been mentioned.
SUMMARY
An object of the invention is to provide apparatus and method for feeding and singulating envelopes and other flat articles, which vary in shape and especially thickness within a lot being processed, as well as when there is reverse shingling. Another object is to processing of flat articles while minimizing the tendency for debris to disruptively accumulate on feeding belts; and, to extend the life of feeder or singulator belts. A still further object is to have consistent singulating performance, whether a feed hopper is full or virtually empty.
In accord with the invention, apparatus comprises at least two substantially similar singulator assemblies which are spaced apart transversely above the article flow path, and means for moving flat articles, such as a transport belt, to move articles from a stack to the nip formed by the singulators. Each singulator is comprised of an endless elastomer belt running around rollers and a body which is pivotably urged downwardly, toward the means for moving. The underside portion of the singulator belt slopes downwardly toward the means for moving, preferably at an angle of 30-45 degrees to the horizontal. The singulating nip is formed between the singulator assembly and the transport belt or other moving means. The elevation of the sloped belt portion is sufficient to enable a plurality of articles from the stack being processed to contact the belt, to become shingled, and to have their leading edges moved in a desirable way toward the singulator nip. Preferably there are two transport belts, one corresponding with each singulator assembly. Alternately, a single transport belt may be used. More than two singulators may be used.
During operation of the apparatus, the singulator belt intermittently touches the transport belt or other moving means, in the moment when articles are not present in the singulator nip. There are means for resisting singulator belt motion, and the belt is for the most time stationary. But the belt incrementally moves around the singulator over time, with repetitive passage of articles through the singulating nip, whenever the threshold resistance to motion which is designed into the singulator is exceeded.
Preferably, the pair of singulators is connected by a rotatable shaft, to which the respective upper rollers are affixed. One of the singulators has a smaller diameter upper roller than the other, and they are otherwise substantially the same. The effect of the different diameter rollers is to create a “fight” between the singulators, and thus the desired resistance to motion. Less preferably, brakes and other means may be used. Additional resistance to singulator belt motion is created by articles pressing against the underside of the singulator belt, due to the drag effect of underlying articles being drawn toward and through the singulator nip. Thus, when both singulator belts touch their respective identically moving transport belts, the desired scuffing is created, and there is a slight incremental movement of the singulator belt around its rollers. Continuous contact of the singulator belt(s) with the transport belts causes the singulator belt to move continuously, inasmuch as the resistance breakaway threshold is exceeded.
Preferably, the articles such as envelopes are contained in a hopper; and the upper end of the each singulator belt protrudes into the downstream wall of the hopper. The protruding belts help alleviate the weight of a heavy stack of envelopes on underlying articles. When envelopes become hung up in the hopper, the absence of envelopes approaching the sloped underside of the singulator causes the singulator belts to contact the transport belt and thus be moved. The belt motion at the upper end of the singulator desirable tends to push the leading edges of the envelopes downwardly, to alleviate the jam.
Preferably, the apparatus includes dual takeaway assemblies, downstream of the singulator assemblies, for carrying away articles, which exit the singulator nips. Each takeaway assembly includes a roller mounted on the shaft which moves the transport belts.
The aforementioned functioning of the apparatus entails a unique method of feeding and singulating articles. The apparatus processes at high speed intermixed articles having varying thickness and shape, especially width, and thicker envelopes that have tapered edges. The foregoing and other objects, features and advantages of the invention will become more apparent from the following description of preferred embodiments and accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top view of apparatus for feeding and singulating envelopes which has various assembly pairs positioned on either side of a support strut and the flow path.
FIG. 2 is a side view of the apparatus of FIG. 1 , showing a stack of envelopes being fed from the hopper.
FIG. 3 is a top view of an alternative singulator body configuration.
FIG. 4 is a partially schematic top view, corresponding with FIG. 1 , showing an alternative embodiment which comprises a single transport belt.
FIG. 5 is a side view of a three roller singulator assembly.
FIG. 6 shows a cut-away portion of the upper end of a singulator assembly, indicating how a brake is used to retard motion of the upper roller and belt.
DESCRIPTION
While the invention is described in terms of handling flat envelopes for slitting, the invention will be suited for feeding other flat articles for other purposes. The apparatus has various mechanical elements, including such as rollers, conveyors and belts, which are similar in construction and material to those in apparatuses described in U.S. Pat. No. 5,971,389 “Feeder for Flat Articles of Varying Thickness” and U.S. patent application Ser. No. 08/962,077 “Sheet Feeding Apparatus”, filed Sep. 14, 1998, for which the applicant here is inventor or co-inventor. The disclosures thereof are hereby incorporated by reference, as is the disclosure of provisional patent application Ser. No. 60/360,919, filed Feb. 28, 2002 by applicant. The apparatus described below is mostly constructed of common aluminum structural alloy. Other metals and structural plastics may be used, within ordinary engineering skill.
FIG. 1 is a top view and FIG. 2 is a side elevation view of the apparatus. Envelopes are drawn from a stack contained in a hopper 10 and are moved downstream along the envelope flow path 13 . The envelopes that are drawn from the hopper pass first through a singulator nip 52 and then through a takeaway nip 50 . The envelope handling is carried out by two nearly identical assemblies, 15 N and 15 F, spaced apart transversely across the flow path. In the FIGS. 1 and 2 embodiment, they are on either side of the strut 25 . The assemblies 15 F and 15 N are substantially identical, but have different size upstream rollers, 23 N and 23 F, described in more detail below. In the Figures and this description, the parts of paired assemblies have identical numbers, but some are called out in the drawing by a suffix, N or F, according to which side of the flow path the particular item lies, to aid in comprehension of the drawings. Other suffixes are used for the corresponding parts of alternative embodiments. An assembly 15 will now be described, as exemplary of the two assemblies 15 F and 15 N.
Assembly 15 is comprised of a three assemblies 20 , 30 , and 40 . Transport assembly 30 moves the envelopes along the flow path from the hopper and through the singulator nip. Singulator assembly 20 is mounted above the transport assembly, with which it cooperates to form nip 52 , which is just downstream of the downstream end of hopper 10 . Takeaway assembly 40 is mounted downstream of the singulator assembly. The subassemblies 20 and 40 are supported off main strut 25 which extends downstream from hopper 10 , above and parallel to the flow path 13 . The hopper and main strut are mounted on an unshown base, as is the transport assembly.
Transport assembly 30 is comprised of elastomer belt 11 which runs over opposing end transporter rollers 54 , 58 . Roller 58 is fixedly mounted on and driven by shaft 60 which is driven by an unshown motor. Roller 54 is an idler running on shaft 55 .
Takeaway assembly 40 is comprised of roller 5 which presses against roller 4 . Roller 4 is on shaft 60 , next to transport belt 11 where it runs over transport roller 58 . Rollers 4 and 58 are both fixedly attached to and rotated by driven shaft 60 . Roller 4 forms a take away nip 50 with roller 5 , which is mounted at the end of H-shape takeaway body 62 . Body 62 is pivotable in the vertical plane from fixed shaft 57 , which projects transversely from strut 25 . Body 62 is spring biased downwardly by spring 7 , which is captured in a cavity within body 62 , and bears against the lever arm of collar 59 , which is fixed to the shaft 57 . The downward spring force applied to roller 5 is sufficient to cause frictional engagement between the envelope and roller 4 , and to move the envelope downstream to the unshown slitter or other processing device, after the envelope exits the singulator nip.
Roller 4 is larger in diameter than belt 11 where it runs around roller 58 . Thus, during operation the effect of rollers 4 and 5 of the takeaway assembly will be to draw envelopes from the singulator nip 52 at a speed faster than the speed of the transport belt 11 , which is nominally the speed with which envelopes are moved through the singulator nip. Roller 5 is made of soft elastomer material such as polyurethane or rubber having 70-80 Shore Durometer hardness, while the driven roller 4 is made of stainless steel or chromium plated carbon steel and has a polished surface.
Singulator assembly 20 comprises belt 56 which runs endlessly around an upper roller 23 N/ 23 F and lower idler roller 21 , at opposing ends of H-shape body 9 . The upper end of body 9 is pivotably mounted on shaft 33 . Shaft 33 is journaled in, and freely rotatable in, a bearing running transversely through strut 25 . The upper rollers 23 N and 23 F are fixed to the common shaft 33 . The underside of belt 56 runs downwardly at an incline. The lower end of belt 56 , where it runs around roller 21 , is adapted to contact the transport assembly belt 11 , and create nip 52 . Gravity and torsion spring 70 urge the body 9 to pivot downwardly, so it contacts transport belt 11 when there is no article in the nip. The phantom 54 of the singulator assembly in FIG. 2 shows how assembly 20 pivots upwardly against the spring bias when an envelope 26 passes through the nip 52 .
The elevation of the shaft 33 relative to the transport belt surface and the length of body 9 are selected so that the bottom surface of the belt 56 runs at an angle B to the horizontal of about 30-45 degrees, preferably about 37 degrees. When singulator belt 56 contacts moving belt 11 in the absence of any envelope in the singulator nip 52 , the belt 56 is moved around its rollers.
As mentioned, singulator assembly 20 N differs from the opposing side assembly 20 F with respect to the rollers 23 . That difference is intended to create “fight” between the motions of the opposing side singulator belts 56 F, 56 N, when the belts engage envelopes or rest on their respective transport belts 11 . The “fight” creates resistance to motion of the belts around their respective rollers. In the embodiment shown in FIGS. 1 and 2 , roller 23 F is slightly but significantly smaller in diameter than roller 23 N. For instance, the ratio between the diameter of roller 23 F to that of 23 N is 25/26. The effect is to make the breakaway threshold, or the point at which a driving force on the belt overcomes the resistance of the belt to motion, a bit lesser for assembly 20 F than for assembly 20 N. Of course, when the force applied to either belt exceeds the breakaway threshold both belts will move.
Since the belts are identical, the tension in the belt 56 F of singulator assembly 20 F will be less than the tension in belt 56 N of singulator assembly 20 N, according to the difference in lengths around the rollers of the two singulators. And also, therefore, the smaller diameter of roller 23 F makes the belt of singulator 20 F want to rotate the roller 23 F faster than does the belt of singulator 20 N want to rotate the roller 23 N. But, both rollers 23 are fixed to the same shaft 33 , and thus the “fight” is created. The result of the fight is resistance to movement by both belts when driving force is simultaneously applied to both belts, as when each belt 56 contacts an envelope moving through nip 52 or same-speed transport belts. Other forces, described below, add to effect of the different diameter rollers in making the belts resist motion. When stationary belts 56 contact moving belts 11 , there is a resultant desirable scuffing action, which tends to clean debris the belts.
The result of the fight and lower tension and lower resistance to motion for belt 56 F of singulator 20 F, compared to belt 56 N, is that belt 56 F will slip in creeping fashion around the roller 23 F, when the forces acting on belt 56 s are sufficient to move the belts 56 . So, over time, there is small, but cumulatively significant, difference in relative movement between the belts 56 F and 56 N in context that both belts move. Over time, both belts 56 move around their respective rollers in the direction indicated by an arrow in FIG. 2 . New portions of the belts will continuously be presented at the nip, as described further below. Thus, wear on the belts 56 due to scuffing action at the nip is distributed along the surface of the belts, as is accumulation of debris which scuffing does not remove. Relatively infrequent operator attention and maintenance is required.
The breakaway threshold, where resistance to motion of the singulator belts is overcome, is predetermined and can be changed by design. For instance in the preferred embodiment being described, tension is lowered in the less tensioned and first-to-slip belt, i.e. belt 56 F. That may be accomplished by changing either diameter of roller 23 F, or the center-to-center distance of the rollers, or less practically, the length of the belt.
The operation of the apparatus is as follows. Referring particularly to FIG. 2 , a first envelope 26 , which lies on the surface of belt 11 , enters singulator nip 52 . As the envelope passes through nip 52 , the leading edge enters the takeaway nip 50 . But until the transport belt causes the trailing edge to exit nip 52 , the takeaway roller 4 slips against the underside of the envelope. Once the envelope exits the singulator nip 52 , it is accelerated by the takeaway nip, to be ejected from the machine. When a first envelope exits nip 52 , the next or second envelope, which has been pressing against the underside of the belt 56 , has to accelerate into the nip. During that process, for a brief moment nothing is in the nip, and belt 56 contacts belt 11 , to achieve the desirable scuffing action, as belt 11 seeks to accelerate belt 56 .
The breakaway threshold for belt motion is by design set so that when there is continuous contact of belt 56 with belt 11 , belt 56 will be driven around its rollers. When processing envelopes continuously, the area and time of contact between the belts 56 and 11 is very small. However, when processing tens of thou sands of envelopes per hour, the cumulative effect of such contact, in combination with the effect of dropping down of envelopes, which are pressing against the sloped upstream underside of the belt 56 , is that there will be a continuous creeping motion of the belt 56 around the rollers. This is further explained below.
When a first and bottommost envelope enters into and is passing through nip 52 , the singulator body 9 rotates upwardly toward phantom position 54 . As the first envelope passes through the nip, overlying envelopes are frictionally dragged downstream toward the nip. However, they are reared from passing through the nip because of contact with the sloped underside of the then-stationary belt 56 . Since the overlying envelopes are continuously dragged downstream, with removal of successive bottommost envelopes, they become shingled and press against the underside of belt 56 . A feature of the sloped underside of the belt 56 is that the leading edges of common envelopes, being tapered or wedge shaped, are deflected downwardly toward the nip, and the result is more assured singulating at the nip.
Once a first envelope has exited the singulator nip, the stacked and shingled overlying envelopes which are pressing against the underside of the belt 56 drop downwardly. When pressing against the belt prior to dropping, the envelopes exert a retarding or resistive force against belt motion. When the envelopes drop downwardly toward the transport belt, the pressing force is momentarily lessened. That aids in the incremental motion of the belt, in the direction which is induced by the scuffing. Motion of belt 56 ceases when the first envelope is passing through the nip, and the stationary belt of course carries out the singulating function by hindering the second envelope from entering the nip. The operation continues until the supply of envelopes in the hopper is exhausted.
The apparatus can handle stacks where there is “reverse shingling” of some or all of the envelopes. Suppose one envelope is in the stack “reverse shingled”. That means the downstream end of an envelope is more upstream than the downstream end of the envelope that overlies it. Suppose that the shingling effect caused by transport belt induced drag is insufficient to overcome the degree of reverse shingle. Even so, the apparatus will function properly, inasmuch as, when the reversed shingle envelope drops down onto the transport belt, it will be caused to advance toward the nip.
The singulator belts are flat and preferably made of molded natural rubber compound having a hardness in the range 60-80 Shore Durometer. The transport belts are preferably a flat laminated timing belt having a polyurethane surface of 50-80 Durometer.
The different diameter singulator rollers may be connected to one another by more complicated means than the simple shaft 33 , for instance by a gear or pulley train. In the generality of the invention, means other than different diameter rollers can be employed for creating the resistance to motion in the opposing side singulator belts 23 . For instance, a brake may be applied to one or two of the rollers 23 in the apparatus of FIG. 1 . For another instance, the rollers 23 may be independently mounted and controlled. See FIG. 6 , where upper singulator roller 23 C rotates on a fixed shaft 33 C which extends transversely from strut 25 . Brake 72 applies adjustable frictional force to the roller to retard rotation. The body 9 is omitted from the Figure for clarity. The opposing side singulator will be similarly constructed. Brakes are less desired because they require more parts, adjustment, and even sensing and control equipment, and concentrated heat is generated. Other means for providing the desired threshold resistance may be employed.
The downstream wall of the hopper 10 is spaced apart from the top surface of transport belt 11 by a distance G. See FIG. 2 . The dimension G is made small enough so that stacked envelopes which are frictionally drawn downstream by the transport belt will contact only the downward sloped portion of belt 56 , on the underside of singulator body 9 . The distance G is made large compared to thickness of envelopes, sufficient to enable a multiplicity of envelopes to contact the sloped belt portion. For instance, G might be 5 cm, where envelopes may vary from 0.1 to 0.6 cm in thickness. In operation, the sloped portion of belt 56 is of such length that during use, it will be contacted by a multiplicity of envelopes at any given time.
Following common practice, the hopper sidewalls are inclined with respect to a vertical centerline plane, so that envelopes in the stack will shift toward one sidewall of the hopper and become aligned in the transverse direction. Thus, when the envelopes are deposited on the transport belt, one edge will be at a known location with respect to the flow path; and envelopes can be appropriately delivered to a slitting device downstream from the takeaway section.
In one embodiment and use, all the envelopes are of substantially similar shape, but of varying thickness. In such case, a pair of singulator assemblies will preferably be located on either side of the centerline of the flow path and of the articles being processed. In another embodiment and use, the envelopes have different shapes, most importantly different widths. They may or may not be of varying thickness. In such case the pair of singulator assemblies will be located so both engage the smaller width articles, which will be guided by a fence 76 , shown in FIG. 1 , running along one side of the apparatus. The fence may be laterally adjustable for aligning envelopes with a slitter. Large width articles intermixed with the small articles will also be guided by the fence. There is no fence on the opposite side of the device/flow path. Thus, there is no constraint on handling the large article. While the centerline of large article will be offset from the centerline of the singulator pair, good functioning is not impaired. Thus, the apparatus and method is quite adaptable to processing different shape and thickness envelopes.
The upper end of each belt 56 , where it rotates around roller 23 , protrudes through a slot at the bottom of the downstream vertical wall of hopper 10 , into the hopper interior. Thus, when the stack is large enough, the downstream ends or leading edges of envelopes, stacked within the hopper, contact the upper end of belt 56 , when move downwardly under force of gravity as underlying envelopes are being removed. To move downwardly past by the upper ends of belt 56 s , the envelopes will necessarily be thrust rearwardly a small amount. The feature is useful in several respects. First, some of the downward force due to weight of the stack is taken off the underlying envelopes. That makes it easier for those envelopes to become shingled when they enter gap space G. Second, there is a friction force on the belt 56 at roller 23 , which provides resistance to belt motion, which is desired. Third, suppose envelopes are jammed within the hopper just above the belt at roller 23 . As underlying envelopes are fed through the singulator, there will quickly be no envelopes pressing against the underside of the belt 56 , and none entering the singulator nip. Belt 56 will thus drop into contact with the belt 11 and be continuously driven. The resultant motion of the belt 56 where it runs around roller 23 will tend to push the leading edges of the envelopes downwardly, into the gap G, alleviating the jam. To protect the belts from undue wear in the event that the hopper is emptied, micro-switch or optical sensing means with controls are used, to shut down the transport drive motor when no new envelope falls onto the transport belts after a pre-set timeout period.
Thus, to summarize, in the preferred embodiment, there are three retarding or resistive forces applied to the belt 56 , namely: (1) frictional resistance to belt motion induced by the different diameters of the upper rollers 23 , alternately by other means; (2) the front ends of the stacked envelopes contact and rub against the underside of belt 56 ; and, (3) the belt 56 running around either roller 23 protrudes into the hopper and engages envelopes in the hopper. The complexity of forces provides good function under a variety of conditions, including the state in which the hopper is heavily loaded and the state in which the envelopes in the hopper are nearly exhausted.
Still other embodiments and variations may be employed. The elements which are mounted from the fixed central strut 25 can be mounted off a different rigid structure, so the same spatial relationships are achieved. More than two singulator assemblies and associated other parts can be used in an apparatus. For example, a third singulator, mounted in parallel with the others can have resistance to motion which is the same as one of the other two, or all three singulators can be set differently. Still more singulators may be used.
As illustrated by FIG. 3 , a singulator (or takeaway) body 9 A can be a simple beam, and not of H-shape, with the belt 56 A running on cantilevered rollers. The singulator can have more than two rollers. As example, FIG. 5 shows a three roller singulator 74 , having a triangle shape body 9 A, including a nip forming roller 21 A and an upper roller 23 A about which the body pivots. While the springs are preferred for downwardly biasing the singulators and takeaway body, other means for accomplishing such may be employed, including other kinds of resilient means and deadweight.
As shown in FIG. 4 , which is a schematic top view which corresponds with FIG. 2 , there may be only a single transport belt 11 A, with opposing side takeaway rollers 4 positioned outboard of the belt. In still another alternative, there is no transport belt. Instead, a series of driven rollers protrude through the surface of a platform running along the flow path, with one resilient surface roller positioned under each singulator, to form the nips. However, in such embodiment the nip roller would be much more subject to wear and fouling than would be the belt.
In the generality of the invention, the takeaway unit can be a separate spaced apart device. Alternatively, there need not be a takeaway unit, and envelopes may be just carried away and discharged by the transport belt, in the same manner as they are delivered to the singulator nip. While a hopper is preferred for depositing articles on the transport belt, other means, including manual means, may be used, although there will then not be the desirable interaction of envelopes with the upper ends of the singulator belts, and performance may be somewhat degraded.
The apparatus which has been described is not only better at handling articles of varied dimension, and at continuing operation with low operator intervention, compared to machines in the prior art, but it is capable of doing so while processing up to forty thousand envelopes per hour.
Although this invention has been shown and described with respect to a preferred embodiment, it will be understood by those skilled in this art that various changes in form and detail thereof may be made without departing from the spirit and scope of the claimed invention.
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Two belt type singulators are used in apparatus which feeds and singulates stacked articles which have varying thickness and shape. The singulators form tandem, spaced apart singulator nips with a transport belt. Each singulator belt has a downwardly sloped underside and moves incrementally around its rollers over time, overcoming certain applied resistive forces. The singulator belt has intermittent contact with the transport belt, when articles are being processed, and there is a resultant scuffing of belts which helps remove debris. Preferably, on off the forces which resists singulator belt motion is created by having a singulator pair with upper rollers, which are rotationally coupled but which have different diameters. The upper ends of the singulator belts project into the hopper which holds the stack and aid in the feeding of articles toward the singulating nips.
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BACKGROUND OF THE INVENTION
1. Field of Invention
The present invention provides a method for cutting concrete in a manner whereby unique three-dimensional shapes are formed.
2. Description of the Prior Art
Apparatus for cutting concrete have been available in the prior art. For example, U.S. Pat. No. 5,579,753 to Chiuminatta et al discloses a saw for cutting grooves in the surface of wet concrete. The speed of a variable speed transmission device connected to the wheels used to propel the saw across the concrete during cutting is controlled, the speed being dependent upon whether the saw is cutting hard aggregate or soft concrete.
U.S. Pat. No. 5,223,200 to Schulz et al discloses a method for making concrete roof tiles. Specifically, a continuous layer of fresh concrete is deposited on pallets supplied in a continuous row and is subsequently compacted, the compacted layer of fresh concrete being cut into roof tile moldings of equal length with a front and a rear edge, the front edge also being trimmed.
Although the prior art exemplified above discloses various concrete cutting apparatus and techniques for forming particularly shaped concrete blocks, the prior art shaped blocks are utilized in construction related projects.
Processes for forming designs from various materials are also well known. For example, porcelain and glass bases for lamps have long been available. However, techniques for cutting formed concrete into designs that have consumer appeal are not currently available. What is thus desired is to provide a process for producing designs from formed concrete, the designs either having utilitarian features or created solely for its aesthetic appearance.
SUMMARY OF THE PRESENT INVENTION
The present invention provides a method of cutting formed concrete into shapes which can be used for specific functions, such as lamp bases, or solely for its aesthetic appearances.
The concrete is cut into the desired shaped piece using a diamond cutting tool. Flat surfaces that result from the cutting are polished using an abrasive disc wheel. An adhesive, clear coating is then applied to the cut aggregate and allowed to dry. Large pieces may have a core portion removed in order to reduce weight. The resulting piece is highly aesthetic and has many uses, such as lamp bases, paper weights and sculpture.
The process is simple and relatively inexpensive and provides a new form of decorative art having many uses.
DESCRIPTION OF THE DRAWINGS
For a better understanding of the invention as well as other objects and further features thereof, reference is made to the following description which is to read in conjunction with the accompanying drawing wherein:
FIG. 1A illustrates a block of concrete aggregate; and
FIG. 1B is a simplified plan view of a diamond concrete cutting tool;
FIG. 2A illustrates the concrete block of FIG. 1 cut to a desired shape; and
FIG. 2B is a simplified view of a abrasive grinding tool;
FIG. 3A illustrates the concrete block after the flat edges are ground; and
FIG. 3B is a view illustrating the application of a clear adhesive to the surfaces of the piece illustrated in FIG. 3A; and
FIG. 4 illustrates the piece of FIG. 3A, after application of the clear adhesive, formed as a lamp base.
DESCRIPTION OF THE INVENTION
Referring now to FIG. 1A, a concrete block 10 is illustrated. Formed concrete having aggregate therein is commonly available in block form, typically from sites whereat old buildings are being, or have been, demolished. As shown in FIG. 1B, a cutting tool 12 having a cutting surface 14 comprising diamonds is positioned to cut block 10 into a predetermined shape. A cutting tool which has been successfully utilized is the Meco 4 Speed Drill, manufactured by Meco Engineering Company, Prescott, Ariz. A cutting surface which has been utilized successfully is the Model PL10C 18×25 diamond cutting bit manufactured by Pro Link Diamond, Irvine, Calif. FIG. 2A illustrates one of numerous shapes that can be cut in accordance with the teachings of the invention. The particular shape illustrated is a wedge shaped piece 16 having flat surfaces 18 , 20 and 22 .
In accordance with the teachings of the invention, a masonry type grinder device 24 , preferably using an abrasive disc wheel 26 , is used to polish flat surfaces 18 , 20 and 22 . FIG. 3A illustrates polished piece 16 . The next step of the inventive method is to apply a coating of clear, shining material to the surfaces of piece 16 . As illustrated in FIG. 3B, a coating material (illustrated as stored in receptacle 26 ) is applied to the surfaces of piece 16 by brush 28 . A preferred material which has been successfully utilized is polyurethane. Polyurethane highlights the color of the aggregate and provides viewing depth. Three coats have been applied to provide the desired effect, the second coating being applied after the first coating dries, the third coating being applied after the second coating dries. The total drying time is approximately twenty-four hours (other coatings, such as lacquer, can be used although lacquer will require more than three coatings).
FIG. 4 illustrates one application of the present invention. In particular, a hole is formed in piece 16 and a lamp structure 30 is secured therein, piece 16 forming a unique lamp base.
Concrete material can be removed from the piece 16 to reduce the weight thereof. In this case, a Model D5246 bit (6 inches) manufactured by Cushion Cut, Torrance, Calif., has been used to remove core material from shaped concrete pieces for weight reduction purposes.
The present invention thus provides a simple and cost effective technique for forming unique and aesthetically pleasing designs from concrete.
While the invention has been described with reference to its preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the true spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its essential teachings.
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A method of forming a decorative shape from a concrete block by cutting the block into a predetermined shaped piece, polishing all flat surfaces and then applying a coating of clear material to the surface of said piece.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application relies on, and claims the benefit of, the filing date of U.S. Provisional Application Ser. No. 60/085,234, filed May 13, 1998, the disclosure of which is hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the field of biochemical assays involving regulated expression of reporter genes, and to mutant strains of bacteria useful in biochemical assays. More particularly, it relates to methods of screening for molecules capable of affecting expression and/or activity of type III secretion machinery in gram-negative bacteria.
2. Description of Related Art
Type III secretion machinery is present in numerous gram-negative bacteria (including members of the species Shigella, Salmonella, Yersinia, Escherichia, Pseudomonas, Xanthomonas, Ralstonia, and Erwinia) that are pathogenic for man, animals, and plants. For example, the Sec-independent type III secretion pathway is involved in secretion of Yersinia anti-host proteins. In Salmonella and Shigella species, it is involved in the process of entry into epithelial cells. It is also implicated in EPEC signal transducing proteins, Pseudomonas aeruginosa toxins, and virulence factors of many plant pathogens, as well as in flagellum assembly of bacteria such as S. typhimurium and Bacillus subtilis.
Features of this secretion pathway can include activation of secretion by contact of the bacterium with host cells (Menard et al., 1994, "The secretion of the Shigella flexneri Ipa invasins is activated by epithelial cells and controlled by IpaB and IpaD.", EMBO J., 13:5293-5302; Watarai et al., 1995, "Contact of Shigella with host cells triggers release of Ipa invasins and is an essential function of invasiveness.", EMBO J., 14:2461-2470; Zierler and Galan, 1995, "Contact with cultures epithelial cells stimulates secretion of Salmonella typhimurium invasion proteins InvJ.", Infect. Immun., 63:4024-4028); that some of the secreted proteins are delivered into the cytoplasm of host cells (Rosqvist et al., 1994, "Target cell contact triggers expression and polarized transfer of Yersinia YopE cytotoxin into mammalian cells.", EMBO J., 13:964-972; Sory and Cornelis, 1994, "Translocation of an hybrid YopE-adenylate-cyclase from Yersinia enterocolitica into HeLa cells.", Mol. Microbiol., 14:583-594; Wood et al., 1996, "SopE, a secreted protein of Salmonella dublin, is translocated into the target eukaryotic cell via a sip-dependent mechanism and promotes bacterial entry.", Mol. Microbiol., 22:327-338; Collazo and Galan, 1997, "The invasion-associated type III system of Salmonella typhimurium directs the translocation of Sip proteins into the host cell.", Mol. Microbiol, 24:747-756); and that transcription of genes encoding secreted proteins is controlled by secretion of regulatory proteins (Hughes et al., 1993, "Sensing structural intermediates in bacterial flagellar assembly by export of a negative regulator.", Science, 262:1277-1280; Pettersson et al., 1996, "Modulation of virulence factor expression by pathogen target cell contact.", Science, 273:1231-1233).
Based on the observations that (1) the secretion machinery is involved in secretion of factors which are active against the host, and (2) secretion mutants are avirulent, the type III secretion machinery provides an attractive target for the screening of molecules that would prevent or inhibit gram-negative bacteria from secreting their virulence factors. However, the search for molecules capable of inhibiting the secretion mechanism has previously required two conditions to be present. First, the type III secretion machinery must be active. And second, the product of the secretion activity, i.e., the secreted proteins, must be measurable. Unfortunately, the secretion machinery is, at best, only weakly active when bacteria are grown in standard laboratory media, making the search for inhibitor molecules difficult or impossible. In addition, there is no way to easily measure the presence of a protein secreted in the culture medium by the type III secretion machinery. These proteins do not have an easily assayable enzymatic activity and their secretion must be evaluated using ELISA, which is time consuming and expensive.
SUMMARY OF THE INVENTION
This invention provides mutant strains of gram-negative bacteria that constitutively secrete proteins via the type III secretion machinery.
This invention also provides methods of identifying molecules that are able to activate or inhibit secretion in wild-type strains of gram-negative bacteria. In embodiments, the method comprises the steps of:
a) exposing gram-negative bacterial cells to a sample molecule, wherein said bacterial cells contain a reporter gene transcriptionally fused to a promoter of a gene activated or otherwise regulated by the type III secretion machinery; and
b) detecting the presence or activity of the product of the reporter gene.
To practice the methods of this invention, genes under transcriptional control of the type III secretion machinery are identified. Transcriptional fusions between the promoters of these genes and a reporter gene, such as the lacZ reporter gene, are constructed and introduced into wild-type gram-negative bacteria and mutants of these bacteria that constitutively secrete proteins via the type III secretion machinery, or into bacteria that are deficient for secretion via the type III secretion machinery. The presence (or activity) of the reporter gene product is evaluated under conditions leading to active secretion to demonstrate that the transcriptional activity of these promoters can be used as an indicator of the secretion activity of the type III secretion machinery.
Using Shigella as a model system for the screening of inhibitors of type III secretion, five genes under transcriptional control of the type III secretion machinery have been identified and the promoters of these genes have been used to create transcriptional fusions with the reporter gene, lacZ. β-galactosidase activity can be induced in recombinant Shigella cells harboring these transcriptional fusion constructs under conditions known to lead to active secretion.
Any gram-negative bacteria containing type III secretion machinery may be used in the methods of this invention. Suitable bacteria include members of the species Shigella, Salmonella, Yersinia, Escherichia, Pseudomonas, Xanthomonas, Ralstonia, and Erwinia. Similarly, any suitable reporter gene may be used to create a transcriptional fusion construct for use in the methods of this invention. Some suitable reporter genes are, for example, lacZ, phoA, luxAB, and gfp. In a preferred method of this invention, the reporter gene is the lacZ gene.
In one method of the invention, the promoter is from a gene selected from the group consisting of virA and the ipaH family of genes, particularly, ipaH9.8, ipaH7.8, ipaH4.5, and ipaH1.4. Promoters such as ipgD, icsB, ipaA, and mxiD are not regulated by the secretion machinery and thus may be used in the methods of this invention as internal controls. Other suitable promoters for use in the methods of this invention may be easily identified following the teachings detailed in this specification.
In a preferred method according to this invention, candidate inhibitor molecules are screened against three strains of bacteria which contain a reporter gene transcriptionally fused to a promoter of a gene regulated by the activity of the type III secretion machinery: a strain in which secretion is regulated, a strain which has a phenotype of constitutive secretion, and a strain which is deficient for secretion.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 depicts secretion of proteins by various Shigella strains. Cultures of M90T (wild type), BS176 (the virulence plasmid-cured strain), and the ipaD (SF622), ΔipaBCDA (SF635), and ipaD mxiD (SF634) mutants were used to prepare either whole culture extracts, by adding Laemmli sample buffer directly to the cultures, or bacterial pellets and culture supernatants, by centrifugation of the cultures. Proteins present in culture supernatants were concentrated 10 times by TCA precipitation. Samples were separated by SDS-PAGE and analyzed by either Coomassie blue staining or immunoblotting using an antiserum raised against aggregated recovered from the medium of the ΔipaBCDA mutant. Numbers indicate the position and the size (in kDa) of standard proteins and arrows indicate the position of the 60- and 46-kDa proteins.
FIG. 2 depicts the structure of plasmids carrying virA and ipaH9.8. A schematic genetic map of a portion of the virulence plasmid pWR100 is shown in the center, along with the position of some relevant restriction sites. Symbols used for restriction sites are: B, BspEI; C, HincII; E, EcoRI; H, HindIII; N, NdeI; P, HpaI; S, Sau3AI; T, StuI; V, BbvI; X, XbaI. The DNA corresponding to virA and ipaH9.8 is shown by shaded bars and the lacZ gene by a solid bar. Arrows indicate the orientation of transcription of the genes. Restriction sites of the virulence plasmid that were used for cloning are indicated in brackets.
FIG. 3 depicts transcription of the virA-lacZ fusion upon addition of Congo red to the growth medium. Congo red (100 μg/ml) was added to the growth medium during the exponential phase of growth of derivatives of the wild-type (open symbols) and mxiD (closed symbols) strains carrying the virA-lacZ fusion. Samples were then collected at 5 minute intervals and assayed for β-galactosidase activity. For both strains, no increase in β-galactosidase activity was detected in the absence of Congo red.
FIG. 4 depicts transcription of the virA-lacZ fusion by intracellular bacteria. Intracellular bacteria recovered after various times of infection of HeLa cells by SF1001 (virA-lacZ) were numbered by plating (open symbols) and used to assay β-galactosidase activity (closed symbols).
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Production of most bacterial virulence factors is tightly regulated in response to environmental signals. In Shigella, for example, both the temperature and the osmolarity of the growth medium modulate transcription of genes involved in entry of the bacteria into epithelial cells (Bernardini et al., 1990, "The two-component regulatory system OmpR-EnvZ controls the virulence of Shigella.", "J. Bacteriol., 172:6274-6281; Maurelli et al., 1984, "Temperarure-dependent expression of virulence genes in Shigella species.", Infect. Immun., 43:195-201). In addition, contact of Shigella with epithelial cells (Menard et al., 1994; Watarai et al., 1995) and exposure of the bacteria to Congo red (Sankaran et al., 1989, "Congo-red mediated regulation of levels of Shigella flexneri 2a membrane proteins.", Infect. Immun., 57:2364-2371; Parsot et al., 1995, "Enhanced secretion through the Shigella flexneri Mxi-Spa translocon leads to assembly of extracellular proteins into macromolecular structures." Mol. Microbiol, 16, 291-300.; Bahrani et al., 1997, "Secretion of Ipa proteins by Shigella flexneri: inducer molecules and kinetics of activation", Infect. Immun., 65:4005-4010) or bile salts (Pope et al., 1995, "Increased protein secretion and adherence to HeLa cells by Shigella spp. following growth in the presence of bile salts", Infect. Immun., 63:3642-3648) activate secretion of IpaB and IpaC.
The Shigella Model
Shigella was used as a model system for application of the methods of this invention. Members of the genus Shigella cause bacillary dysentery in humans by invading the colonic epithelial mucosa and inducing a strong inflammatory response (LaBrec et al., 1964, "Epithelial cell penetration as an essential step in the pathogenesis of bacillary dysentery", J. Bacteriol. 88:1503-1518). In vitro, cell invasion involves two steps: entry and intercellular dissemination. Genes involved in both steps are carried on a 200-kb virulence plasmid (reviewed by Hale, 1991, "Genetic basis of virulence in Shigella species", Microbiol. Rev., 55:206-224; Parsot, 1994, "Shigella flexneri: genetics of entry and intercellular dissemination in epithelial cells", Curr. Topics. Microbiol. Immunol., 192:217-241). A 31-kb fragment of this plasmid is necessary and apparently sufficient for entry into epithelial cells (Maurelli et al., 1985, "Cloning of plasmid DNA sequences involved in invasion of HeLa cells by Shigella flexneri", Infect. Immun., 49:164-171; Sasakawa et a., 1988, "Virulence associated genetic region comprising 31 kilobases of the 230-kilobase plasmid in Shigella flexneri 2a", J. Bacteriol. 170:2480-2484). This fragment is organized in two divergently transcribed regions which, schematically, encode secreted proteins, the IpaA-D proteins, and a type III secretion system, the Mxi-Spa secretion apparatus. The first region contains eight genes, including ipaBCDA, which are transcribed from a promoter located upstream from icsB. The second region contains 20 genes, designated ipg, mxi, and spa, which are clustered in large operons. Inactivation of ipa, mxi, and spa genes leads to a non-invasive phenotype, due to either loss of effector proteins (Sasakawa et al., 1989, "Functional organization and nucleotide sequence of virulence region 2 on the large virulence plasmid of Shigella flexneri 2a", Mol. Microbiol., 3:1191-1201; Menard et al., 1993, "Nonpolar mutagenesis of the ipa genese defines IpaB, IpaC, and IpaD as effectors of Shigella flexneri entry into epithelial cells", J. Bacteriol. 175:58899-5906) or failure to secrete them (Andrews and Maurelli, 1992, "mixA of Shigella flexneri 2a, which facilitates export of invasion plasmid antigens, encodes a homologue of the low-calcium response protein, LcrD, of Yersinia pestis", Infect. Immun., 60:3287-3295; Venkatesan et al., 1992, "Surface presentation of Shigella flexneri invasion plasmid antigns requires the products of the spa locus", J. Bacteriol. 174:1990-2001; Allaoui et al., 1993, "MixD: an outer membrane protein necessary for the secretion of the Shigella flexneri Ipa invasins", Mol. Microbiol., 7:59-68; Sasakawa et al., 1993, "Eight genes in region 5 that form an operon are essential for invasion of epithelial cells by Shigella flexneri 2a", J. Bacteriol. 175:2334-2346).
Bacterial strains and growth media
All Shigella flexneri strains identified in Table I are derivatives of the wild-type strain M90T (Sansonetti et al., 1982, "Involvement of a plasmid in the invasive ability of Shigella flexneri", Infect. Immun., 35:852-860). Bacteria were grown in Luria-Bertani (LB) medium or tryptic soy (TCS) broth. Antibiotics were used at the following concentrations: ampicillin, 100 μg/ml; kanamycin, 30 μg/ml; and streptomycin, 100 μg/ml. Congo red (SERVA, Heidelberg, Germany) was used to induce secretion by bacteria growing in LB medium.
Constitutively secreting strains
Only a small proportion of IpaA-D proteins is secreted by wild-type Shigella growing in laboratory media. Inactivation of ipaD enhances secretion of IpaA, IpaB, IpaC, and about 15 other proteins (Menard et al., 1994; Parsot et al., 1995). These latter proteins are absent or barely detectable in the medium of the wild-type strain unless Congo red, a dye that induces secretion (Bahrani et al., 1997), is present in the culture medium (Parsot et al., 1995).
Inactivation of either ipaB or ipaD and deletion of the ipaB, C, D, and A genes lead to the secretion of about 15 proteins that associate in the extracellular medium (Parsot et al., 1995). Aggregates containing proteins secreted by the ΔipaBCDA mutant (SF635) were used to immunize mice and the resulting anti-serum was tested by Western blotting on extracts of whole cultures, bacterial pellets, and culture supernatants of M90T (wild-type), SF622 (ipaD), SF635 (ΔipaBCDA), SF634 (ipaD mxiD), and BS176 (a virulence-plasmid cured-stain). The serum reacted most strongly with a 46-kDa protein. This protein was present in high amounts in extracts of ipaD and ΔipaBCDA strains; was present in low amounts in extracts of wild-type and ipaD mxiD strains; and was not present in extracts of the virulence plasmid-cured strain (FIG. 1). SDS-PAGE analysis and Coomassie blue staining also revealed that a protein, or possibly a mixture of proteins of about 60 kDa was present in higher amounts in extracts of the ipaD and ΔipaBCDA strains than in extracts of the wild-type and ipaD mxiD strains (FIG. 1). These results suggested that production of 46-kDa and 60-kDa secreted proteins was increased in the constitutively secreting ipaD and ΔipaBCDA strains as compared to the wild-type and secretion deficient ipaD mxiD strains.
Characterization of the gene encoding the 46-kDa secreted protein
The 46-kDa protein secreted by the ΔipaBCDA mutant was transferred onto a PVDF membrane and subjected to Edman degradation and proteolysis by endolysin. The N-terminal sequence of the protein was identified as M-Q-T-S-N-I-T-N-H-E (SEQ ID NO:1) and those of two internal peptides as I-I-T-F-G-I-Y-S-P-H-E-T-L-A (SEQ ID NO:2) and V-H-T-I-T-A-P-V-S-G-N (SEQ ID NO:3). Oligonucleotides based on the N-terminal sequence and one internal peptide were used to screen, by Southern blotting, a set of overlapping cosmids representing the entire virulence plasmid. Both probes hybridized to a 6.4 kb HindIII fragment of cosmid pCos3 which was then cloned into pUC19 to give rise to pBD3 (FIG. 2).
Subcloning experiments and Southern blot analysis of recombinant plasmids using oligonucleotides as probes allowed us to localize the gene encoding the 46-kDa protein on a 3.2-kb HindII-HindIII fragment located upstream from icsA (Bernardini et al., 1989, "Identification of icsA, a plasmid locus of Shigella flexneri that governs bacterial intra and intercellular spread throught interaction with F-actin", Proc. Natl. Acad. Sci. USA 86:3867-3871; Lett et al., 1989, "virG, a plasmid-coded virulence gene of Shigella flexneri: identification of the VirG protein and determination of the complete coding sequence", J. Bacteriol. 171:353-359). Sequence analysis revealed an open reading frame (ORF) starting 487 bp upstream from the icsA translation start codon and oriented in the opposite direction. Amino acid sequences deduced from positions 43 to 71, 159 to 200, and 442 to 473 of the ORF were identical to those determined for the N-terminal end and the two internal peptides of the secreted protein. These sequence data have been submitted to the DDBJ/EMBL/GenBank databases under the accession number AF047364. The deduced sequence of the 46-kDa protein was identical to that of VirA, a secreted protein encoded by the virulence plasmid of an S. flexneri strain of serotype 2a (Uchiya et. al., 1995, "Identification of a novel virulence gene, virA, on the large plasmid of Shigella, involved in invasion and intercellular spreading", Mol. Microbiol. 17:241-250) and, therefore, the corresponding gene of S. flexneri 5 was designated virA. No other ORF was detected immediately upstream or downstream from virA. Restriction analysis of overlapping cosmids indicated that virA was located about 10 kb downstream from the spa operon (Venkatesan et al., 1992; Sasakawa et al., 1993) on the virulence plasmid pWR100.
Characterization of the gene encoding a 60-kDa secreted protein
The 60-kDa proteins which were secreted in high amount by the ΔipaBCDA strain were transferred onto a PVDF membrane and the lower part of the band was used for N-terminal sequence determination and proteolysis by endolysin. Analysis of the N-terminal sequence indicated that the sample contained two proteins; the sequence of the major species was determined as M-L-P-I-N-N-N-F-S-L-P-Q (SEQ ID NO:4). The sequence of an internal peptide was determined as Y-E-M-L-E-N-E-Y-P-Q-R-V-A-D-R (SEQ ID NO:5), which was almost identical to a fragment of the constant region of members of the IpaH family. IpaH proteins are characterized by a constant C-terminal region of about 300 residues which is preceded by a variable N-terminal region composed of repetitive motifs (Hartman et al., 1990, "Sequence and molecular characterization of a multicopy invasion plasmid antigen gene, ipaH, of Shigella flexneri", J. Bacteriol. 172:1905-1915; Venkatesan et al., 1991, "Sequence variation in two ipaH genes of Shigella flexneri 5 and homology to the LG-like family of proteins", Mol. Microbiol. 5:2435-2445). The N-terminal sequence of the 60-kDa secreted protein was different from those deduced from the 5' end of ipaH7.8, ipaH4.5, ipaH2.5 and ipaH1.4 (Hartman et a., 1990; Venkatesan et al., 1991), which suggested that this protein might correspond to the fifth IpaH protein, IpaH9.8, whose gene had not been sequenced yet.
Southern blot analysis using a probe derived from the constant region of ipaH genes indicated that ipaH9.8 was present in cosmid pCos87. Deletion derivatives of pCos87 were constructed to give rise to pBD4 (FIG. 2), whose 2.4-kb insert was entirely sequenced. The amino acid sequences deduced from positions 40 to 75 and 1477 to 1521 of the ORF identified by sequence analysis were identical to those of the N-terminal end and of the internal peptide of the 60-kDa secreted protein. These sequence data have been submitted to the DDBJ/EMBL/GenBank databases under the accession number AF047365. The ipaH9.8 gene encodes a 545-residue protein with a deduced Mr of 61,886. No ORFs were identified upstream or downstream from ipaH9.8. Restriction analysis of overlapping cosmids indicated than ipaH9.8 was located 45 kb downstream from the spa operon.
DNA analysis, PCR, plasmid construction, and transformation of E. coli and S. flexneri strains were performed according to standard methods. Nucleotide sequences were determined by the dideoxy chain termination procedure on alkaline-denatured plasmid DNA. Overlapping cosmids representing the entire virulence plasmid were previously constructed by inserting 40-kb fragments of pWR100 into the vector pJB8 (Maurelli etal., 1985).
Inactivation of ipaD increases transcription of virA and ipaH genes
Western blot analysis indicated that a higher amount of VirA was produced by the ipaD mutant than by the wild-type strain (FIG. 1). To investigate virA transcription, we constructed a virA-lacZ transcriptional fusion. Plasmid pLAC4 (FIG. 2) was constructed by cloning a 1.5-kb XbaI-EcoRI fragment that contains the 5' part of icsA, the icsA-virA intergenic region, and the 5' part of virA, into the SmaI site located upstream from the lacZ reporter gene in the suicide plasmid pLAC1 that confers resistance to ampicillin (Allaoui et al., 1992, "icsB: a Shigella flexneri virulence gene necessary for the lysis of protrusions during intercellular spread", Mol. Microbiol. 6:1605-1616). (Plasmid pLAC4 was deposited in the Collection Nationale Cultures Microoganismes in Paris, France on May 13, 1998 under ascession No.I-2105) pLAC4 was then transferred by conjugation into M90T-Sm and SF622 (ipaD2) to produce recombinant strains SF1001 and SF1002. Since pLAC4 does not replicate in S. flexneri, the Ap r clones arose through homologous recombination between the identical sequences carried by the virulence plasmids M90T-Sm or SF622 and the recombinant plasmid pLAC4, thereby placing the lacZ reporter gene under the control of the virA promoter. Expression of the virA-lacZ fusion was 17 times higher in the ipaD - strain as compared to the ipaD + strain (Table II), indicating that the increased production of VirA by the ipaD mutant was due to an increased transcription of virA. Southern analysis confirmed the structure of the pWR100 derivatives carrying the virA-lacZ transcriptional fusion in recombinant strains designated SF1001 (virA-lacZ virA + ipaD + ) and SF1002 (virA-lacZ virA + IpaD - ).
Plasmid pLAC5 (FIG. 2) was constructed by deleting an NdeI-EcoRI fragment from pLAC4 and thus contains a 380-bp fragment internal to the virA gene. To determine whether VirA is involved in the regulation of the virA promoter, pLAC5 was integrated at the virA locus of the wild-type and ipaD to produce recombinant strains SF1003 and SF1004. Integration of pLAC5 into the virA locus of pWR100 also placed the lacZ gene under the control of the virA promoter but, unlike that of pLAC4, led to the disruption of the virA gene. Inactivation of virA had no effect on transcription of the virA-lacZ fusion in either the ipaD + or ipaD - backgrounds, indicating that virA was not autoregulated. Southern blot analysis confirmed the structure of the pWR100 derivatives carrying the virA-lacZ transcriptional fusion in recombinant strains designated SF1003 (virA-lacZ virA - IpaD + ) and SF1004 (virA-lacZ virA - ipaD - ).
To analyze transcription of the various ipaH genes, the constant region of ipaH9.8 was amplified using the polymerized chain reaction (PCR) technique, and the PCR product was cloned between the KpnI and XbaI sites that are located upstream from the lacZ gene in the suicide vector pLAC2 (Allaoui et al., 1993, "Characterization of the Shigella flexneri ipgD and ipgF genes, which are located in the proximal part of the mxi locus", Infect. Immun. 61:1707-1714) to construct plasmid pLAC6. pLAC6 was then transferred by conjugation into M90T-Sm (wild-type) and SF622 (ipaD). Since pLAC6 carried the constant region of ipaH, integration of the suicide plasmid could occur into any of the five ipaH genes carried on the virulence plasmid. In each case, the lacZ reporter gene is placed under the control of the promoter of the ipaH gene into which the plasmid is integrated. Transconjugants were screened by Southern blot analysis of their virulence plasmid digested by HindIII using a probe from the ipaH constant region. The strains were designated SF1005 (ipaH9.8-lacZ ipaD + ), SF1006 (ipaH9.8-lacZ ipaD - ), SF1007 (ipaH7.8-lacZ ipaD + ), SF1008 (ipaH4.5-lacZ ipaD + ), SF1009 (ipaH4.5-lacZ ipaD - ), SF 1010 (ipaH1.4-lacZ ipaD + ), SF1011 (ipaH1.4-lacZ ipaD - ). The ipaH2.5-lacZ fusion in the wild-type background as well as the ipaH7.8-lacZ and ipaH2.5-lacZ fusions in the ipaD background were not obtained. Expression of ipaH9.8-, ipaH4.5-, and ipaH1.4-lacZ fusions was low in derivatives of the wild-type strain and was increased 5-20 times in derivatives of the ipaD mutant (Table II).
To investigate transcription of genes of the entry region, lacZ transcriptional fusions in icsB and ipaA, which are the first and last genes of the ipaBCDA operon, respectively, and in ipgD and mxiD, which are the first and 12th genes of the mxi operon, respectively (FIG. 2) were used. These fusions were constructed in both the wild-type and ipaD strains. For example, construction of the ipgD-lacZ fusion was achieved using the suicide plasmid pLAC3 (Allaoui et al. 1993). The recombinant plasmid pLAC3 (Allaoui et al., 1993) was constructed by cloning a 1.4-kb SspI fragment that contains the 5' part of icsB, the icsB-ipgD intergenic region, and the 5' part of ipgD (Allaoui et al., 1992,1993) into the SmaI site located upstream from the lacZ reporter gene in the vector pLAC1 (Allaoui et al., 1992). (Plasmid pLAC3 was deposited in the Collection Nationale Cultures Microoganismes in Paris, France on May 13, 1998 under ascession No. I-2104) pLAC3 was then transferred by conjugation into M90T-Sm and SF622 (ipaD2) to produce recombinant strains SF134 and SF806. Since pLAC3 does not replicate in S. flexneri, the Apr clones arose through homologous recombination between the identical sequences carried by the virulence plasmids M90T-Sm or SF622 and the recombinant plasmid pLAC3, thereby placing the lacZ reporter gene under the control of the virA promoter. Southern blot analysis confirmed the structure of the virulence plasmid carrying the ipgD-lacZ transcriptional fusion in the recombinant strains designated SF134 (ipgD-lacZ ipaD + ) and SF806 (ipgD-lacZ ipaD - ). Integration of the suicide plasmids used to construct these fusions did not affect the secretion phenotype of recombinant strains . For each fusion, similar amounts of β-galactosidase were present in derivatives of the wild-type and ipaD strains, indicating that transcription of these genes was not affected by inactivation of ipaD (Table II).
Congo red increases transcription of virA and ipaH genes
Secretion of IpaB and IpaC is enhanced when bacteria grow in the presence of Congo red (Parsot et al., 1995). To investigate the effect of Congo red on virA transcription, the β-galactosidase activity in strain SF1001 (virA-lacZ ipaD + ) after growth in the presence of various concentrations of Congo red was assayed. Transcription of the virA-lacZ fusion was low at concentrations of dye up to 20 μg/ml and then increased with the concentration of the dye to reach a plateau at about 100 μg/ml of Congo red. Likewise, about 3-12 times more β-galactosidase activity was present in strains carrying ipaH9.8-, ipaH7.8-, ipaH4.5-, and ipaH1.4-lacZ fusions after growth in the presence of 100 μg/ml of Congo red (Table II). In contrast, transcription of icsB-, ipaA-, ipgD-, and mxiD-lacZ fusions was not affected by the presence of Congo red in the growth medium (Table II).
Secretion is required for activation of virA transcription
To determine whether regulation of virA transcription was dependent on the type III secretion machinery, the β-galactosidase activities produced by the virA-lacZ fusion in derivatives of wild-type (SF1001) and mxiD (SF1012) strains during growth in the presence of Congo red was compared, along with the production of VirA in ipaD and mxiD ipaD strains.
The presence of Congo red in the growth medium of the derivative of the mxiD strain carrying the virA-lacZ fusion did not lead to an increase in β-galactosidase activity (Table II), and lesser amounts of VirA were present in the ipaD mxiD strain as compared to the ipaD strain (FIG. 1). This indicated that activation of the virA promoter in response to Congo red and inactivation of ipaD required the integrity of the secretion machinery.
To investigate kinetics of activation of the virA promoter, Congo red (100 μg/ml) was added to the growth medium during the exponential phase of growth of derivatives of the wild-type and mxiD strains carrying the virA-lacZ fusion. Samples were then collected at 5 minute intervals and assayed for β-galactosidase activity. An increase in the β-galactosidase specific activity was detected 10 min after addition of the dye to the medium of the derivative of the wild-type strain, whereas no transcriptional activation of the virA-lacZ fusion was detected in the derivative of the mxiD mutant (FIG. 3).
These results differentiated the virA and ipaH genes, the transcription of which was increased after growth in the presence of Congo red or by inactivation of ipaD, from the genes of the entry region, the transcription of which was apparently constitutive with respect to these parameters. Moreover, this suggested that transcription of the virA and ipaH genes was regulated by the Mxi-Spa secretion machinery, since (i) conditions leading to an enhanced transcription of these genes were the same as those known to increase secretion through the Mxi-Spa secretion machinery, and (ii) in these conditions, the secretion machinery was required for the enhanced transcription of the virA-lacZ fusion and for the enhanced production of the VirA protein.
Transcription of virA- and ipaH-lacZ fusions upon entry and during intracellular multiplication
To investigate virA and ipaH transcription during infection of epithelial cells, the β-galactosidase activity that was present in bacteria shortly after entry into epithelial cells was measured. HeLa cells were infected as previously described (Sansonetti et al., 1986, "Multiplication of Shigella flexneri within HeLa cells: lysis of the phagocytic vacuole and plasmid-mediated contact hemolysis", Infect. Immun. 51:461-469). Briefly, cells were infected for 30 minutes to allow entry and then treated with gentamicin for 30 minutes to kill extracellular bacteria. Infected cells were then washed to remove killed bacteria and lysed, and intracellular bacteria were recovered by centrifugation. The number of intracellular bacteria was determined by plating and the β-galactosidase activity present in these bacteria was assayed by using MUG as a substrate. The specific activity was first expressed in units of fluorescence per bacterium and then converted into Miller units. For the strain carrying the ipgD-lacZ fusion, chosen as a representative of genes which were expressed constitutively in vitro, the β-galactosidase activity present within intracellular bacteria recovered after 60 minutes of infection was similar to that found after growth in laboratory medium (Table III). This confirmed that, following gentamicin treatment, washes of infected cells were sufficient to remove killed extracellular bacteria which, otherwise, could have contributed to the total β-galactosidase activity without being numbered by plating. For strains carrying the virA- and ipaH-lacZ fusions, the β-galactosidase activity was 6 to 30 times higher in intracellular bacteria than in bacteria grown in vitro (Table III). This indicated that transcription of virA, ipaH9.8, ipaH7.8, ipaH4.5 and ipaH1.4 had been induced upon entry or shortly thereafter.
To investigate virA transcription during growth in the intracellular compartment, infected cells were lysed after various periods of incubation in the presence of gentamicin and intracellular bacteria were counted by plating and assayed for β-galactosidase activity. The number of intracellular bacteria carrying the virA-lacZ fusion increased with the time of incubation, which was consistent with their intracellular multiplication (FIG. 3). In contrast, the specific β-galactosidase activity present in these bacteria decreased steadily, suggesting that the decrease in specific activity was due to bacterial multiplication. Similarly, the β-galactosidase activity present in bacteria carrying the various ipaH-lacZ fusions was 6 to 13 times lower after 150 minutes of infection as compared to the activity present after 60 minutes of infection (Table III). These results suggested that the virA- and ipaH-lacZ fusions had not been transcribed between 60 and 150 minutes of infection. In contrast, for the strain carrying the ipgD-lacZ fusion, similar amounts of β-galactosidase were present after 60 and 150 minutes of infection (Table III), suggesting that the intracellular compartment had no effect on ipgD transcription.
Protein analysis
All protein analyses were carried out according to the following protocol. Aggregated proteins were collected from the culture medium of SF635 (Δipa) and solubilized in 0.1% SDS. Mice were injected twice with this preparation, at a one week interval. Sera were collected the fourth week, pooled, and absorbed on sonicated extracts of BS176.
Bacteria in the exponential phase of growth were harvested by centrifugation at 14,000 g for 10 minutes. Crude extracts were obtained from the bacterial pellet, and proteins present in the culture supernatant were precipitated by the addition of 1/10 (vol/vol) trichloracetic acid. Electrophoresis in 10% polyacrylamide gels in the presence of sodium dodecyl sulfate (SDS-PAGE) was performed as described (Laemmli, 1970, "Cleavage of structural proteins during the assembly of the head of bacteriophage T4", Nature (London) 227:680-685). After electrophoresis, proteins were either stained with Coomassie brilliant blue or transferred to a nitrocellulose membrane. Immunoblotting procedures were carried out with mouse polyclonal anti-filaments antibodies. Horseradish peroxidase-labelled goat anti-mouse antibodies were used as secondary antibodies and visualized by enhanced chemiluminescence. The N-terminal sequence of VirA and IpaH9.8 and that of internal peptides, which were obtained by endolysin digestion and purified by chromatography, were determined by the Edman degradation procedure.
The β-galactosidase activity present in bacteria growing in laboratory media was assayed by using the substrate o-nitro-phenyl-β-D-galactoside (ONPG) as described (Platt et al., 1972, "Assay of β-galactosidase", In Miller, J. H. (ed.) Experiments in molecular genetics, Cold Spring Harbor Laboratory, Cold Spring Harbor, N.Y., pp. 352-355). The β-galactosidase activity present in intracellular bacteria was assayed by using the substrate 4-methyl-umbelliferyl-β-D-galactoside (MUG) as described (Klarsfeld et al., 1994, "Five Listeria monocytogenese genes preferentially expressed in infected mammalian cells; plcA, putH, parD, pyrE and an arginine ABC transporter gene, arpJ", Mol. Microbiol. 13:585-597). Fluorescence was measured by using a Dynatec apparatus, with 365 nm excitation and 450 nm emission wavelengths. Activities were computed as fluorescence units per hour per bacterium: four fluorescence units were equivalent to one Miller unit and all results are presented in Miller units.
Genes under transcriptional control of type III secretion machinery
Using lacZ transcriptional fusions, we have investigated transcription of virA, of four members of the ipaH family, and of the ipaBCDA and mxi operons. Evidence supports the position that transcription of virA and of four ipaH genes, but not that of the ipaBCDA and mxi operons, is increased when secretion through the type III secretion machinery is enhanced in response to addition of Congo red to the growth medium and to inactivation of ipaD. In addition, transcription of virA- and ipaH-lacZ fusions was activated during entry of bacteria into epithelial cells.
lacZ fusions were used to investigate transcription of virA, ipaH9.8, ipaH7.8, ipaH4.5, and ipaH1.4, as well as that of operons located in the entry region. Transcription of genes of the entry region was high in derivatives of the wild-type strain and was not increased in derivatives of the ipaD mutant or after growth in the presence of Congo red. These results indicate that: (i) the increased secretion observed with the wild-type strain growing in the presence of Congo red and with the ipaD mutant is not due to an increased transcription of the mxi operon; and (ii) transcription of mxi and ipaBCDA operations is the same whether the secretion machinery is poorly active (in the wild-type strain), or deregulated (by addition of Congo red or inactivation of ipaD). This transcriptional analysis and previous Western blot analysis, which indicated that similar amounts of IpaB and IpaC were present in wild-type, ipaD, and mxiD strains (Allaoui et al., 1993; Menard et al., 1993), suggest that expression of genes of the entry region is not controlled by the secretion machinery. In contrast, transcription of the virA and ipaH genes was low in derivatives of the wild-type strain and was increased during growth in the presence of Congo red and in derivatives of the ipaD mutant. These results, together with the low production of VirA in the ipaD mxiD mutant and the low transcription of virA in the mxiD mutant growing in the presence of Congo red, indicate that the secretion machinery is involved in the control mechanism of the virA promoter and suggest that transcription of virA and of four copies of the ipaH family is enhanced in response to an active secretion through the type III apparatus.
Similar amounts of β-galactosidase were present in bacteria carrying the ipgD-lacZ fusion prior to and after 60 minutes of infection. In contrast, the amount of β-galactosidase present in bacteria carrying virA and ipaH-lacZ fusions was about 10 times higher after 60 minutes of infection than prior to infection. Due to the period of incubation in the presence of gentamicin which is required to eliminate extracellular bacteria, it was not possible to investigate whether virA and ipaH transcription was activated upon contact with or shortly after entry into epithelial cells. Only low amounts of β-galactosidase were present in bacteria carrying virA- and ipaH-lacZ fusions after 150 minutes of infection, which suggests that the virA and the ipaH genes had not been transcribed between 60 and 150 minutes of infection. Because there is a correlation between virA and ipaH transcription and active secretion, these results suggest that secretion might not be active when bacteria are multiplying in the cytoplasm of HeLa cells. Alternatively, signals other than secretion might affect negatively transcription of the virA and ipaH genes in the intracellular compartment.
The mechanism involved in the transcriptional control of the virA and ipaH genes in response to active secretion is not known yet. The low transcription of virA by the virA mutant indicates that virA is not autoregulated and the low production of VirA by the ipaD mxiD mutant suggests that IpaD is not the effector of the regulation of the virA promoter. When the secretion apparatus is inactive, a negative regulator might accumulate in the cytoplasm and repress virA and ipaH transcription. Secretion of this regulator, due to the lack of IpaD or in response to external inducers, would decrease its cytoplasmic concentration, thereby leading to the transcriptional activation of its target promoters. Secretion of a negative regulator as a mechanism for the control of gene expression has been documented in Salmonella and Yersinia. In S. typhimurium, transcription of the flagellin gene by an RNA polymerase containing the alternate sigma factor σ 28 requires the integrity of the basal-hook body complex which constitutes an export apparatus related to type III secretion machineries. Secretion of the anti-sigma factor FlgM allows transcription of the flagellin gene by a σ 28 -containing RNA polymerase, thus coupling flagellin expression to flagellar assembly (Hughes et al. 1993; Kutsukake et al., 1994, "Genetic and molecular analysis of the interaction between the flagellum-specific sigma factors in Salmonella typhimurium", EMBO J. 13:4568-4576). In Yersinia, expression of the yop genes is down regulated when Yop secretion is compromised (Cornelis et al., 1987, "Transcription of the yop regulon from Y. enterolitica requires trans-acting pYV and chromosomal genes", Microb. Pathogen. 2:367-379) and secretion of LcrQ via the type III secretion apparatus has been proposed to lead to the transcriptional activation of yop promoters by a mechanism which has not been characterized yet (Pettersson et al., 1996). Differences in the transcriptional regulation of genes encoding proteins secreted by the type III secretion machinery of Shigella are likely to reflect differences in the functional role of these secreted proteins during infection.
TABLE I______________________________________Shigella strains Strain Genotype Reference______________________________________M90T wild type Sansonetti et al., 1985 M90T-Sm spontaneous Sm.sup.R derivative Allaoui et al., 1992 of the M90T BS176 plasmidless derivative of M90T Sansonetti et al. 1985 SF132 icsB-lacZ in M90T-Sm Allaoui et al., 1992 SF134 ipgD-lacZ in M90T-Sm Allaoui et al., 1993 (C.N.C.M. No. I-2016)* SF401 mxiD Allaoui et al., 1993 SF403 mxiD-lacZ in M90T-Sm Allaoui et al., 1993 SF622 ipaD Menard et al., 1993 SF623 ipaA-lacZ in M90T-Sm Menard et al., 1993 SF624 ipaA-lacZ in SF622 (ipaD) Menard et al., 1993 SF634 ipaD mxiD Menard et al., 1994 SF635 ΔipaBCDA Parsot et al., 1995 SF803 icsB-lacZ in SF622 (ipaD) SF806 ipgD-lacZ in SF622 (ipaD) (C.N.C.M. No. I-2017)* SF808 mxiD-lacZ in SF622 (ipaD) SF1001 virA-lacZ in M90T-Sm (virA.sup.+) (C.N.C.M. No. I-2018)* SF1002 virA-lacZ in SF622 (virA.sup.+) (C.N.C.M. No. I-2019)* SF1003 virA-lacZ in M90T-Sm (virA.sup.-) SF1004 virA-lacZ in SF622 (virA.sup.-) SF1005 ipaH9.8-lacZ in M90T-Sm SF1006 ipaH9.8-lacZ in SF622 (ipaD) SF1007 ipaH7.8-lacZ in M90T-Sm SF1008 ipaH4.5-lacZ in M90T-Sm SF1009 ipaH4.5-lacZ in SF622 (ipaD) SF1010 ipaH1.4-lacZ in M90T-Sm SP1011 ipaH1.4-lacZ in SF622 (ipaD) SF1012 virA-lacZ in SF40l (mxiD)______________________________________ *Deposited in the Collection Nationale Cultures Microoganismes in Paris, France on May 13, 1998.
TABLE II______________________________________Expression of lacZ transcriptional fusions by bacteria growing in vitro β-galactosidase activity (Miller units).sup.aFusion ipaD.sup.+ ipaD.sup.- Ratio I.sup.b ipaD.sup.+ + CR Ratio Ii.sup.c______________________________________virA-lacZ 16 280 17 280 17 virA-lacZ mxiD 17 NA NA 18 1.1 ipaH9.8-lacZ 28 580 21 325 12 ipaH7.8-lacZ 20 NA NA 235 12 ipaH4.5-lacZ 31 360 12 110 3.5 ipaH1.4-lacZ 53 280 5.3 270 5.1 ipaA-lacZ 485 510 1.1 390 0.8 icsB-lacZ 290 305 1.1 285 1.0 mxiD-lacZ 275 260 0.9 320 1.2 ipgD-lacz 450 400 0.9 475 1.1______________________________________ .sup.a Activities are the means of at least three independent experiments Standard deviations are within 25% of the reported values. .sup.b Activity present in ipaD.sup.- strains versus activity present in ipaD.sup.+ strains. .sup.c Activity present in derivatives of the ipaD.sup.+ strain grown in the presence of Congo red versus activity present in the same strains grown in the absence of Congo red. NA not applicable.
TABLE III______________________________________Expression of lacZ transcriptional fusions by intracellular bacteria β-galactosidase activity 60 min 150 min (Miller units).sup.aFusion in vitro of infection Ratio I.sup.b of infection Ratio II.sup.c______________________________________ipgD-lacZ 450 490 1.1 463 1.1 virA-lacZ 16 280 18 49 5.7 ipaH9.8-lacZ 28 350 13 49 7.1 ipaH7.8-lacZ 20 590 30 150 3.9 ipaH4.5-lacZ 31 280 9.0 21 13.3 ipaH1.4-lacZ 53 300 5.7 49 6.1______________________________________ .sup.a Activities are the means of at least three independent experiments Standard deviations are within 25% of the reported values. .sup.b Activity present after 60 min of infection versus activity present in bacteria grown in vitro. .sup.c Activity present after 60 min of infection versus activity present after 150 min of infection.
__________________________________________________________________________# SEQUENCE LISTING - - - - <160> NUMBER OF SEQ ID NOS: 5 - - <210> SEQ ID NO 1 <211> LENGTH: 10 <212> TYPE: PRT <213> ORGANISM: Shigella flexneri - - <400> SEQUENCE: 1 - - Met Gln Thr Ser Asn Ile Thr Asn His Glu 1 5 - # 10 - - - - <210> SEQ ID NO 2 <211> LENGTH: 14 <212> TYPE: PRT <213> ORGANISM: Shigella flexneri - - <400> SEQUENCE: 2 - - Ile Ile Thr Phe Gly Ile Tyr Ser Pro His Gl - #u Thr Leu Ala 1 5 - # 10 - - - - <210> SEQ ID NO 3 <211> LENGTH: 11 <212> TYPE: PRT <213> ORGANISM: Shigella flexneri - - <400> SEQUENCE: 3 - - Val His Thr Ile Thr Ala Pro Val Ser Gly As - #n 1 5 - # 10 - - - - <210> SEQ ID NO 4 <211> LENGTH: 12 <212> TYPE: PRT <213> ORGANISM: Shigella flexneri - - <400> SEQUENCE: 4 - - Met Leu Pro Ile Asn Asn Asn Phe Ser Leu Pr - #o Gln 1 5 - # 10 - - - - <210> SEQ ID NO 5 <211> LENGTH: 15 <212> TYPE: PRT <213> ORGANISM: Shigella flexneri - - <400> SEQUENCE: 5 - - Tyr Glu Met Leu Glu Asn Glu Tyr Pro Gln Ar - #g Val Ala Asp Arg 1 5 - # 10 - # 15__________________________________________________________________________
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This invention relates to mutant strains of gram-negative bacteria that constitutively secrete proteins via the type III secretion machinery. It also relates to methods of identifying molecules that are able to activate or inhibit secretion in wild-type strains of gram-negative bacteria by exposing gram-negative bacterial cells to a sample molecule, wherein said bacterial cells contain a reporter gene transcriptionally fused to a promoter of a gene activated or regulated by the type III secretion machinery, and detecting the presence or activity of the product of the reporter gene.
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CROSS REFERENCE TO RELATED APPLICATION
This is a continuation of applicants' prior application Ser. No. 09/397,741, filed Sep. 16, 1999, which issued Apr. 24, 2001 as U.S. Pat. No. 6,220,722 and applicants' prior, now continuation of that parent application, which is application Ser. No. 09/781,485, filed Feb. 12, 2001, now U.S. Pat. No. 6,499,860.
BACKGROUND OF THE INVENTION
The invention relates to a LED lamp comprising a gear column, a lamp cap which is connected to an end of the gear column and a substrate which is connected to the other end of the gear column and which is provided with a number of LEDs.
Such a LED (Light Emitting Diode) lamp is known from English patent publication GB 2,239,306, which more particularly describes a LED lamp which can suitably be used for decorative purposes. The known lamp comprises a customary base with a BC cap or a continental screw cap, a gear column which accommodates the electronic gear necessary to operate the LEDs, as well as a substrate which is circularly symmetrical when viewed in the direction of the longitudinal axis of the lamp, in which substrate a number of individual LEDs are incorporated. The colors generated by the different LEDs during operation of the lamp may differ. By using an adjustable switching time control, it is possible to generate specific lighting effects and lighting patterns with the known lamp.
The known lamp has a number of drawbacks. One of these drawbacks is that the lamp can only be used for signaling purposes, whereby the LEDs of the lamp draw attention via a specific adjustable flashing frequency. The known lamp cannot provide for continuous, uniform lighting with a high luminous flux. In addition, the manufacture of the known lamp is relatively complicated. This applies in particular if the known lamp must be provided with a large number of LEDs.
It is an object of the invention to obviate the above-mentioned drawback. The invention more particularly aims at providing a LED lamp which can be relatively easily mass-produced, and which can be operated such that continuous, uniform lighting with a high luminous flux is obtained.
These and other objects of the invention are achieved by a LED lamp of the type mentioned in the opening paragraph, which is characterized in that the substrate comprises a regular polyhedron of at least four faces, whereby faces of the polyhedron are provided with at least one LED which, during operation of the lamp, has a luminous flux of at least 5 lm, and the gear column is provided with heat-dissipating means which interconnect the substrate and the lamp cap.
The invented lamp enables continuous, uniform, high-intensity lighting to be achieved. It has been found that LEDs having a luminous flux of 5 lm or more can only be efficiently used if the lamp comprises heat-dissipating means. Customary incandescent lamps can only be replaced by LED lamps which are provided with LEDs having such a high luminous flux. A particular aspect of the invention resides in that the heat-dissipating means remove the heat, generated during operation of the lamp, from the substrate via the gear column to the lamp cap and the mains supply connected thereto.
The use of a substrate which is composed of a regular polyhedron of at least four faces enables the intended uniform lighting to be achieved. The regular polyhedron is connected to the gear column, preferably, via a vertex. However, the polyhedron may in principle also be connected to the gear column in the center of one of the faces. The greatest uniformity in lighting is obtained if each one of the faces is provided with the same number of LEDs of the same type.
In experiments leading to the present invention, it has been found that favorable results can be achieved with polyhedrons in the form of an octahedron (regular polyhedron of eight faces) and dodecahedron (regular polyhedron of twelve faces). Better results, however, are achieved with substrates in the form of a hexahedron (polyhedron of six faces, cube). In practice it has been found that a good uniformity in light distribution can already be obtained using substrates in the form of a tetrahedron (regular polyhedron of four faces, pyramid). In an alternative embodiment the substrate comprises a three-dimensional body like a sphere or an ellipsoid, or a pat of a sphere or an ellipsoid.
A favorable embodiment of the LED lamp is characterized in that the lamp is also provided with a (semi-)transparent envelope. This envelope may be made of glass, but is preferably made of a synthetic resin. The envelope serves as a mechanical protection for the LEDs. In addition, the envelope may contribute to obtaining the uniform lighting which can be obtained with the lamp.
A further interesting embodiment of the LED lamp is characterized in that the heat-dissipating means comprise a metal connection between the substrate and the lamp cap. It has been found that such a connection, which may preferably consist of a layer of copper, properly dissipates the heat from the substrate to the lamp cap. In principle, the gear column may entirely consist of a heat-conducting material, for example a metal such as copper or a copper alloy. In this case, it must be ensured that the electronics present in the gear column is properly electrically insulated from the metal gear column. Preferably, also the substrate is made of a metal, such as copper or a copper alloy.
SUMMARY OF THE INVENTION
Yet another embodiment of the LED lamp is characterized in that means are incorporated in the column, which are used to generate an air flow in the lamp. Such means, preferably in the form of a fan, can be used, during operation of the lamp, to generate forced air cooling. In combination with the heat-dissipating means, this measure enables good heat dissipation from the gear column and the substrate.
A further embodiment of the invented LED lamp is characterized in that the faces of the polyhedron are provided with an array of LEDs, which preferably comprises at least one green, at least one red and at least one blue LED or at least one green, at least one red, at least one yellow and at least one blue LED or at least one white LED. By virtue of the shape of the substrate, such an array of LEDs can be readily provided, often as a separate LED array, on the faces of the substrate. This applies in particular when the faces of the polyhedral substrate are substantially flat. Such a LED array generally comprises a number of LEDs which are provided on a flat printed circuit board (PCB). In practice, LEDs cannot be readily secured to a substrate which is not level. If LEDs with a high luminous flux (5 lm or more) are used, then a so-called metal-core PCB is customarily used. Such PCBs have a relatively high heat conduction. By providing these PCBs on the (preferably metal) substrate by means of a heat-conducting adhesive, a very good heat dissipation from the LED arrays to the gear column is obtained.
By using one or more LED combinations in the colors green, red and blue or green, red, yellow and blue for each substrate face, a LED lamp can be obtained which emits white light. Such LED combinations composed of three different LEDs are preferably provided with a secondary optical system, in which the above-mentioned colors are blended so as to obtain white light. Another interesting embodiment of the LED lamp is characterized in that the lamp is provided with means for changing the luminous flux of the LEDs. If the gear column is provided with electronics suitable for this purpose, then this measure enables a dimmable LED lamp to be obtained. The dim function is preferably activated by means of an adjusting ring which is attached to the gear column at the location of the lamp cap. It is obvious that, if an envelope is used in the lamp, the adjusting ring must be situated outside the envelope.
A further interesting embodiment of the invented LED lamp is characterized in that the lamp is provided with means for mutually varying the luminous flux of the LEDs provided on the various faces of the substrate. The electronics necessary for this function is incorporated in the gear column of the lamp. By using this measure, it is possible to change the spatial light distribution of the LED lamp. If LEDs of different colors are used, it is also possible to adjust the color and the color distribution of the LED lamp. The distribution of the color and/or light distribution is preferably adjusted via an adjusting ring, which is connected to the gear column at the location of the lamp cap. It is obvious that, if an envelope is used in the lamp, the adjusting ring must be situated outside the envelope.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a view of a first embodiment of the invented LED lamp,
FIG. 2 is a view of a second embodiment of the invented LED lamp,
FIG. 3 is a diagrammatic, sectional view of two types of LEDs for use in the invented LED lamp,
FIG. 4 shows an example of a possible application of the invented LED lamp.
It is noted that like parts in the different Figures are indicated by like reference numerals.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a first embodiment of the invented Light-emitting diode lamp (LED lamp). This lamp comprises a tubular, hollow gear column ( 1 ), which is connected with one end to a lamp cap ( 2 ). The other end of the gear column ( 1 ) is connected to a substrate ( 3 ), which is provided with a number of LEDs ( 4 ). The space within the hollow gear column ( 1 ) accommodates the electronic gear necessary for controlling the LEDs ( 4 ). During operation of the lamp, these LEDs generate a luminous flux of 5 lm or more. The lamp is further provided with an envelope ( 5 ) of a synthetic resin, which envelops the gear column ( 1 ) and the substrate ( 3 ). It is emphasized that despite the presence of the envelope ( 5 ), the effect of the current invention in the LED lamp is achieved.
In the example described herein, the substrate ( 3 ) has the shape of a regular pyramid with four flat faces and is connected to the gear column ( 1 ) via a vertex of the pyramid. The outer surface of the substrate ( 3 ) is made of a metal or a metal alloy, thereby enabling a good heat conduction from the LEDs ( 4 ) to the column ( 1 ). In the present case, the outer surface of the substrate is made of a copper alloy. Each of the faces of the pyramid is provided with a number (five or six) LEDs ( 4 ), which are secured to the faces by means of a heat-conducting adhesive. In this example, single LEDs of the same type are used, which have only one light point per LED (commonly referred to as single-chip LED). Consequently, the LED lamp shown is monochromatic.
The outer surface of the gear column ( 1 ) of the LED lamp is made of a metal or a metal alloy. This enables a good heat conduction from the substrate ( 3 ) to the (metal) lamp cap ( 2 ) to be attained. In the present example, a copper alloy is used for the column. The use of the above-mentioned heat-dissipating means enables the LEDs with the relatively high luminous flux to be used without heat problems in a LED lamp of the above-described type.
The LED lamp shown in FIG. 1 also includes a f an ( 9 ) incorporated in the gear column ( 1 ), which fan generates an air flow during operation of the lamp. This air flow leaves the gear column ( 1 ) via holes ( 6 ) provided in the gear column, and re-enters the gear column via the holes ( 7 ) provided in the gear column. By suitably shaping and positioning the holes ( 6 ), the air flow is led past a substantial number of the LEDs present on the substrate ( 3 ). By virtue thereof, an improved heat dissipation from the substrate and the LEDs is obtained.
FIG. 2 shows a second embodiment of the invented LED lamp. Like the first embodiment, this embodiment comprises a gear column ( 1 ), a metal lamp cap ( 2 ), a metal substrate ( 3 ) with LEDs ( 4 ), an envelope ( 5 ) (not necessary), as well as outlet holes ( 6 ) and inlet holes ( 7 ) for an air flow generated by forced air cooling.
In the example described with respect to FIG. 2, the substrate ( 3 ) is cube-shaped with six flat faces, and is connected to gear column ( 1 ) via a vertex of the cube. The substrate ( 3 ) is made of a metal or a metal alloy, thereby enabling a good heat conduction from the LEDs ( 4 ) to the gear column ( 1 ) to be achieved. In the present case, the substrate is made of a copper alloy. Each one of the faces of the pyramid is provided with a number (eight or nine) LEDs ( 4 ), which are secured to the faces by means of a heat-conducting adhesive. In this example, multiple-chip LEDs are used, which each have three light points (green, red and blue) per LED or four light points (green, red, yellow, blue) per LED. These colors are mixed so as to obtain white light in the secondary optical system of each of the LEDs. Consequently, during operation of the LED lamp shown, white light is obtained.
The LED lamp in accordance with FIG. 2 is also provided with an adjusting ring ( 8 ) for simultaneously changing the luminous flux of the LEDs. By means of this adjusting ring, the lamp can be dimmed as it were. The lamp may also be provided with a second adjusting ring (not shown), by means of which the luminous flux of the LEDs provided on different faces of the substrate can be changed with respect to each other. This measure enables the spatial light distribution of the lamp to be adjusted. The lamp may also be provided with a further adjusting ring (not shown), by means of which the luminous flux of the three light points of each LED can be changed with respect to each other. This measure enables the color of the light emitted by the lamp to be changed.
FIG. 3 is a schematic, sectional view of three types of LEDs ( 4 ) which can suitably be used in the invented LED lamp. FIG. 3-A shows a LED which comprises single-chip LEDs, which each have only one light point ( 11 ) per LED. This light point ( 11 ) is placed on a so-called MC-PCB ( 12 ), which is responsible for a good heat transfer. Light point ( 11 ) is provided with a primary optical system ( 13 ), by means of which the radiation characteristic of the LED can be influenced. The LED ( 4 ) is also provided with two electrical connections ( 14 ). Via these connections, the LED is soldered onto the substrate ( 3 ). A heat-conducting adhesive between MC-PCB ( 12 ) and substrate ( 3 ) is responsible for a good heat dissipation from the LED to the substrate.
FIG. 3-B shows so-called multiple-chip LEDs, which each have three light points ( 11 ) (green, red and blue) per LED. If necessary, these three colors are blended so as to obtain white light in the primary optical system ( 13 ) of each one of the LEDs. A better color blending to form white light is obtained if a secondary mixing optics is additionally provided above the multiple-chip LEDs. This situation is shown in FIG. 3-C. Also these multiple-chip LEDs comprise a so-called MC-PCB ( 12 ) and connections ( 14 ).
If single-chip LEDs ( 4 ) in the colors green, red and blue are employed on the substrate ( 3 ), it is convenient to group these LEDs in trios, and provide a further secondary optical system ( 15 ) above the primary optical systems. In this manner, a good color blending of green, red and blue light is obtained. This situation is diagrammatically shown in FIG. 3-D.
FIG. 4 diagrammatically shows an application of a LED lamp, which requires an asymmetric light distribution. The LED lamp ( 20 ) is used as outdoor lighting and is situated on a holder ( 21 ) which is secured to the wall ( 22 ) of a building. The necessary luminous flux in the direction of the wall is much smaller than that in the opposite direction. The asymmetric light distribution required for this purpose can be simply adjusted by means of a LED lamp as described with reference to FIG. 3 .
The LED lamp in accordance with the invention can be readily manufactured and exhibits, during operation of the lamp, a relatively high luminous flux.
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An LED lamp has a gear column, which is connected between a cap and substrates. The substrates are arranged as a polyhedron with planar surfaces. Each surface has at least one LED. The gear column also has a heat-dissipater, which interconnects the substrates and the lamp cap.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a sealed-by-resin type semiconductor device and a liquid crystal display module including the same. More particularly, the present invention relates to a COF (chip on flexible printed circuit) in which ICs and chips are implemented on a flexible substrate, and a liquid crystal display module including the same.
2. Description of the Related Art
Recently, there is a demand for smaller-sized, lighter, thinner elements for use in electronic devices such as personal digital assistants. One of such elements is a liquid crystal display (hereinafter referred to as LCD) module which is used as an output section of the electronic devices. Ease of incorporation into the devices is highly required.
Some LCD modules are created by the COF technique to meet the above-described demand. In such an LCD module, an IC for driving a liquid crystal (hereinafter referred to as an LC-driving IC) and other chips are mounted on a flexible substrate made of a polyimide film printed with a conductor pattern, and these elements are coupled to an LCD element via an anisotropic conductive film.
FIG. 5 is a plan view of such a COF LCD module. FIG. 6 is a side view of the COF LCD module.
A “sealing resin” herein means a resin which fills between an LC-driving IC and a flexible substrate so as to protect a contact between the LC-driving IC and the flexible substrate.
As shown in FIG. 5, a COF LCD module 400 includes an LCD element 8 and a COF 300 . The COF 300 includes a flexible substrate 9 on which an LC-driving IC 1 and a chip 10 are mounted.
The flexible substrate 9 is, for example, fabricated in the following way. A copper foil having a thickness of about 2 to 35 μm is coated with a precursor of polyimide which is in turn cured. The resultant polyimide film substrate has a thickness of about 10 to 100 μm. Such a fabricating method is called casting. The substrate is etched to obtain the desired conductor pattern. The substrate is coated with a polyimide resin or an epoxy resin, except for portions of the substrate 9 on which the LC-driving IC 1 and the chip 10 and contacts of the LCD element 8 with the LC-driving IC 1 and the chip 10 . The conductor pattern on which a conductor is exposed is plated with Sn, Ni, Au, or the like. In this way, the flexible substrate 9 is fabricated.
As an alternative way to form the conductor pattern,an additive method may be employed. In this case, a sputtered copper is patterned and then thickened by plating.
The COF 300 is, for example, fabricated in the following way. The LC-driving IC 1 and the chip 10 are mounted on the conductor pattern of the flexible substrate 9 . The LC-driving IC 1 is implemented by flip chip bonding.
The LC-driving IC 1 includes an Au bump (not shown) which is coupled with the conductor pattern. As a method of coupling the Au bump with the conductor pattern, for example, an Sn—Au alloy coupling method, or a coupling method using an anisotropic conductive film may be adopted.
The Sn—Au alloy coupling method is performed in the following way. The LC-driving IC 1 is provided on the flexible substrate 9 so that the Au bump of the LC-driving IC 1 contacts with the Sn-plated conductor pattern. The Au bump is coupled with the conductor pattern by heating and pressing the flexible substrate 9 from the rear side thereof ( 9 A side). Subsequently, the LC-driving IC 1 is sealed by a sealing resin 4 .
The coupling method using an anisotropic conductive film is performed in the following way. The anisotropic conductive film is interposed between the flexible substrate 9 and the LC-driving IC 1 . In this situation, the flexible substrate 9 is heated and pressed from the rear side thereof ( 9 A side) so that the Au bump is electrically coupled with the conductor pattern while the Au bump is fixed on the conductor pattern by the cured anisotropic conductive film.
Thereafter, the COF 300 fabricated as described above is conductive-coupled with the LCD element 8 using an anisotropic conductive film or the like, thereby obtaining the LCD module 400 .
Recently, the pitch of the Au bump is becoming narrower in order to meet a demand for a higher resolution of liquid crystal display and a smaller area of the LC-driving IC 1 . The Au bump is used as the segment output terminal of the LC-driving IC 1 .
In order to improve the ease of incorporating the COF LCD module 400 into a device, the coupling strength between the LC-driving IC 1 and the flexible substrate 9 needs to be enhanced and the COF 300 on which the LC-driving IC 1 is mounted needs to be thinner.
The inventors fabricated and studied a prototype of the COF 300 , in which the LC-driving IC 1 having an Au bump having a narrower pitch, is mounted on the flexible substrate 9 by the Sn—Au alloy coupling.
As a result, when the pitch of the Au bump in the LC-driving IC 1 is about 70 μm or less (a gap between the Au bumps is about 30 μm or less), abnormalities in the liquid crystal display were encountered due to leakage between the Au bumps in a moisture-resistance reliability test in atmosphere having a humidity of about 95% at about 60° C.
The abnormalities in liquid crystal display were investigated to find the causes. As a result, occurrence of migration was recognized between the Au bumps. It was found by elemental analysis that this migration was caused by Au.
In general, it is said that the Au migration is generated by an electric field being applied to a halogen and moisture.
SUMMARY OF THE INVENTION
According to one aspect of the present invention, a sealed-by-resin type semiconductor device includes a substrate; a lead provided on the substrate; and a semiconductor element provided on the lead by flip chip bonding. The semiconductor element includes a plurality of terminals connected to the lead; the sealed-by-resin type semiconductor device further includes a resin for protecting the plurality of terminals; and the resin has a sufficiently low elasticity modulus that occurrence of undesirable migration is suppressed.
In one embodiment of this invention, the elasticity modulus is substantially about 1 GPa or less.
In one embodiment of this invention, the elasticity modulus is substantially about 0.07 GPa or more and about 1 GPa or less.
In one embodiment of this invention, the resin includes a thermosetting resin, an epoxy resin, or a denatured polyimide resin.
In one embodiment of this invention, the resin includes an epoxy resin; and the epoxy resin includes a bisphenol type epoxy resin.
In one embodiment of this invention, the resin includes a denatured polyimide resin; and the denatured polyimide resin includes aromatic tetracarboxylic acid and aromatic diamine.
In one embodiment of this invention, the plurality of terminals include an Au bump.
In one embodiment of this invention, a pitch of the plurality of terminals is substantially about 70 μm or less.
In one embodiment of this invention, the resin has a sufficiently high elasticity modulus that a coupling strength between the substrate and the semiconductor element is sufficient.
According to another aspect of the present invention, a liquid crystal display module includes a sealed-by-resin type semiconductor device including: a substrate; a lead provided on the substrate; and a semiconductor element provided on the lead by flip chip bonding, and a liquid crystal display element coupled with the substrate. The semiconductor element includes a plurality of terminals connected to the lead. The sealed-by-resin type semiconductor device further includes a resin for protecting the plurality of terminals. The resin has a sufficiently low elasticity modulus that occurrence of undesirable migration is suppressed.
In one embodiment of this invention, the liquid crystal display module further includes an anisotropic conductive film for coupling the substrate with the liquid crystal display element.
The inventors conducted an experiment in which an Au bump to which a halogen compound was attached was exposed to high temperature and high humidity. As a result, occurrence of migration was suppressed and a sufficient coupling strength was obtained between the LC-driving IC 1 and the flexible substrate 9 when the elasticity modulus of the sealing resin 4 sealing the LC-driving IC 1 was optimized. This led to achievement of the present invention.
According to the present invention, the electrical coupling reliability of the semiconductor elements and the flexible circuit substrate, such as heat-impact resistance, moisture resistance, and a coupling strength can be enhanced. An epoxy resin or a denatured polyimide resin is used as the sealing resin.
Thus, the invention described herein makes possible the advantages of (1) providing a sealed-by-resin type semiconductor device capable of suppressing migration between Au bumps, and an LCD module including the same and (2) providing a sealed-by-resin type semiconductor device having a sufficient coupling strength between an LC-driving IC and a flexible substrate.
These and other advantages of the present invention will become apparent to those skilled in the art upon reading and understanding the following detailed description with reference to the accompanying figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view of a COF LCD module according to an embodiment of the present invention.
FIG. 2 is a side view of the COF LCD module shown in FIG. 1 .
FIG. 3 is a major cross-sectional view of the COF LCD module shown in FIG. 1 .
FIG. 4 is a graph showing the rate of occurrence of display abnormality due to migration in the COF LCD module shown in FIG. 1 .
FIG. 5 is a plan view of a conventional COF LCD module.
FIG. 6 is a side view of the COF LCD module shown in FIG. 5 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiments of the present invention will be described with reference to the accompanying drawings.
FIG. 1 is a plan view of a COF LCD module 200 according to an embodiment of the present invention. FIG. 2 is a side view of a COF LCD module 200 according to the embodiment of the present invention. The same components as those included in the COF LCD module 400 are indicated by the same reference numerals as those used for the COF LCD module 400 . Detailed description is omitted for those components.
The COF LCD module 200 includes an LCD element 8 and a COF 100 . The COF 100 includes a flexible substrate 9 on which an LC-driving IC 1 and a chip 10 are mounted.
The COF LCD module 200 according to the embodiment of the present invention is different from the foregoing COF LCD module 400 in that in the COF LCD module 200 the LC-driving IC 1 is sealed by a sealing resin 12 , of which the elasticity modulus is optimized, instead of the sealing resin 4 .
FIG. 3 is a cross-sectional view of a major portion of the COF 100 according to the embodiment of the present invention. The sealing resin 12 seals the LC-driving IC 1 .
In the LC-driving IC 1 , a given electronic circuit (not shown) and an electrode pad 1 B are provided on a rear side 1 A of the LC-driving IC 1 . The Au bump 3 is provided on the electrode pad 1 B. For example, the outer dimensions of the LC-driving IC 1 are about 2 mm×20 mm. The bump height H is about 15 μm. The minimum bump pitch P of the Au bump 3 is about 80 μm.
The flexible substrate 9 includes a polyimide film 2 having a thickness of about 20 to 30 μm, a conductor pattern 5 of Cu provided on the polyimide film 2 , a portion on which the LC-driving IC 1 is mounted, a portion on which the chip 10 is mounted, an ink coverlay 6 of polyimide covering portions other than a connecting terminal 9 A which connects an LCD element 8 and the COF 100 , an Sn plating layer 7 with which the conductor pattern 5 is coated.
The flexible substrate 9 and the LC-driving IC 1 are registered so that the conductor pattern 5 is opposed to the Au bump 3 . The LC-driving IC 1 is heated and pressed from the top side thereof (in the direction indicated by arrow A) so as to couple the conductor pattern 5 with the Au bump 3 due to an Sn—Au alloyed junction. The heating temperature is about 280° C. or more which is sufficient so that the Sn plating layer 7 and the Au bump 3 form into an eutectic alloy.
Thereafter, a sealing resin 12 is injected into a gap between the LC-driving IC I and the flexible substrate 9 . The sealing resin 12 is cured to seal the gap. The sealing resin 12 has an elasticity modulus which is sufficiently low so as not to generate undesirable migration.
Thereafter, a resin is applied to the LC-driving IC 1 using a dispenser. The resin is heated for about two hours at about 100° C. and then for about one hour at about 150° C. so as to be cured.
Thereafter, a transparent electrode connecting terminal 8 A of the LCD element 8 is electrically coupled with a connecting terminal 9 A of the flexible substrate 9 via an anisotropic conductive film. Thus, the LCD module 200 is completely fabricated.
EXAMPLES
Example 1
In Example 1, a bisphenol type epoxy resin was used as the sealing resin. Four types of bisphenol type epoxy resins having elasticity modulus of 0.005 GPa, 0.07 GPa, 0.3 GPa, and 1.0 GPa, respectively, were used. The elasticity modulus was measured by a dynamic viscoelasticity method (conducted at a room temperature of about 25° C.).
50 LCD modules were fabricated for each of the four types of bisphenol type epoxy resins having elasticity modulus of 0.005 GPa, 0.07 GPa, 0.3 GPa, and 1.0 GPa, respectively. All the LCD modules were placed in a moisture-resistance reliability test bath having a temperature of about 60° C. and a humidity of about 95%. The rate of occurrence of an LCD abnormality, which is caused by leakage between the Au bumps due to the migration, was evaluated after about 1000 hours had passed.
FIG. 4 is a graph showing the rate of occurrence of the LCD abnormality that is caused by leakage between the Au bumps due to the migration, in Example 1. As is seen from FIG. 4, when the bisphenol type epoxy resin was used as the sealing resin 12 in Example 1, there were substantially no LCD abnormality that is caused by leakage between the Au bumps due to the migration.
The coupling strength between the LC-driving IC 1 and the flexible substrate 9 was evaluated. The flexible substrate 9 was bent into a 90° angle while the LC-driving IC 1 was fixed on the flexible substrate 9 . A load was increasingly imposed on the LC-driving IC 1 while the LCD element 8 was displaying. In this case, the value of the load, which starts to generate the display abnormality in the LCD element 8 , was determined.
The inventors' previous study has found that when the value of the load, which starts to generate the display abnormality in the LCD element 8 , is about 500 gf or more, there are substantially no adverse problems in the process of incorporating the COF LCD module into a device.
The average values of the results obtained by measuring 10 COF LCD modules 200 are shown in Table 1. Table 1 shows the values of loads which start to generate the display abnormality in the LCD elements having the respective elasticity.
TABLE 1
Conventional
Conventional
Example 2
example 1
example 2
Elasticity
Example 1 (epoxy)
(polyimide)
(epoxy)
(silicone)
modulus (GPa)
0.005
0.07
0.3
1.0
0.45
0.65
2.5
3.1
0.0006
Average
380
730
1220
1380
950
970
1510
1500
210
value (gf)
Maximum
410
550
1530
1610
1160
1210
1670
1710
260
value (gf)
Minimum
350
690
1080
1100
880
860
1330
1350
180
value (gf)
As shown in Table 1, in the case of the COF LCD modules 200 of an epoxy resin having an elasticity modulus of 0.07 GPa or more and 1.0 GPa or less, the values of loads are 500 gf or more.
As compared with conventional sealing resins having higher elasticity modulus, the epoxy resins used in Example 1 have shorter cure time, thereby improving productivity.
Example 2
In Example 2, a denatured polyimide including aromatic tetracarboxylic acid and aromatic diamine was used as the sealing resin. Two types of the denatured polyimide having elasticity modulus of 0.45 GPa and 0.65 GPa, respectively. The elasticity modulus was measured by the dynamic viscoelasticity method, similar to Example 1 (conducted at a room temperature of about 25° C.)
50 COF LCD modules 200 were fabricated for each of the two types of the denatured polyimide having elasticity modulus of 0.45 GPa and 0.65 GPa, respectively, in a way similar to Example 1. The sealing resin was heated for two hours at 90° C. and then for two hours at 150° C.
The COF LCD modules thus fabricated were subjected to a moisture-resistance reliability test similar to that of Example 1. The results are shown in FIG. 4 . As is seen from FIG. 4, when the denatured polyimide was used as the sealing resin 12 in Example 2, there were substantially no LCD abnormality caused by leakage between the Au bumps due to the migration.
The coupling strength between the LC-driving IC 1 and the flexible substrate 9 was evaluated in a way similar to that of Example 1 and the results are shown in Table 1. In the case of the denatured polyimide used as the sealing resin 12 in Example 2, the obtained values of loads are 500 gf or more. The denatured polyimide having elasticity modulus of 0.07 GPa or more and 1 GPa or less has the same effect as that of Example 1.
Conventional Example 1
In Conventional Example 1, two types of epoxy resins having elasticity modulus of 2.5 GPa and 3.1 Gpa, which are higher than the elasticity modulus of the sealing resins of Examples 1 and 2, were used.
Similar to Example 1, 50 COF LCD modules were fabricated for each elasticity modulus. The sealing resins were cured for two hours at 120° C. and then for two hours at 150° C. All the COF LCD modules were subjected to a moisture-resistance reliability test similar to that of Example 1.
The results are shown in FIG. 4 . As is seen from FIG. 4, in the case of the sealing resins of Conventional Example 1 having an elasticity modulus which is higher than the elasticity modulus of the sealing resins of Examples 1 and 2, there is observed an LCD abnormality caused by leakage between the Au bumps due to the migration.
Conventional Example 2
In Conventional Example 2, a silicone resin having an elasticity modulus of 0.0006 GPa, which is lower than the elasticity modulus of the sealing resins of Examples 1 and 2, was used.
Similar to Example 1, 50 COF LCD modules were fabricated. The sealing resin was cured for four hours at 150° C. The COF LCD modules were subjected to a moisture-resistance reliability test similar to that of Example 1.
The results are shown in FIG. 4 . As is seen from FIG. 4, in the case of the sealing resins of Conventional Example 2, there is substantially no LCD abnormality caused by leakage between the Au bumps due to the migration.
The coupling strength between the LC-driving IC 1 and the flexible substrate 9 was evaluated in a way similar to that of Example 1 and the results are shown in Table 1. In the case of the resin of Conventional is Example 2, the obtained value of a load does not exceed 500 gf.
As described above, the present invention can provide the sealed-by-resin type semiconductor device capable of suppressing occurrence of migration between the Au bumps, and an LCD module including the same.
Further, the present invention can provide the sealed-by-resin type semiconductor device having a sufficient coupling strength between the LC-driving IC and the flexible substrate, and an LCD module including the same.
In the sealed-by-resin type semiconductor device of the present invention, the epoxy resin or denatured polyimide resin having an elasticity modulus of 0.07 GPa or more and 1 GPa or less is used as a sealing resin protecting semiconductor elements. Therefore, it is possible to suppress occurrence of migration which is responsible for the leakage between the Au bumps. Moreover, a coupling strength between the semiconductor elements and the flexible substrate is sufficient, which is an excellent, characteristic effect.
Various other modifications will be apparent to and can be readily made by those skilled in the art without departing from the scope and spirit of this invention. Accordingly, it is not intended that the scope of the claims appended hereto be limited to the description as set forth herein, but rather that the claims be broadly construed.
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A sealed-by-resin type semiconductor device includes a substrate, a lead provided on the substrate, and a semiconductor element provided on the lead by flip chip bonding. The semiconductor element includes a plurality of terminals connected to the lead. The sealed-by-resin type semiconductor device further includes a resin for protecting the plurality of terminals, and the resin has a sufficiently low elasticity modulus that occurrence of undesirable migration is suppressed.
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This application is a continuation-in-part of and claims the benefit of priority from PCT application PCT/EP2011/064659 filed Aug. 25, 2011 and German Patent Application DE 10 2010 035 944.0 filed Aug. 31, 2010, the disclosure of each is hereby incorporated by reference in its entirety.
The present invention relates to a method for the dry forming of a fiber web as well as to an apparatus for carrying out the method.
BACKGROUND
It is known for the production of non-woven fabrics that the fibers are laid down to a fiber layer on a laydown belt by means of an air flow. This method, ordinarily described as air laid among experts, is based on the fact that the fibers or fiber mixtures are placed uniformly distributed on the surface of a laydown belt by means of a forming head. The zone covered by the forming head on the laydown belt is ordinarily referred to as a forming zone, in which the fibers meet on the laydown belt. Such a method and device are described in, for example, WO 2004/106604 A1. In the case of the known methods and the known device, a multiplicity of fibers or fiber mixtures is fed to a forming head by means of an air flow. Within the forming head means are provided for mixing and distributing the fibers. On the underside of the forming head a forming outlet is constructed which ordinarily is arranged at a short distance above the laydown belt. In this connection, a clearance is formed between the forming head and the laydown belt, the clearance serving to guide a fiber stream escaping from the forming outlet. The laying down of the fibers on the laydown belt is supported by a suction device which absorbs the air of the fiber stream and conducts it away. The fiber layer forming on the surface of the laydown belt is continuously conveyed via the laydown belt out of the forming zone, so that a fiber layer is formed which is subsequently fed to a further treatment, for example solidification.
Depending on the fiber type and fiber size used in such methods, irregularities can arise in the laying down of the fibers, with the irregularities being referred to as beaching. Such irregularities in the fiber distribution are generally attributed to the fact that the distribution and laying down of the fibers is influenced by secondary air flows from the surroundings which are absorbed from the surroundings into the forming zone via the suction device.
In order to eliminate such irregularities in the laying down of the fibers, it is known for example from WO 2006/131122 A1 to influence the suction flow of the suction device in sub-regions of the forming zone. In the case of the known methods and the known device, a guide plate is assigned on an inflow side of the forming zone of the suction device, with the guide plate influencing the suction flow underneath the laying down belt. It is noted that air turbulence arising through suctioned secondary air from the surroundings on the inflow side of the forming zone is supposed to be prevented. However, as a result of the use of such a guide plate, there are differing suction flows in the forming zone which leads to differing laydown behavior of the fibers within the forming zone.
The phenomenon of beaching also could not be ruled out from other systems, such as those known for example from WO 2003/016622 A1. In this connection, the forming head on the inflow side and the outflow side each have sealing rollers, which are in contact with the surface of the laydown belt or the surface of the fiber layer. As a result, it possible to prevent to a great extent an influx in the secondary air from the surroundings. However, in this connection it is disadvantageous that the fiber layer on the surface of the laydown belt is condensed directly on the outflow side by the sealing roller arranged there.
SUMMARY
Hence, the invention addresses the problem of creating a generic method as well as a generic device for the dry forming of a fiber web with which a high uniformity of fiber distribution can be achieved within the fiber layer.
The invention is based on the understanding that the laying down of the fibers is influenced by a fiber stream transverse to a laydown belt essentially through the reorientation of the fibers from an essentially vertical movement to a horizontal movement defined by the laydown belt. Thus it became apparent to the inventors that the residence time of the fibers until impinging on the laydown belt has an influence on the development of the fiber layer. In this respect the laying down of the fibers and the structure of the fiber layer could be advantageously improved by having the fibers of the fiber stream within the forming zone run through the clearance with free sections of different lengths. In this way zones could be realized in which the fibers had greater latitude for the reorientation through long free sections.
The method variant in which the fibers of a fiber stream produced on an inflow side of the forming zone run through a longer free section than the fibers of the fiber stream produced on an outflow side of the forming zone is particularly advantageous. In addition, the great distance between the forming head and the laydown belt on the inflow side can prevent the turbulence effects caused by the inflowing secondary air. On the other hand, the secondary air can be used in a supporting manner for reorientation and laying down of the fibers.
In order to obtain a uniform modification of the free sections within the forming zone, the method variant is preferably used in which case the fiber stream is produced by a forming head inclined vis-à-vis the laydown belt, wherein the free sections of the fibers within the clearance between the inflow side and the outflow side are continuously changing. With this arrangement it is possible to make advantageous use of a horizontally aligned laydown belt for receiving and development of the fiber layer, so that a redistribution of the fibers in the fiber layer cannot occur during transport on an inclined laydown belt.
In order to suppress counter-effects through other secondary air flows within the forming zone, the method variant is particular advantageous in which case the clearance of the forming zone on the outflow side for guiding the fibers is screened by at least one screening means vis-à-vis the surroundings.
In contrast, the clearance of the forming zone on the inflow side for guiding the fibers to the surroundings is kept open. With this, a secondary air flow can be deliberately produced which acts in the direction of the material flow of the laydown belt. Thus, advantageous pre-orientations can be produced on the fiber stream in the direction of the material flow.
In order to be able to generate a uniform fiber layer over the entire width of the laydown belt, in accordance with an advantageous improvement of the inventive method, provision is made that the clearance of the forming zone between the inflow side and the outflow side for guiding the fibers to the surroundings is kept closed. In this way secondary air flows occurring on the long side of the laydown belt can be prevented.
For carrying out of the inventive method in the case of the inventive device the forming head and the laydown belt are kept in a non-parallel arrangement, so that the clearance is formed by differing distances between the laydown belt and the forming outlet of the forming head.
In this connection, the arrangement of the forming head and of the laydown belt is preferably constructed in such a way that the distance between the laydown belt and the forming outlet of the forming head on an inflow side of the forming zone is greater than distance between the laydown belt and the forming outlet of the forming head on an outflow side of the forming zone. In addition, the larger free section for reorientation is realized in the inflow region of the forming zone.
The forming head is preferably held on a inclined plane vis-à-vis the laydown belt so that the distance between the laydown belt and the forming outlet of the forming head from the inflow side to the outflow side of the forming zone is continually changing. With this, a continuous reduction of the free section in the direction of the material flow of the laydown belt can be achieved. Thus, the reduced suction effect due to the already formed fiber layers toward the outflow side of the forming zone can be compensated. The fibers can be received with essentially the same kinetic energy on the surface of the laydown belt or of the fiber layer.
In order to obtain a setting of the free sections in the forming zone optimized for formation of the fiber layer dependent on the fibers and fiber mixtures, the forming head is advantageously held by an adjustable retainer, as a result of which the degree and/or the height of the inclined plane of the forming head can be set.
In order to suppress as much as possible the entry of secondary air on the outflow side, two alternative device variants of the inventive device can be employed. In the case of a first variant, at least one screening means is arranged on the outflow side of the forming head, through which the clearance can be screened vis-à-vis the surroundings. Such screening means are preferably formed by driven sealing rollers which are held in contact with a fiber layer on the laydown belt. This variant is however only suitable when a pre-compression of the fiber layer on the surface of the laydown belt is harmless for any further processing.
For sensitive fiber layers, the device variant is preferably implemented in which case an outflow opening is formed on the outflow side of the forming zone between the forming head and the laydown belt. Such outflow openings are preferably implemented with a small gap height which, depending on the thickness of the fiber layer, can range from 4 mm to 20 mm.
In order to be able to use the secondary flow of ambient air necessary for reorientation, the inventive device is preferably constructed in such a way that an inflow opening is formed on the inflow side of the forming zone between the forming head and the laydown belt.
In this connection, the inflow opening is preferably constructed with a gap height ranging between 40 mm to 400 mm. Thus, preferably laminar secondary flows of the ambient air can be introduced into the forming zone.
The peripheral regions of the forming zone are preferably sealed in accordance with the advantageous improvement of the invention, wherein the clearance to both long sides of the laydown belt vis-à-vis the surroundings is sealed by sealing means between the forming head and the laydown belt. Thus, a uniform fiber layer can be produced over the entire width of the laydown belt.
The fiber stream is preferably produced at the forming outlet of the forming head through a perforated plate or stressed screen cloth, which makes possible a homogenized distribution of the fibers over the entire forming zone.
The inventive method and the inventive device are suitable for the laying down of all fibers and fiber mixtures. For example, synthetic and natural fibers or mixtures of synthetic and natural fibers can be laid down to fiber layers. Due to the high uniformity of the produced fiber layer in the process, preferably even the finest parts such as for example a powder can be advantageously integrated into the mixture.
The inventive method will be explained in more detail with the help of some exemplary embodiments of the inventive device making reference to the attached figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows schematically a cross-section view of a first exemplary embodiment of the inventive device for carrying out the inventive method.
FIG. 2 shows schematically a cross-section view of a further exemplary embodiment of the inventive device for carrying out the inventive method.
DETAILED DESCRIPTION
FIG. 1 shows schematically a first exemplary embodiment of the inventive device for carrying out the inventive method. The exemplary embodiment shows a mixing chamber 1 that is connected via a fiber inlet 2 to a fiber feed not shown in the figure. The fiber inlet 2 can contain one or more connections in order to feed one or more fibers or fiber mixtures by means of an air flow of the mixing chamber 1 . The mixing chamber 1 is connected on an underside to a forming head 3 . The forming head 3 includes several means (not shown in detail here) to uniformly distribute the fibers or fiber mixtures and conduct them away as a fiber stream via a forming outlet 4 constructed on the underside. The forming outlet 4 preferably includes a perforated plate 5 . In the process, the distribution takes place within the forming head preferably via several driven wings, such as is known for example from WO 2004/106604. In this respect, WO 2004/106604 is incorporated herein by reference.
The forming head 3 is arranged above a laydown belt 8 at an inclined plane 21 . The laydown belt 8 is essentially horizontally aligned, so that on an inflow side 10 a greater distance between the forming head 3 and the laydown belt 8 is set than on the opposing outflow side 11 . The distance to the inflow side 10 is marked with the identification letters letter S E . In contrast the distance between the forming outlet 4 and the laydown belt 8 is marked with the identification letters S A .
The location of the forming head 3 or the location of the inclined plane 21 can be set via a retainer 19 of the forming head 3 . The retainer 19 is in this exemplary embodiment formed by two actuators 20 . 1 and 20 . 2 , each of which engages on support arm 22 . 1 and 22 . 2 , with the support arms being connected to the forming head 3 . Thus, through a parallel actuation of the actuators 20 . 1 and 20 . 2 the height of the forming head can be set relative to the laydown belt 8 and thus the height of the inclined plane 21 . By means of unilateral actuation of the actuators 20 . 1 or 20 . 2 it is possible to set the angular position of the forming head 3 and with it the degree of the inclined plane 21 relative to the laydown belt 8 . In each case, a modification of the distances between the forming outlet 4 and the laydown belt 8 occurs.
The laydown belt 8 is gas permeable and is continuously fed in a material conveying direction via several guide rollers 9 , with the material conveying direction being identified by a double arrow. In this respect, the laydown belt 8 continuously runs through the forming zone 6 from the inflow side 10 to the outflow side 11 . In the process, the fibers are laid down on the surface of the laydown belt 8 to a fiber layer 23 .
Below the laydown belt, a suction device 16 is arranged with the suction device being connected via a suction channel 17 to a vacuum source not shown in the figure.
The forming outlet 4 of the forming head 3 is in this case rectangularly constructed, so that an essentially rectangular forming zone 6 is constructed above the laydown belt 8 . The clearance 7 of the forming zone 6 is in this exemplary embodiment only connected to the surroundings via an inflow opening 14 on the inflow side 10 . On the opposing outflow side 11 , a screening means 12 in the form of a sealing roller 13 is arranged between the forming head 3 and the laydown belt 8 . The absorption of secondary air from the surroundings can be prevented in this way. In addition, in the region of the long sides of the forming head 3 , there are two opposing separating plates 15 provided, which seal the clearance 7 of the forming zone 6 to both long sides of the laydown belt 8 vis-à-vis the surroundings.
In the case of the exemplary embodiment of the inventive device shown in FIG. 1 , a synthetic fiber, for example, is fed with a powder jointly via an air flow of the mixing chamber 1 . Within the mixing chamber 1 , static or dynamic means can be constructed, which implement a premixing of the fibers. Subsequently, the mixture of fiber and powder is guided via the air flow to the forming head 3 . Within the forming head 3 , a distribution of the fiber and powder mixture takes place via the distribution means, with the mixture then being guided as a fiber stream into the clearance 7 via the forming outlet 4 . Within the forming zone 6 , a continuously active suction flow is generated via the suction device 16 , with the suction flow on the one hand collecting the fibers entering into the clearance 7 and on the other hand generating a secondary air flow from the surroundings on the inflow side 10 . In the guiding of the fibers within the clearance 7 , the fibers of the fiber stream in the region of the inflow side 10 run through a longer free section until being laid down on the laydown belt 8 . By way of contrast, the fibers on the opposing outflow side 11 are guided on a shorter free section. Thus the fibers guided in the region of the inflow side 10 receive a higher residence time in order to execute the transition from a vertically oriented movement to a horizontally oriented movement. Thus, the fibers can be laid down by the influence of a secondary air flow on the inflow side with a slight pre-orientation in material flow direction. This turns out to be particularly advantageous in particular in the formation of a uniform fiber layer 23 .
Depending on the fiber type and fiber mixtures, it turns out that the distance S E on the inflow side 10 for formation of the inflow opening 14 should be in a range from 40 mm to 400 mm. Too small a distance between the forming head 3 and the laydown belt 8 has the disadvantage that the absorbed secondary air leads to severe turbulence. Too great a distance between the forming head 3 and the laydown belt 8 on the inflow side 10 increasingly reduces the influence of the secondary air, so that this should likewise be avoided.
On the opposing outflow side 11 of the forming head 3 the absorption of a secondary air is prevented by the sealing roller 13 . In this respect, only the influence of the secondary air permitted via the inflow opening 14 remains, with the secondary air being able to be used purposefully for the improvement of the fiber layers.
The inventive method and the inventive device are thus particularly well suited for achieving a high uniformity in the production of fiber layers that are formed of a multiplicity of single finite fiber pieces. In this connection, synthetic or natural fibers or mixtures of synthetic and natural fibers can be laid.
FIG. 2 shows a further exemplary embodiment of the inventive device for carrying out the inventive method. The exemplary embodiment of the inventive device shown in FIG. 2 is essentially identical to the exemplary embodiment in accordance with FIG. 1 , so that only the differences will be explained here and otherwise reference is made to the aforementioned description.
In the exemplary embodiment shown in FIG. 2 , the forming head 3 is likewise held on an inclined plane vis-à-vis the laydown belt 8 , so that on the inflow side 10 a greater distance arises between the forming outlet 4 and the laydown belt 8 than vis-à-vis the outflow side 11 . The distance on the inflow side is marked with the identification letter S E and on the outflow side with the identification letter S A . In this connection, on the outflow side 11 between the forming head 3 and the laydown belt 8 an outflow opening 18 is formed, which connects the clearance 7 of the forming zone 6 to the surroundings. Likewise, on the opposing inflow side 10 , an open inflow opening 14 is shown that is likewise connected to the surroundings. However, through the inclined arrangement of the forming head 3 the outflow opening 18 a significantly lower gap height than the opposing inflow opening 14 is provided. Thus, depending on the fiber and fiber type, the outflow opening 18 is constructed in such a way that a distance in the magnitude of 4 mm to 20 mm ensues between the forming outlet 4 and the laydown belt 8 . The gap height of the outflow opening 18 is arranged or set in the process essentially to the thickness of the fiber layer which is produced on the surface of the laydown belt.
For the setting of the inflow opening 14 and the outflow opening 18 , the forming head 3 is likewise adjustable via an adjustable retainer 19 . The retainer 19 is in this connection identical to the aforementioned exemplary embodiment, so that no further explanation will be given here.
In the exemplary embodiment of the inventive device shown in FIG. 2 , the forming zone and thus the clearance 7 are only screened from the surroundings by the separating plates 15 arranged on the long sides. No additional screening means are provided on either the inflow side 10 or the outflow side 11 .
In the exemplary embodiment shown in FIG. 2 , the fibers within the fiber stream are likewise guided in free sections of differing length within the clearance, so that the residence times for running through the free sections in the inflow region of the forming zone are greater than in the outflow region. In this connection, in this respect the secondary air effects can be used jointly in order to obtain a favorable reorientation of the movement sequences in single fibers. Through the narrow gap on the outflow side it is possible to minimize the absorbed secondary air so that undesired disturbing effects can be avoided.
The above disclosed subject matter is to be considered illustrative, and not restrictive, and the appended claims are intended to cover all such modifications, enhancements, and other embodiments, which fall within the true spirit and scope of the present invention. Thus, to the maximum extent allowed by law, the scope of the present invention is to be determined by the broadest permissible interpretation of the following claims and their equivalents, and shall not be restricted or limited by the foregoing detailed description. While various embodiments of the invention have been described, it will be apparent to those of ordinary skill in the art that many more embodiments and implementations are possible within the scope of the invention. Accordingly, the invention is not to be restricted except in light of the attached claims and their equivalents
REFERENCE LIST
1 Mixing chamber
2 Fiber inlet
3 Forming head
4 Forming outlet
5 Perforated plate
6 Forming zone
7 Clearance
8 Laydown belt
9 Guide rollers
10 Inflow side
11 Outflow side
12 Screening means
13 Sealing roller
14 Inflow opening
15 Separating plate
16 Suction device
17 Suction channel
18 Outflow opening
19 Retainer
20 . 1 , 20 . 2 Actuator
21 Inclined plane
22 . 1 , 22 . 2 Support arm
23 Fiber layer
Distance S E , S A
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A method and a device for the dry forming of a fiber web, in which a multiplicity of fibers or fiber mixtures are fed to a forming head by means of an air flow is described. The forming head produces a fiber stream which is introduced into a clearance of a forming zone between the forming head and a laydown belt. To obtain as uniform a construction of the fiber layer as possible during the laying down of the fibers, the fibers of the fiber stream run through the clearance within the forming zone with free sections of different lengths. To this end, the forming head and the laydown belt are held in a non-parallel arrangement, with the result that the clearance is formed by different spacings between the laydown belt and the forming outlet of the forming head.
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CROSS-REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. Provisional Application No. 61/215,254, filed May 4, 2009.
TECHNICAL FIELD
Embodiments of the present invention relate to flame retardant fabrics.
BACKGROUND
Phosphorus only based flame retardants (“FRs”) are typically not effective on nylon. It has been noted that in many cases phosphorus treated nylon fabrics will burn at a greater rate than the untreated fabric. It is believed that in the combustion process the phosphorus containing material forms an acidic environment which causes the nylon polymer to unzip to supply more fuel for combustion. In theory the combustion matrix needs a component that will lower the “acidity” during combustion to minimize the “unzipping” of the nylon polymer.
Many of the phosphorus containing systems for nylon require a halogen with the phosphorus system to be effective. It is not sure how the bromine works but it is assumed that it serves as a free radical scavenger as well as possibly modifying the melt properties of the nylon polymer. However, there is a trend in the industry to minimize the use of halogens as FR materials due to environmental concerns.
The use of sulfur containing materials has been used for years to treat nylon composites to meet various FR standards. The more common systems are based on thiourea and formaldehyde components. However, the hand of the treated fabrics is usually very stiff and there is an odor associated with the finished product. The finished product also has a high level of formaldehyde present. The mechanism of the sulfur containing materials for reducing the flammability is based on modifying the melt behavior of the nylon polymer.
For nylon/cotton blends with 10 percent or higher of nylon, there is generally a molten puddle of the nylon polymer present with flame front in the combustion process, even with FR treated fabrics. In a fire it is perceived that this molten puddle of nylon sticks to the skin of a person wearing the garment and can seriously burn the person. FR cellulosic containing fabrics form a char which helps to provide some insulation to minimize the burn injuries. On the other hand, 100% synthetic containing fabrics and high nylon containing blends can melt and stick to the skin causing serious burns more so than cellulosic fabrics.
Fabric and clothing manufacturers continue to seek improvements in FR fabrics and methods for manufacturing FR fabrics.
SUMMARY
Embodiments of the present invention use melamine-based resins in combination with phosphorus-based flame retardants to greatly improve flame retardant performance, durability, and further promote char formation in the combustion zone of fabrics and fabric blends. Method embodiments of the present invention include a melamine resin in combination with a treatment with a tetrakis(hydroxymethyl)phosphonium-based (“THP”) compound, improving the FR performance. There is little effect on the hand and strength loss of the treated fabrics. This improved FR performance may be due to a synergistic effect between phosphorus of the THP and nitrogen of the melamine where the nitrogen may catalyze or promote phosphorylation or char formation in the combustion process. Another object of embodiments of the present invention is to produce a nylon/cellulosic FR fabric which will produce a minimum of molten nylon polymer in the combustion process. Another object is to utilize a reaction of THP chemistry with melamine resin to form a durable FR finish that will meet the flammability requirements after 100 home launderings, especially on lightweight fabrics. Historically, fabrics with high nylon content were treated with a high concentration of a THP-based aqueous solution to increase the final phosphorous loading on the fabric. These fabrics performed extremely poorly on the National Fire Protection Association's (“NFPA”) 12 second bottom vertical test. Fabrics produced using methods of the present invention have a greatly improved durability to laundering, and these fabrics pass the NFPA 12 second bottom vertical test after numerous launderings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a flow diagram of a method for manufacturing flame retardant fabrics in accordance with one or more embodiments of the present invention.
FIG. 2 shows a molecular structure of melamine and molecular structures of melamine-based compounds found in melamine-based resins.
FIG. 3 shows a table summarizing examples of various fabrics treated in accordance with one or more embodiments of the present invention.
DETAILED DESCRIPTION
Embodiments of the present invention are directed to methods for manufacturing flame retardant (“FR”) fabrics and to fabrics produced by the methods described below. FIG. 1 shows a flow diagram of a method for manufacturing flame retardant fabrics. In step 101 , a melamine-based compound is applied to the fabric. Examples of suitable melamine-based compounds for pre-treating the fabric include, but are not limited to, trimethoxymethyl melamine (“TMMM”) and hexamethoxymethyl melamine (“HMMM”). FIG. 2 shows molecular structural formulas of melamine 202 and structural formulas of TMMM 204 and HMMM 206 .
Returning to FIG. 1 , step 101 , the melamine-based compound can be in the form of a resin which is diluted in water to form a melamine-based aqueous solution. The melamine-based aqueous solution is applied to the fabric and the fabric is padded, meaning the fabric can be placed in a vat of the melamine-based aqueous solution followed by running the fabric through a pair of narrowly spaced rollers that squeeze or press the fabric. Next, the fabric is cured by placing the fabric in an oven. The oven dwell time and oven temperature depend on the type of fabric. The oven temperatures can range from approximately 300° F. to approximately 450° F., and the temperature of the fabric in the oven ranges from approximately 300° F. to approximately 400° F. The dwell time can range from approximately 20 seconds to approximately 20 minutes, depending on the temperature in the oven and the fabric temperature.
In step 102 , a THP-based compound is applied to the fabric. Examples of suitable THP-based compounds include, but are not limited to, tetrakis(hydroxymethyl)phosphonium sulfate urea (“THPS-urea”) and tetrakis(hydroxymethyl)phosphonium chloride urea (“THPC-urea”). THPS-urea and THPC-urea are FR compounds. The THP-based compound is combined with water to form a THP-based aqueous solution that can be neutralized to a pH in the range of approximately 5.0 to approximately 7.0 using approximately 5% caustic NaOH or using one or more other suitable alkali agents. Note this pH range is suitable for good fabric strength and FR efficiency, but the process can also run at an even wider range of pHs, such as pHs ranging from approximately 3.0 to approximately 8.0. The THP-based aqueous solution is applied to the fabric and the fabric is padded, as described above in step 101 . After the fabric is treated with the THP-based compound, the fabric is dried.
In step 103 , the fabric is ammoniated by placing the fabric in an ammonia chamber in order to form a flame retardant polymer containing phosphorous 3. For example, the fabric can be ammoniated by spraying the fabric with, or exposing the fabric to, an anhydrous ammonia gas.
In step 104 , the fabric is oxidized, washed and framed. The fabric can be oxidized by placing the fabric in an aqueous solution composed of approximately 10% peroxide. The oxidation process may occur in the same chamber as the ammonia chamber or in a separate chamber. Other suitable oxidizing agents include, but are not limited to, sodium percarbonate or ozone. After the fabric is ammoniated, oxidation sets the melamine-based compound and the THP-based compound as a flame retardant polymer in the fabric by converting the phosphorous 3 to phosphorous 5.
Note that embodiments of the present invention are not limited to step 1 being performed before step 2. In other embodiments, step 2 can be performed before step 1. For example, the process of applying a THP-based compound to a fabric described in step 2 can be applied before application of the melamine-based compound described in step 1.
The fabric can be composed of a cellulosic material including, but not limited to, cotton, rayon, tencel or flax. It can be composed of a blend of nylon and one or more cellulosic materials. The fabric can also be a blend of one or more cellulosic materials and one or more synthetic materials, such as nylon, spandex, acrylic, acetate or triacetate. Examples of nylon blended fabrics include, but are not limited to, a nylon/cellulose blend, a nylon/cotton blend, a cotton/nylon/spandex blend, or a rayon/nylon/spandex blend.
EXAMPLES
Examples of fabrics treated using the above described methods are now described. FIG. 3 shows a table summarizing the various flame retardant fabrics produced in the following examples in accordance with one or more embodiments of the present invention.
Example 1
The fabric treated in this example was a 5.4 ounces per square yard interlock 65% cotton 35% nylon blend. The pretreatment consists of padding a bath containing approximately 20 liters of TMMM product per 50 gallons. The wet pick up was approximately 86%. The resin treated fabric was cured at approximately 370° F. for about two minutes. In the second step the pretreated fabric was padded with a mix containing 22 gallons of THPS-Urea condensate per 50 gallons of water. The FR treated fabric was dried at approximately 270° F. to about 10% moisture after which the FR treated fabric was ammoniated, oxidized, washed and framed. The fabric was then evaluated for hand and drape and was extremely soft. The char length was only 3.1 inches after 150 home laundries.
Example 2
The fabric treated in this example was a light 4.1 ounces per square yard jersey cotton/nylon/spandex having approximately 77% cotton, 19% nylon, and 4% spandex. The fabric has a minimum tear strength, but it was not possible to make a fabric with more nylon content because of the difficulty in making this blend flame resistant. The fabric was padded with a bath containing approximately 10 liters of the TMMM per 50 gallons. The wet pick up was approximately 80%. The resin treated fabric was cured at approximately 370° F. for about one and a half minutes. In the second step, the resin treated fabric was padded with a mix containing 16 gallons of THPS-Urea condensate per 50 gallons of water. The FR treated fabric was dried at approximately 270° F. to about 10% moisture. The FR treated fabric was ammoniated, oxidized, washed and framed. The fabric was then evaluated for hand and drape, and the hand was extremely soft. The fabric was stronger, and the char length was 4.5 inches after 30 home laundries. Historically, when treated with a high concentration of a THP-based aqueous solution to increase final phosphorous loading on the fabric, this fabric would have a char length greater than 7 inches after only 5 home laundries. The burst strength of the fabric used in this example was 44 pounds per square inch, compared to 40 pounds per square inch using traditional methods.
Example 3
The fabric treated in this example was a light 4.1 ounces per square yard of jersey cotton/nylon/spandex, with approximately 62% cotton, 34% nylon, and 4% spandex. The fabric was pretreated with a mix containing approximately 15 liters of TMMM per 50 gallons. The wet pick up was approximately 82%. The resin treated fabric was cured at approximately 370° F. for about one and a half minutes. In the second step the pretreated fabric was padded with a mix having 20 gallons of THPS-Urea condensate per 50 gallon of mix. The FR treated fabric was dried at approximately 270° F. to about 10% moisture. The FR treated fabric was ammoniated, oxidized, washed and framed. The fabric was then evaluated for hand and drape. The fabric was stronger, and the char length was only 4.5 inches after 30 home laundries. The burst strength of the fabric used in this example was 52 pounds per square inch, compared to 40 pounds per square inch using traditional methods.
Example 4
The fabric treated in this example was a 9.6 ounces per square yard Ponte di roma 73% rayon, 18% nylon, and 9% spandex blend. The fabric was pretreated with a resin mix containing approximately 20 liters of TMMM per 50 gallons. The wet pick up was approximately 80%. The resin treated fabric was cured at approximately 370° F. for about two minutes. In the second step the pretreated fabric was padded with a mix containing 22 gallons of THPS-Urea condensate per 50 gallons of water. The FR treated fabric was dried at approximately 270° F. to about 10% moisture. The FR treated fabric was ammoniated, oxidized, washed and framed. The fabric was then evaluated for hand and drape. It also had a good hand. Much like Example 1, the char length was only 3.1 inches after 150 home laundries.
Example 5
The fabric treated in this example was a 7.5 ounces per square yard ripstop 52% nylon and 48% cotton blend. The fabric was pretreated with a resin mix containing approximately 30 liters of TMMM per 50 gallons. The wet pick up was approximately 86%. The resin treated fabric was cured at approximately 370° F. for about two minutes. In the second step the resin treated fabric was padded with a mix containing 26 gallons of THPS-Urea condensate per 50 gallons of water. The FR treated fabric was dried at approximately 270° F. to about 10% moisture. The FR fabric was ammoniated, oxidized, washed and framed. The fabric was then evaluated for hand and drape. It was not soft. Durability of the flame retardant process was good, but this was an off the shelf ripstop with 52 fills per inch. It may be necessary to design a more open ripstop fabric to get a more acceptable fabric, perhaps 46-48 fills per inch. The char length was only 4.1 inches after 50 home laundries. A similar fabric produced using traditional methods and tested even before a single home laundry would not stop burning, and the test sample was consumed. Instead, in our example there was no molten nylon polymer in the burning zone. The char would break down to a fine powder when pressed between the fingers and thumb. There was no rigid plastic-like residue.
Example 6
The fabric treated in this example was a 4.4 oz./sq. yd. jersey comb cotton. The fabric was pretreated with a resin mix having 10 liters of TMMM per 50 gallons. The treated fabric was cured at approximately 330° F. In the second step the resin treated fabric was padded with a mix containing 16 gallons of THPS-Urea Condensate per 50 gallons of water [pH approximately 6.2]. The FR treated fabric was dried at approximately 270° F. to about 10% moisture. The FR treated fabric was ammoniated oxidized, washed, and framed. The average char length was 3 inches after 170 home laundries. Using traditional methods, a fabric that performed this well on the burn test would have a significantly harsher hand.
The foregoing description, for purposes of explanation, used specific nomenclature to provide a thorough understanding of the invention. However, it will be apparent to one skilled in the art that the specific details are not required in order to practice the invention. The foregoing descriptions of specific embodiments of the present invention are presented for purposes of illustration and description. They are not intended to be exhaustive of or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in view of the above teachings. The embodiments are shown and described in order to best explain the principles of the invention and its practical applications, to thereby enable others skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the following claims and their equivalents:
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Embodiments of the present invention use melamine-based resins as a pretreatment on fabrics and fabric blends in combination with phosphorus-based flame retardants to improve flame retardant performance, durability, and further promote char formation in a combustion zone of the fabric.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Applications for which benefit is being claimed:
[0002] 1. Provisional application No. 62/283,778 filed by William D. Rogers and Richard D Rogers entitled Plate Shear Guide Bars (Line Finder) on Sep. 10, 2015.
[0003] 2. provisional application No. 62/390,764 filed by William D Rogers and Richard D Rogers on Apr. 8, 2016 entitled Line Finder and Holding System for Brakes and Shears.
BACKGROUND OF THE INVENTION
[0004] Manufacturing of metal goods has long been an important part of our national economy and a major source of our national wealth. As competition from a global economy pressures our manufacturing base, it becomes extremely important that metal working machines be improved in productivity, accuracy and quality of work produced. One such group of machines are metal brakes, coper notchers, and particularly, shears. At present, sheet metal shears, although adequate in most respects, are difficult with regard to accuracy of cut. These machines consist primarily of two knives, one movable and one stationary. In most cases the lower knife is stationary and the upper knife is moved up and down. In order to accommodate materials of different thickness, there must be a considerable amount of space between the two knives while the machine is at rest. In order to minimize the force needed to make the cut, the upper, moving knife must have a cutting surface that is at an angle, called a rake angle, with respect to the lower, stationary knife. These factors leave the operator with no way to align the cut other than viewing and aligning with the edge of the lower knife. Often the plate is as wide as the bottom blade leaving it totally hidden. The cutting line on which the stock is to be sheared is, of course, drawn on the top surface of the stock. It is not possible for the operator to look straight down at the stock being sheared as the knives are recessed within the machine for safety and other purposes, therefore the operator must guess at the proper alignment. As thickness of stock being sheared increases, the difficulty of alignment increases. The result is lost work time and ruined material, decreasing the quality of work and the efficiency with which it is done. The manufacturer is left with a great need for a more efficient method of alignment. The present invention fulfills this need by providing a tool by which the desired line of cut by a sheet metal shear or similar device can easily and accurately be obtained.
DESCRIPTION OF THE PRIOR ART
[0005] At present, accurate cutting with shearing machines is accomplished by use of an apparatus mounted behind the cutting knife which provides a stop for the material being sheared. Such devices require adjustment for individual cuts. In addition, these devices provide only for square cutting and do not accommodate cutting stock at an angle. Solutions to these problems were offered in the provisional application No. 62/283,778 filed by William D. Rogers and Richard D Rogers entitled Plate Shear Guide Bars (Line Finder) on Sep. 10, 2015. Further solutions were offered in the provisional application No. 62/390,764 filed by William D Rogers and Richard D Rogers on Apr. 8, 2016 entitled Line Finder and Holding System for Brakes and Shears. These solutions are further addressed by this application.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a front elevation view of the shear alignment tool mounted to a sheet metal shear.
[0007] FIG. 2 is a side elevation view of the shear alignment tool showing the angle of sight of an operator.
[0008] FIG. 3 is a side elevation view showing two shear alignment tools affixed to a shear, one to the front side of the upper knife, and one to the back side of the lower knife.
[0009] FIG. 4 is a front elevation view of the two-shear alignment tool mounting arrangement.
[0010] FIG. 5 is a front elevation view of an elongated shear alignment tool equipped with a level.
DETAILED DESCRIPTION
[0011] Referring to the drawings and more specifically to figure one, it can be seen that the shear alignment tool 1 comprises essentially a base 2 , a set of facial magnets 3 imbedded into base 2 , and two adjustment screws 4 . Base 2 is formed from non-magnetic material such as aluminum or plastic. This assures that the magnetic attraction is applied at the proper place and keeps magnetic waste materials from clinging to the tool. Facial magnets 3 are positioned in base 2 so as to make contact and thus magnetically adhere to upper knife 5 . Adjustment screws 4 are so adjusted so as to make contact with frame 6 located above upper knife 5 while providing the desired opening between line identifying edge 7 of shear alignment tool 1 and lower knife 8 . Adjustment screw magnets 9 are affixed to the upper ends of adjustment screws 4 . These magnets affix the upper ends of adjustment screws 4 to frame 6 . In some shears, frame 6 may not be located or formed in a suitable way to accommodate adjustment screws 4 . In such a case, a special adapter bar may be mounted on the shear for this purpose. Both frame 6 and lower knife 8 are immovable thus the position of line identifying edge 7 above lower knife 8 , as determined by adjustment screws 4 , is maintained. Through the use of adjustment screws 4 , the space between line identifying edge 7 and lower knife 8 is set to be just larger than the thickness of the material being sheared. Upper knife 5 , lower knife 8 , and line identifying edge 7 are in the same vertical plane. Line identifying edge 7 is also set to be parallel to lower knife 8 so as to maintain a constant space width. By producing this small, even space between line identifying edge 7 and lower knife 8 , the rake angle is effectively eliminated and the distance between upper knife 5 and lower knife 8 is effectively reduced to a manageable level for the operator. As upper knife 5 lowers during the shearing process, shear alignment tool 1 continues to magnetically adhere to upper knife 5 as the surface of upper knife 5 slides along the shear alignment tool 1 . Shear alignment tool 1 is maintained at its fixed position by way of sliding action of upper knife 5 against facial magnets 3 and by the fixed position magnets 9 . During reset of upper knife 5 , adjustment screws 4 force shear alignment tool 1 to maintain its position relative to lower knife 8 , returning the setting to its rest position.
[0012] Also referring to figure one, it can be seen that close hold down accessory 10 is affixed to shear alignment tool 1 . Hold down adjustment screw 11 can be adjusted so as to contact, or nearly contact, the surface of the stock being sheared. Close hold down provides a means for holding material stationary after it becomes too short to reach the OEM standard hold down mechanism. This will allow the use of remnants now thrown in the scrap bin.
[0013] Referring to figure two, it can be seen that the bottom of shear alignment tool 1 is tapered so as to produce a very thin lower line identifying edge 7 . As the operator uses shear alignment tool 1 , he can ascertain his line of sight 12 according to his height and posture. Through the skill naturally acquired and the freedom from blockage provided by the tapered line identifying edge 7 , the space between line identifying edge 7 and the stock being sheared is further negated for a near perfect shear. Also depicted are upper knife 5 , lower knife 8 , frame 6 , and work table 14 . For simplification, close hold down accessory 10 is not depicted.
[0014] Referring to figure three, it can be seen that two shear alignment tools 1 may be used in order to obtain an accurate shear while shearing wide pieces of plate. Again for simplification, close hold down accessory 10 is not depicted. In figure three, one of the shear alignment tools 1 A is mounted and used as described above. Another shear alignment tool 1 B is placed on the back side of lower knife 8 and affixed magnetically to lower cutting edge 13 of upper knife 5 by way of adjustment screw magnets 9 and to lower knife 8 by the attraction of facial magnets 3 . The rake angle of upper knife 5 is shown in the drawing as hashed lines. This angle may cause shear alignment tool 1 B to be mounted in a tilted position relative to lower knife 8 . Further adjustment of adjustment screws 4 may be made in order to obtain a level position if desired. A tilted position poses no operational problem as side edge 15 of shear alignment tool 1 B, due to its tilted position, will move away from the edge of the stock being sheared as upper knife 5 moves it downward. This allows shear alignment tool 1 B to move up and down with the movement of upper knife 5 while maintaining contact with lower knife 8 . Adjustment screw magnets 9 , maintaining contact with upper knife 5 assured the return of shear alignment tool 1 B to its rest position after the shear is complete. This gives the operator an indication of the location of the knives that can be seen from a distance as well as an angle. Through this placement of shear alignment tools, the operator may use line identifying edge 7 to align the stock in front of him while using the side edge 15 of shear alignment tool 1 B for the alignment of the stock far to his left or right. The operator may also look from the side of both shear alignment tools, using the very edge of both tools to acquire a near perfect setting along the line to be sheared. Likewise, in the one shear alignment tool application, a series of arches or notches may be cut into the bottom of shear alignment tool 1 . In this case, a series of views of the absolute position of line identifying edge 7 with regard to the layout line on which the stock is being sheared is provided.
[0015] Referring to figure four, it can be seen that shear alignment tool 1 B is affixed to the rear of lower knife 8 and being held in place magnetically by adjustment screw magnets 9 . It can also be seen that shear alignment tool 1 A is magnetically affixed to upper knife 5 and held fast to frame 6 by adjustment screw magnets 9 . As upper knife 5 lowers to make the cut, shear alignment tool 1 B slides along lower knife 8 and shear alignment tool 1 A remains fixed as upper knife 5 slides along its surface. After the shear is made, as upper knife 5 raises, shear alignment tool 1 B is returned to its rest position. The position of shear alignment tool 1 A remains fixed as upper knife 5 regains its relative position with shear alignment tool 1 A.
[0016] Shear alignment tools 1 A and 1 B may also be used wherein both tools are located on the operator's side of the shear. In fact, it is often advantageous to use multiple tools in this configuration, especially when wide sheets of stock are being sheared. Also, shear alignment tools of different lengths may be employed, depending upon the needs of the operator. In such uses, it is important that the entire line identifying edge be parallel to the cutting edge of lower knife 8 in order to obtain an accurate cut. In figure five, it can be seen that this is accomplished by the presence of a level 16 properly affixed to elongated shear alignment tool 17 . With the shear machine being installed so that lower knife 8 is level, line identifying edge 7 can be set parallel to lower knife 8 by use of adjustment screws 4 and level 16 .
[0017] Through this multifaceted tool, the operator is given several methods of alignment, all of which provide a massive improvement in accuracy with regard to the use of shears and other similar tools.
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An apparatus for improving the accuracy of machines which shear plate materials in general and sheet metals in particular. The apparatus comprises an indicator that is magnetically mounted to the shearing blade and extends downward toward the work table of the machine to give an indication of where the blade will pass through the metal.
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This application is a continuation of U.S. patent application Ser. No. 11/850,311 filed on Sep. 5, 2007 to issue on Feb. 17, 2009 as U.S. Pat. No. 7,491,009.
BACKGROUND
One of the most dangerous maneuvers in driving in the United States is making a left turn. In the United States, traffic drives on the right-hand side of the road and on-coming traffic drives on the left-hand side of the road. To make a left turn, a vehicle must cross the on-coming traffic.
In other countries, such as the United Kingdom, traffic drives on the left-hand side of the road and on-coming traffic drives on the right-hand side of the road. In those countries, a right turn is dangerous because it requires crossing on-coming traffic. Throughout the rest of this disclosure we will discuss left turns but a person of ordinary skill would readily recognize that the same concepts and techniques apply to right turns in countries with traffic conventions such as those in the United Kingdom.
A traditional method for reducing the danger of left turns, illustrated in FIG. 1 , uses lanes that are dedicated to left turns and traffic lights that include lights that regulate left turns. FIG. 1 shows an intersection between two four-lane roads. An intersection can be two roads crossing at substantially right angles, or it can be one road teeing into another, or it can be two or more roads coming together at an angle, such as in a Y intersection. A road can have any number of lanes and can have any surface.
A road may allow travel in two substantially opposite directions although a road can also be one-way. In FIG. 1 , one road has two A lanes for travel in the A direction, i.e., from left to right on the page, and two lanes for travel in the A-prime direction, i.e., from right to left on the page. A second road that intersects with the first road has two B lanes for travel in the B direction, i.e., from top to bottom on the page, and two B-prime lanes for travel in the B-prime direction, i.e., from bottom to top on the page. For simplicity of discussion, it will be assumed for all of the drawings of intersections discussed herein that the top of the page is the north as indicated by the compass included on some or all of the Figure pages. Further, the “arm” of an intersection extending in a particular direction will be referred to in that manner (e.g., the “east arm” referring to the arm of the intersection extending to the right, or east, on the page). However, it will be understood that the orientation of the roads with respect to the compass is not limiting. For example, FIG. 1 may be oriented such that north on the compass is at the top of the drawing or it may be to the right of the drawing or any other orientation.
In the traditional approach illustrated in FIG. 1 , each set of lanes is provided with a right-turn lane. For example, a vehicle would use right-turn lane 105 to turn from the A lanes to the B lanes. Similarly, each set of lanes is provided with a left-turn lane. For example, a vehicle would use left-turn lane 110 to turn from the A lanes to the B-prime lanes.
In addition, in the traditional approach illustrated in FIG. 1 the intersection may be controlled by traffic indicators, such as traffic lights. A different set of traffic lights may be devoted to some or all of the directions that traffic can travel through the intersection. Each direction may have the traditional red (for stop), yellow (for caution), and green (for proceed) lights, each color representing a state of the traffic flow. A turn may have a green arrow, indicating that the turn can be made, instead of the traditional green light. Similarly, the yellow and red lights for a turn can be replaced with yellow and red arrows, respectively. As an alternative to lights, the states may be represented by mechanical indicators, such as wooden, metal, or cloth flags. The traffic indicators may be attached to a pole adjacent the road or they may be suspended from a cable strung across the intersection.
The traffic indicators may have phases. A traffic indicator “phase” defines the state of the traffic indicators at an intersection. For example, one phase may be defined by the left turn indicator for the turn from the A lanes to the B-prime lanes being green and all other lights being red. Another phase may be for the lights over the A lanes and the A-prime lanes to be green and all other lights to be red. Each phase may define a set of one or more protected paths through an intersection. A “protected path” is one in which traffic has right of way superior to that of traffic following intersecting paths. For example, an intersection between two bi-directional roads may have four phases, such as those illustrated in FIGS. 1A-D . In the first and third phases ( FIGS. 1A and 1C ), left turns are protected paths and through traffic is not allowed. In the second and fourth phases ( FIGS. 1B and 1D ), through traffic lanes are protected paths and left turns are not protected paths (and may not be allowed). A “cycle” is a progression through the phases of the one or more traffic indicators. In some cases of “running through a cycle,” a phase may be skipped. For example, in the intersection illustrated in FIG. 1 , a detector may be situated to detect whether traffic is waiting to turn left. If there is no such traffic one or more of the left-turn phases may be skipped.
SUMMARY
In general, in one aspect, the invention features an article of manufacture for use in an intersection between two roads. The intersection has one or more traffic indicators to control the flow of traffic through the intersection. The one or more traffic indicators collectively have one or more traffic indicator phases. Each traffic indicator phase specifies the traffic allowed to flow through the intersection during that traffic indicator phase. The intersection includes one or more A lanes for traffic proceeding in direction A, one or more A-prime lanes for traffic proceeding in direction A-prime, substantially opposite direction A, one or more B lanes for traffic proceeding in direction B intersecting the A lanes and the A-prime lanes, and one or more B-prime lanes for traffic proceeding in direction B-prime, substantially opposite direction B. The intersection also includes a protected turn-around lane situated between the B lanes and the B-prime lanes. The protected turn-around lane is reached by turning from the A lanes to the B lanes. The protected turn-around lane allows traffic proceeding in direction B to turn around and proceed in direction B-prime. The protected turn-around lane provides for a protected turn from the A lanes to the B-prime lanes without having a traffic indicator phase dedicated to protecting such a turn.
Implementations of the invention may include one or more of the following. The protected turn-around lane may have a generally elliptical shape. The generally elliptical shape may have one or more radii of curvature. The radii of curvature may be sufficient to allow a vehicle of a predetermined size to turn through the protected turn-around lane. The intersection may include a do-not-block area in the B-prime lanes adjacent the protected turn-around lane, where through traffic is not to stop. The intersection may include a merge lane allowing traffic to merge from one of the B-prime lanes into the protected turn-around lane. The intersection may include using a second protected turn-around lane opposite the protected turn-around lane as an extended merge lane for merging into the B-prime lanes.
In general, in another aspect, the invention features an article of manufacture for use in an intersection between two roads. The intersection includes one or more A lanes for traffic proceeding in direction A, one or more A-prime lanes for traffic proceeding in direction A-prime, substantially opposite direction A, one or more B lanes for traffic proceeding in direction B intersecting the A lanes and the A-prime lanes, and one or more B-prime lanes for traffic proceeding in direction B-prime, substantially opposite direction B. The intersection includes an overpass to allow the B lanes and the B-prime lanes to pass over the A lanes and the A-prime lanes. The intersection includes an A exit lane from the A lanes, allowing traffic exiting the A lanes to travel in direction B. The intersection includes a path through the overpass allowing traffic moving in direction B to turn around and travel in direction B-prime. The path is a protected path. The A exit lane connects to an entrance side of the path. A B-prime entrance lane connects to an exit side of the path. The B-prime entrance lane allows traffic to enter the B-prime lanes.
Implementations of the invention may include one or more of the following. The intersection may include B access lanes parallel and adjacent to the B lanes. The A exit lane connection to the entrance side of the path may be under the B access lanes. A B entrance lane may be connected to the A exit lane. The B entrance lane may allow traffic to enter the B lanes. The path may be a tunnel. The intersection may include a B exit lane from the B lanes. The B exit lane may connect to an entrance side of the path. An A entrance lane connecting to an exit side of the path. The A entrance lane may allow traffic to enter the A lanes. The intersection may include an A-prime exit lane from the A-prime lanes, allowing traffic exiting the A-prime lanes to travel in direction B-prime. The intersection may include a second path through the overpass allowing traffic moving in direction B-prime to turn around and travel in direction B, the path being a protected path. The A-prime exit lane may connect to an entrance side of the second path. The intersection may include a B entrance lane connecting to an exit side of the second path. The B entrance lane may allow traffic to enter the B lanes. The intersection may include a B-prime exit lane from the B-prime lanes. The B-prime exit lane may connect to an entrance side of the second path. The intersection may include an A-prime entrance lane connecting to an exit side of the second path. The A-prime entrance lane may allow traffic to enter the A-prime lanes. The intersection may include B-prime access lanes parallel and adjacent to the B-prime lanes. The A-prime exit lane connection to the entrance side of the second path may be under the B-prime access lanes. The intersection may include a B-prime entrance lane connected to the A-prime exit lane. The B-prime entrance lane allows traffic to enter the B-prime lanes.
In general, in another aspect, the invention features an article of manufacture for use in an intersection between two roads. The intersection includes one or more A lanes for traffic proceeding in direction A, one or more A-prime lanes for traffic proceeding in direction A-prime, substantially opposite direction A, one or more B lanes for traffic proceeding in direction B intersecting the A lanes and the A-prime lanes, and one or more B-prime lanes for traffic proceeding in direction B-prime, substantially opposite direction B. The intersection also includes an overpass to allow the B lanes and the B-prime lanes to pass over the A lanes and the A-prime lanes. The intersection includes a protected turn-around lane situated between the B lanes and the B-prime lanes. The protected turn-around lane is reached by turning from the A lanes to the B lanes crossing under one or more B lanes through the underpass. The protected turn-around lane allows traffic proceeding in direction B to turn around and proceed in direction B-prime.
Implementations of the invention include one or more of the following. The intersection may include an A exit lane from the A lanes, allowing traffic exiting the A lanes to travel in direction B. The intersection may include a protected turn-around lane situated between the A lanes and the A-prime lanes. The protected turn-around lane may be reached by turning from the B-prime lanes to the A lanes crossing over one or more A lanes as part of the overpass. The protected turn-around lane allows traffic proceeding in direction A to turn around and proceed in direction A-prime. The intersection may include a B-prime exit lane from the B-prime lanes, allowing traffic exiting the B-prime lanes to travel in direction A.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top view of a prior art intersection.
FIGS. 1A-1D illustrate phases associated with the prior art intersection shown in FIG. 1 .
FIG. 2 is a top view of one embodiment of an intersection.
FIG. 3 is a top view of one embodiment of an intersection.
FIG. 4 is a top view of one embodiment of an intersection.
FIGS. 4A-4B illustrate the phases associated with the intersection embodiment shown in FIG. 4 .
FIGS. 4C-4D illustrate variations of the intersection embodiment shown in FIG. 4 .
FIG. 5 is a top view of one embodiment of an intersection.
FIGS. 5A-5C illustrate the phases associated with the intersection embodiment shown in FIG. 5 .
FIG. 6 is a top view of one embodiment of an intersection.
FIGS. 6A-6C illustrate the phases associated with the intersection embodiment shown in FIG. 6 .
FIG. 7 is a top view of one embodiment of an intersection.
FIGS. 7A-7D illustrate the phases associated with the intersection embodiment shown in FIG. 7 .
FIG. 8 is a top view of one embodiment of an intersection.
FIGS. 8A-8D illustrate the phases associated with the intersection embodiment shown in FIG. 8 .
FIG. 9 is a top view of a prior art intersection.
FIGS. 9A-9C illustrate the phases associated with the prior art intersection shown in FIG. 9 .
FIG. 10 is a top view of one embodiment of an intersection.
FIGS. 10A-10B illustrate the phases associated with the intersection embodiment shown in FIG. 5 .
FIGS. 10C-10D illustrate variations on the intersection embodiment shown in FIG. 10 .
FIG. 11 is a top view of one embodiment of an intersection.
FIGS. 11A-11B illustrate the phases associated with the intersection embodiment shown in FIG. 5 .
FIG. 12 is a top view of one embodiment of an intersection.
FIG. 13 is a side view of the intersection embodiment shown in FIG. 12 .
FIG. 14 is a top view of one embodiment of an intersection.
FIG. 14 a is a top view of one embodiment of an intersection.
FIG. 15 is a perspective view of the intersection embodiment shown in FIG. 14 .
FIG. 16 is a side view of the intersection embodiment shown in FIG. 14 .
FIG. 16 a is a side view of a modified version of the intersection embodiment shown in FIG. 14 .
FIG. 17 is a top view of one embodiment of an intersection.
FIG. 17A illustrates the phase associated with the intersection embodiment shown in FIG. 17 .
FIGS. 18 and 19 are side views of the intersection embodiment shown in FIG. 17 .
FIG. 20 is a perspective view of the intersection embodiment shown in FIG. 17 .
DETAILED DESCRIPTION
An improved intersection reduces the number of traffic indicator phases and in some cases eliminates traffic indicator phases entirely. This has two positive effects. First, reducing the number of phases may improve the amount of time required for a vehicle to clear an intersection. This is because a vehicle may be required to wait through the intersection's other phases before crossing the intersection in the phase in which traffic is allowed flowing in the direction the vehicle desires to travel. Second, because reducing the number of phases reduces the number of phase transitions in each cycle, the number of red light accidents will be reduced.
One embodiment of an improved intersection, illustrated in FIG. 2 , includes protected turn-around lanes 205 , 210 , 215 , 220 . The “protected turn-around lanes” can be as shown in FIG. 2 . That is, it can be defined by a concrete structure, e.g. 225 , between the lanes traveling in one direction (e.g., the A direction) and the lanes traveling in substantially opposite direction (e.g., the A-prime direction). Alternatively, the “protected turn-around lane” can be defined with paint. For example, the concrete structure 225 in FIG. 2 could be replaced by painted stripes or any other device to guide traffic. FIG. 2 shows protected turn-around lanes 205 , 210 , 215 , 220 in each arm of the intersection. It will be understood by the person or ordinary skill that an improved intersection could also be made with fewer than all of the concrete structures and protected turn-around lanes.
The intersection illustrated in FIG. 2 provides a protected left turn from any direction without dedicating a traffic indicator phase to that left turn. A “protected turn” is a protected path that involves a turn. So, in the example shown in FIG. 2 , a vehicle traveling in direction A arriving at the intersection and wishing to turn left into direction B-prime can turn right onto the B lanes (a) when the indicator for lanes proceeding in direction A is red, in which case the turn is not a protected path and a merge is required, or (b) when the indicator for lanes proceeding in direction A is green, in which case the turn is a protected path and no merge is required. Thus, the turn can be made without being forced to merge.
In either case, once the vehicle turns from the A lanes to the B lanes it can move into the protected turn-around lane 220 , which allows the vehicle to turn around from the B direction to the B-prime direction. Once this maneuver is complete, the vehicle has made the desired left turn from the A direction to the B-prime direction. Upon completing the turn, the vehicle must wait at the intersection until the traffic indicators provide that passing through the intersection in the B-prime direction is permissible. Left turns from the other lanes (i.e., from the A-prime lanes to the B lanes, from the B lanes to the A lanes, and from the B-prime lanes to the A-prime lanes) is accomplished in a similar fashion.
The intersection shown in FIG. 2 requires more area than the intersection shown in FIG. 1 . In particular, the road is approximately 10 lanes wide in the vicinity of the concrete structures 225 , 230 , 235 , and 240 in FIG. 2 compared to approximately 5 lanes wide without the concrete structures in FIG. 1 . The improvement in safety and efficiency compensates for the additional land requirements.
A merge lane 305 , 310 , 315 , 320 , as shown in FIG. 3 , may be added to allow large vehicles, such as fire trucks or busses that might require a greater turning radius than that allowed by the protected turn-around lanes 205 , 210 , 215 , 220 shown in FIG. 2 . For example a large vehicle wishing to make a left turn from the A lanes to the B-prime lanes might enter the merge lane 305 and enter the protected turn-around lane 205 and then make a traditional unprotected left turn (assuming the intersection does not include a left turn arrow making the turn a protected one). Alternatively, the protected turn-around lanes 205 , 210 , 215 , 220 may be designed to have a turning radius to handle any sized vehicle.
The concrete structures 325 , 330 , 335 , 340 have a teardrop shape in FIG. 3 as compared to the round shape of the concrete structures 225 , 230 , 235 , and 240 in FIG. 2 . The concrete structures can have any suitable shape. They can be asymmetrical, as shown in FIGS. 4C and 4D .
Do-not-block areas 405 , 410 , 415 , 420 , as shown in FIG. 4 (they are also shown in FIGS. 5-8 and 10 - 11 ), which may be demarked with cross-hatched paint, such as is shown in FIG. 4 , or any other suitable means, define turning regions where vehicles traveling in the through lanes are not allowed to stop. They allow greater clearance for vehicles turning in the protected turn-around lanes.
Extended merge lanes 425 , 430 , 435 , 440 , as shown in FIG. 4 (they are also shown in FIGS. 5 and 6 ), provide a path through the turn-around lanes that doubles as an extended merge area. This allows the length of the merge lane to no longer be limited by the placement of the turn-around lane.
The intersections shown in FIGS. 2 , 3 , and 4 have two traffic phases, as shown in FIGS. 4A and 4B . In one phase ( FIG. 4A ), traffic flows in the B direction and the B-prime direction. Also, traffic that had turned from the A lanes into the protected turn-around lane 220 can complete a left turn into the B-prime lanes and traffic that had turned from the A-prime lanes into the protected turn-around lane 210 can complete a left turn into the B lanes. In the other phase ( FIG. 4B ), traffic flows in the A direction and the A-prime direction. Also, traffic that had turned from the B lanes into the protected turn-around lane 205 can complete a left turn into the A lanes and traffic that had turned from the B-prime lanes into the protected turn-around lane 215 can complete a left turn into the A-prime lanes.
Thus, the intersection shown in FIGS. 2 , 3 , and 4 provides the same left-turn functionality as the intersection shown in FIG. 1 , with fewer traffic phases. This improves the efficiency of the intersection.
Other configurations of intersections are also possible. For example, as shown in FIG. 5 , it may be that not all arms of the intersection are provided with protected turn-around lanes. In FIG. 5 , protected turn-around lanes are provided for traffic turning from the A lanes to the B-prime lanes, from the B lanes to the A lanes, and from the A-prime lanes to the B lanes, but not from the B-prime lanes to the A-prime lanes.
The intersection shown in FIG. 5 has three phases. In the first, shown in FIG. 5A , traffic proceeds in the B-prime direction and turns left from the B-prime lanes to the A-prime lanes. In the second phase, illustrated in FIG. 5B , traffic proceeds in the B direction and in the B-prime direction. The second phase also allows protected left turns from the A-prime lanes to the B lanes using the protected turn-around lane 520 in the north arm of the intersection and protected left turns from the A lanes to the B-prime lanes using the protected turn-around lane 515 in the south arm of the intersection. In the third phase, illustrated in FIG. 5C , traffic proceeds in the A direction and in the A-prime direction. The third phase also allows protected left turns from the B lanes to the A-prime lanes using the protected turn-around lane 510 in the west arm of the. The first phase could be eliminated by providing a protected turn-around lane from the B-prime lanes to the A-prime lanes. It may be necessary to have an intersection configured as shown in FIG. 5 if, for example, it is not possible to acquire land to accommodate the wider footprint needed by the protected turn-around lane.
FIG. 5 also illustrates another configuration of the concrete structure 505 . Concrete structure 505 has more of the shape of a traditional median strip and extends from the turn-around lane to the A lanes.
FIG. 6 illustrates another possible intersection configuration, in which two opposite arms of the intersection have protected turn-around lanes but the other two do not. In the example shown in FIG. 6 , protected turn-around lanes are provided for turns from the A-prime lanes to the B lanes and from the A lanes to the B-prime lanes but not from the B-prime lanes to the A-prime lanes or from the B lanes to the A lanes.
The intersection shown in FIG. 6 has three phases. The first, shown in FIG. 6A , allows turns from the B-prime lanes to the A-prime lanes and from the B lanes to the A lanes. The second phase, shown in FIG. 6B , allows traffic to proceed in the B lanes and the B-prime lanes. The second phase also allows protected left turns from the A lanes to the B-prime lanes using the protected turn-around lane 605 in the south arm of the intersection and protected left turns from the A-prime lanes to the B lanes using protected turn-around lane 610 in the north arm of the intersection. The third phase, shown in FIG. 6C , allows traffic to proceed in the A lanes and the A-prime lanes.
FIG. 7 illustrates another possible intersection configuration, in which two adjacent arms of the intersection have protected turn-around lanes but the other two do not. In the example shown in FIG. 7 , protected turn-around lanes are provided for turns from the A lanes to the B-prime lanes and from the B-prime lanes to the A-prime lanes but not from the A-prime lanes to the B lanes or from the B lanes to the A lanes.
The intersection shown in FIG. 7 has four phases. The first, shown in FIG. 7A , allows traffic to proceed in the B direction and for turns from the B lanes to the A lanes. The second phase, shown in FIG. 7B allows traffic to proceed in the B direction and in the B-prime direction. The second phase also allows protected left turns from the A lanes to the B-prime lanes using the protected turn-around lane 710 in the south arm of the intersection. The third phase, shown in FIG. 7C , allows traffic to proceed in the A-prime direction and to turn from the A-prime lanes to the B lanes. The fourth phase, shown in FIG. 7D , allows traffic to proceed in the A direction and the A-prime direction. The third and fourth phases also allow protected left turns from the B-prime lanes to the A-prime lanes using the protected turn-around lane 705 in the east arm of the intersection.
FIG. 8 illustrates another possible intersection configuration, in which one arm of the intersection has a protected turn-around lane but the other three do not. In the example shown in FIG. 8 , protected turn-around lanes are provided for turns from the A lanes to the B-prime lanes but not from the B-prime lanes to the A-prime lanes, from the A-prime lanes to the B lanes, or from the B lanes to the A lanes.
The intersection shown in FIG. 8 has four phases. The first, shown in FIG. 8A , allows turns from the B lanes to the A lanes and from the B-prime lanes to the A-prime lanes. The second phase, shown in FIG. 8B allows traffic to proceed in the B direction and in the B-prime direction. The second phase also allows protected left turns from the A lanes to the B-prime lanes using the protected turn-around lane. The third phase, shown in FIG. 8C , allows traffic to proceed in the A-prime direction and to turn from the A-prime lanes to the B lanes. The fourth phase, shown in FIG. 8D , allows traffic to proceed in the A direction and the A-prime direction.
FIG. 9 illustrates a prior art “T” intersection, in which the east-west road dead ends into the intersection but the north-south road extends beyond the intersection. The intersection in FIG. 9 has three phases. In the first phase, shown in FIG. 9A , traffic is allowed to turn from the A lanes to the B lanes and the B-prime lanes. In the second phase, shown in FIG. 9B , traffic is allowed to proceed in the B-prime direction and to turn from the B-prime lanes to the A-prime lanes. In the third phase, shown in FIG. 9C , traffic is allowed to proceed in the B direction and the B-prime direction and turns are allowed from the B lanes to the A-prime lanes.
A “T” intersection incorporating a protected turn-around lane is illustrated in FIG. 10 . In FIG. 10 , a protected turn-around lane is provided for turns from the A lanes to the B-prime lanes. The resulting intersection has two phases. The first phase, illustrated in FIG. 10A , allows traffic to proceed in the B direction and the B-prime direction and a right turn from the B lanes to the A-prime lanes. The first phase also allows a yielded right turn from the A lanes to the B lanes. The second phase, illustrated in FIG. 10B , allows traffic to proceed in the B-prime direction and for turns from the B-prime lanes to the A-prime lanes and from the A lanes to the B lanes. The second phase also allows a yielded right turn from the B lanes to the A-prime lanes.
In FIG. 10 , the concrete structure 1005 that forms the protected turn-around lane bulges to the west. FIGS. 10C and 10D illustrate two different configurations of the concrete structure. In FIG. 10 C, the concrete structure 1010 bulges to the west. In FIG. 10D , the concrete structure 1015 deviates to the east and then bulges to the east. The latter configuration accommodates situations in which it is not possible or desirable to have the B lanes deviate to the west around the protected turn-around lane.
A “Y” intersection can also benefit from protected turn-around lanes, as shown in FIG. 11 . In FIG. 11 , a protected turn-around lane is provided for turns from the A direction to the C direction. The “Y” intersection in FIG. 11 has two phases. The first phase, shown in FIG. 1A , allows traffic to turn from the B-prime lanes to the C lanes, from the C-prime lanes to the A-prime lanes and from the C-prime lanes to the B lanes. The first phase also allows a yielded right turn from the A lanes to the B lanes. The second phase, shown in FIG. 1B , allows traffic to turn from the B-prime lanes to the C lanes, from the B-prime lanes to the A-prime lanes and from the A lanes to the B lanes. The second phase also allows a yielded right turn from the C-prime lanes to the A-prime lanes.
Another type of intersection, illustrated in FIG. 12 , provides unrestricted traffic flow in all directions and protects all left turns. The intersection employs an overpass. An overpass is as understood in the art. It is limited to the portion of a first road passing over a second road that is in close proximity to the place where the crossing occurs. It does not include an extended elevated road. So, for example, an extended portion of road that is elevated over more than one road is not a single overpass but multiple overpasses. An overpass includes only that portion of the road that passes over the road below, the structure necessary to support it, and the adjacent structure. A cloverleaf intersection is not an overpass, for example, because, while it incorporates one road passing over another road, it also includes elements that are apart from the portion of one road that passes over another.
The intersection in FIG. 12 , illustrated in plan view in FIG. 13 , includes paths 1305 , 1310 , and 1315 (and another path that cannot be seen in the view shown in FIG. 13 ) that go through the structure of the intersection. A down ramp 1325 provides access from the lanes moving from the left to the right on the overpass of FIG. 13 to path 1315 . An up ramp 1330 provides access from the path 1305 to the lanes moving from the left to the right on the overpass of FIG. 13 . Similar ramps, which cannot be seen in the view of FIG. 13 , provide access to and from the lanes moving from the right to the left on the overpass of FIG. 13 . For sake of illustration, the ramps are shown with exaggerated steepness. The actual ramps would have more gradual slopes. As will be seen more clearly in FIG. 12 , paths 1305 , 1310 , and 1315 provide access between the lanes moving in and out of the page and those moving left and right in the page.
Reference is now made to FIG. 12 , which is a top view of the intersection illustrated in FIG. 13 ( FIG. 13 shows view 13 of the intersection illustrated in FIG. 12 ). The A lanes have an unobstructed path 1320 under the B lanes and the B-prime lanes. In addition, protected left and right turns can be made from the A lanes to the B lanes and the B-prime lanes, respectively. Exit lane 1205 from the A lanes connects to entrance lane 1210 to the B lanes, providing a path to turn right from the A lanes to the B lanes. Exit lane 1205 also connects to the path 1305 . Path 1305 connects to the on ramp 1330 , which provides a path to the B-prime lanes. The exit lane 1205 , path 1305 , and on ramp 1330 provide a protected left turn from the A lanes to the B-prime lanes.
A similar arrangement is provided for the A-prime lanes. The A-prime lanes have an unobstructed path 1320 under the B lanes and the B-prime lanes. Exit lane 1215 from the A-prime lanes connects to entrance lane 1220 to the B-prime lanes, providing a path to turn right from the A-prime lanes to the B-prime lanes. Exit lane 1215 also connects to the path 1315 . Path 1315 connects to the on ramp 1225 , which provides a path to the B lanes. The exit lane 1215 , path 1315 , and on ramp 1225 provide a protected left turn from the A-prime lanes to the B lanes.
A different arrangement is provided for the B lanes. Exit lane 1230 from the B lanes, which is at the same level as the A lanes and the A-prime lanes, connects to entrance lane 1235 to the A-prime lanes, providing a path to turn right from the B lanes to the A-prime lanes. A branch of exit lane 1230 also ascends up ramp 1225 , crosses the A-prime lanes and the A lanes, descends down ramp 1240 , and connects to path 1310 . Path 1310 connects to the on ramp 1245 , which provides a path to the A lanes. The exit lane 1230 , path 1310 , and on ramp 1245 provide a protected left turn from the B lanes to the A lanes.
The arrangement for the B-prime lanes is similar to that for the B lanes. Exit lane 1250 from the B-prime lanes, which is at the same level as the A lanes and the A-prime lanes, connects to entrance lane 1245 to the A lanes, providing a path to turn right from the B-prime lanes to the A lanes. A branch of exit lane 1250 also ascends up ramp 1330 , crosses the A-prime lanes and the A lanes, descends down ramp 1325 , and connects to path 1315 . Path 1315 connects to the on ramp 1235 , which provides a path to the A-prime lanes. The exit lane 1250 , path 1315 , and on ramp 1235 provide a protected left turn from the B-prime lanes to the A-prime lanes.
Another embodiment of the intersection, illustrated in FIGS. 14 , 15 , and 16 , provides for “access lanes” adjacent to the B and B-prime lanes shown in previous embodiments. Access lanes 1405 are adjacent to and run in the same direction as the B lanes. Access lanes 1410 are adjacent to and run in the same direction as the B-prime lanes. While FIG. 14 shows 3 access lanes in the B direction and 3 access lanes in the B-prime direction, a person of ordinary skill would understand that the number of access lanes is not limiting. Medians 1415 , 1420 , 1425 , and 1430 separate the B lanes from access lanes 1405 and the B-prime lanes from access lanes 1430 . As with the previous embodiment, the B lanes and the B-prime lanes cross the A lanes and the A-prime lanes on an overpass.
The same features are illustrated in FIG. 15 , which provides a perspective view of the intersection shown in FIG. 14 . Access lanes 1405 ascend an up ramp 1505 , cross the A lanes and A-prime lanes, and descend a down ramp 1510 . A transition lane 1515 , adjacent to the B lanes and access lanes 1405 , and accessible to both, descends a down ramp (as shown in FIG. 15 ), and travels through path 1435 (see FIG. 14 ) to exit 1520 (see FIGS. 14 , 15 , 16 , and 16 a , which shows a plan view of the intersection of FIG. 14 ).
The access lanes 1410 traveling in the B-prime direction ascend an up ramp 1525 , cross the A lanes and A-prime lanes, and descend a down ramp 1530 . The overpass distance to the down ramp 1530 is shorter in FIG. 16 a . A transition lane 1535 , adjacent to the B-prime lanes and access lanes 1410 , and accessible to both, descends a down ramp (as shown in FIG. 15 ), and travels through path 1440 (see FIG. 14 ) to exit 1445 (see FIG. 14 ).
The intersection shown in FIGS. 14 , 15 , and 16 allows protected right and left turns from the A, A-prime, B, and B-prime lanes. An exit lane from the A lanes 1450 connects to an entrance lane 1455 to the access lanes 1405 , which allow access to the B lanes, providing a right turn from the A lanes to the B lanes. A branch of exit lane 1450 also connects to path 1460 , which travels through the overpass exiting at 1462 , and ascends up ramp 1525 to allow a vehicle to merge into the B-prime lanes. Exit lanes 1450 , path 1460 , and ramp 1525 allow a protected left turn from the A lanes to the B-prime lanes.
An exit lane from the A-prime lanes 1465 connects to an entrance lane 1470 to the access lanes 1410 , which allow access to the B-prime lanes, providing a right turn from the A-prime lanes to the B-prime lanes. A branch of exit lane 1465 also connects to path 1475 , which travels through the overpass exiting at 1480 , and ascends up ramp 1505 to allow a vehicle to merge into the B lanes. Exit lanes 1465 , path 1475 , and ramp 1505 allow a protected left turn from the A-prime lanes to the B lanes.
Turning right from the B lanes to the A-prime lanes requires exiting the B lanes to the access lanes 1405 at a point off the top of FIG. 14 and exiting the access lanes 1405 using exit lane 1485 to enter the A-prime lanes using entrance lane 1490 . Turning left from the B lanes to the A lanes requires following the transitional lane 1515 through path 1435 to exit 1520 and onto the A lanes. This sequence of turns is shown graphically in FIG. 15 . FIG. 14 a illustrates a way to avoid use of the transitional lane 1515 by shortening the median strip between the access lanes 1405 and the right-most lane 1498 of the B lanes. That change allows traffic to merge from the access lanes 1405 to the B lanes in anticipation of making a left turn from the B lanes to the A lanes. FIG. 14 a also shows symbolically the paths that would be followed in making turns from one set of lanes to another. The symbols indicate which turn they illustrate. A key for the symbols is:
Symbol
Meaning
LN
Left turn from north-bound lanes (B-prime lanes)
RN
Right turn from north-bound lanes (B-prime lanes)
LS
Left turn from south-bound lanes (B lanes)
RS
Right turn from south-bound lanes (B lanes)
LE
Left turn from east-bound lanes (A lanes)
RE
Right turn from east-bound lanes (A lanes)
LW
Left turn from west-bound lanes (A-prime lanes)
RW
Right turn from west-bound lanes (A-prime lanes)
Turning right from the B-prime lanes to the A lanes requires exiting the B-prime lanes to the access lanes 1410 at a point off the bottom of FIG. 14 and exiting the access lanes 1410 using exit lane 1495 to enter the A lanes using entrance lane 1497 . Turning left from the B-prime lanes to the A-prime lanes requires following the transitional lane 1535 through path 1440 to exit 1445 and onto the A-prime lanes.
Another embodiment of the intersection with an overpass, illustrated in FIGS. 17 , 18 , 19 , and 20 , allows protected left and right turns from the A, A-prime, B, and B-prime lanes. Each arm of the intersection includes a protected turnaround lane structure 1705 , 1710 (the structures in the east and west arms of the intersection are not shown because of space limitations).
A right turn from the A lanes to the B lanes is accomplished by using the exit lane 1715 from the A lanes to reach the entrance lane 1720 to the B lanes. A left turn from the A lanes to the B-prime lanes is accomplished by using the exit lane 1725 to proceed through the overpass following the path shown in FIG. 17 , around the protected turnaround lane structure 1710 and onto the B-prime lanes.
A right turn from the A-prime lanes to the B-prime lanes is accomplished by using the exit lane 1730 from the A-prime lanes to reach the entrance lane 1735 to the B-prime lanes. A left turn from the A-prime lanes to the B lanes is accomplished by using the exit lane 1740 to proceed through the overpass following the path shown in FIG. 17 , around the protected turnaround lane structure 1705 and onto the B lanes.
A right turn from the B lanes to the A-prime lanes is accomplished by using the exit lane 1745 from the B lanes to reach the entrance lane 1750 to the A-prime lanes. A left turn from the B lanes to the A lanes is accomplished by using the exit lane 1755 to proceed over the A-prime lanes following the path shown in FIG. 17 , around a protected turnaround lane structure (not shown) and onto the A lanes.
A right turn from the B-prime lanes to the A lanes is accomplished by using the exit lane 1760 from the B-prime lanes to reach the entrance lane 1765 to the A-prime lanes. A left turn from the B-prime lanes to the A-prime lanes is accomplished by using the exit lane 1770 to proceed over the A lanes following the path shown in FIG. 17 , around a protected turnaround lane structure (not shown) and onto the A-prime lanes.
The intersection illustrated in FIG. 17 produces a single-phase intersection, as illustrated in FIG. 17A . That is, traffic in all directions is protected. In such an intersection, no traffic light is required.
While the traffic intersection has been described in connection with the preferred embodiments of the various figures, it is to be understood that other similar embodiments may be used or modifications and additions can be made to the described embodiment for performing the same function of the traffic intersection without deviating therefrom.
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A method for constructing a traffic intersection is disclosed. One version of the intersection includes a protected turn-around lane that allows traffic to turn around and proceed in the opposite direction. The protected turn-around lane provides for a protected turn without having a traffic indicator phase dedicated to protecting such a turn. Another version of the intersection includes an overpass and a protected path through the overpass allowing traffic to turn around and travel in substantially the opposite direction. Another version of the intersection includes an overpass and a protected turn-around lane.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to carburetors and, more particularly, to a throttle valve linkage for use with a multi-carburetor assembly comprising a plurality of carburetors disposed between engine cylinders arranged in a pair or pairs, as in the case of V-type engine for two-wheeled vehicles, each carburetor being provided for one of the cylinders.
2. Description of the Prior Arts
The type of engines has been known in the field of two-wheeled vehicles which has a plurality of cylinders arranged in a row extending transversely of the longitudinal axis of the vehicle. In this type of engines, carburetors are arranged also in a row transverse to the longitudinal axis of the vehicle so that the throttle shafts of these carburetors are disposed on a common axis. In this case, therefore, there is no substantial difficulty in designing and constructing a throttle valve linkage for operating the throttle valves of all carburetors similarly and in synchronization.
This type of engine, however, inevitably has a large length in the direction transverse to the longitudinal axis, i.e., the running direction, of the vehicle and makes the operation of the two-wheeled vehicle difficult.
Under this circumstance, in recent years, two-wheeled vehicles have been put into use which are designed to have V-type engines in each of which a plurality of cylinders are arranged in V-shape as viewed from lateral side of the vehicle. In this type of engine, a multi-carburetor assembly comprising a plurality of carburetors provided each for one cylinder, are disposed in a limited space between the cylinders arranged in a pair or pairs. The multi-carburetor assembly is arranged such that the direction of suction of air by a first carburetor associated with a first cylinder is opposite to that of a second carburetor associated with a second cylinder and the throttle valves of these carburetors are not arranged on a common axis but are mounted on separate throttle shafts having parallel axes spaced from each other. The two throttle shafts are connected to each other by means of a wire which is wound at both ends thereof in opposite directions around two throttle shafts. One of the throttle shafts is operatively connected to an accelerator adapted to be operated by the driver. As the driver operates the accelerator for accelerating the vehicle, the throttle shaft operatively connected to the accelerator and, hence, the throttle valve carried by this throttle shaft are rotated in one direction. Simultaneously, the rotation of this throttle shaft is transmitted to the other throttle shaft through the wire to rotate the other throttle shaft and the throttle valve in the direction opposite to the direction of rotation of the first-mentioned throttle shaft and throttle valve. The first-mentioned throttle shaft and throttle valve directly operated by the accelerator will be referred to as "driving throttle shaft and throttle valve," while the throttle shaft and throttle lever driven through the wire will be referred to as "driven throttle shaft and throttle valve," hereinafter.
The conventional wire-type throttle linkage between the driving and driven throttle shafts involves the following problems. Namely, this conventional linkage cannot provide good synchronism and similarity of operation of two throttle valves. More specifically, the operation of the driven throttle valve tends to be lagged behind the operation of the driving throttle valve particularly in a part throttle engine operation range. In addition, the wire is undesirably elongated in a relatively short period of time due to the tension applied thereto and deteriorates the synchronism and similarity of operations of the two throttle valves.
The prior art throttle valve linkage which utilizes a wire is not satisfactory because of the problems discussed above, although the prior art linkage can be installed in a limited space.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide an improved throttle valve linkage for use with a multi-carburetor assembly including at least one pair of carburetors disposed between engine cylinders arranged in pair, each carburetor being associated with one of said cylinders, said carburetors being arranged such that the direction of the intake air through one of said carburetors is opposite to the direction of the intake air through the other carburetor, the carburetors having throttle shafts extending substantially in parallel relationship to each other and being adapted to be rotated in the opposite directions by operation of an accelerator to thereby open and close the throttle valves of the carburetors.
It is another object of the present invention to provide an improved throttle valve linkage of the class specified above and which does not utilize wire, can be installed within a limited space and is operative to transmit the rotation of the throttle shaft of one of the carburetors to the throttle shaft of the other carburetor so that the direction of rotation of the other carburetor throttle shaft is inverted.
The throttle valve linkage according to the present invention comprises:
first and second levers adapted to be rotated with said throttle shafts of said first and second carburetors, respectively;
first and second link members pivotally connected at their one ends to the free ends of said first and second levers, respectively;
a common pivot pin pivotally connecting the other ends of said first and second link members;
means defining a substantially elongated guide channel for slidably guiding said common pivot pin;
one of said throttle shafts being operatively connected to said accelerator;
the arrangement being such that the rotation of said one throttle shaft is transmitted to the other throttle shaft so that the direction of the rotation of said other throttle shaft is inverted.
The throttle valve linkage according to the present invention having the construction and arrangement briefly discussed above does not utilize wire which is essentially used in the prior art throttle valve linkage. Accordingly, the problem due mainly to the elongation of the wire is eliminated in the throttle valve linkage of the invention. This greatly improves the response of operation of the driven throttle valve to that of the driving throttle valve. In addition, the throttle valve linkage according to the present invention can be mounted in an extremely narrow space.
The above and other objects, features and advantages of the invention will become more apparent from the following description of preferred embodiments in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of a two-wheeled vehicle having a V-type engine incorporating a multi-carburetor assembly equipped with a throttle linkage of the invention;
FIG. 2 is an enlarged perspective view of the engine shown in FIG. 1;
FIG. 3 is a front elevational view of the multi-carburetor assembly shown in FIGS. 1 and 2;
FIG. 4 is a side elevational view of an embodiment of the throttle linkage of the invention taken along line IV--IV in FIG. 3;
FIG. 5 is a sectional view of the throttle linkage taken along line V--V in FIG. 4;
FIG. 6 is an enlarged view of a part of the throttle linkage taken along line VI--VI in FIG. 4;
FIG. 7 is a schematic illustration of the link mechanism shown in FIG. 4;
FIG. 8 is an illustration of the prior art;
FIG. 9 is a graph showing the operation characteristic of the embodiment shown in FIGS. 4 and 7 in comparison with the operation characteristic of the prior art shown in FIG. 8;
FIG. 10 is a schematic illustration of a throttle linkage constructed in accordance with a second embodiment of the invention;
FIG. 11 is a graph showing the operation characteristic of the second embodiment in comparison with that of the first embodiment;
FIG. 12 is a schematic illustration of a throttle linkage constructed in accordance with a third embodiment of the invention;
FIG. 13 is a graph showing the operation characteristic of the third embodiment in comparison with that of the first embodiment;
FIG. 14 is a side elevational view of a part of a throttle linkage constructed in accordance with a fourth embodiment, in which a broken line illustrates a modification;
FIG. 15 is a graph showing the operation characteristics of the fourth embodiment and the modification thereof;
FIG. 16 is a schematic illustration of a link mechanism constructed in accordance with a fifth embodiment of the invention; and
FIG. 17 is a graph showing the operation characteristics of the fifth embodiment in comparison with that of the first embodiment.
DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows a two-wheeled vehicle having a V-type engine unit including first and second cylinders 10, 12 arranged in V shape as viewed in the direction transverse to the longitudinal axis of the vehicle. A multi-carburetor assembly 14 is disposed in the V-shaped or triangular space defined between the two cylinders 10, 12. The multi-carburetor assembly consists of a carburetor 16 for the first cylinder 10 and a carburetor 18 for the second cylinder 12. These two carburetors 16, 18 are so arranged that they suck intake air in opposite directions. Namely, as will be most clearly seen in FIG. 2, an air horn 20 of the first carburetor 16 is disposed in the vicinity of the second cylinder 12, while an air horn 22 of the second carburetor 18 is disposed in the vicinity of the first cylinder 10, so that the intake air to be supplied to both cylinders 10, 12 flows into the air horns 20, 22 of the carburetors 16, 18 as indicated by arrows 16a, 18a, respectively.
Referring now to FIGS. 3 and 4, an intake air passage 24 of the first carburetor 16 has an upstream end 26 connected to the air horn 20 and a downstream end 28 connected to the intake port of the cylinder 10. Similarly, an intake air passage 30 of the second carburetor 18 has an upstream end 32 connected to the air horn 22 and a downstream end 34 connected to the intake port of the cylinder 12. As will be best seen in FIG. 4, the upstream end 26 of the intake air passage 24 of the first carburetor 16 and the downstream end 34 of the intake air passage 30 of the second carburetor 18 are disposed at one side (i.e., at the left side) of the multi-carburetor assembly 14, as viewed in FIG. 4, while the downstream end 28 of the intake air passage 24 of the first carburetor 16 and the upstream end 32 of intake air passage 30 of the second carburetor 18 are disposed at the other side (i.e., at the right side) of the carburetor assembly 14, as viewed in FIG. 4. These carburetors 16, 18 are connected to each other at their lower ends by means of a connector 36 (which is generally called as "bracket") to form the multi-carburetor assembly.
Butterfly-type throttle valves 38, 40 are disposed in the intake air passages 24, 30 of the first and second carburetors 16, 18, respectively. These throttle valves 38, 40 are fixed to throttle shafts 39, 40 rotatably mounted on the carburetors 16, 18 and extending therethrough transversely of respectively intake air passages 24, 30 and are rotatable together with these throttle shafts 39, 40. An arm 44 is fixed at its one end to the end of the throttle shaft 39 opposite to the carburetor 18, while the other end of the arm 44 is connected to a wire 46 of an accelerator. The idle position of the throttle valve 38 is adjustable by means of an adjust screw 48.
The throttle shafts 39, 42 are disposed on two separate axes extending substantially in parallel with each other, as shown in FIG. 4. These throttle shafts 39, 42 are drivingly connected to each other at their inner ends, i.e., at their adjacent ends, by means of a throttle valve linkage 50. The arrangement is such that, when the accelerator is operated in the accelerating direction, the throttle valve 38 of the first carburetor 16 is rotated clockwisely as viewed in FIG. 4 and this rotation is inverted and transmitted to the throttle shaft 42 of the second carburetor 18 by the throttle valve linkage 50. For this reason, the throttle valve 38 and the throttle shaft 39 associated with the first carburetor will be referred to hereunder as "driving throttle valve and throttle shaft" while the throttle valve 40 and the throttle shaft 42 associated with the second carburetor 18 will be referred to as "driven throttle valve and throttle shaft."
The throttle valve linkage 50 will be described in more detail with specific reference to FIGS. 4 to 6. The throttle valve linkage 50 includes a layer 52 fixed to the driving throttle shaft 39. The lever 52 is pivotally connected at its free end to the upper end of a first link member 54 by means of a pivot pin 56. The first link member 54 is pivotally connected at its lower end by a pin 60 to the lower end of a second link member 58 having a shape similar to that of the first link member 54. As will be seen in FIG. 5, a roller 62 made of a wear-resistant material such as a sintered metal is rotatably mounted on the pivot pin 60 between the two link members 54, 58. The afore-mentioned bracket 36 has a flattened portion 36a extending substantially in the same plane as the throttle linkage 50. An upwardly opened elongated slot or notch 64 is formed in the flattened portion 36a and receives the roller 62 as shown in FIG. 5.
The link member 58 is pivotally connected at its upper end to one end of a lever unit 66 by a pivot pin 68. The lever unit 66 includes a substantially L-shaped lever 70 pivotally connected at its central portion to the link member 58 and rotatably mounted at its one end on the driven throttle shaft 42, a lever 72 fixed at its lower end to the throttle shaft 42, and an adjust screw 74 adjustably connecting the upper end of the lever 72 and the other end of the L-shaped lever 70. More specifically, the lever 72 has a substantially U-shaped upper end constituted by two arms 72a, 72b between which is placed a bent upper end 70a of the L-shaped lever 70. The adjust screw 74 extends through a threaded hole formed in the arm 72a of the lever 72 and makes a contact at its end with the bent upper end 70a of the lever 70. A compression spring 76 is disposed between the upper end 70a of the lever 70 and the arm 72b of the lever 72 to normally bias the upper end 70a of the lever 70 into contact with the inner end of the adjust screw 74. It is possible to adjust the idle position of the driven throttle valve 40 by rotating the adjust screw 74. Once the adjustment is made, the levers 70, 72 and the adjust screw 74 rotate as a unit about the axis of the throttle shaft 42 in accordance with the movement of the second link member 58. For this reason, the lever unit 66 constituted by these three members 70, 72, 74 will be regarded and mentioned hereunder as a single lever for the purpose of simplification of description.
In the throttle valve linkage having the described construction, when the accelerator is operated to rotate the driving throttle valve 38 from the idle position in the clockwise direction as indicated by an arrow showing in FIG. 4, the lever 52 is rotated in the same direction to move the link member 54 downwards. As stated before, the roller 60 is attached to the lower end of the link member 54 through the pivot pin 60 and is received in the slot-like notch 64, so that the downward movement of the link member 54 is guided by the notch 64.
The downward movement of the roller 62 causes a downward movement of the other link member 58 so that the lever 66 is rotated counter-clockwise together with the driven throttle shaft 42 and the driven throttle valve 40.
Referring now to FIG. 7, a line P is a bisector line which is perpendicular to a line L interconnecting the axes of the two throttle shafts 39, 42 and divides the line L into two sections of equal lengths. In the embodiment described in connection with FIGS. 3 to 6, the longitudinal axis of the notch 64 for guiding the movement of the roller 62 coincides with the above-mentioned line P. In addition, the length l 1 of the lever 52 is substantially equal to the effective length l 2 of the lever 66 and the link members 54 and 58 have substantially equal lengths. Therefore, when the driving throttle valve 38 has been rotated to a certain position, the driven throttle valve 40 is rotated to a position of an opening degree substantially equal to that of the driving throttle valve 38. This operation characteristic is represented by straight lines A shown in FIGS. 11, 13 and 17.
On the other hand, in the prior art throttle valve linkage shown in FIG. 8, a wire 3 is wound at its one end around a throttle shaft 2 of a driving throttle valve 1 and at its other end around a throttle shaft 5 of a driven throttle valve 4 in the direction opposite to the direction of winding of the first-mentioned end, so that the rotation of the driving throttle valve 1 is inverted and transmitted to the driven throttle valve 4. In this prior art linkage, however, the opening degree of the driven throttle valve 4 is considerably small as compared with that of the driving throttle valve 1 especially in the part-throttle engine operating range, as represented by a curve X in FIG. 9. This is believed to be due to the fact that, in the initial stage of the throttle opening operation, the tension force applied to the wire 3 by the driving throttle shaft 2 is effective only to tighten the twist of the wire 3 and, therefore, cannot be used effectively to drive the driven throttle shaft 5.
This problem is completely eliminated in the throttle valve linkage of the invention. Namely, the throttle valve linkage of the invention permits the driving and driven throttle valves 38, 40 to be opened at a substantially equal rate, as indicated by a line A' in FIG. 9.
As has been described, the throttle valve linkage according to the invention links the driving and driven throttle shafts in such a manner that the driven throttle valve is opened substantially at the same rate as the driving throttle valve, so that an air-fuel mixture is charged into the first and second cylinders 10, 12 through respective carburetors 16, 18 at a substantially equal rate. Considered theoretically, this will ensure equal outputs from both cylinders as a result of combustion of the mixture charges into these cylinders.
Some of the multi-cylinder engines incorporating the throttle valve linkage of the above-described embodiment, however, will have a problem that there is a difference in the level of output between the first and second cylinders. Referring to the V-type engine shown in FIG. 2, as an example, the exhaust pipe connected to the first cylinder 10 is bent at a radius of curvature which is as large as possible to ensure a smooth flow of the exhaust gas, whereas the exhaust pipe connected to the rear-side cylinder, i.e., the second cylinder 12, is inevitably curved at a much smaller radius of curvature as compared with that of the exhaust pipe of the first cylinder 10 due to the limitation in the space. In consequence, the exhaust gas from the second cylinder encounters a higher resistance that the resistance to the exhaust gas from the first cylinder, with a resultant higher back pressure against the second cylinder than against the first cylinder. As a result, there occurs an desirable tendency that the second cylinder produces an output which is appreciably smaller than the output from the first cylinder.
In the engines having a difference in output between the first and second cylinders, therefore, it is desired to equalize the outputs from both cylinders by supplying the mixture at a greater rate in to the cylinder of the smaller output than into the cylinder of the larger output. To cope with this desirability, the present inventors propose the following embodiments.
Referring to FIG. 10 showing a second embodiment of the invention, the length l 1 of the lever 52 is equal to the length l 2 of the lever 66 and the link members 54, 58 are designed to have equal lengths. In this embodiment, however, the slot-like notch 64 for guiding the roller 62 is inclined. More specifically, the longitudinal axis 64B' of the slot-like notch 64B is inclined to the aforementioned line P at an angle θ which is 10° in this case. The operation characteristic of this throttle valve linkage is shown by a line B in FIG. 11. It will be seen that the driven throttle valve is opened at a greater degree than the driving throttle valve. The line A represents the operation characteristics of the first embodiment, as pointed out previously.
In a third embodiment shown in FIG. 12, the axis of the notch 64 coincides with the line P; namely, the angle θ is zero. In this case, however, the lever 52 is designed to have a length l 1 which is smaller than the length l 2 of the lever 66. The throttle valve linkage of this third embodiment exhibits an operation characteristic graphically shown by a line C in FIG. 13 which resembles the line B representing the operation characteristic of the second embodiment. It will be apparent to those skilled in the art that an operation characteristic represented by a broken line C' is obtained by modifying the third embodiment shown in FIG. 12 such that the length l 1 is greater than the length l 1 . As stated before, the line A represents the operation characteristic of the first embodiment.
In the fourth embodiment shown in FIG. 14, the notch 64D has a substantially oval shape. The left side edge portion of this notch 64D is curved to present an arcuate form to guide the roller 62. In a modification of this embodiment shown by a broken line, the notch 64d has a left side edge portion curved to present a laterally directed or turned V shape for guiding the roller 62. Curves D and d shown in FIG. 15 represent the operation characteristic of the fourth embodiment having the notch 64D and its modification having the notch 64d, respectively. The operation characteristics shown in FIG. 15 are useful in the case where the throttle valve of one of the carburetors, namely, the carburetor 18 associated with the cylinder 12, is designed to have a throttle opening characteristic which is more moderate or less sharp than that of the throttle valve of the other carburetor 16 so that the output of the cylinder 12 is prevented from being sharply varied in the part throttle engine operation range to thereby assure an improved engine drivability and emission control performance. It will be apparent to those in the art that the notches 64D and 64d shown in FIG. 14 may be further modified to have curved right side edges to provide modified operation characteristics which will be substantially opposite to those shown in FIG. 15.
In a fifth embodiment of the invention shown in FIG. 16, the length l 1 of the lever 52 is smaller than the length l 2 of the lever 66 and the notch 64E for guiding the roller 62 is inclined to the line P at an angle θ in the counterclockwise direction (i.e., θ<0). This embodiment exhibits an operation characteristic represented by a curve E shown in FIG. 17 wherein the line A represents the operation characteristic of the first embodiment of the invention, as pointed out previously.
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A throttle valve linkage for use with a multi-carburetor assembly comprising a pair of carburetors has first and second levers secured respectively to the throttle shafts of the first and second carburetors, first and second link members respectively connected at one ends to the free ends of the first and second levers. The other ends of the first and second link members are pivotally connected by a common pivot pin which is slidably movable in a guide channel. The rotation of the first carburetor throttle shaft is transmitted by the linkage to the second carburetor throttle shaft so that the latter is rotated in a direction opposite to the direction of rotation of the first carburetor throttle shaft.
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TECHNICAL FIELD OF THE INVENTION
[0001] The present invention relates to an apparatus for separating air into its components. More specifically, embodiments of the present invention are related to an apparatus for producing merchant or non-merchant grade liquid nitrogen using a pair of turbo-boosters to provide refrigeration and energy for the process.
SUMMARY OF THE INVENTION
[0002] An apparatus is provided for producing nitrogen through the cryogenic separation of air. In one embodiment, the apparatus can include a heat exchanger configured to receive a main air feed comprising filtered purified and compressed air at a pressure of at least 5 bar; an air separation unit in fluid communication with a cool side of the heat exchanger, the air separation unit configured to receive cooled air from the heat exchanger and produce gaseous nitrogen and waste gaseous oxygen, wherein the air separation unit comprises a single column having a bottom reboiler and a top condenser; a recycle compressor in fluid communication with a warm side of the heat exchanger such that the recycle compressor is configured to receive a nitrogen recycle from the heat exchanger, wherein at least a portion of the nitrogen recycle is made up of gaseous nitrogen from the air separation unit; a first turbine-booster having a first booster and a first turbine, the first booster in fluid communication with the recycle compressor such that the first booster is configured to receive a compressed nitrogen recycle from the recycle compressor; a second turbine-booster having a second booster and a second turbine, the second booster in fluid communication with the first booster such that the second booster is configured to receive a boosted nitrogen from the first booster, wherein an outlet of the second booster is in fluid communication with the heat exchanger such that the boosted nitrogen from the second booster is cooled within the heat exchanger, wherein the second turbine is in fluid communication with the heat exchanger such that the second turbine is configured to receive a cooled fluid under pressure from the heat exchanger and then expand the cooled fluid to provide refrigeration for the apparatus; and a liquid/gas separator in fluid communication with the heat exchanger, the liquid/gas separator configured to receive an expanded fluid comprising nitrogen from the second booster turbine and separate the expanded fluid into a nitrogen-enriched gas and a nitrogen-enriched liquid, the liquid/gas separator in fluid communication with the second booster and the heat exchanger such that the liquid/gas separator is configured to receive a portion of the boosted nitrogen after fully cooling in the heat exchanger, the liquid/gas separator is also configured to send the nitrogen-enriched gas to the cool side of the heat exchanger.
[0003] According to other optional aspects of the invention:
the top condenser is in fluid communication with the single column, wherein the bottom reboiler is in fluid communication with the single column, wherein the top condenser is configured to provide condensing duty for the single column, wherein the bottom reboiler configured to provide reboiling duty for the single column; the apparatus includes a subcooler in fluid communication with the single column such that the subcooler is configured to receive a fluid from the single column that is operable to provide subcooling for the subcooler; the fluid received from the single column is an oxygen-rich liquid from the bottom of the single column; the fluid received from the single column is an oxygen-rich liquid from a middle section of the single column; the subcooler is in fluid communication with the liquid/gas separator, the subcooler being configured to subcool the nitrogen-enriched liquid from the liquid/gas separator; the second turbine is mechanically coupled to the second booster; the first turbine is mechanically coupled to the first booster; and the recycle compressor is in fluid communication with the heat exchanger, the bottom reboiler and the single column, such that the recycle compressor is configured to have a fraction of partially compressed nitrogen recycle withdrawn from an internal stage of recycle compressor, cooled in the heat exchanger, used by the bottom reboiler as a boiler heating fluid; and then introduced flashed into a top portion of the single column.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] These and other features, aspects, and advantages of the present invention will become better understood with regard to the following description, claims, and accompanying drawings. It is to be noted, however, that the drawings illustrate only several embodiments of the invention and are therefore not to be considered limiting of the invention's scope as it can admit to other equally effective embodiments.
[0013] FIG. 1 provides an embodiment of the present invention.
[0014] FIG. 2 provides another embodiment of the present invention.
[0015] FIG. 3 provides an additional embodiment of the present invention.
DETAILED DESCRIPTION
[0016] While the invention will be described in connection with several embodiments, it will be understood that it is not intended to limit the invention to those embodiments. On the contrary, it is intended to cover all the alternatives, modifications and equivalence as may be included within the spirit and scope of the invention defined by the appended claims.
[0017] FIG. 1 provides a basic embodiment of the present invention. Main air feed 2 , which has already been purified and compressed to a pressure of about 5 to about 6 bar, is introduced to heat exchanger 10 and cooled down to a temperature near its dew point or lower to form fully cooled air feed 12 . Fully cooled air feed 12 is then introduced to air separation unit 19 , in order to separate the various components of air. Waste gaseous oxygen 22 is recovered from air separation unit 19 and is passed through the cold side of heat exchanger 10 in order to provide cooling to heat exchanger 10 . After exiting heat exchanger 10 , waste gaseous oxygen 22 can be vented to the atmosphere, used to regenerate the air adsorbers (not shown) or sent to a system of columns (not shown) if recovery of the oxygen is desired.
[0018] Gaseous nitrogen 28 is also withdrawn from air separation unit 19 and passed through the cold side of heat exchanger 10 to provide additional cooling. However, instead of venting to the atmosphere, gaseous nitrogen 28 is recycled in the process. Nitrogen recycle 38 exits air separation unit 19 and is introduced to recycle compressor 40 and compressed to form compressed nitrogen recycle 46 . Compressed nitrogen recycle 46 is then cooled in second aftercooler 43 before being boosted in first booster 50 and cooled in third aftercooler 51 to form boosted nitrogen 52 . Boosted nitrogen 52 is then introduced to second booster 53 in order to further compress boosted nitrogen 52 before being cooled in fourth aftercooler 55 to form fully boosted nitrogen 56 . In one embodiment fully boosted nitrogen 56 can be at ambient temperature and a pressure of about 45 to about 65 bar prior to entering heat exchanger 10 .
[0019] Fully boosted nitrogen 56 is then introduced to heat exchanger 10 for cooling. In one embodiment, one portion of fully boosted nitrogen 56 is fully cooled in heat exchanger 10 to form liquefied nitrogen 58 , which is subsequently introduced to liquid/gas separator 60 by flashing via valve 59 . In another embodiment, another portion of fully boosted nitrogen 56 is only partially cooled in heat exchanger 10 to form partially cooled boosted nitrogen 78 . In one embodiment, partially cooled boosted nitrogen 78 is at or above its super critical pressure. Partially cooled boosted nitrogen 78 is then introduced into second turbine 80 in order to expand partially cooled boosted nitrogen 78 to form second expanded nitrogen 82 . In one embodiment, second expanded nitrogen 82 can have a temperature that is near or below its dew point and a pressure of about 5 to about 6 bar. In one embodiment, second expanded nitrogen 82 is a two phase fluid consisting of gas and liquid phases. In a preferred embodiment, second expanded nitrogen 82 is introduced to liquid/gas separator 60 in order to separate any gaseous nitrogen from liquid nitrogen. Recovered liquid nitrogen 62 is withdrawn from liquid/gas separator 60 and collected as product. In one embodiment, gaseous nitrogen 68 is withdrawn from a top portion of liquid/gas separator 60 and combined with gaseous nitrogen 28 before introduction to the cold side of heat exchanger 10 and subsequently recycled.
[0020] In one embodiment, fraction of compressed nitrogen recycle 48 is withdrawn from compressed nitrogen recycle 46 and fed to the warm end of heat exchanger 10 , where fraction of compressed nitrogen recycle 48 is partially cooled before being expanded in first turbine 70 to form first expanded nitrogen 72 . In one embodiment, first expanded nitrogen 72 is reintroduced to heat exchanger 10 , preferably at an intermediate point, and combined with gaseous nitrogen 28 and subsequently recycled. In one embodiment, first turbine 70 is connected by a common shaft with first booster 50 and helps to provide the energy needed for first booster 50 to compress compressed nitrogen recycle 46 . Likewise, second turbine 80 is connected by a common shaft with second booster 53 and helps to provide the energy needed for second booster 53 to compress boosted nitrogen 52 . In one embodiment, first turbine 70 and second turbine 80 provide substantially all of the refrigeration needs for the process.
[0021] First turbine 70 and second turbine 80 produce refrigeration by work expansion. Their respective boosters, first booster 50 and second booster 53 , utilize the produced work to further compress their respective nitrogen streams.
[0022] FIG. 2 provides an alternate embodiment of the invention, which includes two recycle compressors (recycle compressor 40 and second recycle compressor 45 ), recycle aftercooler 41 , single column 20 and subcooler 30 . In one embodiment, single column 20 operates at about 5 bar. In one embodiment, nitrogen recycle 38 is partially compressed in recycle compressor 40 and cooled in recycle aftercooler 41 to form partially compressed nitrogen recycle 42 . In one embodiment, partially compressed nitrogen recycle 42 has a pressure of about 8 bar. Partially compressed nitrogen recycle 42 is then further compressed in second recycle compressor 45 and cooled in second aftercooler 43 to form compressed nitrogen recycle 46 , which preferably has a pressure of about 25 to about 27 bar. Fraction of partially compressed nitrogen recycle 44 is withdrawn from partially compressed nitrogen recycle 42 and fed to the warm end of heat exchanger 10 . Whereas fraction of compressed nitrogen recycle 48 is only partially cooled in heat exchanger 10 , fraction of partially compressed nitrogen recycle 44 is fully cooled in heat exchanger 10 . In one embodiment, the split between compressed nitrogen recycle 48 and compressed nitrogen recycle 46 is about 40/60. In another embodiment, the split can be determined by balancing the needs for obtaining the desired temperature approach at the warm end of heat exchanger 10 and maintaining appropriate turbine side versus booster side flow rates based on each device's efficiencies.
[0023] After exiting the cold end of heat exchanger 10 , fraction of partially compressed nitrogen recycle 44 is used to provide heat to bottom boiler 21 before being introduced via valve 93 near a top portion of single column 20 . Those of ordinary skill in the art will recognize that even though recycle compressor 40 and second recycle compressor 45 are pictured as two different compressors, it is possible to use one compressor and remove fraction of partially compressed nitrogen recycle 44 from an inner stage of that single compressor.
[0024] As with all distillation columns, liquids tend to collect near the bottom, while gases rise to the top. In this embodiment, oxygen-rich liquid 24 is withdrawn from the bottom of single column 20 and introduced to subcooler 30 via valve 29 . In one embodiment, oxygen-rich condensing fluid 26 is withdrawn from oxygen-rich liquid 24 and introduced via valve 35 near top condenser 23 . In one embodiment, top condenser is a bath type condenser.
[0025] Gaseous nitrogen near the top of single column 20 travels up tube 27 , with a portion being withdrawn as gaseous nitrogen 28 and the rest condensing within top condenser 23 before being reintroduced to single column 20 . Oxygen-rich condensing fluid 26 introduced near top condenser 23 provides the needed cooling to condense the nitrogen. Waste gaseous oxygen 22 is withdrawn and used to provide refrigeration to heat exchanger 10 . In one embodiment, safety purge 83 can be withdrawn as a safety precaution.
[0026] Recovered liquid nitrogen 62 is then introduced to subcooler 30 in order to further cool recovered liquid nitrogen 62 to produce liquid nitrogen product 64 . Oxygen-rich liquid 24 is used to provide the necessary cooling. Any gas forming within subcooler 30 is withdrawn as oxygen-rich waste gas 34 and may be combined with waste gaseous oxygen 22 before entering the warm end of heat exchanger 10 . In one embodiment not shown, oxygen-rich waste gas 34 may be warmed in heat exchanger 10 separately from waste gaseous oxygen 22 in order to allow for deeper subcooling of liquid nitrogen product 64 . Oxygen purge 32 can be withdrawn from the bottom of subcooler 30 as necessary. Recycled liquid nitrogen 66 can be withdrawn from recovered liquid nitrogen 62 and introduced to the top of single column 20 as reflux via valve 36 . In an optional embodiment (shown as dotted line 66 a ), recycled liquid nitrogen 66 can originate from liquefied nitrogen 58 via line 66 a.
[0027] FIG. 3 provides an additional embodiment of the invention. FIG. 3 is similar to FIG. 2 , except that FIG. 3 provides for increased safety by reducing the risk of hydrocarbons concentrating in subcooler 30 . In this embodiment, oxygen-rich fluid 25 is withdrawn from single column 20 at a point above the bottom portion of single column 20 and introduced to subcooler 30 instead of using the oxygen-rich liquid from the bottom of single column 20 . Essentially, instead of sending a portion of the bottoms liquid to subcooler 30 , all of the withdrawn bottoms liquid is sent to top condenser 23 as oxygen-rich condensing fluid 26 via valve 35 . Recycled liquid nitrogen 67 can be withdrawn from liquefied nitrogen 58 and introduced to the top of single column 20 as reflux via valve 36 .
[0028] In certain embodiment, the feed gas to the single column is air, as opposed to a feed gas having a concentration having higher nitrogen content. The single column has both a bottom reboiler and a top condenser, and in certain embodiments, the reboiler is driven by gaseous nitrogen withdrawn from the recycle compressor, preferably at a first stage discharge of the recycle compressor. In another embodiment, the single column can be partly refluxed with liquid nitrogen split-off from a Joule-Thompson stream (e.g., high pressure nitrogen stream exiting the cool end of the heat exchanger such as stream 58 ). In another embodiment, column bottoms may be split for both product subcooling and for driving the top condenser, or all of column bottoms can used for driving the top condenser with product subcooling being done via an oxygen-rich liquid column sidedraw stream.
[0029] While the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications, and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications, and variations as fall within the spirit and broad scope of the appended claims. The present invention may suitably comprise, consist or consist essentially of the elements disclosed and may be practiced in the absence of an element not disclosed. Furthermore, language referring to order, such as first and second, should be understood in an exemplary sense and not in a limiting sense. For example, it can be recognized by those skilled in the art that certain steps or devices can be combined into a single step/device.
[0030] The singular forms “a”, “an”, and “the” include plural referents, unless the context clearly dictates otherwise.
[0031] Optional or optionally means that the subsequently described event or circumstances may or may not occur. The description includes instances where the event or circumstance occurs and instances where it does not occur.
[0032] Ranges may be expressed herein as from about one particular value, and/or to about another particular value. When such a range is expressed, it is to be understood that another embodiment is from the one particular value and/or to the other particular value, along with all combinations within said range.
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An apparatus for producing liquid nitrogen is provided. The apparatus includes a heat exchanger, a pair of turbine-boosters, a warm compressor, an air separation unit having a single column, a top condenser and a bottom reboiler, a liquid/gas separator, and an optional subcooler. The apparatus is configured to produce merchant or non-merchant grade liquid nitrogen using the pair of turbine-boosters to provide refrigeration and energy for the process.
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BACKGROUND OF THE INVENTION
The present invention relates to a drying apparatus and more particularly to an apparatus for drying fruit that has been treated with an aqueous coating.
In the commercial preparation of fruit, such as citrus fruit, for market, it is common to treat the fruit with an aqueous coating of wax or other material to replace the natural wax which is removed during the washing process, thereby serving to protect the fruit during periods of storage and handling, during transit to market, and ultimately, to enhance the appearance of the fruit at the marketplace. Once this coating has been applied, it is desirable to dry the fruit to facilitate handling, packing, and shipping.
Prior devices that have been used for this purpose have employed relatively high operating temperatures, in the range of 120 to 160 degrees Fahrenheit, low velocity air flow, in the range of 200 to 300 feet per minute, and direct fired heaters to elevate the temperature of the drying air. Direct fired heaters have been employed to reduce the cost of the apparatus but have unnecessarily increased the cost of operation. Because a direct fired heater exhausts combustion gases, including water vapor, into the drying chamber, much higher drying temperatures are necessary to accomplish the desired drying effect. These higher temperatures, in turn, create higher surface temperatures in the fruit, which have been implicated in the occurrence of rind breakdown in citrus fruit either through direct stress on the fruit or through the formation of a "glassy" layer within the wax, which can impede the natural transfer of gases through the coating, e.g. reduce the transfer of carbon dioxide out of the fruit as well as oxygen into the fruit. Moreover, the high dryer temperatures of the prior art increase the overall temperature of the fruit, further exacerbating the inefficiency of these systems by requiring greater amounts of energy to cool the fruit for subsequent storage and handling. In addition, especially in the case of citrus fruit, when insufficient velocity of airflow is used, uneven or incomplete drying can occur because citrus continuously releases water through respiration as well as from the wax, causing humid air to accumulate between pieces of fruit or between layers of fruit on the conveyor.
To overcome some of these drawbacks, other prior devices have used chilled air to dry the fruit, based on the principle of using refrigerated coils to remove humidity from the air. These systems can be engineered to remove moisture from the fruit, but they experience other problems. Although the wax coating of the fruit is dry when the fruit exits the dryer, the fruit is also cold, resulting in severe sweating under humid conditions.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a novel drying apparatus for drying objects, such as fruit, which apparatus overcomes the problems experienced with prior devices.
A primary object of the invention is to provide a dryer that is effective and efficient in the setting of an overall fruit packing facility.
Another object of the invention is to provide a drying apparatus that is effective while operating at relatively low temperatures in order to avoid potentially damaging fruit by exposure to excessive heat.
Another object of the invention is to provide for drying of fruit with high velocity air flow in order to achieve even and complete drying of the fruit coating.
Another object of the invention is to provide a drying apparatus that uses indirect heat to achieve the desired drying temperature thereby preventing the counter-productive introduction of water vapor and other combustion gases into the fruit treatment environment.
It is yet another object of the invention to provide a fruit drying apparatus that is capable of achieving the above objects and is still easy to maintain, efficient in operation, and non-disruptive to the working environment of a fruit handling and packing facility.
These and other objects of the invention are achieved by providing a uniquely shaped drying apparatus through which fruit or other objects are conveyed and within which mildly heated air is forced at high velocity through a series of four zones. The drying air is heated by an indirect fired heater and passes over the fruit or other objects to be dried twice within the drying apparatus, first in one direction and then in the opposite direction, in order to achieve even and complete drying.
The present invention contemplates a dryer apparatus that is characterized by a unique diverging and converging overall shape through which fruit or other objects to be dried are conveyed on a continuous conveyor means. Drying air is forcibly withdrawn at a very high volume flow rate from a diverging chamber and forced into an adjacent converging chamber where it is then caused to pass over the fruit or other objects to be dried. After passing over the fruit, the drying air is collected in another chamber of diverging shape and is again forcibly withdrawn from that chamber and forced at a high volume flow rate into yet another converging chamber. In that chamber, the air again passes over the fruit or objects to be dried, this time in the opposite direction from the first pass, and is collected on the other side of the fruit in the diverging chamber from which it was first withdrawn. Using this reverse airflow system allows for large air flows to pass twice over the fruit in opposite directions thereby minimizing the possibility of pockets of dead air where humidity can accumulate.
In addition, the apparatus of the present invention is preferably provided with removable side panels that permit easy access to the interior of the apparatus for the purpose of conducting regular maintenance. These panels and other housing panels are preferably provided with a suitable layer of insulation for the dual purpose of conserving heat loss and providing sound insulation, and the supply air intake and exhaust ducts are preferably conducted to a point outside of the area where the apparatus is located. With this arrangement, the apparatus of the present invention is easy to maintain, efficient in operation, and does not introduce unwanted noise, heat, or humidity to the work space surrounding the apparatus.
These and other aspects of the invention will be more apparent from the following description of the preferred embodiment thereof when considered in connection with the accompanying drawings and appended claims.
BRIEF DESCRIPTION OF THE DRAWING
The present invention is illustrated by way of example and not limitation in the accompanying drawing in which like references indicate similar parts, and in which:
FIG. 1 is a side elevational view, taken partly in section, of the drying apparatus of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A dryer apparatus embodying this invention is generally shown at 10 in FIG. 1 and is comprised of a housing 12 through which extends a continuous conveyor 14 for carrying fruit or other objects to be dried within the housing. The conveyor 14 can be of conventional design and enters the housing 12 at its entrance end 16 and extends longitudinally through the central portion of the housing 12 emerging from the housing at its exit end 18. After exiting the housing 12, the conveyor 14 is drawn over a drive roller 20 and returns to the entrance end 16 on a path that is below and external of the housing 12. At the entrance end 16 of the housing 12, the conveyor 14 passes over an entrance end roller 22 to complete the continuous circuit of the conveyor means. In the embodiment shown, the conveyor 14 is powered by a variable speed drive motor 24 that provides motive force to the drive roller 20 through a drive belt or chain 26.
In operation, fruit or other objects to be dried are deposited on the conveyor 14 where it passes on top of the entrance end roller 22 and is then conveyed through the housing 12 toward the exit end 18 where it is transferred to another conveyor (not shown) for further processing or handling. Due to the high air velocity used in the apparatus of the present invention, it is not necessary to provide for excessive fruit rotation during the drying process. In fact, such rotation is undesirable as it tends to increase scuffing of the wax and detracts from the appearance of the finished product. Instead, fruit contact points are broken and the fruit is rotated only once at or about the mid-point in the dryer. For this purpose, contact points are broken by a conveyor lifter 28 of conventional and well known design, and the conveyor lifter 28 is located at or about the mid-point of the procession of the conveyor 14 through the dryer 10.
Dryers intended to remove moisture from an aqueous coating of wax applied to fruit, such as citrus fruit, generally function by increasing the surface temperature of the fruit to a temperature sufficient to raise the vapor pressure of the water in the wax to a level above the partial pressure of water in the air inside the dryer. The surface temperature of the fruit is normally increased by adding heat to the air in the dryer. In the apparatus of the present invention, for the purpose of adding heat to the air in the dryer, an air heater, indicated generally at 30, draws supply air into the heater 30 by force of a heater fan 32. The fan 32 draws air into a fresh air inlet 34. Inside the heater 30, air is heated through a series of coils or heat exchangers 36, and that heated air is forced into the dryer 10 via a hot air inlet 38.
As indicated above, prior dryers intended for this purpose have been characterized by inefficiency and other problems that have remained unsolved. In accordance with the present invention, a dryer is provided, especially suited for drying aqueous coatings on fruit, which dryer employs a unique, four-chamber air flow pattern using high velocity air flow that passes the fruit twice in opposite directions and at relatively low temperature. To achieve this, a uniquely shaped diverging and converging housing 12 is used in combination with high powered fans, indicated generally at 40, to move the drying air through the four chambers and over the fruit for a uniform drying effect. In addition, the heater 30 is preferably an indirect heater that is capable of maintaining the desired treatment temperature inside the dryer 10 without introducing water vapor and other undesirable combustion gases into the fruit drying atmosphere.
The fans 40 are mounted within the housing 12 and serve to force drying air to circulate through the chambers of the dryer 10. A first fan or set of fans 42 is mounted in the upper mid-portion of the housing 12 and is positioned to force a large volume of air into a portion of the housing designated as Zone 1 in the drawing. Zone 1 is located at the entrance end of the housing 12 and above the conveyor 14. From the perspective of the fan or fans 42, air is forced by the fan 42 into a chamber (Zone 1) that converges from the end of the chamber defined by fan 42 toward the entrance end of the housing 16. This forcing of air at a high volume rate into Zone 1, and the converging shape of Zone 1, combine to create a uniform air pressure above the fruit on the conveyor defining the bottom of Zone 1.
To further facilitate uniform flow of air down through the layer of fruit on the conveyor 14, an air distribution panel 44 can be interposed in the air flow path above the conveyor 14 in Zone 1. This air distribution panel 44 can be comprised of perforated sheet metal, or any other desired material, and can be provided with any desired degree of openness. An openness of 35 to 65 percent is currently preferred.
Below the portion of the conveyor that passes through Zone 1 is a chamber, designated as Zone 2 in the drawing, that is characterized by a diverging shape from the entrance end 16 of the housing 12 toward its mid-portion. The mid-portion end of diverging Zone 2 is defined by a second fan or set of fans 46, which serve to draw air at a high volume flow rate out of Zone 2 and into a downstream chamber, designated in the drawing as Zone 3. The resulting reduced pressure in Zone 2, when combined with the high uniform pressure maintained in Zone 1 by the first fan 42, pulls air downwardly past the fruit on the conveyor 14 at a high and uniform velocity across the portion of the conveyor defining the border between Zones 1 and 2.
Zone 3 is located below the conveyor 14 and runs from the mid-portion of the dryer 10 to the exit end 18 of the housing 12. The second fan or set of fans 46 withdraws air from the diverging chamber Zone 2 and forces that air at a high volume flow rate into the adjacent, converging chamber Zone 3, which is located below the conveyor 14 and downstream of Zones 1 and 2. As is the case with Zone 1, this forcing of air at a high volume flow rate into Zone 3, and the converging shape of Zone 3, combine to create a uniform air pressure below the conveyor defining the top of Zone 3. Again, as in Zone 1, a second air distribution panel 48 can be interposed in the air flow path below the conveyor in Zone 3.
Across the conveyor 14 from converging chamber Zone 3 is another diverging chamber designated as Zone 4 in the drawing. As can be seen in the drawing, it is from this diverging chamber Zone 4 that the first fan or set of fans 42 withdraws air to create the uniform air pressure in Zone 1. The resulting reduced pressure in Zone 4 pulls air upwardly past the fruit on the conveyor 14 at a high and uniform velocity across the portion of the conveyor 14 that defines the border between Zones 3 and 4.
More specifically, in the preferred embodiment of the present invention, the conveyor 14 traverses a total length of about 35 feet within the housing 12 and is about 3 feet to 9 feet wide. The first fan 42 is either a set of two 30 inch diameter, 10 horsepower fans or a single 36 inch diameter, 15 horsepower fan that blows air at a volumetric flow rate of up to 30,000 cubic feet per minute per foot of dryer width into Zone 1, creating a positive pressure in Zone 1 of about 2 inches of water and a negative pressure in Zone 4. The second fan 46 is also preferably a set of two 30 inch diameter, 10 horsepower fans that maintain a similar positive pressure in Zone 3 and negative pressure in Zone 2. The resulting pressure differentials between Zones 1 and 2, and between Zones 3 and 4, cause air in the dryer 10 to flow downwardly across the fruit in Zone 1 and upwardly through the fruit in Zone 4 at a velocity in excess of 1000 feet per minute. Further, the air distribution panels 44 and 48 in the currently preferred embodiment of the invention have a degree of openness of less than 50%.
In order to achieve the desired drying effect in the present dryer using a very high velocity air flow, it is not necessary to maintain extremely high operating temperatures within the housing 12. It has been found that by maintaining the temperature of the air in Zone 1 at a maximum of about 95 to 100 degrees Fahrenheit, sufficient heat is transferred to the surface of the fruit thereby increasing the vapor pressure of the water in the wax, and excellent drying results are achieved. Moreover, as the fruit is conveyed through Zone 1, the high velocity air flow removes water vapor from the aqueous surface coating of the fruit as well as from the gaps between individual pieces of fruit.
For the purpose of maintaining the desired temperature within the dryer 10 without introducing water vapor and other undesirable combustion gases, the heater 30 is preferably an indirect, gas-fired heater instead of a direct fired type heater. This arrangement eliminates unnecessary introduction of water vapor and other combustion gases, including carbon monoxide and nitrogen oxides, into the drying environment as well as into the packing environment, if the dryer is installed indoors. If a direct fired heater were used, as has been common in dryers in the past, water vapor and other combustion gases are injected into the dryer substantially increasing the partial pressure of water in the dryer air. Accordingly, in order to raise the water vapor pressure of the water in the wax above the high partial water pressure of the drying air, relatively high operating temperatures were required.
In the present invention, by using an indirect fired heater, the combustion gases used to heat the heat exchangers 36 are vented outside of the dryer 10, and if the dryer is installed indoors, the gases are preferably vented outside of the building through appropriate ducting (not shown). In order to obtain supply air having a minimum humidity, the fresh air inlet 34 is also preferably connected by appropriate ducting (not shown) to a source of air outside of the building in which the dryer 10 might be installed.
When the preferred embodiment of the present invention, as described above, is in operation, between 5,000 and 10,000 cubic feet per minute of air is passively exhausted to the outside through a vent 50 in the side wall of the housing 12 in Zone 4. To compensate for the loss of that vented humid air, make-up fresh air is heated by heater 30 to a temperature necessary, after being combined with return air from Zone 4, to maintain the temperature in Zone 1 at a maximum of about 95 to 100 degrees Fahrenheit. All make-up fresh air is preferably brought in from outside of the packing environment because outside air is generally less humid than the air inside of a fruit packing facility. In addition, in order to monitor and maintain the desired temperature and humidity conditions within the dryer 10, temperature sensors 52 and humidity sensors 54 may be placed inside the dryer 10, and can be monitored by an operator outside of the dryer. Preferably, these sensors 52 and 54 are placed in Zones 1 and 3, as shown.
Lastly, in order to reduce the noise of operation and to provide for efficient retention of heat, the housing 12 is preferably lined with a suitable layer of insulation 56. Also, the panels 58 comprising one side of the housing 12 are preferably removable to facilitate easy maintenance of the interior of the dryer 10. Only a few or all of the panels 58 may be arranged to be removable.
It will be apparent to those skilled in the art that the drying apparatus of the present invention provides an efficient and effective means for drying objects, particularly fruit having an aqueous coating of wax or citrus coating thereon, that overcomes problems that existed in previous dryers. The apparatus of the present invention is capable of achieving effective drying while operating at a relatively low drying temperature, thereby minimizing damage to the fruit being dried, conserving energy, and reducing the cost of operation. Moreover, the apparatus is arranged to cooperate well with other processes typically encountered in a packing facility, and does so without having negative effect of the work environment, by minimizing noise of operation and eliminating the introduction of noxious fumes into the work place.
Various modifications and changes may be made by those having ordinary skill in the art without departing from the spirit and scope of the invention. Therefore, it must be understood that the illustrated embodiment has been set forth only for the purpose of example, and that it should not be taken as limiting the invention as defined in the following claims.
The words used in this specification to describe the present invention are to be understood not only in the sense of their commonly defined meanings, but to include by special definition, structure, material, or acts beyond the scope of the commonly defined meanings. The definitions of the words or elements of the following claims are, therefore, defined in this specification to include not only the combination of elements which are literally set forth, but all equivalent structure, material, or acts for performing substantially the same function in substantially the same way to obtain substantially the same result.
In addition to the equivalents of the claimed elements, obvious substitutions now or later known to one of ordinary skill in the art are defined to be within the scope of the defined elements.
The claims are thus to be understood to include what is specifically illustrated and described above, what is conceptually equivalent, what can be obviously substituted, and also what essentially incorporates the essential idea of the invention.
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A drying apparatus is provided for drying objects such as citrus fruit that has been coated with an aqueous coating such as wax. The apparatus includes a housing that is divided into four distinct zones, two each above and below a conveyor for conveying fruit through the dryer. An indirect fired heater is provided, and fans that circulate drying air at high velocity in a reverse air flow pattern. The housing of the dryer is constructed in a unique shape so each successive zone is alternately converging and diverging. With this arrangement, air is balanced in the treatment zones and passes over the fruit twice, first in one direction, and then in the other, to achieve even and complete drying.
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TECHNICAL FIELD
[0001] This invention is relates to a tree delimbing method and device for delimbing a tree trunk in a compliant gripping state defined by a set of limbing knives enclosing the trunk, comprising repeated adjustment of the limbing knives through a control unit for adaption of the gripping state to a varying thickness of the trunk when the trunk is advanced between the knives for the delimbing of the trunk.
BACKGROUND
[0002] When delimbing tree trunks using a tree processing assembly, it is desirable to cut the branches as close as possible to the trunk. During a delimbing operation it is therefore necessary to adapt the grip of the surrounding knives to the varying thickness of the trunk section that is currently in the grip.
[0003] In a prior art delimbing device of the above mentioned type and disclosed in U.S. Pat. No. 4,898,218, the compliance of the gripping state is predetermined by changing a closing extent of a gripping means provided with the limbing knives each time a top face of the trunk has been moved a predetermined distance in a direction of movement for a resiliently compliant limbing knife. In the example disclosed in the above patent, there is provided a switch which is actuated by the compliant limbing knife so as to when the switch is not actuated by the limbing knife, the closing extent of the gripping means increases to lift the tree trunk in the delimbing device until the compliant limbing knife actuates the switch that then interrupts the closing of the gripping means. When the tree trunk advances further in the delimbing device in the direction to its top end, the switch again becomes non-actuated by the returning resiliently compliant limbing knife such that the closing extent of the gripping means once more increases. This procedure is repeated until the whole tree trunk has been advanced through the delimbing device.
[0004] A disadvantage of the prior art device is that the compliance of the gripping state, i.e. the remaining free stroke of travel of the resilient limbing knife, is invariable after each increase of the extent of closing of the grip of the trunk. However, in order to obtain a good delimbing operation, it may be necessary to cut the branches of different types of tree trunks with mutually different compliance or remaining free stroke of travel of the resilient limbing knife. Birch trees, for example, can have coarse branches that may excessively load the processing assembly when attempting to cut the branches too close to the trunk. The gripping state should then have a relatively large compliance, capable of allowing the tree trunk to move away from the limbing knives, or allowing the limbing knives to move away from the tree trunk a further distance, when one or more such coarse branches are coming into knife engagement. The compliance, play or remaining free stroke of travel of the gripping state should then be about 30 to 40 mm. On the other hand, spruce trees, for example, may have a linearly tapering trunk with relatively thin branches. The gripping state should then have a relatively small compliance so as to cut the branches close to the trunk. If the compliance then is too large, the elastic branches may resiliently bend toward the trunk and slide along the limbing knives without being cut. The compliance, play or free stroke of travel of the gripping state may then be about 5 mm.
DISCLOSURE OF THE INVENTION
[0005] An object of the present invention is to further develop a method and a device of the type defined above so that it is capable of more effectively delimbing tree trunks of mutually differing branch qualities.
[0006] Another object may be considered as to adapt the delimbing operation to the requirements of the actual tree trunk.
[0007] These objects are obtained by the features of the appended claims.
[0008] In one aspect of the invention, a method according to the invention comprises
[0009] setting a desired compliance of the gripping state in the control unit;
[0010] detecting an actual compliance of the gripping state; and
[0011] performing each adjustment of the limbing knives through the control unit until the actual compliance corresponds to the desired compliance.
[0012] Thereby the compliance of the gripping state can be adapted to the quality of the actual tree trunk. The desired compliance may empirically be determined by an operator of the device based on a judgment of the tree trunk and its branches and be set in an input unit as a category such as “Spruce”, “Birch”, etc. but also as a direct distance value, for example 40 mm.
[0013] While the compliance of the gripping state may be included by all limbing knives, according to one embodiment of the invention, the compliance comprises a remaining free stroke of one limbing knife resiliently engaging the trunk.
[0014] Other features and advantages of the invention may be apparent from the claims and the following detailed description of embodiments.
BRIEF DESCRIPTION OF THE DRAWING
[0015] FIG. 1 is a front view of a vertically oriented tree processing assembly that may be incorporated with a device according to the invention;
[0016] FIG. 2 is a diagrammatic side view with parts broken away of a tree trunk received in a horizontally oriented tree processing assembly;
[0017] FIG. 3 is a view corresponding to FIG. 2 illustrating an increasing distance between the tree trunk and a bottom face of the assembly when the trunk is advanced therethrough;
[0018] FIG. 4 is a diagrammatic front view of a horizontally oriented tree processing assembly gripping a tree trunk;
[0019] FIG. 5 is a view corresponding to FIG. 4 where the assembly is gripping a thinner section of the trunk; and
[0020] FIG. 6 is a graph showing a characteristic of a proximity sensor that may be incorporated with a device according to the invention
[0021] Throughout the drawing, components having similar function have identical reference numbers.
DETAILED DESCRIPTION OF EMBODIMENTS
[0022] FIG. 1 shows a front face of a vertically oriented tree processing assembly 10 of the single-grip type. Assembly 10 has a main body 12 supporting inter alia a pair of opposite feed wheels 14 , a lower forward limbing knife 18 , a pair of upper forward limbing knives 24 , 26 and an upper rearward limbing knife 28 .
[0023] The two feed wheels 14 are pivotally connected to the main body 12 to clamp and longitudinally feed a tree trunk 60 ( FIGS. 2-5 ) felled by the assembly 10 . The likewise pivotally connected limbing knives 18 , 24 , 26 , 28 , likewise pivotally connected to the main body 12 , enclose the tree trunk to cut off branches therefrom when the trunk is advanced through the assembly.
[0024] Each feed wheel 14 and the limbing knives 18 , 24 , 26 are adjusted to their positions enclosing the trunk by means of actuators. In the examples shown, the feed wheels 14 are adjusted by respective hydraulic cylinders 16 , and the lower limbing knife 18 as well as the upper forward limbing knives 24 , 26 are also adjusted by respective hydraulic cylinders 20 and 56 , 56 ( FIG. 4 ). The upper rearward limbing knife 28 is resiliently forced to the tree trunk 60 by means of a spring 30 ( FIGS. 4 , 5 ).
[0025] The diagrammatic representation of FIG. 2-5 shows a horizontally oriented tree processing assembly 10 gripping a tree trunk 60 by the upper forward limbing knives 24 , 26 and by the upper rearward limbing knife 28 . Accordingly, the upper forward limbing knives 24 , 26 as well as the lower forward limbing knife 18 (indicated only in FIG. 2 ) support the weight of the horizontally oriented tree trunk 60 received in the processing assembly 10 .
[0026] To facilitate the description, the function of the adjustable lower forward limbing knife 18 is omitted. If the assembly 10 is provided with such a limbing knife 18 , in the following description, limbing knife 18 is understood to be controlled in a manner corresponding to the control of the adjustable upper forward limbing knives 24 , 26 .
[0027] When the horizontally oriented, thus gripped tree trunk 60 is advanced to the left through the assembly in the manner that is diagrammatically shown in FIGS. 2 and 3 , i.e. from the butt end to the top end, the actual distance d from the trunk to a bottom face of the main body 12 of the assembly 10 will increase. The spring-loaded limbing knife 28 will then follow the movement downwards of the top face of the trunk 30 and—to a limited extent—also upwards. Distance d may then be considered as a measurement of the compliance of the enclosing engagement of the limbing knives to the vertical movements and variations of thickness during the feed of the trunk. The bottom face of the main body may represent an upper end position, formed by an upper stop (not shown) for the spring-loaded limbing knife 28 , the lower end position of which may be defined by a lower stop 32 ( FIGS. 4 , 5 ) of the assembly 10 .
[0028] The distance d is critical for a correct delimbing operation. Distance d may be regarded as representing the play or remaining stroke of travel of the spring-loaded limbing knife 28 —and thereby also the play in the vertical direction of the horizontally oriented tree trunk 30 .
[0029] If, on the one hand, the play is too small, the trunk may get stuck in the assembly 10 or subject the limbing knives to a far too high load by cutting into far too massive wood sections of the branches or the trunk 60 . If, on the other hand, the play is too large, the branches of the trunk 60 may bend to the trunk and slide under the the knives whereby they will not be cut off during the delimbing operation.
[0030] As is apparent from FIGS. 4 and 5 , the actual distance d is detected by a proximity sensor 42 , such as an analog inductive or magnetic proximity sensor. Proximity sensor 42 is continuously signaling the actual distance d, for example as an electric current i, via a signal connection 44 to an electronic control unit 46 of a control system 40 . In one embodiment, a processor (not shown) in the control unit 40 can be programmed to emit a control signal via a signal connection 48 to a magnet valve 50 when the electric current indicates that the distance d has risen to a critical value D 1 ( FIG. 6 ) that may be stored in a memory (not shown) in the control unit 46 . Valve 50 then opens a path between a hydraulic pump 52 and the respective hydraulic cylinders 56 . The limbing knives 24 , 26 will then further tighten the grip of the tree trunk 60 , whereby the distance d decreases to an adjoining value D 2 ( FIG. 6 ) when the tree trunk 60 is lifted further up in the assembly 10 . During the continuing feed of the trunk 60 in the assembly 10 , the distance d may further increase until it again reaches the critical value D 1 , whereupon the above process is repeated. The number of repetitions of this process depends on the magnitude of the interval D 1 -D 2 and the length of the tree trunk. The magnitude of the interval D 1 -D 2 may vary depending on the accuracy, for example, depending on inertia and delay in the hydraulic system and influence of hysteresis, of the control system 40 and the sensor 42 .
[0031] As indicated in FIG. 6 , in certain circumstances, D 1 and D 2 may have relatively large values that typically amount to between 30 and 40 mm. This means that the limbing knife 28 has a relatively large play above the tree trunk 60 . Such a case may be suitable for trunks of birch, the branches of which may be relatively massive close to the trunk. The large play of the limbing knife 28 will then allow the knife to be forced further out from the trunk before it cuts the branch. The spring-loaded limbing knife 28 and also the other limbing knives can have such a cutting angle that they are guided away from the trunk to a certain amount during the cutting operation. The process may then also allow that the whole trunk 60 is forced away from the adjustable limbing knives 24 , 26 when these knives encounter massive branches. The result, however, is that a larger play d will generally allow coarse branches to be cut off at a larger distance from the trunk 60 than will a smaller play. The spring-loaded limbing knife 28 and the weight of the trunk 60 will, however, provide for that the thinner branches still are cut close to the trunk.
[0032] A relatively small play where D 1 and D 2 have relatively small values of about 5 mm may be suitable when delimbing trunks of spruce, for example, where generally the trunk surface tapers relatively linearly and the branches are relatively thin and therefore are quite easy to cut off. The branches are then cut close to the trunk 60 and are thereby prevented from bending against the trunk and sliding along and past the limbing knives 18 , 24 , 26 , 28 .
[0033] In order to take account for varying quality of tree trunks where at least certain branches need to be cut off at different distances from the trunk to obtain a good delimbing result for a certain processing assembly, the desired play or the above-mentioned critical value D 1 can be set in the control unit 46 prior to each delimbing operation. To this end, the control unit 46 is provided with an input unit 47 , having one or more push buttons or keys 49 , for example, in the vehicle (not shown) that supports the assembly 10 . In one embodiment of the invention, the operator (not shown) then makes a visual examination of the tree to be felled, and, after an empirical conclusion, makes a decision about the quality of the trunk, for example in the form of a category, that is entered into the unit 47 . Apart from “Birch” and “Spruce”, in a set of categories to be entered, also other tree species, sub-categories such as “Slender Birch”, as well as varying qualities such as decay or rotten wood, may be included. An experienced operator may also enter the value of D 1 directly, if the control unit 46 so allows. The set of keys 49 of the control unit 47 may be located accessible for the operator in the proximity of a joy stick (not shown), for example, provided for controlling another function of the tree processing assembly.
[0034] To relieve the operator, in the scope of the appended claims, it is at least imaginable to perform the setting of tree trunk category automatically by using a camera and an image processing system (not shown) having the capability of identifying the different categories of tree trunks.
[0035] The foregoing detailed description is given primarily for clearness of understanding and no unnecessary limitations are to be understood therefrom. Modifications will become obvious to those skilled in the art upon reading this disclosure and may be made without departing from the spirit of the invention or the scope of the appended claims.
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Method and device for delimbing a tree trunk ( 60 ) in a compliant gripping state defined by a set of limbing knives ( 18, 24, 26, 28 ) enclosing the trunk. The limbing knives are repeatedly adjusted through a control unit ( 46 ) for adaption of the gripping state to a varying thickness of the trunk when the trunk is advanced between the knives for the delimbing of the trunk. The invention comprises entering a desired compliance (D 1 ) of the gripping state in the control unit ( 46 ), detecting an actual compliance (d) of the gripping state, and performing each adjustment of the limbing knives via the control unit until the actual compliance (d) corresponds to the desired compliance (D 1 ).
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This application is a divisional of application Ser. No. 08/942,430, filed Oct. 1, 1997, U.S. Pat. No. 5,848,665, issued.
BACKGROUND OF THE INVENTION
The present invention relates to a safety and debris net system which are used as fall catching prevention type apparatus found in the construction industry, and deals more particularly with an improvement in the safety net material whereby the material realizes increased strength and effectiveness as a fall prevention device and deals as well with improvements in the connections between component parts of a net system and the securement devices used to secure the net system to supporting structure.
In the past safety net construction has been primarily limited to meshes made from nylon. While nylon meshes are still popular, some problems attendant to their use as using safety nets exist. First, nylon is not resistant to ultraviolet light and therefore must be treated to prevent the negative effects of exposure to such light. The treating process is usually accomplished by dyeing by dipping in a solution, and in this dyeing/dipping process causes shrinkage of the nylon. Even after this treatment is complete, the nylon material tends to undesirably stretch with use. Accordingly, in some applications, some sort of sag control measures must be incorporated into the support structure at the job sight to prevent net sagging . This is particularly important and needed in the application of netting which is used in tunnels or in bridges where the passage of vehicles below the netting, in particular trucks, could interfere or even cause entanglement with the moving vehicles below and thereby presenting a hazardous situation. Also, sag is undesirable because it would allow someone falling into a safety net to hit what was below it due to the travel which occurred at impact. Further, with the increasing concern for products which are made from environmentally safe processes, the dipping of a net into a chemical bath such as, described above, is likewise undesirable.
Also, in the connection between the debris and safety nets with the structure responsible for holding it in place, it is long been the practice to sew or lash the debris net or safety net to the border piece. This practice is very labor intensive and contributes to the major cost in net fabrication. Not only is the connection between the net and its border usually done by a sewing or lashing procedure, but also in the case with debris netting, the connecting rings which are used to connect the debris nets together have been sewn or lashed to the base material. The hem or border member of each debris net also defines an overlapping flap between successive debris net segments and must be sufficiently strong to bear the loads imposed on any connection it makes with another net. Likewise, the use of hooks which attach safety nets to supporting cables also use a hemming, lashing or sewing process which had the potential of becoming unraveled and hence the spacing between clip hooks would become undone. Additionally, hitherto the debris and the safety nets were fabricated as separate items, and thus were required to be assembled together at a given on-site location to assume the layered orientation, e.g., the debris net superimposed over the safety net. This process took time and added to labor expense. It also contributed to the need to provide a connection system which could orient these nets in this manner.
Accordingly, it is an object of the invention to provide a improved net of the type which is used as a safety net for personnel or as a rack guard or conveyor guards wherein the net mesh is connected to its supporting border in a manner which significantly reduces its manufacturing costs and production time.
Still a further object of the invention is to provide a combined debris and safety net which is fabricated as one unit thus avoiding the hitherto problems associated with assembling the two on site.
It is yet a further object of the invention to provide a net of the aforementioned type which is resistant to deterioration because of exposure to ultraviolet radiation hence making it unnecessary to color it by dyeing or treating which hitherto has been standard practice in the industry and avoids the problem of shrinkage of material due to such dyeing process as well as avoiding the negative effects of such treatment on the environment.
A further object of the invention is to provide an improved connection between a safety net and or a debris net with parameter structure which connects to static supports of a safety system.
SUMMARY OF THE INVENTION
The invention resides in an improvement in safety net wherein the net is formed from a material which is resistant to weakening by ultraviolet radiation, hence does not need to be dyed or treated, and therefore is shrink and sag controlled. The invention further resides in a connection and method for making such connection between a safety net and a debris net for supporting same as a unit in an assembled condition.
More specifically, the invention resides in a safety net comprised of an elongate substantially flexible border member having a cross section which is substantially uniform through out its length. The border member has first and second opposite distal ends which are connected to one another to define a closed interior area. A mesh structure is provided and includes first and second elongate members intersecting at spaced nodal points to define a matrix of interconnecting members which define the mesh structure. A plurality of flex C-ring fasteners are also provided and are capable of being deformed around an underlying area of the border member and about the cross section thereof to cause fastening of the mesh structure with the border member at points therealong corresponding to spacings which evenly distribute loads through out the net through the periphery of the mesh structure. The flex C-rings are steel members which are deformed from an expanded condition to a deformed reduced condition so as to nonreleaseably capture a portion of the perimeter of the mesh structure and the border member in a fastened condition thereby avoiding the hitherto known problems with stitching of articles to the component members of the net.
The aspect of the invention which employs a method of fastening using deformable metallic flex C-ring fasteners instead of stitching is further employed by way of attaching a safety net and a debris net to one another. This is done by aligning the debris net with the safety net such that a flap constituted by the overlying debris net extends beyond the safety net and the underlying safety net extends coextensively with the end of the debris net at the opposite end of the debris net. In this way, the safety nets are connected end to end with one another with the debris net flap covering the joint between serially connected safety nets, or, alternatively, the debris net may simply be made coextensive with the safety net at both opposite ends, such that the joint between serially connected safety nets remains exposed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partially fragmented side elevation view of a debris and safety net system embodying the invention shown in its assembled condition.
FIG. 2 is a partially fragmentary top plan view of the system of FIG. 1.
FIG. 3 is a partially fragmentary plan view of a netting unit.
FIG. 4 is a partially fragmentary plan view of the debris net employed in the unit of FIG. 3.
FIG. 5 illustrates a safety net shown separate from the netting unit of FIG. 3.
FIG. 6 is a section view taken along line 6--6 in FIG. 4.
FIG. 7 is a section view taken along line 7--7 in FIG. 3.
FIGS. 8a, 8b, and 8c show mesh border connection for the net of FIG. 5.
FIG. 9a shows one embodiment of a hook clip connection.
FIG. 9b shows another embodiment of a hook clip connection.
FIG. 10a illustrates one embodiment of the mesh strands for the net of FIG. 5.
FIG. 10b illustrates another embodiment of the mesh strands for the net of FIG. 5.
FIG. 11 illustrates an eye splice connection using the fastener of FIGS. 13a and 13b.
FIG. 12 illustrates a "T" connection using the fastener of FIGS. 13 and 13b.
FIG. 13a is a side elevation view of the fastener shown in FIGS. 11 and 12.
FIG. 13b is a sectional view taken along line 13b--13b of FIG. 13a.
FIG. 13c is a perspective end view of the fastener shown on FIGS. 11 and 12.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIGS. 1 and 2 illustrate a safety and debris netting system in its assembled condition. The system 2 includes a primary cable 4 disposed outwardly spaced from a structure, in this case a building 1, in a clothes-line fashion by a post 6 connected to the structure 1 at its lower end, and a secondary cable 3 disposed along the periphery of the structure and anchored thereto at location(s) 7 so as to be disposed coextensively and parallel to the primary cable 4. In the illustrated example, the post 6 is hingedly connected at its lower end to the existing structure and is cantilevered outwardly thereof and is maintained at an angle relative to the structure 1 by a plurality of combined debris net and safety net assembly units 11 which extend therebetween. Each unit 11,11 is comprised of a debris net 8 and a safety net 10, each respectively superimposed over one another in that order. Each net unit 11, 11, connects to the system along each of the primary and secondary cables 4 and 3 so as to be cantilevered outwardly of the structure in the manner illustrated in FIG. 2.
Referring now to FIGS. 3-6, and to the construction of the net assembly units 11,11, it should be seen that each unit is in fact the result of the superposition connection of the debris net 8 of FIG. 4 onto the safety net 10 shown in FIG. 5. Each debris net segment has a left end 12 primarily defined by a flap region 17 and a right end 19 defined by the reminder of the net. These regions are respectively further defined by a transversely extending seam 18, separating one region of each net segment from the other. A border member 25 is likewise formed about the perimeter of the net to protect against unraveling of the strands and to serve as a part of the net which can be used to secure it to another debris and/or safety net. A second transversely extending seam 14 is provided within the right end segment of the debris net 8, and as will be discussed later, is used as a securement along which appropriate connecting hardware is attached. As best seen in FIG. 6, the border as well as the seams are defined by bunched debris netting fabric 13 sewn around an internal cord 16 provided for the purpose of creating a mounting strip along which a plurality of securements can be made to the debris net. To this end, connecting ring means 23,23 are attached along the seam 14 of the net at spaced intervals S1,S1, and the left end 14 of each of the debris net is provided with lashings 24,24 each respectively secured to the net at spaced intervals S2,S2 corresponding to the spacings S1,S1 such that the connecting rings 22,22 of one net can be connected to the rightmost next net by being tied by the corresponding placed ones of the lashings 24,24 in the manner shown in FIG. 6.
It is a feature of the invention to connect the plurality of connecting rings 23, 23 and the seam 14 to one another through the intermediary of the improved connecting mean shown in FIGS. 6 and 7. This connection means includes at least one deformable flex C-ring fastener 9,9 which mechanically connect each connecting ring to the debris net 8 along the seam 14. In the preferred embodiment, the flex C-ring fasteners are three-sixteenth to eleven thirty seconds gauge steel cylindrical connectors having a wire diameter of 0.70" and are capable of being deformed about and/or through a given member to take its final deformed O-ring shape about the captured member. These fasteners are commercially sold by Stanley Products of New Britain Ct. under the tradename Spenax, under part number 5G100, while the applicator tool is also sold by Stanley under the tradename Spenax and under model number SC50. The tool referenced is particularly well suited for deforming the fastener through the material making up each seam of the debris net so as to bind the gathered material and the ring together. This avoids the heretofore known process of having to stitch the rings 23,23 into the seams at the points of connection. Also, in the past, the only way by which the lashings 24,24 were attached to the debris net was by sewing or stitching, which again is subject to the same problems associated with the stitched connection of the rings 23,23. Thus, the lashings 24,24 are also attached to the debris net at the leftmost border end 12 using the aforementioned flex C-ring fasteners and related tool. This is accomplished by taking a length of lashing line and doubling it back on itself and then securing it midway of its length to the border end 12 using the aforementioned flex C-rings fasteners as best illustrated in FIG. 7.
As best illustrated in FIG. 5, the safety net 10 is comprised of a border member 32 usually made up of a five-eighths inch twisted polypropylene rope to which is attached at securement points a,a and b,b a mesh member 36. The mesh member is usually a standard knotted mesh as illustrated in FIGS. 8a-8c, but it is contemplated within the purview of the invention to include any mesh structure or material capable of being secured to the border in the manner hereto disclosed. In particular, the design of the mesh may take many different forms as reflected by either a diamond mesh or a square-type mesh. In the preferred embodiment however, as illustrated in FIG. 5, the net is a four inch diamond design which is connected to the border member 32 in a manner which will be discussed in greater detail below.
In the safety net 10, the connection between the mesh structure and the border member 32 is effected by using the previously discussed flex C-ring connections that are discussed previously. It should be seen that in the case of a diamond configuration mesh structure, the perimeter of the netting is defined by outwardly directed V-shaped nodes 38,38. These V-nodes connect to the border member at points a,a and b,b. As with the ring connections associated with the debris net discussed above, in the past it was commonly the practice to use stitching and/or other tying methods to attach one member to the other. However, it has been found that the connection between the border member and the mesh structure 36 can be made less expensively and with the same degree of reliability and strength using the fastening method discussed above. This would be accomplished by providing at least one flex C-ring fastener to connect the mesh at each node a,a and b,b to the border member as best illustrated in FIGS. 8a, 8b. In the illustrated example of FIG. 8a, the node aa is located interiorly of the border member 32, whereas, in the embodiment of FIG. 8b, the node aa is dispose outwardly of the border member 32 by threading the border member 32 through each node. Also, as illustrated in FIG. 8c, more than one C-ring fastener 9,9 may be used to connect the mesh structure 36 is connected to the border member 32, Such fasteners 9,9 are 11/2 inch flex C-ring fasteners each having a wire diameter equaling approximately 0.12 inch and being sold by Stanley Inc. under part number 11SS40. Further to these ends, it should be seen that the border member 32 being a continuous piece of rope, is capable of being connected at its distal ends by a lapping joint 40 using a mechanical connection which will be discussed in further detail later in accordance with another aspect of the invention.
As illustrated in FIGS. 5, 9a, and 9b, disposed about the periphery of the safety net 10, is provided a means 42 for locking the net into place along the cables 3 and 4 at two border edges 41,41' of the net 10 marked with the nodes aa, aa, and for coupling one net to the other along opposed border ends 43,43' marked by the nodes bb,bb. This means is readily connectable to the cables 3 and 4 by a plurality of eye hooks 42,42 which are securedly disposed about the border member 32 for the purpose of locking onto the cables 3 and 4. Each eye hook as illustrated in FIG. 9a, has a base portion 44 and a body portion 46 which are integrally connected to one another. The body portion which defines the hook end of the members 42,42 has a crescent shape and is provided with an outwardly biassed locking element 48 which is maintained in a normally closed condition by the biassing means of the hook so as to be maintained in an otherwise closed condition. The base portion 44 has an opening 50 through which is received the border member 32. The hooks 42,42 are maintained in a linearly spatial relationship relative to one another along the border member 32 so as to distribute loads equally throughout the netting. To these ends, each hook is secured to the border member against relative linear movement by a pair of flex C-rings 13, 13 disposed on opposite sides of the involved hook and by a holding strip 52 which straddles the base of each hook and is secured to border member by the C-ring pair 13,13. In the illustrated embodiment of FIG. 9b, the eye hook 42' therein shown has a modified base portion 44' which, instead of including an opening 50, has a bifurcated offset clevis portion comprised of members 72 and 74 which straddle the border member 32 along its opposite sides. Each of the clevis members 72 and 74 includes an opening 76, 78 sized to receive a locking bolt 80 therein which is held in place by an appropriate holding member, such as, a bolt or pin 82. This arrangement is particularly useful in the fabrication of the safety net 10 in that it allows for the hooks 42', 42' to be connected to the net after the mesh 36 is attached to the border member 32 thereby saving labor costs and allowing the net to be custom fitted with the hooks 42',42' at the spacings requested by the customer.
Referring back to FIG. 3, and to the net unit 11, the aspect of the invention which employs a method of fastening using deformable metallic C-ring fasteners is further employed by way of attaching the safety net 10 and the debris net 8 to one another in the manner illustrated in FIG. 7. This is done by aligning the debris net with the safety net in the manner described below and connecting same at points cc along the border 32 of the safety net 32. The spacing between points cc, cc may vary according to design, but in the preferred embodiment, the spacing is equal to about two feet between connection points. To these ends, it should be seen that since the length of the debris net 8 in the illustrated embodiment exceeds that of the safety net 10 by the length of the flap region 17, the seam 18 of the debris net 8 is hence aligned with the left border run 43 of the safety net 10 and the right end border 19 of the debris net 8 with the right border run 43' of the safety net 10 such that at the left of the unit 11, the flap region 17 of the overlying debris net 8 extends beyond the left border 43 of the safety net 10, and, on the right side, the underlying safety net 10 and the overlaying debris net extend coextensively with one another. In this way, as best shown in FIG. 2, the net "A" connects to net "B" along line A-B by clipping the hooks 42,42 disposed along end 43' of the safety net "A" to the border length 43 of the net "B", then by clipping the hooks 42 42 disposed along border length 43 in net "B" to the border length 43' of net "A", and then by securing the debris net by attaching the lashings 24,24 to the rings 23,23 such that the flap portion 17 covers the connection line A-B.
Referring now to FIGS. 10-12, it should be see that another aspect of the invention resides in the material by which the strands 37,37 of the safety net mesh material 36 can be made in order to overcome the hitherto known problems associated with stretching and shrinkage due to the results of dying materials previously used for safety nets as well the known problems associated with on-sight sagging which is prevalent in commonly used materials, such as, nylon. The mesh structure of the embodiments can take numerous forms. In the first form, as shown in FIG. 10a, the mesh strand 37' is a dual component material having a inner core member 45 and an outer sheathing member 47 which together combined to create a tensile strength which is required in the industry for safety standards. The inner core 45 is comprised of a single polypropylene or nylon strand or equivalent material and the surrounding braided sheathing member 47 is formed from a DACRON polyester braided sock. Alternatively, the sheathing member 47 may take the form of a twisted or straight sock or other like material which is abrasion and/or U.V resistant. This arrangement is particularly conducive to the prevention of the degradation of the core material since without the protection of the sheathing material, the core member would be subject to the adverse degrading effects of ultraviolet exposure, thereby making it necessary to dye or dip the monofilament core material as is presently done in the art. While the sheathing member is considerably durable and would not readily lend itself to abrading, it is nevertheless possible that through usage, it can become worn and the additional strength and protection that offers to the core material 45 could somehow be compromised. In view of this, the core member 45 may itself be formed from for example as a colorfast material with for example a red pigment extruded with the polypropylene material such that if the sheathing does become worn to the point that a hole develops, the color of the core member will show through as an indicator of a possible failure condition in the net. As seen in FIG. 10b, the mesh strands 37" can alternatively be formed from a twisted three strand DACRON rope with a polypropylene or nylon monofilament(s) 33,33 intertwined within the remaining twisted rope strands to enhance its strength.
In another alternative embodiment, the strands 37 of the safety net 10 take on a typical knotted structure of the type discussed with reference to the safety net shown in FIGS. 8a-c above, in that they are readily connectable to the border member 32 using the improved connection method employing flex C-ring fasteners 9,9, particularly because the knots 50,50 provide the locations of the attachment nodes aa and bb. In the present embodiment, the strands 37,37 are twisted and knotted in a conventional manner, but are however made from a single homogeneous material having properties which resist sagging and shrinkage relative to other materials that have previously been used in the art. Preferably, the material best suited to achieve these results is a twisted polyester DACRON rope made by Everson Cordage of Everson, Washington State. The configuration of mesh structures which employ material of this type are not limited to any particular design. That is, the mesh structure can take the form of either a square net type arrangement or a diamond design depending on the performance characteristics of the net.
Referring now to FIGS. 11 and 12, and as discussed previously with respect to FIG. 6 and the connection 40, it should be seen that the ends of rope can be lapp joined with a mechanical fastener, such as shown as 60 in FIGS. 13a-c, or, alternatively a single rope length can be doubled back on itself and then mechanically fastened in the manner shown in the illustrated embodiments of FIGS. 11 and 12. As shown in FIG. 11, two ropes 62 and 64 are interconnected using interconnected eye splices 66 and 68, respectively associated with each rope length. Each rope length has a doubled back portion 70, 72 which is passed through the fastener 60 and is secured against movement relative to the remaining rope length. For this purpose, the fastener 60, is illustrated in FIGS. 13a and 13b, is provided as a commercially available hour glass swedge having a hollow generally cylindric shape with an internal confine 74 provided for receiving the rope lengths. The fastener is made from a deformable material, such as brass or lead, and is die crimped onto the surrounded rope lengths. As shown in FIG. 12, a transverse rope connection is made between two orthogonally oriented twisted ropes 80 and 82 by causing the rope 80 to pierce the rope 82 at 86 and then to double back the piercing rope 80 onto itself so as to pass through the fastener 60 whereupon the fastener is crimped.
By the foregoing, a safety and debris net system has been discussed by way of illustration rather than by way of limitation. Numerous modifications and substitutions can be made without the departing from the spirit of the invention. For example, as shown in FIG. 10, in the mesh structure 36 of the safety net 10 could alternatively be formed from braided strands and/or chords which are braid at intersections, and/or formed from other materials, such as, nylon, attached to the border member 32 using the flex C-ring fasteners of the invention. Also, as used herein, the terms "right" and "left" are not used to limit the invention to specific orientations, but are used rather only to more easily describe the invention.
Accordingly, the invention has been described by way of illustration rather than limitation.
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The invention resides in an improvement in safety net system wherein the safety net is formed from an improved material which is resistant to weakening by ultraviolet radiation, hence does not need to be dyed or treated, and therefore is shrink and sag controlled. The invention further resides in a connection and method for making such connection between a safety net and a debris net for supporting same as a unit in an assembled condition and/or an improved connection between a border member of a safety net and its associated mesh.
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RELATED APPLICATIONS
The present application is a divisional of U.S. patent application Ser. No. 08/723,556, filed on Sep. 30, 1996, now abandoned entitled "CATALYST FOR HYDROGENATION OF LIVING POLYMER AND HYDROGENATION METHOD USING THE SAME", presently pending.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a catalyst for hydrogenation of living polymer. More particularly, to an organic titanium catalyst of homogeneous phase having high activity in a reaction in which unsaturated double bonds in conjugated diene units of living polymers are selectively hydrogenated. Also, the present invention is concerned with a method for hydrogenating living polymer, using the catalyst.
2. Description of the Prior Art
Copolymers of conjugated diene monomers, such as 1,3-butadiene and isoprene, with copolymerizable aromatic vinyl monomers, such as styrene, are widely used as elastomers. The block copolymers of conjugated diene monomer and aromatic vinyl monomer are thermoplastic elastomers and can be used as modifiers for polyolefin and polystyrene resins to prepare transparent resins having impact resistance. These copolymers can be vulcanized by the presence of olefinic double bonds in polymers, but have disadvantages that durability and resistance to oxidation against oxygen and ozone in atmosphere are lowered. Thus, such copolymers can be applied only within a limited range where they are not exposed to the air or the outside.
Generally, it can be achieved to improve durability and resistance to oxidation of such copolymers by hydrogenating the olefinic double bonds in the polymers partially or wholly saturating the double bonds.
Many methods for hydrogenation of polymers having olefinic double bonds have been reported. In general, they can be divided into two type methods: one using a heterogeneous catalyst of which metals, such as nickel, paladium, platinum, ruthenium, etc. are dispersed in supports, such as carbon, silica, aluminum, calcium carbonate, etc.; and the other using a homogeneous catalyst of Ziegler catalyst consisting of organic salts of nickel, cobalt, iron, chromium, titanium, or the like and reducing compound such as an organoaluminum or the like, or organometal compound, such as rhodium and titanium.
In the case of using the heterogeneous catalyst, hydrogenation is comprised of dissolving olefinic polymers in appropriate solvents and contacting with hydrogen in the presence of the heterogeneous catalyst. In this method, the contact between reactant and catalyst cannot easily be carried out owing to the steric hindrance and relatively high viscosity of polymer. Also, owing to the strong adsorption between polymer and catalyst, it is very difficult for other unsaturated polymers to access to the active point. For complete addition of hydrogen to the remaining unsaturated polymers, the hydrogenation reaction is required to be carried out at high temperature and at high pressure in the presence of a large amount of catalyst. Such conditions often result in the decomposition of the polymer and gelation thereof and, in the case of the copolymer of conjugated diene and aromatic vinyl monomer, saturation of the aromatic double bonds is simultaneously proceeded. It is therefore difficult to perform selective hydrogenation of olefinic polymer. In addition, it is very difficult for the catalyst to be physically separated from the hydrogenated polymer solution and some heterogeneous catalysts are virtually impossible to be completely removed due to their strong adsorption for the polymers.
In contrast with the heterogeneous catalyst, the homogeneous catalyst shows high activity in hydrogenation and thus, high hydrogenation yield is expected even with a small amount of catalyst under reaction conditions at a low temperature and a low pressure. In addition, hydrogenation can be selectively executed at the double bonds, exclusive of the aromatic moiety, in the copolymer of conjugated diene and aromatic vinyl hydrocarbon under appropriate hydrogenation conditions.
Hydrogenation or selective hydrogenation of conjugated diene polymers is described in many literatures.
U.S. Pat. Nos. 3,494,942, 3,634,594, 3,670,054 and U.S. Pat. No. 3,700,633 disclose use of catalysts containing metal of Periodic Table VIII group or precursors thereof for hydrogenation or selective hydrogenation of ethylenically unsaturated pwymers and ethylenically unsaturated polymers with aromatic groups. In said patents, metal of Periodic Table VIII group, especially, nickel or cobalt compound is formulated with a reducing agent, such as aluminum alkyl, to prepare useful catalyst. Also, there is described in the prior arts that aluminum alkyl is preferred reducing agent, but I-A, II-A and III-B group metals of Periodic Table, especially, lithium and magnesium alkyls or hydrides thereof are effective reducing agents. The mole ratio of I-A, II-A or III-B group metal to VIII group metal is in the range of 0.1:1 to 20:1 and preferably 1:1 to 10:1.
U.S. Pat. No. 4,501,857 suggests that the double bonds present in conjugated diene polymers can be selectively hydrogenated by hydrogenating the polymers in the presence of at least one of bis(cyclopentadienyl)titanium compounds and at least one of lithium hydrocarbon compounds.
U.S. Pat. No. 4,980,421 describes that alkoxy lithium compounds formulated with bis(cyclopentadienyl)titanium compounds and optionally at least one of reducing organometallic compound such as aluminium, zinc and magnesium compounds have analogous hydrogenation activity, wherein alkoxy lithium compounds could be directly added or be added as a reaction mixture of organic lithium compounds with alcoholic or phenolic compounds.
U.S. Pat. No. 4,673,714 showed that bis(cyclopentadienyl)titanium compounds could preferably hydrogenate the double bonds of conjugated diene without using alkyl lithium. It was mentioned that this titanium compound was bis(cyclopentadienyl)titanium diaryl compounds and that an advantage of this catalyst system is no use of lithium hydrocarbon compound.
U.S. Pat. No. 5,039,755 discloses a hydrogenation method in which conjugated diene monomers are polymerized or copolymerized with a polymerization initiator of organic alkali metal, to produce living polymers. The polymerization of the produced living polymer is terminated by adding hydrogen. The selective hydrogenation of the double bonds in conjugated diene units of the terminated polymer is carried out with (C 5 H 5 ) 2 TiR 2 (R=arylalkyl).
However, since the homogeneous catalyst appears that its hydrogenation activity is largely changed depending on the reduction state of the catalyst, it is difficult to obtain hydrogenated polymer having high yield and reproducibility. In addition, the active ingredients of the catalyst are tend to be changed into inactive ones by impurities in the reaction system. So, the impurities serve as a factor which lowers the reproducibility of the catalyst. Such inactivation of the homogeneous catalyst causes a serious problem in the hydrogenation of polymer for improving durability and resistance to oxidation.
In general, hydrogenation using homogeneous catalysts is not sufficiently rapid in hydrogenation rate and its activity depends on the reduction state of catalyst and impurities in the reaction system. Hence, the conventional homogeneous catalysts are problematic in applying the hydrogenation reaction of polymer on an industrial scale. Therefore, there has been strongly required a catalyst which is able to show high hydrogenation rate and produce highly hydrogenated polymer, without being affected by impurities of the reaction system and the preparation condition of catalyst.
The above-mentioned problems, however, cannot be solved by the catalysts suggested in the literatures and patents published thus far.
SUMMARY OF THE INVENTION
The above problems can be solved by using a catalyst comprising cyclopentadienyl titanium compound as main catalyst and alkoxy lithium compound as a cocatalyst according to the present invention. That is, the hydrogenated polymers can be prepared from living polymers which consists mainly of conjugated double bond monomers and aromatic vinyl monomers, in high hydrogenation rate and reproducibility, by using the catalyst, according to the present invention, having high activity and not being affected by impurities in the reaction system and the preparation conditions of catalyst.
Accordingly, it is an object of the present invention to provide a catalyst for hydrogenation of living polymers which consists mainly of conjugated double bond monomers and aromatic vinyl monomers, comprising cyclopentadienyl titanium compound, represented by the following general formula I as main catalyst: ##STR2## wherein R 1 , R 2 and R 3 may be the same or different and are independently selected from the group consisting of halogen groups, C 1 -C 8 alkyl groups, C 1 -C 8 alkoxy groups, C 6 -C 20 aryloxy groups, C 6 -C 20 cycloalkyl groups, silyl groups, and carbonyl groups; and alkoxylithium compound represented by the following general formula II as a cocatalyst:
R.sub.4 O--Li [II]
wherein R 4 is a hydrocarbon.
It is another object to provide a method for hydrogenating living polymers which consists mainly of conjugated double bond monomers and aromatic vinyl monomers, in which at least one of conjugated diene compound is polymerized or copolymerized in an inert solvent by using a polymerization initiator of organic alkali metal, to prepare a living polymer and the produced polymer is contacted with hydrogen in the presence of a catalyst comprising cyclopentadienyl titanium compound of the above formula I and alkoxylithium compound of the above formula II.
DETAILED DESCRIPTION OF THE INVENTION
By the hydrogenation catalyst according to the present invention can be selectively hydrogenated unsaturated double bonds in conjugated diene units of conjugated diene living polymers, and living copolymers or random or block copolymers of conjugated diene monomer and copolymerizable vinyl-substituted aromatic monomer, having molecular weight of 500 to 1,000,000. Without using a cocatalyst, hydrogenation occurs partially at 1,2-vinyl bond units but does not proceed at 1,4-butadiene units. Therefore, it is necessary to use the catalyst in combination with a cocatalyst to selectively hydrogenate the olefinic unsaturated double bonds in high yield. Preferably, the cocatalyst is an alkoxy lithium compound.
Ethylenically unsaturated and aromatically unsaturated polymers are prepared by homopolymerizing at least one of polyolefin, especially, diolefin or copolymerizing them with at least one of alkenyl aromatic hydrocarbon monomers, if necessary.
Copolymers may be not only of linear or radial type but also of random, tapered, block or any combination thereof.
Ethylenically unsaturated copolymers or ethylenically and aromatically unsaturated copolymers may be prepared by using an anionic initiator or polymerization catalyst, such as organolithium compound. The preparation of such polymers can be carried out by bulk, solution or emulsion technique. Conjugated dienes which can be polymerized in anionic type include conjugated dienes containing C 4 -C 12 carbon atoms, such as 1,3-butadiene, isoprene, pipenylene, phenylbutadiene, 3,4-dimethyl-1,3-hexadiene and 4,5-diethyl-1,3-octadiene, and preferably conjugated dienes containing C 4 -C 8 carbon atoms. Copolymerizable alkenyl aromatic hydrocarbons include vinyl aryl compounds, such as styrene, alkyl-substituted styrene, alkoxy-substituted styrene, 2-vinylpyridine, 4-vinylpyridine, vinylnaphthalene, and alkyl-substituted vinylnaphthalene.
In accordance with the present invention, the living polymer solution obtained by polymerizing conjugated diene monomers in an inert solvent is used, in hydrogenation as such. Therefore, the hydrogenation is succesively carried out. Herein, the term of living polymer means a polymer having activity in terminal. The inert solvent is a solvent which does not react with any reactants for polymerization or hydrogenation, at all, and is preferably exemplified by aliphatic hydrocarbons, such as n-pentane, n-hexane, n-heptane, n-octane and the like, cyclic hydrocarbons, such as cyclohexane, cycloheptane and the like, and ethers, such as diethyl ether, tetrahydrofuran and the like, and the mixtures thereof. Aromatic hydrocarbons, such as benzene, toluene, xylene and ethylbenzene, can be employed, which do not allow the double bonds of the aromatic moieties to be saturated with hydrogen under selected hydrogenation conditions.
The hydrogenation of the present invention is carried out with a living polymer concentration of 1 to 50% by weight based on the total weight of the solvent and preferably with a living polymer concentration of 5 to 25% by weight. Particularly, it is necessary that the living polymer provided for hydrogenation is not inactivated by the moisture or impurities in the solution.
In accordance with the present invention, hydrogenation is carried out by maintaining a living polymer solution at a certain temperature under a hydrogen or inert atmosphere, adding hydrogenation catalyst with or without stirring and providing hydrogen gas at a constant pressure. Herein, the inert atmosphere means one which does not react with any reactants for hydrogenation at all, including helium, nitrogen, argon and the like. Air or oxygen is not so desirable that hydrogenation catalyst may be oxidized or decomposed to result in lowering catalyst activity. Organic titanium compound and alkoxy lithium compound are mixed with each other in a suitable solvent under an inert atmosphere to prepare catalyst and then catalyst is introduced into a reactor. The mixing mole ratio of alkoxy lithium to titanium is preferably in the range of 1 to 3. For example, if the mole ratio of alkoxy to titanium is less than 1, the catalyst has not so sufficient activity as to occur effective hydrogenation in mild conditions. On the other hand, if the mole ratio of alkoxy lithium to titanium is over 3, the activity is not outstandingly increased. On the contrary, it is disadvantageous in view of economics to use alkoxy lithium excessively. In effecting hydrogenation on the living polymer according to the present invention, the mole ratio of reducing lithium to titanium in the living polymer is advantageously in the range of 2:1 to 10:1. Thus, hydrogenation catalyst must be maintained in an amount of 0.05-5 mmol per 100 g of living polymer, in order to maintain the ratio of lithium to titanium of 1 to 10.
Generally, hydrogenation is performed at a temperature of 0 to 150° C. For example, at less than 0° C., catalyst for hydrogenation comes to have low activity, resulting in a decrease of hydrogenation rate. In this case, a large quantity of catalyst is therefore needed, causing an economical loss and lowering the solubility of the hydrogenated polymer. Thus, it is easy to be deposited. On the other hand, at temperatures more than 150° C., the catalyst is also inactivated and the polymer is subjected to gelation or decomposition. In addition, since a hydrogenation can easily occur at the double bonds of aromatic moieties at high temperatures, hydrogenation selectivity is lowered. Preferred reaction temperature ranges from 50 to 140° C.
A particular limit is not given to the pressure of hydrogen used for hydrogenation. Typically, hydrogenation is performed under a hydrogen pressure of 1-100 kg/cm 2 . For example, if hydrogen pressure is below 1 kg/cm 2 , hydrogenation rate is low. On the other hand, a hydrogen pressure of higher than 100 kg/cm 2 causes gelation as a side-reaction. Thus, the preferred hydrogen pressure is 2 to 30 kg/cm 2 , and the optimal hydrogen pressure is selected in consideration of the hydrogenation conditions including the amount of the catalyst. In general, when an amount of hydrogenation catalyst is low, it is preferred that higher pressure is selected.
In the presence of the hydrogenation catalyst of the present invention, the hydrogenation is performed for a period of from several seconds to, in extreme cases, five hundred hours. Within this range, the reaction time of hydrogenation may be selected depending on the change of hydrogenation conditions.
Any process type, for example, batch type, continuous type or any combination thereof can be employed to proceed the hydrogenation using the catalyst of the present invention and the progress state of hydrogenation can be identified by determining the absorption amount of hydrogen.
In accordance with the present invention, it is possible to obtain hydrogenated polymers in which more than 50%, preferably 90%, of unsaturated double bonds in conjugated diene units of polymers are hydrogenated. More preferably, when copolymers of conjugated diene monomers and vinyl-substituted aromatic hydrocarbons are hydrogenated, it is also possible to obtain hydrogenated copolymer in which hydrogenation yield is at least 90% for the conjugated diene unit and simultaneously not more than 10% for the aromatic double bonds.
After completing hydrogenation, the hydrogenated polymer can be easily isolated, if necessary, by removing catalyst residue from the polymer solution. For example, a polar solvent, such as acetone or alcohol, is added to the polymer solution to precipitate the polymer, the solution is placed in a hot bath and stirred to separate polymer from solvent, or reaction solution is directly heated to vaporize solvent.
As described hereinbefore, based on the present invention, it is possible to hydrogenate conjugated diene polymer under a mild condition in the presence of a highly active catalyst, especially to selectively hydrogenate unsaturated double bonds in conjugated diene units of copolymer consisting of conjugated diene and vinyl-substituted aromatic hydrocarbon. Particularly, the present invention has several economical advantages which are very useful for industrial application. For example, since living polymers are used as materials, hydrogenation is continuously executed in the same reactor. In addition, the hydrogenation catalyst of the present invention has very high activity so that it may be added in small amounts. Further, no deashing process is required after hydrogenation.
A better understanding of the present invention may be obtained in light of following examples which are set forth to illustrate, but are not to be construed to limit, the present invention.
Hydrogenation was carried out in the presence of a cocatalyst in Examples, while it was carried out without using the cocatalyst in Comparative Example.
SYNTHESIS EXAMPLE I
In a 2 gallon autoclave reactor, 4,500 g of cyclohexane was placed. 9 g of tetrahydrofuran, 112.5 g of styrene monomer and 1.6 g of n-butyllithium were charged into the reactor and then the reaction mixture was subjected to polymerization for 1 hour. Thereafter, 525 g of 1,3-butadiene monomer were injected into the reactor to polymerize for one hour. Finally, 112.5 g of styrene monomer was added and then polymerized for one hour to obtain styrene-butadiene-styrene living block copolymer with a number average molecular weight of about 60,000 which had a styrene content of 30.54% (block styrene content of 30.3%) and 1,2-vinyl bond content of 39.80% (27.8% when reduced into whole polymer). Living lithium in the polymer was present in an amount of 1.67 mmol per 100 g of polymer.
SYNTHESIS EXAMPLE II
In a 2 gallon autoclave reactor, 4,500 g of cyclohexane was placed. 9 g of tetrahydrofuran, 112.5 g of styrene monomer and 1.7 g of n-butyllithium were charged into the reactor and then the reaction mixture wsa subjected to polymerization for 1 hour. Thereafter, 525 g of 1,3-butadiene monomer were injected into the reactor to polymerize for one hour. Finally, 112.5 g of styrene monomer was added and then polymerized for one hour to obtain styrene-butadiene-styrene living block copolymer with a number average molecular weight of about 50,000 which had styrene content of 30.87% (block styrene content of 30.1%) and 1,2-vinyl bond content of 41.31% (28.9% when reduced into whole polymer). Living lithium in the polymer was present in an amount of 2.00 mmol per 100 g of polymer.
SYNTHESIS EXAMPLE III
In a 2 gallon autoclave reactor, 4,500 g of cyclohexane was placed. 9 g of tetrahydrofuran, 112.5 g of styrene monomer and 1.3 g of n-butyllithium were charged into the reactor and then the reaction mixture was subjected to polymerization for 1 hour. Thereafter, 525 g of 1,3-butadiene monomer was injected into the reactor to polymerize for one hour. Finally, 112.5 g of styrene monomer was added and then polymerized for one hour to obtain styrene-butadien-styrene living block copolymer with a number average molecular weight of about 100,000 which had a styrene content of 29.9% (block styrene content of 29.5%) and 1,2-vinyl bond content of 39.6% (27.9% when reduced into whole polymer). Living lithium in the polymer was present in an amount of 1.00 mmol per 100 g of polymer.
SYNTHESIS EXAMPLE IV
In a 2 gallon autoclave reactor, 4,500 g of cyclohexane was placed. 9 g of tetrahydrofuran and 1.5 g of n-butyllithium were charged into the reactor, followed by simultaneously injecting 225 g of styrene monomer and 525 g of 1,3-butadiene monomer into the reactor to polymerize for 1 hour. As a result, styrene-butadiene-styrene living block copolymer with a number average molecular weight of about 50,000 was obtained in which the styrene content amounted to 29% and 1,2-vinyl bond content to 30.5% (21.4% when reduced into whole polymer). Living lithium in the polymer was present in an amount of 1.6 mmol per 100 g of polymer.
COMPARATIVE EXAMPLE I
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example I was poured and heated to 90° C. with shaking at 450 rpm. Simultaneously, 0.6 mmol of cyclopentadienyl titanium trichloride dissolved in 10 ml of tetrahydrofuran was added in the reactor. Then, the pressure of reactor was risen with 10 kg/cm 2 of hydrogen pressure to hydrogenate for 3 hours. After completion of the reaction, the reactor was cooled and lowered to the ambient pressure and the reaction solution was poured in a water-vapor mixture solution.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 44% for the whole polymer, 95% for 1,2-vinyl bond unit and 5% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE I
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example I was poured and heated to 90° C. with shaking at 450 rpm. 0.3 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 0.5 to react for one hour at room temperature, and then, the reactants were added in the reactor. Then, the pressure of reactor was risen with 10 kg/cm 2 of hydrogen pressure to hydrogenate for 3 hours. After completion of the reaction, the reactor was cooled and lowered to the ambient pressure and the reaction solution was poured in a water-vapor mixture solution.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 60% for the whole polymer, 95% for 1,2-vinyl bond unit, and 35% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE II
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example I was poured. Under the same conditions as those in Example I, 0.6 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 1 to react for one hour at room temperature. Thereafter, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 99% for the whole polymer, 100% for 1,2-vinyl bond unit, and 98% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE III
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example I was poured. Under the same conditions as those in Example I, 1.2 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 2 to react for one hour at room temperature. Thereafter, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 99% for the whole polymer, 100% for 1,2-vinyl bond unit, and 98% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE IV
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example I was poured. Under the same conditions as those in Example I, 1.2 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.4 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 3 to react for one hour at room temperature. Thereafter, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 97% for the whole polymer, 100% for 1,2-vinyl bond unit, and 95% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE V
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example II was poured. Under the same conditions as those in Example I, 0.6 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 1 to react for one hour at room temperature. Following this, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 100% for the whole polymer, 100% for 1,2-vinyl bond unit, and 100% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE VI
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example II was poured. Under the same conditions as those in Example I, 1.2 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 2 to react for one hour at room temperature and then, added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 99% for the whole polymer, 100% for 1,2-vinyl bond unit, and 98% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE VII
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example I was poured. Under the same conditions as those in Example II, 1.8 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 3 to react for one hour at room temperature. The resulting reaction was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 99% for the whole polymer, 100% for 1,2-vinyl bond unit, and 98% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE VIII
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example III was poured. Under the same conditions as those in Example I, 0.5 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.5 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 1 to react for one hour at room temperature. Thereafter, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 97% for the whole polymer, 100% for 1,2-vinyl bond unit, and 95% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE IX
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example IV was poured. Under the same conditions as those in Example I, 0.6 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 1 to react for one hour at room temperature. Thereafter, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 99% for the whole polymer, 100% for 1,2-vinyl bond unit, and 98% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE X
In a one gallon autoclave reactor 1,050 g of the solution of 14.3 percent by weight living polymer solution obtained in Synthesis Example II was poured. Under the same conditions as those in Example I, 0.6 mmol of 2,6-di-tertiary-butyl-4-methylphenol lithium and 0.6 mmol of cyclopentadienyl titanium trichloride were dissolved in 10 ml of tetrahydrofuran in such a way that the mole ratio of alkoxylithium to titanium might be 1 to react for one hour at room temperature. Thereafter, the resulting solution was added in the reactor.
H-NMR of the resulting hydrogenated polymer revealed that the yield of hydrogenation was 99% for the whole polymer, 100% for 1,2-vinyl bond unit, and 98% for 1,4-butadiene unit. No hydrogenation occurred in styrene moieties.
EXAMPLE XI to XVI
In these examples, the effect of various cocatalysts, i.e. alkoxy lithium compounds, was investigated by using the hydrogenation procedure under the same conditions as those in Example I and the living polymer solution obtained in Synthesis Example II. Table 1 below shows kinds and amounts of the catalyst and cocatalysts as used, the RO-Li/Ti ratio, and the degree of hydrogenation.
TABLE 1______________________________________Example XI XII XIII XIV XV XVI______________________________________Catalyst Cyclopentadienyl titanium trichlorideCocatalyst 4-methylphenoxy 4-tert- 4-octyl- lithium butyl- phenoxy phenoxy lithium lithiumAmount of 0.4 0.3 0.32 0.2 0.3 0.3 catalyst, mmol/100 g of polymer Amount of 0.8 0.8 0.7 0.4 0.6 0.8 cocatalyst, mmol RO--Li/Ti 1 1.33 1.09 1 1 1.33 Degree of 96.2 94.8 98.0 89.3 97.3 98.0 hydrogenation______________________________________
Other features, advantages and embodiments of the present invention disclosed herein will be readily apparent to those exercising ordinary skill after reading the foregoing disclosures. In this regard, while specific embodiments of the invention have been described in considerable detail, variations and modifications of these embodiments can be effected without departing from the spirit and scope of the invention as described and claimed.
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A method for hydrogenating living polymers that include mainly conjugated double bond monomers and aromatic vinyl monomers. At least one conjugated diene compound is polymerized or copolymerized in an inert solvent by using a polymerization initiator of organic alkali metal. The produced polymer is contacted with hydrogen in the presence of a catalyst. The catalyst is formed of a cyclopentadienyl titanium compound represented by: ##STR1## wherein R 1 , R 2 and R 3 are independently selected from halogen groups, C 1 -C 8 alkyl groups, C 1 -C 8 alkoxy groups, C 6 -C 20 aryloxy groups, C 6 -C 20 cycloalkyl groups, silyl groups, and carbonyl groups. A cocatalyst is provided of alkoxylithium compound represented by:
R.sub.4 O--Li
wherein R 4 is a hydrocarbon. This cocatalyst selectively hydrogenates the unsaturated double bonds in the conjugated diene units of the living polymer.
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BACKGROUND OF THE INVENTION
The present invention relates to a plastic screw cap with tamper-evident ring.
Caps of the above type are already known commercially and comprise a cylindrical cup which is internally threaded in order to be screwed onto the top of the container (bottle).
A so-called tamper-evident ring is coupled to the rim of the cup by means of breakable bridges and is internally provided with engagement elements constituted by flaps or by a collar which, when the cap is applied so as to close the container, engage under an annular raised retention portion of the container. By unscrewing the cap, the flaps or the collar abut against the annular raised portion and retain the ring, while the resulting axial traction force breaks the bridges.
Conventional caps entail the problem of ensuring that during application to the container the flaps or collar can widen or otherwise be elastically deformed in order to pass over the raised retention portion of the bottle and then close again below said raised portion, so as to allow the separation of the tamper-evident ring during the unscrewing of the cap and clearly indicate that the container has been opened.
However, in currently commercially available caps the tamper-evident ring, in order to ensure that the teeth or collar remain engaged below the annular raised portion of the container during unscrewing and can thus ensure the breaking of the bridges, has an excessively rigid structure and therefore passing over the raised portion when the cap is applied to the container is critical.
SUMMARY OF THE INVENTION
The aim of the present invention is to provide a plastic cap which is capable of substantially obviating the shortcomings of conventional caps.
This aim is achieved by a plastic screw cap of the type composed of a cylindrical cup provided with an internal thread and with a tamper-evident ring which is coupled to the rim of the cup by means of a plurality of bridges forming a fracture line, said ring having a retention means for retaining it below an annular raised portion of a container whereto the cap is applied, incisions being formed on the outside of said tamper-evident ring, said incisions do not cross the entire thickness of the ring and allow an elastic radial expansion of the ring, such as to pass beyond said annular raised portion during the application of the cap to the container.
BRIEF DESCRIPTION OF THE DRAWINGS
Further characteristics and advantages of the present invention will become apparent from the following detailed description, on the basis of the accompanying drawings, wherein:
FIG. 1 is a perspective view of a cap provided with a tamper-evident ring, whose outside diameter is smaller than the diameter of the cup, and with an internal annular expansion provided with retention flaps;
FIG. 2 is a partially sectional view, taken along an axial plane, of the screw cap of FIG. 1;
FIG. 3 is an enlarged-scale view of a detail of FIG. 2;
FIG. 4 is a partially sectional view, taken along an axial plane, of the cap in the position for application to a container;
FIG. 5 is a partially sectional view, taken along an axial plane, of a variation of the cap;
FIG. 6 is an enlarged-scale view of the cross-section of the tamper-evident ring of the cap of FIG. 5;
FIG. 7 is a partially sectional view of another variation of the cap;
FIG. 8 is an enlarged-scale view of the cross-section of the tamper-evident ring of the cap of FIG. 7;
FIG. 9 is a partially sectional view of another variation of the cap;
FIG. 10 is an enlarged-scale view of the cross-section of the tamper-evident ring of the cap of FIG. 9;
FIGS. 11 and 12 are partially sectional views, taken along an axial plane, of the cap according to two further variations;
FIGS. 13 to 15 are partially sectional views, taken along an axial plane, of three variations of a cap provided with a tamper-evident ring, whose outside diameter is equal to the outside diameter of the cup, and with an internal retention collar.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to FIGS. 1, 2 and 3 , the reference numeral 1 generally designates a cap according to the present invention, formed by molding plastics according to conventional methods. The cap 1 comprises a cylindrical cup 2 which is composed of a bottom 3 , which is internally covered by a liner 4 , and of a cylindrical wall 5 inside which a thread 6 is formed.
A tamper-evident ring 7 protrudes from the rim of the cylindrical wall 5 of the cup 2 and is composed of a cylindrical wall whose rim is connected to the rim of the cup 2 by means of a plurality of bridges 8 which are spaced by slits 9 . The bridges 8 and the slits 9 form a fracture line which allows to separate the tamper-evident ring 7 from the cup 2 when the cap is unscrewed from the container whereto it has been applied.
The opposite rim of the ring 7 is internally provided with an annular expansion 10 , whose inside diameter is substantially equal to the inside diameter of the wall 5 . The bridges 8 and the slits 9 can be provided in any manner, for example during the molding of the cap by providing suitable mold shapes or by means of cutting operations performed after molding.
A connecting region is formed between the rim of the cup 2 and the expansion 10 and is constituted by a wall 11 whose outside diameter is smaller than the outside diameter of the wall 5 and whose inside diameter is greater than the inside diameter of the expansion 10 , so that the wall 11 is significantly thinner than the wall 5 of the cup. This difference in thickness allows the wall 11 , by exploiting the elasticity of the plastics material, to follow any widening occurring during the application of the cap to a container and to assume a conical shape which tapers toward the bottom 3 of the cup 2 , as occurs for example during application to a container.
From the above description it is thus evident that the expansion 10 is significantly thicker than the wall 11 and protrudes from the inner face thereof, so that the inside diameter of the expansion 10 is significantly smaller than the inside diameter of the wall 11 .
The greater thickness of the annular expansion 10 ensures that said expansion has, in relation to the elasticity of the plastics material the cap is made of, a reduced ability to widen with respect to the wall 11 .
The difference in inside diameter between the expansion 10 and the wall 11 forms a steplike connecting region, wherefrom multiple flaps 12 protrude toward the inside of the cup 2 ; said flaps are inclined toward the bottom 3 of the cup at a preset angle. The flaps 12 are equidistant and mutually separated by spaces 13 and their thickness is preferably greater than the thickness of the wall 11 but smaller than the thickness of the expansion 10 . Moreover, the upper and lower faces of the flaps 12 are connected to the internal faces of the wall 11 and of the expansion 10 by radiused regions 14 and 15 .
The different thickness of the wall 11 , of the expansion 10 and of the flaps 12 causes on the one hand easier application of the cap to a container 16 (shown in dashed lines in FIG. 4) and, on the other hand, firmer retention of the tamper-evident ring 7 below the annular raised portion 17 of the container 16 whereto the cap 1 is applied and, ultimately, safer separation thereof when the cap is unscrewed.
However, the greater thickness of the annular expansion 10 constitutes a considerable critical point in the application of the cap to the container. Indeed, when applying the cap, due to the lower elasticity of the expansion 10 the contrast to the widening of the thinner region of the wall 11 which is close to the expansion 10 can cause the bridges 8 to break.
According to an important aspect of the present invention, this drawback can be obviated with surprisingly positive results by providing a plurality of incisions 18 which are distributed along the outer peripheral region of the tamper-evident ring 7 and affect the region of the expansion 10 . Said incisions 18 have an axial orientation and do not pass through the thickness of the expansion. In this manner, when the cap is applied to the container 16 , the radial expansion of the tamper-evident ring 7 is facilitated by the opening of the score lines 18 in a circumferential direction (see FIG. 4 ), which by entailing an increase in the diameter of the expansion allow the tamper-evident ring 7 to slide above the annular raised portion 17 of the container below which it must engage.
It should be observed that since the incisions 18 are not through cuts, they do not compromise the strength of the expansion 10 and therefore the engagement of the flaps 12 below the annular raised portion 17 of the container.
The number of the incisions 18 is chosen as a function of the greater flexibility to be given to the tamper-evident ring 7 .
It should be observed that the ability of the tamper-evident ring 7 to expand radially is limited so that the tamper-protection of the container is not compromised. Moreover, the greater flexibility of the tamper-evident ring and the reduced stresses whereto the bridges 8 are subjected during the application of the cap allow to reduce the thickness of the bridges and therefore to facilitate their breakage when the cap is unscrewed.
In its practical embodiment, the cap according to the present invention is susceptible of numerous modifications and variations, all of which are within the scope of the same inventive concept.
FIGS. 5 and 6 are views of an embodiment in which instead of the axial incisions a circumferential incision 19 is provided in the outer face of the wall 11 , arranged between the fracture line formed by the slits 9 and the expansion 10 . It is of course possible to combine axial incisions 18 with a circumferential incision 19 , as provided in the embodiment of FIGS. 7 and 8. In particular, it should be observed that the axial incisions can partially extend into the wall 11 as well and join the circumferential incision 19 .
FIGS. 9, 11 and 12 relate to the application of the inventive concept to a cap in which the tamper-evident ring 7 is not provided with the annular expansion 10 and retention of the cap on the container is achieved with a continuous internal collar 20 instead of with flaps 12 . Advantageously, the axial incisions 18 , as shown in FIG. 10, affect the region of the collar 20 and continue into the wall 11 . FIGS. 13 to 15 illustrate a cap according to still a further aspect of the invention, wherein the tamper-evident ring has an outside diameter which is equal to that of the cup 2 . In this case also, the axial incisions 18 can continue into the wall 11 . In the practical embodiment of the invention, the incisions 18 , 19 can be formed during molding. However, said incisions are preferably formed by means of a cutting machine provided with a blade which allows to precisely adjust the depth of the incisions.
The disclosures in Italian Patent Application No. BO98A000296 from which this application claims priority are incorporated herein by reference.
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A plastic screw cap includes a cylindrical cup provided with an internal thread and with a tamper-evident ring which is coupled to the rim of the cup by means of a plurality of bridges forming a fracture line; the ring has a collar or expansion for retaining it below an annular raised portion of a container whereto the cap is applied. Incisions are formed on the outside of the tamper-evident ring, the incisions do not cross the entire thickness of the ring and allow an elastic radial expansion of the ring, such as to pass beyond the annular raised portion during the application of the cap to the container.
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BACKGROUND OF INVENTION
The present invention relates to a novel and industrially advantageous process for the preparation of azide derivatives useful as drugs, perfumes or intermediates of dyes.
PRIOR ART
Up to this time, azide derivatives have been prepared by the reaction of sodium azide with halides, sulfonyl esters or phosphate esters.
Meanwhile, a process of directly reacting various alcohols with diphenyl phosphorazidate in the presence of 1,8-diazabicyclo[5.4.0]-7-undecene has been disclosed in WO-95/01970 as a process of converting alcohols into azides not through halides or the like.
However, the above process of reacting sodium azide with a halide or the like had problems that the operation had to be conducted extremely carefully due to the explosiveness of sodium azide used as the raw material, that the yields of the azides derived from secondary alcohols were low, and that the stereoselectivity of the reaction was poor.
The process disclosed in WO-95/01970 was still problematic in that the yields of azides derived from secondary alcohols were low, though it was freed from the problem of safeness of sodium azide and that of poor stereoselectivity.
As described above, an industrially satisfactory process for the preparation of azide derivatives has not been established yet, so that the development of a novel and more advantageous process has been expected.
The inventors of the present invention have intensively studied to solve the above problems. As a result of these studies, they have found that the objective azide derivatives can be prepared in high yields and at high stereoselectivity by the reaction with di-p-nitrophenyl phosphorazidate in the presence of 1,8-diazabicyclo[5.4.0]-7-undecene. The present invention has been accomplished on the basis of this finding.
SUMMARY OF INVENTION
The present invention will now be described in detail.
The present invention relates to a process for the preparation of an azide derivative (II) from an alcohol derivative (I) as represented by the following reaction formula characterized by reacting an alcohol derivative (I) with di-p-nitrophenyl phosphorazidate in the presence of 1,8-diazabicyclo[5.4.0]-7-undecene. ##STR1## wherein R is a group represented by the following general formula: ##STR2## (wherein R 1 is hydrogen, lower alkyl or lower alkoxycarbonyl; R 2 is linear or branched alkyl, linear or branched alkenyl, linear or branched alkynyl, alkoxyalkyl, alkoxycarbonylalkyl, cyanoalkyl, optionally substituted aryl, optionally substituted aralkyl, optionally substituted heteroaryl, optionally substituted heteroarylalkyl, allyl or optionally substituted arylallyl; and R 3 is hydrogen, lower alkyl, lower alkenyl, lower alkoxycarbonyl or optionally substituted aralkyl), a C 3 -C 8 cycloalkyl group optionally substituted with lower alkyl or lower alkoxycarbonyl, a C 3 -C 8 cycloalkenyl group optionally substituted with lower alkyl or lower alkoxycarbonyl, a saccharide residue wherein part of the hydroxyl groups are protected, or a C 3 -C 8 cycloalkyl group fused with an aromatic ring which is optionally substituted.
The term "lower alkyl" used in the above definition of R 1 in the general formula (I) or (II) refers to a C 1 -C 6 alkyl group, and examples thereof include methyl, ethyl, n-propyl, i-propyl, n-butyl, i-butyl, t-butyl, n-pentyl, i-pentyl, t-pentyl, neopentyl and hexyl.
The term "lower alkoxycarbonyl" used therein refers to an alkoxycarbonyl group wherein the alkoxy moiety is a C 1 -C 6 lower alkoxy group selected from among methoxy, ethoxy, n-propoxy, i-propoxy, n-butoxy, i-butoxy, t-butoxy, pentyloxy, hexyloxy and the like. Specific examples of such an alkoxycarbonyl group include methoxycarbonyl, ethoxycarbonyl, propoxycarbonyl and hexyloxycarbonyl, though the lower alkoxycarbonyl group is not limited to these groups.
The term "linear or branched alkyl" used in the definition of R 2 refers to an alkyl group having at most 50 carbon atoms, i.e., any of methyl to pentacontanyl groups, which may have more than one branch therein.
The term "linear or branched alkenyl" refers to an alkenyl group having at most 50 carbon atoms, i.e., vinyl or any of propenyl to pentacontaenyl groups, which may have more than one double bond or branch therein.
The term "linear or branched alkynyl" refers to an alkynyl group having at most 50 carbon atoms, i.e., ethynyl or any of propynyl to pentacontynyl groups, which may have more than one triple bond or branch therein.
The term "alkoxyalkyl" refers to a linear or branched C 3 -C 50 alkyl group as described above which has a C 1 -C 6 lower alkoxy group therein. Specific examples thereof include methoxypropyl, ethoxypropyl, methoxybutyl, ethoxybutyl, propoxypentyl and hexyloxypentacontanyl, though the alkoxyalkyl group is not limited to these groups.
The term "cyanoalkyl" refers to a linear or branched C 1 -C 50 alkyl group having a cyano group therein. Specific examples thereof include cyanopropyl, cyanobutyl, cyanopentyl, cyanohexyl and cyanopentacontanyl, though the cyanoalkyl group is not limited to these groups.
The term "optionally substituted aryl" refers to phenyl, naphthalenyl or the like, which may be substituted with halogeno, lower alkyl, lower alkoxy, cyano, nitro, amino or the like.
The term "optionally substituted aralkyl" refers to benzyl, phenethyl or the like, which may be substituted with halogeno, lower alkyl, lower alkoxy, cyano, nitro, amino or the like.
The term "optionally substituted heteroaryl" refers to pyridyl, pyrazinyl, pyrimidyl, furanyl, pyrrolyl, thienyl, thiazolyl or the like, which may be substituted with halogeno, lower alkyl, lower alkoxy, cyano, nitro, amino or the like.
The term "optionally substituted heteroarylalkyl" refers to pyridylmethyl, pyrazinylethyl, pyrimidylpropyl, furanylbutyl, pyrrolylpentyl, thienylhexyl or the like, which may be substituted with halogeno, lower alkyl, lower alkoxy, cyano, nitro, amino or the like.
The term "allyl" refers to a group represented by the formula: CH 2 ═CHCH 2 --.
The term "optionally substituted arylallyl" refers to allyl substituted with an optionally substituted aryl group as described above, for example, cinnamyl.
The term "a C 3 -C 8 cycloalkyl group optionally substituted with lower alkyl or lower alkoxycarbonyl" refers to cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, cyclooctyl or the like, which may be substituted with the above lower alkyl or lower alkoxycarbonyl.
The term "a C 3 -C 8 cycloalkenyl group optionally substituted with lower alkyl or lower alkoxycarbonyl" refers specifically to cyclopropylenyl, cyclobutylenyl, cyclopentenyl, cyclohexenyl, cycloheptenyl, cyclooctenyl or the like, which may be substituted with the above lower alkyl or lower alkoxycarbonyl.
The term "a saccharide residue wherein part of the hydroxyl groups are protected" refers to a monosaccharide (such as ribose, xylose, glucose, galactose or mannose), disaccharide (such as sucrose or lactose), or other oligosaccharide wherein at least one hydroxyl group remains in a free state and the other hydroxyl groups are protected with hydroxyl-protective groups conventionally used in organic syntheses. Preferable examples of the protective group include acetyl, benzoyl, benzyl, dimethylketal residue (isopropylidene) and phenylacetal residue (benzylidene), though the protective group may be any one inert to the reaction according to the present invention.
The term "a C 3 -C 8 cycloalkyl group fused with an aromatic ring which is optionally substituted" includes indanyl, tetrahydronaphthyl, benzocycloheptyl, benzocyclooctyl and tetrahydroanthryl, which may be each substituted with lower alkyl, lower alkoxy, halogeno, lower haloalkyl or the like on the aromatic ring.
In the present invention, 1,8-diazabicyclo[5.4.0]-7-undecene, CAS Registry No. 6674-22-2, and di-p-nitrophenyl phosphorazidate, CAS Registry No. 51250-91-0, are used, which are both known compounds and commercially available as reagents or industrial chemicals. Further, the latter can also be prepared according to the process disclosed in JP-A 48-80545, JP-A 48-67202 or the like.
DETAILED DESCRIPTION OF INVENTION
The present invention can be carried out as follows.
The order of addition of the alcohol derivative (I), 1,8-diazabicyclo[5.4.0]-7-undecene, and di-p-nitrophenyl phosphorazidate is not limited. In other words, the three compounds may be mixed at once, or two of the compounds may be premixed, followed by the addition of the remainder. In order to attain a higher yield and a higher stereoselectivity, however, it is preferable that 1,8-diazabicyclo[5.4.0]-7-undecene be added to a mixture of the alcohol derivative (I) with di-p-nitrophenyl phosphorazidate.
The amount of di-p-nitrophenyl phosphorazidate to be used is generally 1.0 to 10 equivalents, preferably 1.05 to 5 equivalents, still preferably 1.1 to 2 equivalents per equivalent of the alcohol derivative (I), though the amount is not limited.
The amount of 1,8-diazabicyclo[5.4.0]-7-undecene to be used is generally 1.0 to 10 equivalents, preferably 1.05 to 5 equivalents, still preferably 1.1 to 2 equivalents per equivalent of the alcohol derivative (I), though the amount is not limited.
The reaction may be conducted in the presence of a solvent since the use of a solvent is effective in facilitating the control of reaction temperature. The solvent usable in the present invention is not limited, but may be any one inert to the alcohol derivative (I), 1,8-diazabicyclo[5.4.0]-7-undecene and di-p-nitrophenyl phosphorazidate. Examples thereof include benzene, toluene, xylene, petroleum benzine, pentane, hexane, petroleum ether, diethyl ether, diisopropyl ether, t-butyl methyl ether, tetrahydrofuran (hereinafter abbreviated to "THF"), dioxane, dioxolane, ethylene glycol dimethyl ether, chloroform, methylene chloride, 1,2-dichloroethane, acetonitrile, ethyl acetate, butyl acetate, N,N-dimethylformamide (hereinafter abbreviated to "DMF"), 1-methyl-2-pyrrolidone, dimethyl sulfoxide (hereinafter abbreviated to "DMSO") and hexamethylphosphoramide (hereinafter abbreviated to "HMPA"), among which toluene, THF and DMF are preferable.
The amount of the solvent to be used is generally 0 to 100 ml, preferably 0.5 to 50 ml, still preferably 1 to 20 ml per gram of the alcohol derivative (I), though it is not limited.
The reaction temperature is not limited, though it may be generally up to the reflux temperature of the solvent used. Specifically, it may be selected within the range of -78 to 150° C., preferably -50 to 100° C., still preferably -30 to 50° C., in accordance with the reactivity of the starting compound.
Although the reaction time depends on the amount of the solvent used, reaction temperature and so on, the reaction is generally completed within 24 hours. After the completion of the reaction, water is added to the reaction mixture and the resulting mixture is left standing to cause phase separation; and the recovered organic phase is suitably subjected to water washing, drying and/or concentration and thereafter purified conventionally by recrystallization, various column chromatography, distillation or the like.
Examples and Comparative Examples will now be described to explain the present invention specifically, though it is needless to say that the present invention is not limited by them.
EXAMPLE
Example 1
Synthesis of 1-azidodecane ##STR3##
To a solution of 1.58 g (10 mmol) of 1-decanol in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 16 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.40 g of the title compound as a colorless liquid (yield: 76%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 3.25(2H,t,J=6.8 Hz), 1.60(2H,tt,J=7.2,6.8 Hz), 1.22-1.40(14H,m), 0.88(3H,t,J=7.2 Hz). IRν max(neat); 2927, 2856, 2096, 1466, 1261 cm -1 .
Example 2
Synthesis of 2-azidodecane ##STR4##
To a solution of 1.58 g (10 mmol) of 2-decanol in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 50° C. for 6 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.49 g of the title compound as a colorless liquid (yield: 81%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 3.41(1H,tq,J=6.8,6.4 Hz), 1.24(3H,d,J=6.4 Hz), 1.23-1.56(14H,m), 0.88(3H,t,J=7.2 Hz). IRν max(neat); 2927, 2856, 2099, 1465, 1248 cm -1 .
Example3
Synthesis of 3-azidodecane ##STR5##
To a solution of 1.58 g (10 mmol) of 3-decanol in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 50° C. for 6 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.59 g of the title compound as a colorless liquid (yield: 87%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 3.18(1H,tt,J=7.6,6.4 Hz), 1.22-1.63(14H,m), 0.98(3H,t,J=7.6 Hz), 0.89(3H,t,J=6.8 Hz). IRν max(neat); 2929, 2857, 2096, 1463, 1273 cm -1 .
Example 4
Synthesis of (S)-(+)-2-azidooctane ##STR6##
To a solution of 1.30 g (10 mmol) of (R)-(-)-2-octanol (e.e. (GC): 96.5%) in 10 ml of THF was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 50° C. for 6 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.40 g of the title compound as a colorless liquid (e.e. (GC): 96.3%, yield: 90%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 3.41(1H,tq,J=6.8,6.4 Hz), 1.24(3H,d,J=6.4 Hz), 1.22-1.56(10H,m), 0.89(3H,t,J=6.8 Hz). IRν max(neat); 2930, 2858, 2100, 1468, 1249 cm -1 . [α] 20 D ; +39.6° (c=1.25,CHCl 3 ).
Example 5
Synthesis of methyl (2R,3S)-2-azido-3-methylpentanoate ##STR7##
To a solution of 1.46 g (10 mmol) of methyl (2S,3S)-2-hydroxy-3-methylpentanoate (d.e. (NMR): 97.4%) in 10 ml of THF was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 50° C. for 6 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 1.21 g of the title compound as a colorless liquid (d.e. (NMR): 92.4%, yield: 71%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 3.90(1H,d,J=4.8 Hz), 3.80(3H,s), 1.92-2.02(1H,m), 1.40-1.51(1H,m), 1.24-1.36(1H,m), 0.94(3H,t,J=7.2 Hz), 0.92(3H,d,J=6.8 Hz). IRν max(neat); 2967, 2109, 1745, 1204 cm -1 . [α] 20 D ; +54.9° (c=1.40,CHCl 3 ).
Example 6
Synthesis of methyl (2S,3S)-2-azido-3-methylpentanoate ##STR8##
To a solution of 731 mg (5.0 mmol) of methyl (2R,3S)-2-hydroxy-3-methylpentanoate (d.e. (NMR): 97.4%) in 5 ml of THF was added 2.20 g (6.0 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 900 μl (6.0 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 50° C., for 6 hours.
The resulting reaction mixture was diluted with 30 ml of diethyl ether, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 578 mg of the title compound as a colorless liquid (d.e. (NMR): 93.4%, yield: 68%).
1 H-NMR(400 MHz,CDCl 3 ); δ (ppm) 3.80(3H,s), 3.72(1H,d, J=6.4 Hz), 1.91-2.01(1H,m), 1.48-1.57(1H,m), 1.21-1.32(1H,m), 0.97(3H,d,J=6.8 Hz), 0.92(3H,t,J=7.6 Hz). IRν max(neat); 2967, 2109, 1745, 1202 cm -1 . [α] 20 D ; -22.6° (c=0.86,CHCl 3 ).
Example 7
Synthesis of ethyl 2-azidophenylacetate ##STR9##
To a solution of 1.80 g (10 mmol) of ethyl mandelate in 10 ml of THF was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for one hour.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 1.99 g of the title compound as a colorless liquid (yield: 97%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.37-7.44(5H,m), 4.94(1H,s), 4.17-4.31(2H,m), 1.26(3H,dd,J=7.6,6.8 Hz). IRν max(neat); 2984, 2112, 1738, 1244, 1198 cm -1 .
Example 8
Synthesis of 2,3,4,6-tetra-O-benzyl-β-D-glucopyranosyl azide ##STR10##
To a solution of 540 mg (1.0 mmol) of 2,3,4,6-tetra-O-benzyl-D-glucopyranose in 2 ml of DMF was added 438 mg (1.2 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to -20° C. under stirring, followed by the dropwise addition of 180 μl (1.2 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at -20° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 20 ml of ethyl acetate, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (toluene/ethyl acetate) to give 428 mg of the title compound as a colorless syrup (yield: 76%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.25-7.35(18H,m), 7.12-7.16(2H,m), 4.89(1H,d,J=11.2 Hz), 4.87(1H,d,J=10.4 Hz), 4.82(1H,d,J=11.2 Hz), 4.80(1H,d,J=10.8 Hz), 4.75(1H,d,J=10.4 Hz), 4.62(1H,d,J=8.8 Hz), 4.62(1H,d,J=12.0 Hz), 4.54(1H,d,J=12.0 Hz), 4.54(1H,d,J=10.8 Hz), 3.62-3.76(4H,m), 3.50-3.56(1H,m), 3.33-3.41(1H,m). IRν max(neat); 2115, 1092, 736, 697 cm -1 . [α] 20 D ; +6.6° (c=0.91,CHCl 3 ).
Example 9
Synthesis of 2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl azide ##STR11##
To a solution of 348 mg (1.0 mmol) of 2,3,4,6-tetra-O-acetyl-D-glucopyranose in 2 ml of DMF was added 438 mg (1.2 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to -20° C. under stirring, followed by the dropwise addition of 180 μl (1.2 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at -20° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 20 ml of ethyl acetate, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (toluene/ethyl acetate) to give 128 mg of the title compound as a colorless powder and 195 mg of the starting compound (corrected yield: 78%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.22(1H,dd,J=9.6,9.2 Hz), 5.11(1H,dd,J=10.0,9.6 Hz), 4.96(1H,dd,J=9.2,8.8 Hz), 4.65(1H, d, J=8.8 Hz), 4.28(1H,dd,J=12.4,4.8 Hz), 4.18(1H,dd,J=12.4,2.4 Hz), 3.80(1H,ddd,J=10.4,4.8,2.4 Hz), 2.11(3H,s), 2.08(3H,s), 2.04(3H, s), 2.01(3H,s). IRν max(neat); 2120, 1753, 1369, 1229, 1040 cm -1 . mp ; 125° C. [α] 20 D ; -19.1° (c=0.90,CHCl 3 ).
Example 10
Synthesis of 2,3,4,6-tetra-O-benzyl-D-galactopyranosyl azide ##STR12##
To a solution of 540 mg (1.0 mmol) of 2,3,4,6-tetra-O-benzyl-D-galactopyranose in 2 ml of DMF was added 438 mg (1.2 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to -20° C. under stirring, followed by the dropwise addition of 180 μl (1.2 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at -20° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 20 ml of ethyl acetate, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (toluene/ethyl acetate) to give 534 mg of the title compound as a colorless syrup (α/β: 1/9, yield: 94%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.25-7.38(20H,m), 5.29 (1/10H,d,J=4.0 Hz), 4.59(9/10H,d,J=4.0 Hz), 4.39-4.95(8H,m), 4.11 (1/10H,dd,J=10.0,4.0 Hz), 4.02(1/10H,brdd,J=6.8,6.0 Hz), 3.92-3.96(1H,m), 3.74-3.81(1H,m), 3.50-3.64(1H,m). IRν max(neat); 2113, 1102, 735, 697 cm -1 . [α] 20 D ;+4.0° (c=1.00,CHCl 3 ).
Example 11
Synthesis of 2,3,4,6-tetra-O-benzyl-α-D-mannopyranosyl azide ##STR13##
To a solution of 540 mg (1.0 mmol) of 2,3,4,6-tetra-O-benzyl-D-mannopyranose in 2 ml of DMF was added 438 mg (1.2 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to -20° C. under stirring, followed by the dropwise addition of 180 μl (1.2 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at -20° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixutre was diluted with 20 ml of ethyl acetate, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 427 mg of the title compound as a colorless syrup (yield: 75%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.25-7.37(18H,m), 7.15-7.18(2H,m), 5.04(1H,d,J=2.4 Hz), 4.86(1H,d,J=10.4 Hz), 4.73(1H, d,J=12.4 Hz), 4.69(1H,d,J=12.4 Hz), 4.67(1H,d,J=12.0 Hz), 4.61 (1H,d,J=11.6 Hz), 4.58(1H,d,J=11.6 Hz), 4.54(1H,d,J=12.0 Hz), 4.51(1H,d,J=10.4 Hz), 4.02(1H,dd,J=9.6,9.6 Hz), 3.89(1H,ddd,J=9.6,4.4,2.0 Hz), 3.78-3.83(2H,m), 3.74(1H,dd,J=11.2,2.0 Hz), 3.63(1H,dd,J=2.8,2.4 Hz). IRν max(neat); 2111, 1099, 737, 697 cm -1 . [α] 20 D ;+100.7° (c=1.28,CHCl 3 ).
Example 12
Synthesis of (E)-2-octen-1-yl azide/1-octen-3-yl azide Mixture ##STR14##
To a solution of 1.28 g (10 mmol) of (E)-2-octen-1-ol in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.26 g of the title mixture {i.e., a 1:1 (E)-2-octen-1-yl azide/1-octen-3-yl azide mixture} as a colorless liquid (yield: 82%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.69-5.80(1H,m), 5.52 (1/2H,dtt,J=14.8,6.8,1.2 Hz), 5.23-5.29(1H,m), 3.80(1/2H,dt, J=7.6,7.2 Hz), 3.69(1H,d,J=6.4 Hz), 2.08(1H,dt,J=7.2,6.8 Hz), 1.24-1.58(7H,m), 0.89(3H,t,J=6.8 Hz). IRν max(neat); 2958, 2929, 2098, 1237, 971 cm -1 .
Example 13
Synthesis of 2-cyclohexen-1-yl azide ##STR15##
To a solution of 980 mg (10 mmol) of 2-cyclohexen-1-ol in 10 ml of THF was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 913 mg of the title compound as a colorless liquid (yield: 74%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.98-6.03(1H,m), 5.68-5.73 (1H,m), 3.88(1H,brs), 1.56-2.14(6H,m). IRν max(neat); 2941, 2029, 2098, 1257, 1230, 894 cm -1 .
Example 14
Synthesis of 3-methyl-2-cyclohexen-1-yl azide/1-methyl-2-cyclohexen-1-yl azide mixture ##STR16##
To a solution of 1.12 g (10 mmol) of 3-methyl-2-cyclohexen-1-ol in 10 ml of THF was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.06 g of the title mixture {i.e., an 8: 1 3-methyl-2-cyclohexen-1-yl azide/1-methyl-2-cyclohexen-1-yl azide mixture} as a colorless liquid (yield: 77%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.96(1/9H,ddd,J=10.0, 4.0,3.6 Hz), 5.60(1/9H,ddd,J=10.0,3.2,2.4 Hz), 5.45-5.47(8/9H,m), 3.88(8/9H,brs), 1.73(24/9H,s), 1.54-2.08(6H,m), 1.30(3/9H,s). IRν max(neat); 2936, 2093, 1447, 1247, 890 cm -1
Example 15
Synthesis of (E)-3-azido-5-methoxycarbonyl-1-cyclohexene ##STR17##
To a solution of 1.56 g (10 mmol) of (Z)-3-hydroxy-5-methoxycarbonyl-1-cyclohexene in 10 ml of THF was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for one hour.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 1.53 g of the title compound as a colorless liquid (E/Z: 97/3, yield: 84%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 6.05(1H,dddd,J=10.0,5.2, 2.8,1.2 Hz), 5.80(1H,m), 4.03(1H,brm), 3.71(3H,s), 2.77(1H, dddd,J=11.6,10.0,5.2,2.8 Hz), 2.40(1H,brddd,J=18.4,5.2,5.2 Hz), 2.24(1H,dddd,J=18.4,10.0,4.4,2.8 Hz), 2.14(1H,dm,J=13.6 Hz), 1.89(1H,ddd,J=13.6,11.6,4.8 Hz). IRν max(neat); 2953, 2100, 1732, 1435, 1254 cm -1 .
Example 16
Synthesis of geranyl azide/neryl azide/linalyl azide Mixture ##STR18##
To a solution of 1.54 g (10 mmol) of geraniol in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.68 g of the title mixture {i.e., a 9:5:2 geranyl azide/neryl azide/linalyl azide mixture} as a colorless liquid (yield: 94%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.78(2/16H,dd,J=17.2, 10.4 Hz), 5.31-5.36(14/16H,m), 5.23(2/16H,dd,J=17.2,0.8 Hz), 5.21 (2/16H,dd,J=10.4,0.8 Hz), 5.06-5.12(16/16H,m), 3.77(18/16H,d,J=7.6 Hz), 3.75(10/16H,J=7.2 Hz), 2.05-2.17(56/16H,m), 1.97-2.03 (4/16H,m), 1.80(15/16H,d,J=1.2 Hz), 1.71(27/16H,d,J=0.8 Hz), 1.69(48/16H,s), 1.61(48/16H,s), 1.52-1.60(4/16H,m), 1.36 (6/16H,s). IRν max(neat); 2969, 2928, 2097, 1250 cm -1
Example 17
Synthesis of geranyl azide/neryl azide/linalyl azide Mixture ##STR19##
To a solution of 1.54 g (10 mmol) of nerol in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 30 minutes.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 1.70 g of the title mixture {i.e., a 3:4:1 geranyl azide/neryl azide/linalyl azide mixture} as a colorless liquid (yield: 95%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.78(1/8H,dd,J=17.2, 10.4 Hz), 5.31-5.36(7/8H,m), 5.23(1/8H,dd,J=17.2,0.8 Hz), 5.21 (1/8H,dd,J=10.4,0.8 Hz), 5.06-5.12(8/8H,m), 3.77(6/8H,d,J=7.6 Hz), 3.75(8/8H,J=7.2 Hz), 2.05-2.17(28/8H,m), 1.97-2.03 (2/8H,m), 1.80(12/8H,d,J=1.2 Hz), 1.71(9/8H,d,J=0.8 Hz), 1.69 (24/8H,s), 1.61(24/8H,s), 1.52-1.60(2/8H,m), 1.36(3/8H,s). IRν max(neat); 2969, 2928, 2097, 1250 cm -1
Example 18
Synthesis of geranyl azide/neryl azide/linalyl azide Mixture ##STR20##
To a solution of 1.54 g (10 mmol) of linalool in 10 ml of toluene was added 4.38 g (12 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 537 mg of the title mixture {i.e., a 7:10:3 geranyl azide/nerylazide/linalyl azide mixture} as a colorless liquid and 936 mg of the starting compound (corrected yield: 77%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 5.78(3/20H,dd,J=17.2, 10.4 Hz), 5.31-5.36(17/20H,m), 5.23(3/20H,dd,J=17.2,0.8 Hz), 5.21 (3/20H,dd,J=10.4,0.8 Hz), 5.06-5.12(20/20H,m), 3.77(14/20H,d,J=7.6 Hz), 3.75(20/20H,J=7.2 Hz), 2.05-2.17(68/20H,m), 1.97-2.03 (6/20H,m), 1.80(30/20H,d,J=1.2 Hz), 1.71(21/20H,d,J=0.8 Hz),1.69 (60/20H,s), 1.61(60/20H,s), 1.52-1.60(6/20H,m), 1.36(9/20H,s). IRν max(neat); 2969, 2928, 2097, 1250 cm -1
Example 19
Synthesis of (S)-1-phenylethyl azide ##STR21##
To a solution of 611 mg (5.0 mmol) of (R)-1-phenylethanol (e.e.(GC): 100%) in 5 ml of THF was added 2.20 g (6.0 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 900 μl (6.0 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for one hour.
The resulting reaction mixture was diluted with 30 ml of diethyl ether, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 691 mg of the title compound as a colorless liquid (e.e. (GC): 100%, yield: 94%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.29-7.41(5H,m), 4.61(1H, q,J=6.8 Hz), 1.53(3H,d,J=6.8 Hz). IRν max(neat); 2980, 2105, 1454, 1248, 699 cm -1 . [α] 20 D ; -105.0° (c=1.10, CHCl 3 ).
Example 20
Synthesis of (S)-1-azidoindan ##STR22##
To a solution of 671 mg (5.0 mmol) of (R)-1-indanol (e.e. (GC): 100%) in 5 ml of THF was added 2.20 g (6.0 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 900 μl (6.0 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 2 hours.
The resulting reaction mixture was diluted with 30 ml of diethyl ether, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 654 mg of the title compound as a colorless liquid (e.e. (GC): 81.3%, yield: 82%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.39(1H,dd,J=7.2,0.4 Hz), 7.23-7.31(3H,m), 4.86(1H,dd,J=7.2,4.4 Hz), 3.07(1H,ddd,J=16.0 8.4,6.4 Hz), 2.87(1H,ddd,J=16.0,8.4,5.2 Hz), 2.44(1H,dddd,J=13.2,8.4,7.2,6.4 Hz), 2.12(1H,dddd,J=13.2,8.4,5.2,4.4 Hz). IRν max(neat); 2946, 2092, 1325, 1287, 755 cm -1 . [α] 20 D ; -9.0° (c=0.99,CHCl 3 ).
Example 21
Synthesis of (S)-2-phenyl-1-(2-thiazolyl)-ethyl azide ##STR23##
To a solution of 103 mg (0.5 mmol) of (R)-2-phenyl-1-(2-thiazolyl)ethanol (e.e. (HPLC): 95.9%) in 0.5 ml of THF was added 219 mg (0.6 mmol) of di-p-nitrophenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 90 μl (0.6 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 3 hours.
The resulting reaction mixture was diluted with 20 ml of diethyl ether, washed thrice with 10 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 105 mg of the title compound as a colorless liquid (e.e. (HPLC): 95.6%, yield: 91%).
1 H-NMR(400 MHz, CDCl 3 ); δ (ppm) 7.81(1H,d,J=3.2 Hz), 7.22-7.33(6H,m), 5.01(1H,dd,J=8.8,4.8 Hz), 3.42(1H,dd,J=14.0,4.8 Hz), 3.17(1H,dd,J=14.0,8.8 Hz). IRν max(neat); 3029, 2105, 1497, 1308, 1247, 732, 700 cm -1 . [α] 20 D ;-36.2° (c=1.03,CHCl 3 ).
Comparative Example 1
Synthesis of 1-azidodecane (According to the Process using diphenyl phosphorazidate)
To a solution of 1.58 g (10 mmol) of 1-decanol in 10 ml of toluene was added 2.59 ml (12 mmol) of diphenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 25° C. for 24 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 95 mg of the title compound as a colorless liquid (yield: 5%).
Comparative Example 2
Synthesis of 2-azidodecane (According to the Process using diphenyl phosphorazidate)
To a solution of 1.58 g (10 mmol) of 2-decanol in 10 ml of toluene was added 2.59 ml (12 mmol) of diphenyl phosphorazidate. The resulting mixture was cooled to 0° C. under stirring, followed by the dropwise addition of 1.8 ml (12 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene. The resulting mixture was stirred at 0° C. for 30 minutes and then at 50° C. for 6 hours.
The resulting reaction mixture was diluted with 50 ml of diethyl ether, washed thrice with 20 ml of water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane) to give 63 mg of the title compound as a colorless liquid (yield: 3%).
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A process for the preparation of azide derivatives useful as drugs, perfumes or intermediates of dyes by reacting an alcohol derivative with di-p-nitrophenyl phosphorazidate in the presence of 1,8-diazabicyclo[5.4.0]-7-undecene.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to computer software and business methods. More specifically, the present invention relates to systems and method for automatically administering exams, analyzing test results and formulating study strategies.
[0003] 2. Description of the Related Art
[0004] Standardized tests are used to assess a test taker's knowledge, ability and/or likelihood of success for a variety of educational, governmental and commercial positions. In the educational arena, a score on an SAT, ACT, or Graduate Records Examination (GRE), and other tests is used as significant component of a college admissions evaluation and selection process. Obviously, one's score on such exams is of paramount importance. For this reason, a number of preparatory courses are currently on the market. Such courses include Kaplan SAT Online, the Princeton Review and Peterson's Test Prep by way of example. These courses generally feature online distribution of course material and administration of practice exams and provide raw test scores or simple metrics such as percent correct. However, raw test scores and simple metrics do not provide the student with much guidance as to how to improve the test score.
[0005] Hence, a system or method is needed for administering a test, analyzing test results, diagnosing a student's strengths and weaknesses and suggesting studying strategies based on the diagnosis.
SUMMARY OF THE INVENTION
[0006] The present invention sets out to address the need in the art in the field of test preparation with a focus specifically on but not limited to standardized, admissions testing. The present invention provides a mathematically driven system which can be used to diagnose a student's strengths and weaknesses and provide studying strategies based on these strengths and weaknesses. The present invention bases studying suggestions not on raw test scores or on simple metrics such as “percent correct”, but on the student's potential to increase their test score by studying a particular topic.
[0007] The inventive method includes the steps of administering an exam with composite questions relating to a subject and an associated study strategy therefor; analyzing results of said exam to diagnose strengths and weaknesses of a student with respect to said subjects and strategies; and outputting data with respect to optimal strategies for the student with respect to said subjects.
[0008] In the best mode, the step of diagnosing strength and weaknesses includes the step of computing an AspenRank. The step of computing the AspenRank includes the steps of: 1) computing as a raw score the number of questions answered correctly divided by the number of questions posed in said exam; 2) computing a weighted score equal to the raw score times a weight, the weight being based on a difficulty of said questions posed; and 3) computing a weighted incorrect score equal to a number of questions answered incorrectly times a weight, the weight being again based on the difficulty of said questions posed. The step of computing the AspenRank includes the step of ascertaining a student's strength in an area based on all of the above factors plus the overall frequency of a certain type of question on a given test. AspenRank score is a measure of potential yield in said scores if a student studies a subject or strategy area.
[0009] The invention is disclosed herein with respect to the SAT, but the present teachings are not limited thereto.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a diagram of a typical client-server architecture for use in connection with the present teachings.
[0011] FIG. 2 is a flow diagram illustrative of the method of the present invention.
DESCRIPTION OF THE INVENTION
[0012] Illustrative embodiments and exemplary applications will now be described with reference to the accompanying drawings to disclose the advantageous teachings of the present invention.
[0013] While the present invention is described herein with reference to illustrative embodiments for particular applications, it should be understood that the invention is not limited thereto. Those having ordinary skill in the art and access to the teachings provided herein will recognize additional modifications, applications, and embodiments within the scope thereof and additional fields in which the present invention would be of significant utility.
[0014] The present invention operates on the assumption that a student can increase his or her test score in two ways:
By increasing his understanding of specific subjects covered by the test. By increasing his awareness of specific test-taking strategies that can either
Help the student eliminate incorrect answers Help the student identify correct answers Decrease the amount of time that it takes to identify correct answers
[0020] Test questions can therefore be described in terms of one or more subjects and one or more strategies that apply to that specific question. A student's performance on an individual question then essentially “casts a vote” for his familiarity with the underlying subjects and strategies assigned to that question.
[0021] If the student gets a question right, this is evidence that he understands the underlying subjects and strategies assigned to that question. If the student gets a question wrong, this is evidence that he does not understand these subjects and strategies. This information, once aggregated, suggests a student's strengths and weaknesses in particular subject areas and with particular test-taking strategies.
[0022] The present invention, then, takes this information into consideration along with some additional factors to suggest to the student, on a subject-by-subject or strategy-by-strategy basis, which subjects or strategies the student should study to get the highest yield in the form of higher test scores on future tests.
[0023] In accordance with the present teachings, an AspenRank score is calculated for each subject that is tested within a given test and for each strategy that applies to a given test.
[0024] The AspenRank score for a specific subject or strategy takes into Consideration the following:
RAW_SCORE=number of correct/number of questions posed WEIGHTED_CORRECT_SCORE=weighted number of correct answers/number of questions posed with correct answers weighted based on the difficulty of the question (1-5, 5 being the most difficult) WEIGHTED_INCORRECT_SCORE=weighted number of incorrect answers/number of questions posed with incorrect answers weighted based on the difficulty of the question (−1 to −5, −5 being assigned to getting an easy question wrong and −1 assigned when getting a difficult question wrong) UNANSWERED=number of questions left unanswered TOTAL_POSED=number of questions on the test for a given subject or strategy
[0030] To clarify, for WEIGHTED_CORRECT_SCORE and WEIGHTED_INCORRECT_SCORE, the following table is used:
Difficulty Correct Incorrect Easiest 1 +1 −5 2 +2 −4 3 +3 −3 4 +4 −2 Hardest 5 +5 −1
[0031] Thus, the student is rewarded more for getting hard questions correct and penalized more for getting easy question wrong. These two pieces of information taken together most realistically describe a student's strength in an area.
[0000] Consider the following example:
[0032] A student gets 5 questions correct out of 10 posed. A grade of 50%
[0033] Now suppose the difficulties of these questions were: 1, 1, 2, 2, 3, 3, 4, 4, 5, 5
[0034] Now suppose there is Student A and Student B, both of whom scored 5/10. But their correct answers are indicated by bold (no questions left unanswered):
Student A Student B 1 , 1 , 2 , 2 , 3 , 3, 4, 4, 5, 5 1, 1, 2, 2, 3, 3 , 4 , 4 , 5 , 5 Un-weighted score: 5/10 = 50% 5/10 = 50% Weighted correct: 9/30 = 30% 21/30 = 70% Weighted incorrect: 21 − 9/−3 = 370% −921/−30 = 730%
[0035] Student B has a much better understanding of the subject matter, as evidenced by getting harder questions correct. Student B also has higher potential to improve his score because he merely needs to answer a few simple questions correctly to improve his score whereas Student A may have a more fundamental lack of understanding on his hands.
[0036] In the example above, the WEIGHTED_CORRECT and WEIGHTED_INCORRECT are equal, but this is not always the case because a) difficulty distributions are not always even, as they were in the example and b) often a student will leave a question unanswered, which is does not mean it was incorrect per se.
[0037] In accordance with the present teachings, other factors are taken into consideration such as how often a specific subject or strategy appears on a test (TOTAL_POSED) and how many questions were left unanswered (UNANSWERED). UNANSWERED is relevant because, on many tests, unanswered questions are actually preferable to incorrectly answered questions because there is a penalty for wrong answers. Therefore, a strategy to improve one's score is often to stop getting answers wrong as opposed to getting more right or, in most cases, to stop guessing altogether.
[0038] TOTAL_POSED is highly important to the present invention because it suggests the amount of potential yield a student could get by studying a particular area based on how often that subject is actually on the test.
[0000] Consider this:
[0039] Two students, Student A and Student B, get identical scores on a particular subject. Correct answers again indicated by bold.
Student A Student B Questions 1, 5 1, 1, 1, 1, 5 , 5 , 5 , 5 Un-weighted Score ½ = 50% 4/8 = 50% Weighted Correct Score 5/6 = 83% 20/24 = 83% Weighted Incorrect Score −51/−6 = 1783% −204/−24 = 1783%
[0040] Even though these two students have identical weighted correct and weighted incorrect scores, the TOTAL POSED factor would ensure that Student B would have a higher AspenRank for this subject area because there are more questions that he can pick up by studying that subject area. There is not as much yield to be had by Student A since, at best, he could only pick up one additional question correct.
[0000] AspenRank in Practice
[0041] All of the factors described above are weighted and averaged to come up with an AspenRank that ranges from 0 to 5 in increments of 0.5. An AspenRank of 5 indicates high potential yield if the student studies that subject or strategy area. An AspenRank of 0 indicates low to no potential yield if the student studies that subject or strategy area.
[0042] Based on the discussion above, the following is true:
[0043] An AspenRank of zero can be achieved in two ways:
1. If the student gets 100% of the questions right there is no score improvement to be had by studying that subject, thus no potential yield and an AspenRank of zero. 2. If the student gets 0% of the questions right there is no indication that the student has any understanding of the subject or strategy area, thus the problem is more structural and not easily remedied by a “brush up” tutorial on the topic.
[0046] An AspenRank of five is achieved when a student gets some questions right, some wrong, and when those he got right outweigh those he got wrong when the difficulties of the questions are taken into consideration. Also, a subject or strategy area with an AspenRank of five likely means that there are a fair amount of questions on the test that cover that specific subject or strategy area.
[0047] The loftier the score improvement that the student wants to achieve, the lower in the AspenRanking scores the student will focus when studying. Inversely, if only a minor improvement is wanted, a student need only study the subjects and strategies with the highest AspenRank.
[0048] FIG. 1 is a diagram of a typical client-server architecture for use in connection with the present teachings. The architecture 10 includes a database server which executes the software 100 of the present invention. In the illustrative architecture, the database server 12 feeds an Internet server 14 . The server communicates with users via a network 15 and numerous client computers of which five are shown 16 , 18 , 20 , 22 and 24 . Those skilled in the art will appreciate that the network 15 may be the Internet, a local area network or another network without departing from the scope of the present teachings.
[0049] FIG. 2 is a flow diagram illustrative of the method of the present invention. In the best mode, the process illustrated in FIG. 2 is implemented in software 100 . At step 102 , a test is administered. At step 110 , the test data is analyzed in accordance with the present teachings. As a first step in the analysis of the data, weighted possibly correct and incorrect scores are computed at step 112 . For each correct answer, the total weighted possible correct answers are computed as being equal to the total possible correct answers, each multiplied (weighted) by a plus a measure of the level of difficulty of the question. Likewise for each incorrect answer, the total weighted possible incorrect answer is computed as being equal to the sum of the weight of the incorrect answers for all the questions posed, the weight being computed based on the difficulty level of the question (−1 being assigned to getting a difficult question wrong and −5 being assigned to getting an easy question wrong).
[0050] At step 114 , the number of correct, incorrect and not answered responses is computed. In other words, the total number of correct, incorrect and unanswered questions is incremented. We increment the totals at step 114 to obtain the raw number of correct, incorrect and unanswered questions from the student responses.
[0051] Next, at step 116 the weighted number of correct and incorrect answers is computed. For each correct answer, the total weighted number of correct answers is equal to the total weighted number of correct answers plus the level of difficulty of the question. For each incorrect answer, the total weighted number of incorrect answers is computed as the sum of the weight of the incorrect answers for the questions with incorrect answer, the weight being computed based on the difficulty level of the question (−1 being assigned to getting a difficult question wrong and −5 being assigned to getting an easy question wrong).
[0052] Finally, at step 118 , the Aspen score and the Aspen rank are computed in accordance with the present teachings using the factors determined above and at step 120 , data is output to the student which indicates which subjects and strategies have higher Aspen rank and yield relative to subjects and strategies with lower Aspen rank and yield.
[0053] Thus, the present invention has been described herein with reference to a particular embodiment for a particular application. Those having ordinary skill in the art and access to the present teachings will recognize additional modifications applications and embodiments within the scope thereof.
[0054] It is therefore intended by the appended claims to cover any and all such applications, modifications and embodiments within the scope of the present invention.
[0055] Accordingly,
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A mathematically driven system which can be used to diagnose a student's strengths and weaknesses and provide studying strategies based on these strengths and weaknesses. The invention bases studying suggestions not on raw test scores or on simple metrics such as “percent correct”, but on the student's potential to increase their test score by studying a particular topic. The inventive method includes the steps of administering an exam with composite questions relating to a subject and an associated study strategy therefor; analyzing results of said exam to diagnose strengths and weaknesses of a student with respect to said subjects and strategies; and outputting data with respect to optimal strategies for the student with respect to said subjects.
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[0001] This application is a division of application Ser. No. 12/800,622 filed May 19, 2010.
[0002] This invention relates to a tool used in wells extending into the earth and, more particularly, to a tool for isolating one section of a pipe string from another section.
BACKGROUND OF THE INVENTION
[0003] There are a number of situations, in the completion of oil and gas wells, where it is desirable to isolate one section of a subterranean well from another. For example, in U.S. Pat. No. 5,924,696, there is disclosed an isolation tool used alone or in combination with a packer to isolate a lower section of a production string from an upper section. This tool incorporates a pair of oppositely facing frangible or rupturable discs or half domes which isolate the well below the discs from pressure operations above the discs and which isolate the tubing string from well bore pressure. When it is desired to provide communication across the tool, the upper disc is ruptured by dropping a go-devil into the well from the surface or well head which falls into the well and, upon impact, fractures the upwardly convex ceramic disc. The momentum of the go-devil normally also ruptures the lower disc but the lower disc may be broken by application of pressure from above, after the upper disc is broken, because the lower disc is concave upwardly and thereby relatively weak against applied pressure from above.
[0004] An important development in natural gas production in recent decades has been the drilling of horizontal sections through zones that have previously been considered uneconomically tight or which are shales. By fracing the horizontal sections of the well, considerable production is obtained from zones which were previously uneconomical. For some years, the fastest growing segment of gas production in the United States has been from shales or very silty zones that previously have not been considered economic. The current areas of increasing activity include the Barnett Shale, the Haynesville Shale, the Fayetteville Shale, and the Marcellus Shale in the United States, the Horn River Basin of Canada and other shale or shaley formations in North America and Europe.
[0005] It is no exaggeration to say that the future of natural gas production in the continental United States is from these heretofore uneconomically tight gas bearing formations. In addition, there are many areas of the world where oil and gas is produced and costs are, from the perspective of a United States operator, exorbitantly high. These areas currently include offshore Africa, the Middle East, the North Sea and deep water parts of the Gulf of Mexico. Accordingly, a development that allows well completions at overall lower costs is important in many areas of the world and in many different situations.
[0006] Disclosures of interest relative to this invention are found in U.S. Pat. Nos. 7,044,230; 7,210,533 and 7,350,582 and U.S. Printed Patent Applications S.N. 20070074873; 20080271898 and 20090056955.
SUMMARY OF THE INVENTION
[0007] The device disclosed in U.S. Pat. No. 5,924,696 can be used in a horizontal section of a well to isolate the well below the tool from pressure operations above the tool. However, the upper disc has to be broken or weakened in a mechanical fashion requiring a bit trip, typically a coiled tubing trip in modern high tech wells or a bit trip with a workover rig in more traditional environments, to fracture the upper disc because a go-devil dropped through the vertical section of the well does not have sufficient momentum to reach and then fracture the upper disc. Theoretically, sufficient pressure could be applied from above to break the upper disc from the concave side but this pressure is commonly so high that it would damage or destroy other components of the production string. It has been realized that it would be desirable to provide an isolation tool which can be used in a horizontal section of a well without requiring a bit trip.
[0008] As disclosed herein, a pressure differential that is uniform across the pressure disc is created by manipulating pressure at the surface or through the well head to fracture a first of the discs. The other disc may be ruptured using pressure in the well. The exact sequence of breaking the discs may depend on the particular design employed and whether the isolation tool is located above or below a packer or other sealing element isolating the production string, typically from a surrounding pipe string
[0009] Several embodiments of an isolation tool are disclosed that may be used in wells to temporarily isolate a section of the well below the tool from a section above the tool. These embodiments use a pressure differential to fracture a first of the discs. In one embodiment, a capillary tube is provided from above the upper disc to a location between the discs. In a second embodiment, a check valve admits pressurized well fluid between the discs so that one of the discs may be broken by reducing the pressure on one side of the isolation tool. In a third embodiment, an unvalved opening admits pressurized well fluid between the discs so that one of the discs may be broken by reducing the pressure on one side of the isolation tool. In a fourth embodiment, a movable member is displaced by pressure supplied from above to break a first of the discs.
[0010] It is an object of this invention to provide an improved down hole well tool to isolate one section of a well from another.
[0011] A more specific object of this invention is to provide an improved isolation sub that can be manipulated by a pressure differential to place isolated sections of a well into communication.
[0012] These and other objects and advantages of this invention will become more apparent as this description proceeds, reference being made to the accompanying drawings and appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a cross-sectional view of one embodiment of an isolation tool that incorporates a pair of oppositely facing pressure discs;
[0014] FIG. 2 is an exploded view of a component of the device of FIG. 1 ;
[0015] FIG. 3 is a schematic view of a well in which the isolation tool of FIG. 1 is employed;
[0016] FIG. 4 is a cross-sectional view of another embodiment of an isolation tool that incorporates a pair of oppositely facing pressure discs;
[0017] FIG. 5 is an enlarged view of a valve assembly used in the embodiment of FIG. 4 ;
[0018] FIG. 6 is a view similar to FIG. 2 , illustrating operation of the embodiment of FIGS. 4 and 5 ;
[0019] FIG. 7 is a partial view of another embodiment of this invention, based on the embodiment of FIG. 4 ;
[0020] FIG. 8 is a cross-sectional view of another embodiment of an isolation tool that incorporates a pair of oppositely facing pressure discs, illustrating the tool in a position where upper and lower sections of the well are isolated;
[0021] FIG. 9 is a cross-sectional view of the embodiment of FIG. 5 illustrating the tool in the process of breaking one of the pressure discs;
[0022] FIG. 10 is an isometric view of a modified pressure dome; and
[0023] FIG. 11 is a view of the pressure dome of FIG. 10 in an isolation tool.
DETAILED DESCRIPTION OF THE INVENTION
[0024] Referring to FIGS. 1-2 , there is illustrated an isolation tool or sub 10 comprising a housing 12 having a passage 14 therethrough, upper and lower rupturable pressure discs 16 , 18 and a capillary tube 20 opening into a chamber 22 between the discs 16 , 18 .
[0025] The housing 12 may comprise a lower end, pin body or pin 24 , a central section 26 , an upper end or box body 28 and suitable sealing elements or O-rings 30 , 32 captivating the discs 16 , 18 in a fluid tight manner. Except for the capillary tube 20 , those skilled in the art will recognize the isolation sub 10 , as heretofore described, as being typical of isolation subs sold by Magnum International, Inc. of Corpus Christi, Tex. and as also described in U.S. Pat. No. 5,924,696.
[0026] The capillary tube 20 may be external to the housing 12 , or an internal passage may be provided, and may terminate in an extension of the central section 26 or in the upper section 28 . One problem that is occasionally encountered is sufficient debris above the upper disc 16 which might seal off pressure from reaching the capillary tube 20 . To overcome this problem, the capillary tube 20 may be of greater length as by providing one or more pipe sections 34 of any suitable length connected to a collar or other sub 36 thereby elongating the housing 12 . This will accommodate debris, such as sand or the like, from bridging off access to the top of the capillary tube 20 .
[0027] The discs 16 , 18 may be of any suitable type having the capability of being stronger in one direction than in an opposite direction. Conveniently, the discs 16 , 18 may be curved or generally hemispherical domes made of any suitable material, such as ceramic, porcelain, glass and the like. Suitable ceramic materials, such as alumina, zirconia and carbides are currently commercially available from Coors Tek of Golden, Colo. These materials are frangible and rupture in response to either a sharp blow or in response to a pressure differential where high pressure is applied to the concave side of the discs 16 , 18 . Because of their curved or hemispherical shape, half domes may be a preferred selection because of their considerable ability to resist pressure from the convex side, their much lower ability to resist pressure from the concave side, cost, reliability and frangibility. Ceramic discs of this type are available in a variety of strengths but a typical disc may have the capability of withstanding 25,000 psi applied on the convex side but only 1500 psi applied on the concave side. In a typical situation, the discs 16 , 18 may be 10-20 times stronger against pressure applied to the convex side than to the concave side. Any pressure disc which has greater strength in one direction than in the opposite may be used, another example of which are metal Scored Rupture Disc Assemblies available from Fike Corporation of Blue Springs, Mo. or BS&B of Tulsa, Okla. The Fike discs that are stronger in one direction than the other are also concave on the weak side and convex on the other which is a convenient technique for making the discs stronger in one direction than in an opposite direction and thus responsive to different sized pressure differentials.
[0028] The capillary tube 20 includes a tube 38 of any suitable outside and inside diameter so long as it transmits pressure, either higher or lower than hydrostatic pressure in the well applied from above the tool 10 . The tube 20 may be connected to the central section 26 in a recess 40 by a nipple 42 threaded, pressed or otherwise connected to the central section 26 . The nipple 42 communicates with a passage 44 opening into the chamber 22 so any pressure, higher or lower than hydrostatic pressure, applied above the tool 10 is delivered between the discs 16 , 18 . A connector 46 may be threaded into the nipple 42 as driven by a wrench (not shown) acting on a polygonal nut 48 . A similar or dissimilar fitting 50 may connect an upper end of the tube 38 to the collar 36 .
[0029] Referring to FIG. 3 , a typical example of using the isolation tool 10 is illustrated. The isolation tool 10 may comprise part of a horizontal or inclined section of a production string 52 inside a casing string 54 which intersects a productive zone where one or more pipe joints 56 may be disposed below the tool 10 and a series of pipe joints 58 may be disposed above the tool 10 leading to the surface or well head so formation fluids may be produced. A typical use of the isolation tool 10 is to isolate the productive zone below a packer 60 from pressure operations above the tool 10 which operations typically set the packer 60 . Another typical use of the isolation tool 10 is in setting a liner during drilling of a deep well.
[0030] At the outset and throughout the packer setting operation, there is hydrostatic pressure inside the production string 52 and in the annulus between the production string 52 and the casing string 54 , meaning there is hydrostatic pressure above the upper disc 16 , in the chamber 22 and below the lower disc 18 , so there is no pressure differential operating on the discs 16 , 18 which would tend to break them. The packer 60 is set by applying pressure downwardly through the production string 52 . Any pressure applied from above acts on both sides of the upper disc 16 so the upper disc 16 sees no pressure differential and there is no tendency of the upper disc 16 to fail. So long as the packer 60 is set by a pressure that is less than the sum of hydrostatic pressure at the tool 10 and the strength of the disc 18 against pressure applied on the concave side, the packer 60 may be manipulated without fracturing the lower disc 18 .
[0031] After the packer 60 is set, pressure is applied from above and transmitted through the capillary tube 20 to a location between the discs 16 , 18 . This applied pressure is greater than the hydrostatic pressure in the well and creates a pressure differential which is uniform over the area of the disc 18 and which exceeds the ability of the concave side of the lower disc 18 to withstand it. The lower disc 18 then shatters or ruptures allowing well pressure to enter the chamber 22 . When pressure in the production string 52 above the tool 10 is lowered, as by stopping the pumps which have created the pressure to set the packer 60 , by swabbing the production string 52 , gas lifting the production string 52 or simply opening the production string 52 to the atmosphere at the surface or well head, well pressure acting on the concave side of the upper disc 16 exceeds its ability to withstand pressure in this direction whereupon the upper disc 16 fails thereby placing the production string 52 , above and below the tool 10 , in communication and allowing the well to produce. Thus, the tool 10 allows breaking of the discs 16 , 18 to place the heretofore isolated parts of the well in communication by the application of pressure from above. In this situation, the pressure that breaks the lower disc 18 is applied from above and produces a pressure at the tool 10 that is greater than hydrostatic pressure but far less than what would rupture the disc 16 if applied from above.
[0032] Many, if not most, hydraulically set packers require more pressure above hydrostatic than the concave side of the lower disc 18 can withstand. To overcome this problem, an inline pressure disc 62 may be provided in the capillary tube 20 as shown best in FIG. 3 . In some embodiments, the pressure disc 62 may be located between the nipple 42 and the passage 44 , may be located inside the nipple 42 , inside the fitting 50 or any other suitable location. The pressure disc 62 may be of any suitable type to provide a sufficient resistance to allow the packer 60 to be hydraulically set without rupturing the lower disc 18 . In some embodiments, the pressure disc 62 is commercially available from Fike Corporation of Blue Springs, Mo. and known as Scored FSR Rupture Disc Assembly. In a typical situation, the packer 60 may require an applied pressure of 3500 psi above hydrostatic to set. In such situations, the pressure disc 62 may be selected to rupture at a substantially greater pressure, e.g. 4500 psi. Thus, the packer 60 would be set and then additional pressure would be applied to rupture the disc 62 which would place sufficient pressure in the chamber 22 to fracture the lower disc 18 . The upper disc 16 would not rupture immediately because there is initially no pressure differential across the upper disc 16 because the pressure applied from the surface is on both sides of the upper disc 16 . After the lower disc 18 fails, pump pressure applied from the surface is reduced whereupon formation pressure applied from below produces a pressure differential sufficient to rupture the upper disc 16 .
[0033] In some embodiments, a check valve (not shown) may be provided in the fitting 50 to allow flow inside the tubing string 58 to enter the chamber 22 but prevent flow out of the chamber 22 .
[0034] It will be seen that the tool 10 is designed to cause one of the pressure discs 16 , 18 to fail by creation of a pressure differential that is substantially below the differential pressure which would cause failure if applied to the strong or convex side of the pressure discs 16 , 18 .
[0035] Referring to FIG. 4 , there is illustrated another isolation tool 70 providing a passage 72 therethrough and comprising, as major components, a housing 74 , first and second pressure discs 76 , and a valve assembly 80 allowing hydrostatic pressure from outside the tool 70 to enter a chamber 82 between the pressure discs 76 , 78 .
[0036] The housing 74 may comprise a lower end or pin body 84 , a central section or collar 86 providing a passage 88 into the chamber 82 , an upper end or box body 90 and suitable sealing elements or O-rings 92 , 94 captivating the discs 76 , 78 in a fluid tight manner. The pressure discs 76 , 78 may be of the same type and style as the pressure discs 16 , 18 and are capable of resisting a greater pressure from one direction than the other. Except for the valve assembly 80 , those skilled in the art will recognize the isolation sub 70 , as heretofore described, as being typical of isolation subs sold by Magnum International, Inc. of Corpus Christi, Tex. and as also being described in U.S. Pat. No. 5,924,696.
[0037] The valve assembly 80 comprises a check valve which allows flow into the chamber 82 so hydrostatic pressure is delivered between the discs 76 , 78 during normal operations, such as when the tool 70 is being run into a well. The valve assembly 80 may comprise a spring 96 biasing a ball check 98 against a valve seat 100 . It will be seen that the check valve 80 allows the maximum hydrostatic pressure to which the tool 70 is subjected to appear in the chamber 82 . Under normal conditions, there is no tendency for the pressure in the chamber 82 to rupture the discs 76 , 78 because the same pressure exists on the inside and outside of the tool 70 .
[0038] Referring to FIG. 6 , the isolation tool 70 is illustrated in a production string 102 inside a casing string 104 . A pressure actuated packer 106 may be above the isolation tool 70 . The production string 102 may extend past the tool 70 toward a hydrocarbon formation. Initially, the isolation tool 70 pressure separates the production string 102 into two segments. Because of the inherent strength of the convex side of the illustrated disc 76 , the applied pressure may be sufficiently high to conduct any desired pressure operation. After the packer 102 is set or when it is desired to place the well below the tool 70 in communication with the production string 102 above the tool 70 , steps are conducted to reduce pressure above the upper disc 76 . This may be done in any suitable manner, as by opening the production string 102 at the surface or through the well head, swabbing the production string 102 , gas lifting the production string 102 or the like. When the pressure above the upper disc 76 declines sufficiently, a pressure differential is created across the upper disc 76 which is sufficient to rupture the upper disc 76 . This pressure differential is much smaller than a pressure differential caused by the application of positive pressure to the convex side of the upper disc 76 that is sufficient to rupture it. For example, the convex side of the disc 76 may be rated to withstand a pressure differential of 25,000 psi but the embodiment of FIG. 4 acts to rupture the upper disc 76 upon creating a much smaller pressure differential applied to the concave side of the disc 76 .
[0039] After the upper disc 76 ruptures, pressure may be applied at the surface through the production string 102 by a suitable pump (not shown) to create a pressure differential across the lower disc sufficient to rupture it. In this manner, the heretofore pressure separated sections of the well are now in communication.
[0040] Referring to FIG. 7 , there is illustrated another isolation tool 110 which may be identical to the tool 70 except that the check valve assembly 80 has been eliminated. Thus, the tool 110 may include a collar 112 having one or more continuously open or unvalved passages 114 therein communicating between the pressure discs. By continuously open, it is meant that the passage 114 is open when the tool 110 is in the well. Surprisingly, the tool 110 works in the same manner as the tool 70 because the passage 114 allows hydrostatic pressure to build up between the discs. When liquids above the upper disc are removed, a pressure differential is created across the upper disc in its weak direction thereby rupturing the upper disc. The lower disc is broken in the same manner as the lower disc 78 which may be by pumping into the tool 110 . Besides the advantage of simplicity, the tool 110 also has an advantage when it becomes necessary or desirable to remove the production string and packer from the well without setting the packer. In the embodiment of FIGS. 4-5 , pulling the tool 70 from the well will reduce pressure above the upper disc 76 and below the lower disc 78 so the trapped pressure in the chamber 82 will likely cause one of the discs 76 , 78 to fail. By removing the check valve assembly 80 , the isolation tool 110 may be pulled from the well without rupturing either of the pressure discs because hydrostatic pressure will bleed off from between the discs at the same rate as it falls above the upper disc and below the lower disc. By eliminating the check valve assembly 80 , there is created an isolation tool which will not rupture when the tool is pulled from the well.
[0041] Referring to FIGS. 8-9 , there is illustrated another isolation tool 120 providing a passage 122 therethrough and comprising, as major components, a housing 124 , first and second frangible pressure discs 126 , 128 and an assembly 130 responsive to pressure inside the tool 120 to rupture the discs 126 , 128 .
[0042] The housing 124 may comprise a lower end or pin body 132 , a central section or collar 134 , a section 136 that cooperates with the assembly 130 , an upper end or box body 138 , and suitable sealing elements or O-rings 140 , 142 captivating the discs 126 , 128 in a fluid tight manner. Another set of seals or O-rings 144 seal between the section 136 and the box body 138 .
[0043] The section 136 includes a wall 146 of reduced thickness providing a recess 148 open to the exterior of the tool 120 through one or more passages 150 . The assembly 130 may include a sleeve 152 having an annular rim 154 comprising a pressure reaction surface. An O-ring or other seal 156 may seal between the rim 154 and the inside of the wall 146 to provide a piston operable by a pressure differential between hydrostatic pressure in the well acting through the passage 150 against the underside 158 of the rim 154 and pressure applied from above acting on the top 160 of the rim 154 . The sleeve 152 may normally be kept in place by a shear pin 162 or other similar device.
[0044] It will be seen that a pressure applied from above through the inside of the tool 120 passes through an opening 164 in the box body 138 and acts on the top 160 of the rim 154 . When the downward force applied in this manner sufficiently exceeds the upward force on the rim 134 by hydrostatic pressure outside the tool 120 , the shear pin 162 fails and the sleeve 152 moves from an upper position shown in FIG. 8 to a lower position shown in FIG. 9 .
[0045] The bottom of the sleeve 152 may be equipped with a suitable aid to fracture the upper disc 126 . This may be a pointed element 166 attached to the inside of the sleeve 152 in any suitable manner, as by a lattice work frame 168 .
[0046] As in the previously described embodiments, the isolation tool 120 may be used in any situation where it is desired to pressure separate one section of a hydrocarbon well from another. Assuming the tool 120 is run in a production string analogous to those shown in FIGS. 2 and 6 , pressure applied from above is sufficient to hydraulically set a packer (not shown) but is not sufficient to shear the pin 162 . After the packer (not shown) is set, additional pressure is applied from above which is sufficient to shear the pin 162 but is not sufficient to fracture the convex side of the disc 126 . When the pin 162 shears, the sleeve 152 moves downwardly with sufficient force that the point 166 impacts the frangible disc 126 thereby rupturing it. Pressure inside the tool 120 is sufficient to rupture the much weaker lower disc 128 because the pressure differential is applied to the concave side of the disc 128 .
[0047] Thus, in common with the tools 10 , 70 , the isolation tool 120 opens communication between the previously isolated parts of a well upon the application of pressure from above that is less than the rated capacity of the convex side of the upper disc 126 .
[0048] Referring to FIGS. 10-11 , an improved pressure disk 170 is illustrated having a generally hemispherical central section 172 providing a circular edge 174 , a convex outer surface 176 , a concave inner surface 178 and a cylindrical skirt 180 extending substantially from the circular edge 174 below the curved portion of the disk 170 . The cylindrical skirt 180 includes an inner cylindrical wall 182 and an outer cylindrical wall 184 providing an extended sealing area as shown in FIG. 11 where multiple sealing elements or O-rings 186 , 188 seal between the disk 170 and a housing 190 which may be part of an isolation tool 192 or other tool where a frangible pressure disk is necessary or desirable.
[0049] The advantage of the elongate cylindrical skirt 180 is it provides sufficient area for multiple sealing elements, such as a pair of O-rings or other seals or one or more seals with a backup seal or device. It is much simpler to seal against the outer cylindrical wall 184 than against a curved portion of the hemi-spherical central section 172 . In fact, seals heretofore used with hemispherical pressure disks of the type disclosed herein were crushed to accommodate and seal against the arcuate side of the pressure disk. Sealing against the cylindrical surface 182 is much simpler, more reliable, more reproducible and more efficient. Thus, the skirt 180 may be of any suitable length sufficient to provide a cylindrical surface of sufficient length to receive at least one seal member on the O.D. and, preferably, two seal members. Thus, in a typical situation in disks 170 of 2″ diameter and greater the skirt 180 may be at least 1″ long.
[0050] The disk 170 may be made of any frangible material, such as ceramic, porcelain or glass, i.e. from the same materials as the pressure disks previously described.
[0051] It will be apparent that the outer cylindrical wall 184 may be manufactured in a variety of techniques. One simple technique is to grind the outer diameter of a hemispherical disk to provide the cylindrical wall 184 . A preferred technique may be to manufacture the disk 170 with an elongate cylindrical skirt 180 as illustrated in FIGS. 10-11 and then grind the outer diameter to a smoothness compatible with O-ring type seals. This smoothness, known to machinists as a seal finish or O-ring seal finish is known more technically as 63-32 on a scale known as RMS or Root Mean Square. 7n this system, and simplified for purposes of illustration, the number is a measure, in microns, of the difference between the heights of small protrusions and the depths of small depressions in the surface. The smaller the number, the smoother the surface.
[0052] Although this invention has been disclosed and described in its preferred forms with a certain degree of particularity, it is understood that the present disclosure of the preferred forms is only by way of example and that numerous changes in the details of operation and in the combination and arrangement of parts may be resorted to without departing from the spirit and scope of the invention as hereinafter claimed.
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A down hole pressure isolation tool is placed in a pipe string and includes a pair of pressure discs having one side that is highly resistant to applied pressure and one side that ruptures when much lower pressures are applied to it. The weak sides of the pressure discs face each other. Rather than rupturing the discs by dropping a go-devil into the well, a first of the discs is ruptured or broken by the application of fluid pressure from the well head or surface. Formation pressure is then used, in different ways according to the different embodiments, to rupture the remaining disc.
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BACKGROUND OF THE INVENTION
[0001] This invention relates to gas turbine combustion systems and, specifically, to a fuel nozzle design which minimizes combustor damage during a combustion flame flashback or flame holding event.
[0002] A gas turbine combustor mixes large quantities of fuel and compressed air and burns the resulting mixture. Conventional combustors for industrial gas turbines typically include an annular array of cylindrical combustion “cans” in which air and fuel are mixed and combustion occurs. Compressed air from an axial compressor flows into the combustor. Fuel is injected through fuel nozzle assemblies that extend into each can. The mixture of fuel and air burns in a combustion chamber of each can. The combustion gases discharge from each can into a duct that leads to the turbine.
[0003] Combustion cans, designed for low emissions, include premix chambers and combustion chambers. Fuel nozzle assemblies in each combustion can inject fuel and air into the chambers of the can. A portion of the fuel from the nozzle assembly is discharged into the premix chamber of the can, where air is added to and premixed with the fuel. Premixing air and fuel in the premix chamber promotes rapid and efficient combustion in the combustion chamber of each can, and low emissions from the combustion. The mixture of air and fuel flows downstream from the premix chamber to the combustion chamber which supports combustion and under some conditions receives additional fuel discharged by the front of the fuel nozzle assembly. The additional fuel provides a means of stabilizing the flame for low power operation, and may be completely shut off at high power conditions.
[0004] A flashback or flame holding condition may occur in combustion cans having premix chambers. The premix chambers are not intended to support combustion. Flashback occurs when flame propagates into the premix chamber from the downstream combustion chamber, typically caused by momentary transient conditions. Flame holding occurs when a flame is initiated in the premixing zone, possibly by an external source such as a spark or hot foreign object ejected by the compressor, and the flame then stabilizes in a recirculation zone or weak boundary layer zone immediately downstream of the portion of the fuel nozzle assembly discharging fuel into the premix chamber. The damage resulting from flashback or flame holding may include burning combustor components not intended to be subjected to the heat of combustion. The damage caused by burning these combustor components may cause the components to malfunction and break up. If broken sections of the combustor flow into the combustion gas stream, they potentially may damage the hot gas path, e.g., turbine in the gas turbine.
[0005] Fuses in fuel nozzle assemblies prevent flame holding by diverting fuel away from the fuel nozzles for the premix chamber. The diversion of fuel from the premix chamber causes the abnormal flame to burn out and prevents further combustion in the premix chamber. However, conventional fuse designs, such as disclosed in U.S. Pat. No. 5,685,139, are not suited to all types of fuel nozzle assemblies. Accordingly, there is a need for novel designs of fuses.
BRIEF DESCRIPTION OF THE INVENTION
[0006] A fuel nozzle assembly for a combustor of a gas turbine has been developed comprising: a nozzle body having a front and an inner tube defining a fuel passage extending through the nozzle body; an outer tube around the inner tube and defining an air passage between the outer tube and the inner tube; a weakened region of the outer tube which burns through in event of a flashback thereby causing a portion of premix fuel to bypass the injectors and to be discharged from the weakened region; an expandable conduit arranged in the air passage and having an outlet adjacent the weakened region, wherein fuel flows through the expandable conduit when the weakened region of the outer tube burns through and the fuel flow is discharged from the conduit, through the weakened region and towards the front of the nozzle body, and a collar attached to the nozzle body, the collar including a premix fuel passage and ports discharging fuel from the collar, wherein the expandable conduit has an inlet open to the premix fuel passage.
[0007] A method has been developed for quenching a flashback condition in a combustor of a gas turbine, the method comprising: injecting fuel and compressed air from a fuel injector assembly to a premix chamber of the combustor, wherein the injected fuel and compressor air does not normally combust in the premix chamber; combusting the fuel and compressed in a combustion chamber downstream of the premix chamber in the combustor; providing air to the combustion chamber from a front of the injector assembly through an air passage extending through a nozzle body of the fuel injector; injecting fuel to the combustion chamber from a fuel passage having an outlet at the front of the injector assembly; opening an outlet of a conduit in response to a flashback condition adjacent the fuel injector assembly, wherein the outlet is proximate the front of the injector assembly and the conduit extends through the air passage; diverting fuel from the premix chamber to the conduit by the opening of the outlet, and quenching flames of the flashback condition by the diversion of fuel.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a side view showing in partial cross-section a conventional combustion can of a gas turbine.
[0009] FIG. 2 is a perspective view of a fuel nozzle assembly.
[0010] FIG. 3 is a perspective view of a fuse assembly that is incorporated in the fuel nozzle body of the fuel nozzle assembly.
[0011] FIG. 4 is a side, cross sectional view of the fuse assembly in the rear collar of the fuel nozzle assembly.
[0012] FIG. 5 is a side, cross-sectional view of a front portion of the nozzle body.
DETAILED DESCRIPTION OF THE INVENTION
[0013] FIG. 1 is side view, showing in partial cross section, a conventional combustor 10 of a gas turbine 12 that includes a compressor 13 (represented by compressor casing 14 ), and a turbine section 15 represented by a single turbine blade 16 . The combustor includes an annular array of combustion cans 18 arranged around the compressor casing 14 . The compressor 13 is driven by the turbine which is drivingly connected along a common axis to the compressor.
[0014] Pressurized air from the compressor enters each combustion can 18 the combustor 10 and flows (see air arrow 19 ) through an annular duct 20 formed between a cylindrical sleeve 22 and an inner cylindrical liner 24 of the can. Compressed air flows through the duct 20 towards the end cover assembly 26 of the can in a reverse flow direction to the combustion gases formed in the can (see combustion gas arrow 28 ). Air enters the combustion chamber 30 and premix chambers 32 in each can through various openings in the liner 24 and through the premixer inlets 25 in the fuel nozzle assemblies 34 .
[0015] A mixture of fuel and air is supplied to the premix chambers 32 and the combustion chamber by fuel nozzle assemblies 34 arranged at the front of the can and attached to the end cover. The fuel and compressed air mix in the premix chamber and flow to the combustion chamber 30 . The mixture burns in the combustion chamber and the resulting combustion gases flow (see combustion flow arrow 28 ) from the cans to a transition duct 36 that directs the combustion gases to the turbine blades 16 .
[0016] Each combustion can 18 includes a substantially cylindrical combustion casing 38 which is secured at an open aftward end to the compressor casing 14 . The forward end of the combustion can is closed by the end cover assembly 26 which may include conventional fuel supply tubes, manifolds and associated valves for feeding gas, liquid fuel and air (and water if desired) to the combustor can. The end cover assembly 26 supports multiple fuel nozzle assemblies 34 for each can. For example, fuel nozzle assemblies may be arranged in a circular array around a center nozzle assembly. These nozzle assemblies may be treated has having the same structure, at least for purposes of describing the fuse system.
[0017] FIG. 2 is a perspective view of a fuel nozzle assembly 34 . The nozzle assembly 34 includes a nozzle body 40 , a rear collar 42 and a rear section 44 that connects to the end cover assembly of a combustor can. Fuel and air is supplied to the end cover assembly which directs the fuel to the rear section of the fuel nozzle assembly. The rear collar 42 forms an outer ring of an annular air passage 48 that provides premix air to the premix chamber of the combustion can. Within the annular air passage 48 are radial vanes 50 that impart a spiral flow to the premix air flowing through the passage 48 . The vanes 50 contain fuel discharge ports 52 ( FIG. 4 ) through which fuel is discharged from the fuel nozzle assembly into the premix chamber, where it mixes with the air flowing in air passage 48 . One or more fuel gas passages and fuel discharge ports may be arranged in the vanes 50 . The front 46 of the nozzle body includes the forward fuel nozzle ports that deliver fuel directly to the combustion chamber in the combustor can.
[0018] FIG. 3 is a perspective view of a fuse assembly 54 that is incorporated in the fuel nozzle assembly and, specifically, in the collar and nozzle body. The fuse assembly 54 includes a cylindrical array of helical conduits 56 that extend from a cylindrical rear fuse base 58 mounted in the rear collar to a cylindrical front fuse and nozzle base 60 mounted in the front of the nozzle body. The conduits 56 may be brazed to the bases 58 , 60 . The helical shape of the conduits 56 allows the conduits to expand or contract in an axial direction, such as due to thermal expansion. The rear fuse base 58 includes openings 61 , 62 that are aligned with a fuel passage or fuel passages in the collar when the fuse base 58 is inserted in the rear collar. Arranging the openings 61 , 62 in two or more rows (as shown in FIG. 3 ) allows the multiple conduits 56 to receive fuel from multiple premix fuel passages in the collar 42 . The openings 61 , 62 lead to respective passages in the fuse base 58 and the conduits 56 .
[0019] Fuel from the fuel passage, that would normally flow to the premix chamber, flows through the rear fuse base 58 and the helical conduits 56 to the nozzle base 60 when the fuse is activated by a flashback event. After the fuse has been activated, the fuel flowing through the helical conduits 56 diverts fuel from the premix chamber(s) to prevent further combustion of fuel in that chamber(s).
[0020] Openings 63 , 64 on the front fuse and nozzle base 60 allow the fuel from the helical conduits 56 to discharge through the front of the nozzle body and into the combustion chamber. The openings 63 , 64 are normally blocked to prevent the flow of fuel through the helical conduits. When the openings 64 are not blocked, the flow of fuel through helical conduits diverts fuel from the premix chamber, so as to quench a flash back or flame holding condition. The front fuse and nozzle base also includes air nozzles 66 for air discharged from the front of the fuel nozzle. The discharged air forms an air curtain around the fuel flowing from the front 46 of the fuel nozzle.
[0021] FIG. 4 is a side, cross sectional view of the fuel nozzle assembly and, specifically, the rear collar 42 and rear section 44 of the fuel assembly. The rear fuse base 58 is mounted in the rear collar. A cylindrical gas passage 68 is defined by an inner tubular section 69 aligned with the axis of the fuel nozzle and extending through the rear section 44 , the rear collar 42 and the nozzle body 40 of the fuel assembly. An annular gas passage 70 is defined between the inner tube 69 and an outer wall of the passage. Fuel flows through the annular fuel gas passage 70 from the rear section 44 of the fuel assembly to the rear collar 42 .
[0022] As indicated by flow arrow 72 , the fuel gas flows from the gas passage 70 , through passages 71 in the rear fuse base 58 , the openings 61 , 62 that lead to the radial vanes 50 of the rear collar, out the fuel ports 52 in the vanes and into the premix chamber. The gas flows as indicated by arrow 72 , unless the fuse has been activated. An single flow arrow 72 is shown to indicate a premix gas path through the rear collar 42 and passages in the vanes 50 . However, one or multiple premix gas paths may be in the rear collar and vanes. Each of the premix gas paths may be associated with a different one of the helical conduits 56 . Further each of the premix gas paths may be associated with one or more of the helical conduits.
[0023] When the fuse is activated, the gas flows from passage 70 , through the passages 71 in the rear fuse base 58 and to the helical conduits 56 as indicated by flow arrow 74 . The conduits 56 provide a flow path that diverts most of the fuel in passage 70 away from the vanes 50 and the fuel ports 52 .
[0024] The helical conduits 56 are arranged in an annular air passage 76 between the tube 69 of the gas passage 68 and an outer tubular casing 78 of the nozzle body 40 . Air enters through ports 77 in the rear collar 42 and flows into the air passage 76 . The air flows through the passage 76 , across outer surfaces of the helical conduits 56 and to the front fuse and nozzle base. The size and number of the conduits 56 are such that the air flowing through the passage 76 is sufficient for the curtain of air flow needed at the front of the fuel nozzle. Preferably, the helical conduits occupy less than one half of the volume of the passage 76 .
[0025] FIG. 5 is a side, cross-sectional view of a front portion of the nozzle body 40 . The helical conduits 56 are arranged in the annular air passage 76 defined between the inner cylindrical tube 69 of the gas passage 68 and the tubular casing 78 of the nozzle body 40 . The helical shape of the conduits 56 allows for axial expansion of the conduits. The front fuse and nozzle base 60 is seated between the wall of the gas passage 68 and the tubular casing 78 .
[0026] The openings 64 in the front fuse and nozzle base 60 are adjacent a weakened section 80 , e.g., a relatively thin annular section, of the casing 78 . The weakened sections 80 may be a segmented annular region of the casing 78 that has been machined to remove some of the thickness of the casing wall adjacent the openings 64 of the base 60 . The weakened sections 80 are susceptible to burning through in the event of a flashback. Once burned through, the opened weakened sections 80 allow fuel to flow out the openings 64 in the fuse and nozzle base 60 and flow through the helical conduits 56 . The flow of fuel through the helical conduits diverts fuel from the premix chamber and starves and quenches any flame occurring in the premix chamber to stop the flash back condition.
[0027] The inner cylindrical wall of the gas passage 68 has a front end that fits into a quasi-conical inner sleeve assembly 82 that supports the front nozzle 84 . The inner sleeve assembly allows for thermal expansion between the cylindrical wall of the gas passage and the front nozzle. Air from the annular passage 76 flows through the front fuse and nozzle base 60 and through swirl vanes 86 before being discharged around the front of the center fuel discharge nozzle ports 88 for the gas passage 68 .
[0028] While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
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A fuel nozzle assembly for a combustor of a gas turbine including: a nozzle body having a front and an inner tube defining a fuel passage extending through the nozzle body, wherein the front proximate to a combustion section of the combustor; an outer casing around the inner tube, wherein an air passage is defined between the outer casing and the inner tube; a gas conduit arranged in the air passage and having an outlet proximate to the front of the nozzle body, wherein fuel starts flowing through the expandable conduit only after a flashback condition occurs in the combustor, and a premix fuel passage and port discharging fuel to a premix section of the combustor, wherein the gas conduit has an inlet open to the premix fuel passage.
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BACKGROUND OF THE INVENTION
This invention relates to multiple pole coupling discs of the type used in an electromagnetic coupling such as an electromagnetic clutch or brake. The coupling disc may be part of a rotary or non-rotary field or may be a rotary or non-rotary armature.
A typical electromagnetic coupling is disclosed in Silvestrini et al U.S. Pat. No. 4,187,939 and, in that particular case, the coupling is an electromagnetic clutch having a rotary armature disc made of magnetic material such as steel and having a field with a rotary coupling disc or rotor which also is made of magnetic material. When the coil of the field is excited, magnetic flux threads a path between the rotor and the axially opposing armature and attracts the armature into engagement with the working face of the rotor to couple the two for rotation in unison.
In the coupling disclosed in the Silvestrini et al patent, the armature is formed with a ring of angularly spaced "banana" slots while the rotor is formed with two concentric rings of angularly spaced banana slots located on opposite sides of the ring of slots in the armature. The banana slots form high reluctance air gaps causing the rotor and armature to define four magnetic poles which increase the torque of a coupling having a coil of a given diameter. By forming an additional ring of slots in each of the rotor and armature, the coupling may be constructed as a six-pole coupling with even higher torque capacity.
Until just recently, the banana slots conventionally have been stamped in the rotor and armature. Presently available stamping techniques dictate that, as a general rule, the radial width of the slots cannot be substantially less than approximately 3/4 the thickness of the disc. As a result, difficulty is encountered in stamping multiple rings of slots in a comparatively thick disc which is relatively small in diameter. In addition, stamping of the slots leaves burrs at the edges of the slots and tends to impose restrictions on the location of the slots in the disc and on the shape of the slots. It is difficult to maintain concentricity between adjacent rows of slots and it is difficult to keep all portions of the disc of a uniform thickness. The design of the disc thus tends to be dictated by tooling considerations rather than magnetic characteristics.
As an alternative to slotting the rotor and armature to form high reluctance air gaps, channels may be machined in the disc and then filled with non-magnetic material to define high reluctance barriers between the poles. Subsequently, the disc is machined to remove the bottoms of the magnetic channels and eliminate the flux leakage paths which otherwise would be created across the bottoms of the channels. This manufacturing process is relatively expensive and becomes even more so when each disc is formed with two or more high reluctance rings.
Formation of the slots in a coupling disc through the use of a laser beam is disclosed in commonly assigned Booth et al U.S. Pat. No. 4,685,202. In the method disclosed in that patent, the laser beam forms continuous slots which are immediately backfilled with non-magnetic material. Alternatively, the method contemplates the formation of angularly spaced banana slots separated by non-magnetic bridges which are formed by backfilling the spaces between the slots with non-magnetic material.
The methods disclosed in the aforementioned Booth et al patent represent remarkable improvements in the art of magnetic coupling discs. Even those methods, however, have some limitations. For example, the formation of slots of any substantial radial width requires the use of a very powerful laser having a beam of substantial diameter. In addition, backfilling of the slots or portions thereof imposes some restriction on the cross-sectional shape and/or the orientation of the slots.
Commonly assigned Booth et al U.S. application Ser. No. 133,145, filed Dec. 14, 1987now U.S. Pat. No. 4,818,840, discloses another method of forming slots in an electromagnetic coupling disc through use of a laser. Specifically, the laser beam traces around the perimeter of each slot to be formed and forms the slot by cutting a slug of material from the disc. This method enables relatively precise control of the shape, location and edge finish of the slots but is somewhat slow from a manufacturing standpoint since the entire perimeter of each slot must be traced by the laser beam. In addition, it is necessary to reprogram the path of travel of the laser beam each time the slot configuration, location or size is changed.
SUMMARY OF THE INVENTION
The general aim of the present invention is to provide a new and improved electromagnetic coupling disc, and a method of making the same, which enables a coupling having a coil of a given diameter to produce higher torque and which, at the same time, is less vulnerable to variations in the manufacturing process.
A more detailed object is to achieve the foregoing through the provision of a coupling disc in which the magnetic poles are delineated by closed-end grooves in the non-working face of the disc rather than through slots so as to avoid many of the manufacturing difficulties which arise in the formation of slots by stamping or by laser cutting.
An important object of the invention is to form the grooves in the disc by means of a relatively simple but precise metal rolling method.
Still another object is to use the material displaced by the rolling method to form various functional components on the disc.
The invention also resides in the provision of strengthening bridges between adjacent grooves and in the novel formation of a second set of grooves in the working face of the disc in order to better define and delineate the magnetic poles of the disc.
These and other objects and advantages of the invention will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing one type of a new and improved electromagnetic coupling disc incorporating the unique features of the present invention.
FIG. 2 is an enlarged perspective view of a portion of the disc shown in FIG. 1.
FIG. 3 is an enlarged top plan view of the disc as taken along the line 3--3 of FIG. 1.
FIG. 4 is an enlarged cross-section taken along the line 4--4 of FIG. 3 and schematically shows the grooves being formed in the non-working face of the disc.
FIG. 5 is a cross-section taken along the line 5--5 of FIG. 3.
FIG. 6 is a fragmentary view of the working face of the disc as taken along the line 6--6 of FIG. 5.
FIG. 7 is a cross-section generally similar to FIG. 4 but shows a variation of the groove formation in the working face of the disc.
FIG. 8 is a cross-section similar to FIG. 7 but shows still another variation of the groove formation in the working face of the disc.
FIG. 9 is an enlarged fragmentary view of a portion of a disc and shows yet another variation of the groove formation in the working face of the disc.
FIG. 10 is a cross-sectional view of a coupling disc which is formed with an integral locating flange for a bearing.
FIG. 11 is a view similar to FIG. 10 but shows a coupling disc which is formed with an integral locating flange for a pulley.
FIG. 12 is another view similar to FIG. 10 but shows a coupling disc which is formed with an integral grease guard.
FIG. 13 is still another view similar to FIG. 10 but shows a coupling disc with a modified magnetic pole construction.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The drawings illustrate the present invention as being incorporated in a coupling disc 20 for use in an electromagnetic coupling such as an electromagnetic brake or clutch. While the disc could be an armature, it herein is shown as forming part of a clutch rotor 21 which may, for example, be of the type disclosed in the aforementioned Silvestrini et al patent. In this particular instance, the rotor is circular in shape and includes an axially extending outer flange 22 and an axially extending inner hub 23 which preferably are integral with one face 24 of the disc 20. The opposite face 25 (FIG. 4) of the disc forms the working face of the rotor 21 and is adapted to frictionally engage the armature of the clutch. The flange 22 and the hub 23 define the outer and inner pole rings, respectively, of the rotor 21.
As is conventional, the rotor 21 is made of low reluctance magnetic material such as steel. While the rotor could be cast and then machined, it preferably is formed by a stamping or drawing operation.
The specific rotor 21 which has been illustrated in FIGS. 1 to 6 forms part of a six-pole clutch and thus the disc 20 includes three concentric rings 30 (FIG. 3) which carry less magnetic flux than the remaining areas of the disc. One magnetic pole is defined by that annular area of the disc located radially inwardly of the inner ring, two poles are defined by the annular area between the inner ring and the middle ring, two additional poles are defined by the annular area between the middle ring and the outer ring, and the sixth pole is defined by the annular area located outwardly of the outer ring.
In accordance with the primary aspect of the present invention, the rings 30 are defined by closed-end grooves which are formed in the non-working face 24 of the disc 20 in a unique manner. As compared to coupling discs having magnetic barriers formed by either open slots or by slots filled with non-magnetic material, the grooved disc 20 is easier to manufacture on a high speed production basis, is less vulnerable to minor manufacturing variations and is less subject to fatigue failure.
The preferred method of forming the grooves 30 in the non-working face 24 of the disc 20 is illustrated in FIG. 4. In carrying out this method, provision is made of a circular ring-like die 31 having a forming face 32 adapted to be disposed in opposing relation with the non-working face 24 of the disc 20. Formed on and projecting axially from the forming face of the die are three radially spaced and circumferentially extending ribs 33 which are used to form the grooves 30.
After the rotor 21 has been stamped, it is placed on the die 31 with the outer and inner pole rings 22 and 23 straddling the die and with the non-working face 24 of the disc 20 lying against the crests of the ribs 33. With the rotor 21 in this position, the rotor and the die 31 are slowly rotated in unison about the axis of the rotor. During such rotation, a roller 35 (FIG. 4) is traversed radially back and forth across the working face 25 of the disc 20 and is forced in a direction pressing the non-working face 24 of the disc against the ribs 33 of the die 31. The roller rotates about an axis which is perpendicular to the disc and, as it traverses across and pushes on the working face 25, it causes the ribs to displace the metal of the non-working face 24 of the disc and thereby form the grooves 30 by cold flow of the metal. The height of the ribs is less than the thickness of the disc and thus the grooves are formed with closed ends or bottoms and do not interrupt the working face 25 of the disc.
A typical disc 20 has a thickness of approximately 0.165" and is formed with grooves 30 having a nominal depth of 0.120". Each groove preferably is formed with a concavely curved closed end and is formed with side walls which flare away from one another as they progress from the closed end of the groove toward the non-working face 24 of the disc 20. By way of example, each side wall may flare at an angle of approximately fifteen degrees.
The construction of the disc 20 as described thus far enables the rotor 21 to effectively function in a multiple pole electromagnetic coupling. The voids created by the grooves 30 establish air gaps which are resistant to the flow of magnetic flux and thus cause magnetic poles to be set up on opposite sides of each groove. While there is some flux leakage through those webbed areas located between the closed ends of the grooves 30 and the working face 25 of the disc 20, such flux leakage is not sufficiently great to be detrimental in certain types of couplings. When formed as described, the grooves 30 are of a very precise shape, are very accurately located and are precisely concentric. The webbed areas at the closed ends of the grooves 30 have virtually the same thickness at all three rows of grooves and, in addition, there are virtually no variations from rotor-to-rotor. The existence of the continuous webs at the closed ends of the grooves strengthens the disc 20 and makes the disc less likely to fail in fatigue when compared to a disc with through-slots. Moreover, the grooves 30 enable the use of a disc 20 of smaller radial width than is the case when a disc is slotted by conventional stamping techniques. This permits a coupling capable of producing torque of a given magnitude to be constructed as a smaller-diameter package.
In the preferred embodiment of the disc 20, the grooves 30 of each row or ring are spaced angularly from one another and are separated by radially extending bridges 36 (FIG. 2) which increase the structural integrity of the disc. Herein, the bridges 36 are formed simply by interrupting the ribs 33 of the die 31 at angularly spaced locations. As a result, the disc 20 is not grooved at those locations but instead is left with bridges 36 which have a thickness approximtely equal to the original thickness of the disc. To reduce stress areas, the ends of the ribs 33 are concavely radiused so that the bridges 36 are convexly radiused when viewed from the non-working face 24 of the disc 20 as is apparent from FIG. 2. The bridges 36 of adjacent rings of grooves 30 are offset angularly from one another in order to reduce flux leakage between adjacent rings (see FIG. 3).
With certain couplings, the rotor 21 may be used as constructed in the manner described above and without any machining operations whatsoever. In some instances, it may be desirable to just lightly machine the working face 25 of the disc 20 in order to bring the working face into more precise squareness and flatness and to remove any small dimples which might have been created during formation of the grooves 30. Such machining improves the magnetic characteristics of the disc but, since only light machining is required, it may be accomplished faster and easier than is the case where slots are stamped in the disc.
To further improve the magnetic characteristics of the disc 20, shallow and circular grooves 40 may be formed in the working face 25 of the disc as illustrated in FIGS. 5 and 6. The grooves preferably are circumferentially continuous and, in the embodiment shown in FIGS. 5 and 6, are alined radially with the grooves 30. The grooves 40 are not so deep as to extend completely to the grooves 30 or to the non-working face 24 of the disc 20. Instead, each groove 40 has a nominal depth of only about 0.035" and thus an axially thin web 41 (FIG. 5) having a nominal thickness T of about 0.010" is left between radially alined grooves 30 and 40. The grooves 40 reduce flux leakage, establish better magnetic pole definition in the disc 20 and may be formed either by conventional machining or by laser cutting. In each case, less time is required than is necessary for through-slots since the grooves 40 extend only through a fraction of the thickness of the disc.
A disc 20A with a modified working face 25A is shown in FIG. 7. In this instance, each groove on the working face includes a portion 45 of relatively large radial width immediately adjacent the working face and a portion 46 of smaller radial width adjacent the closed end of the groove 30A. While a stepped groove configuration of this type is more difficult to manufacture, it establishes even better definition of the magnetic poles while maintaining relatively good structural integrity.
A disc 20B with yet a different type of working face 25B is shown in FIG. 8. In this instance, the grooves 40B in the working face are offset radially outwardly from the grooves 30B in the non-working face 24B. Such offset increases the effective length of the torque arm of each pole and enables the coupling to transmit torque of a higher magnitude.
In the disc 20C shown in FIG. 9, the grooves 40C in the working face 25C are not formed with parallel side walls but instead each groove is formed with inclined side walls which flare away from one another at an angle X of about twenty degrees as the side walls progress toward the working face. As a result, each groove 40C has a relatively large radial width at the working face 25C and tapers to a progressively smaller radial width. By virtue of this arrangement, each groove 40C becomes narrower as the coupling wears in and as the air gap between the disc 20C and the coacting armature increases. This enables the static and dynamic torque of the coupling to be relatively high during the early life of the coupling and to modulate as the coupling wears in.
FIG. 10 shows a disc 20D in which the grooves 30D are of a multi-stepped configuration. In addition, a circular flange 50 projects radially inwardly from the inner side of the inner pole ring 23D adjacent the junction of that ring with the disc 20D. The flange 50 serves as a locator and stop shoulder for a mounting bearing 51 for the rotor 21D. The flange 50 is integral with the inner ring 23D and is created by the excess metal resulting from rolling the grooves 30D in the disc 20D. That metal is directed toward the inner ring 23D by appropriate dies and/or rollers and is extruded to form the flange 50. This takes advantage of the excess material and eliminates the need for an initially thick inner ring where much of the material must be machined away to leave a flange. In the present instance, no machining is required to produce and locate flange 50.
A similar concept is embodied in the disc 20E shown in FIG. 11. In this instance, however, the excess material resulting from rolling the grooves 30E is directed outwardly to form a circular flange 53 which projects radially outwardly from the outer side of the outer pole ring 22E adjacent the junction of that ring and the disc 20E. The flange 53 may serve as a locator and stop shoulder for a drive pulley 54.
In the disc 20F shown in FIG. 12, the excess material is extruded axially to form a circular flange 55 which projects axially outwardly from the working face 25F of the disc 20F adjacent the inner side of the inner pole ring 23F. The flange serves as a guard to help protect the working face 25F from lubricants in the area of the bearing 51.
FIG. 13 shows a disc 20G with a radially inwardly projecting flange 50' formed in the same general manner as the flange 50 of the disc 20D of FIG. 10. In this embodiment, however, a groove 60 is rolled into the working face side of the flange 50' to create an additional magnetic pole face.
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The non-working face of a coupling disc (i.e., the armature or rotor) of an electromagnetic coupling such as a clutch or brake is formed with radially spaced rows of angularly spaced grooves separated by radially extending bridges. The grooves terminate short of the working face of the disc and delineate magnetic poles in the disc. In some embodiments, radially spaced rows of grooves also are formed in the working face of the disc. In still other embodiments, excess metal resulting from rolling of the grooves in the non-working face of the disc is used to form integral locating flanges or the like adjacent the disc.
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BACKGROUND OF THE INVENTION
The invention concerns a mounting device for fixing a furniture hinge including a base plate to be fixed to a furniture part, in particular a side wall of a furniture carcass. A fixing device is provided for preferably releasably fixing the hinge to the mounting device, wherein the fixing device is mounted moveably on the base plate.
In the pivotal movement of furniture parts connected pivotably relative to each other by a hinge from the closed position into the open position there is basically the risk that collisions with adjacent furniture parts can occur. That involves in particular furniture doors which are pivotable by the hinge and which serve for closing off a furniture carcass and which can collide with adjacent furniture doors or other projecting furniture parts upon being opened or closed.
To resolve that problem, AT 369 107 discloses an especially constructed wide-angle hinge with which it is possible to achieve a lifting-away movement for pivoting the door from the end edge of the furniture carcass, during the opening movement of the furniture door. In that case, fixed to the furniture carcass is a mounting housing having two slots which are disposed one behind the other and in which pins connected to the hinge arm are moveably mounted, whereby the hinge arm is guided displaceably and partially pivotably. In that situation, a gear meshing with two toothed racks which are moveable relative to each other serves to drive the hinge arm whereby the latter moves relative to the mounting housing which is fixed to the furniture carcass and a greater opening movement of the furniture door is achieved.
DE 43 18 607 also discloses a wide-angle hinge in which the door is pivoted away from the furniture carcass during the opening movement to avoid collisions with adjacent furniture doors. Once again, arranged in a mounting housing fixed to the furniture carcass are a plurality of slots in which pins connected to the hinge arm are displaceably mounted. To drive the hinge arm, a pulling means is fixed in the hinge cup, the pulling means being held in a constantly stressed condition.
The above-mentioned hinges suffer from the disadvantage of a complicated structure which is thus susceptible to faults. As these hinges are not necessary for all furniture doors, the complication and expenditure involved in the production of those kind of hinges is excessively high.
Another possible way of achieving an increased opening movement is disclosed in WO 2006/053364. The hinge described there has an intermediate portion between the hinge cup and the hinge arm. The intermediate portion is positively coupled to the hinge arm by two levers, and the levers are rotatably mounted both to the intermediate portion and also to the hinge arm by suitable spindles. The intermediate portion which is moveable relative to the hinge arm provides that the furniture door has an increased motion component in a direction out of the furniture carcass.
DE 34 07 174 C2 also discloses a cross-link hinge with an increased opening movement, which is made possible by a two-part hinge arm. A lower part of the hinge arm is fixedly secured to a mounting plate on the furniture carcass. Arranged on the moveably mounted upper part of the hinge arm is a hinge lever having a gear segment meshing with a toothed bar on the lower part. The hinge lever is connected to a hinge arm of the cross-link hinge, thereby permitting motional coupling of the hinge arm and the upper part. Besides the disadvantage that the increased opening stroke movement is made possible only for cross-link hinges, the hinge arm has to be connected to the base plate in a complicated structure with a complex fixing device, thereby involving a particularly high level of assembly complication and expenditure. In addition, that device has the disadvantage that further moveably mounted small parts are added to the parts which are already present in the hinge and which are moveable relative to each other, thereby increasing the complexity and susceptibility to defect of the hinge.
The disadvantage of these types of hinge is that they are in turn designed only for a specific purpose of use, thereby giving a high level of complication and expenditure both for the hinge manufacturer and also for the assembly fitter who must always have all possible types of hinge available to him.
However, a device which is independent of the hinge and with which the problem of collisions can be resolved in the case of an excessively small opening movement is desirable, in which respect the device can be used with a large number of the commercially available hinges.
On the other hand the extent of the increase in the opening movement, that is linked to that hinge, may still be too slight for many uses. For that situation it would be necessary to provide a device which permits an additional increase in the opening movement.
SUMMARY OF THE INVENTION
Therefore, the object of the invention is to provide such a device with which the above disadvantages are avoided and which provides a solution to the collision problems in the case of furniture parts which are pivotable by means of hinges, as independently of the hinge itself as possible.
A mounting device to which furniture hinges are fixed serves to attain that object. The mounting device itself has a base plate which is to be fixed to a furniture part for example by screws or other fixing means. In particular, the base plate is to be fixed to a side wall of a furniture carcass, in which case the furniture hinge serves for opening and closing of a furniture door.
The mounting device further includes a fixing device, by way of which the hinge is fixed to the mounting device. Preferably, a releasable fixing of the hinge permits simple fitment and removal of the hinge when the mounting device is already fixed in place. The hinge is fixed with a fitment portion to the mounting device. That fitment portion can be, for example, the hinge arm of the hinge.
The fixing device itself is mounted moveably to the base plate whereby a hinge fixed to the fixing device is also mounted moveably to the base plate.
The mounting device further includes a connecting element mounted moveably to the base plate, wherein that connecting element is moveable by way of at least one hinge lever. Besides the fixing device, the connecting element also serves for connecting the hinge to the mounting device. For that purpose, the connecting element can be fixed to a part which is moveable in the opening and closing movement of the hinge. By virtue of the fact that, in the condition of being connected to the hinge, the connecting element is fixed to a part of the hinge that is moved in the opening and closing movement of the hinge, and also moves during that movement with the moveable part of the hinge, the movements of the connecting element and the moveable part of the hinge to which the connecting element can be fixed are coupled.
Insofar as it is now provided that the fixing device is moveable relative to the base plate by way of the hinge lever so that the connecting element is mounted moveably to the base plate, the movement of the connecting element that is coupled to the movement of the hinge can be transmitted to the fixing device. The extent and the direction of the movement of the fixing device are dependent on the movement of the connecting element which controls the movement of the fixing device.
In the mounted condition of the hinge, the hinge is moved by the mobility of the fixing device together with the fixing device relative to the base plate, the movement being guided and controlled by the connecting element. If accordingly during the opening stroke movement of the fitted hinge, the part moveable on the hinge moves outwardly in the furniture carcass, the coupling effect means that the fixing device and therewith the hinge fixed to the fixing device are also moved outwardly whereby the opening stroke movement of the hinge is increased. In that case, the at least one hinge lever affords a structurally simple method of coupling and guiding the movement, without complicated pulling devices which are susceptible to defects or pin arrangements which are guided in slots.
Because the mounting device and the hinge to be fixed to the mounting device are separate components, the increased opening stroke movement is achieved independently of the hinge, by the mounting device. If a hinge is used which itself already has an increased opening stroke movement, those increases in the opening movements are added together and provide overall an even greater opening movement. The mounting device according to the invention, however, can also be used in relation to commercial hinges without an increased opening movement, whereby the increase in the opening stroke movement is effected by the mounting device and independently of the hinge itself.
Insofar as that increase in the opening stroke movement is to be attributed to the mobility of the fixing device relative to the base plate, large parts of commercial hinges can be connected to such a fixing device insofar as the latter is designed for fixing such hinges. Depending on the respectively prevailing factors in respect of the furniture parts to be pivoted, the mounting fitter can then decide whether he uses a commercial non-moveable mounting device or a mounting device according to the invention with the moveable fixing device. It is possible, however, in both cases to use the same type of hinge, whereby both the manufacturing complication and expenditure and also the mounting complication and expenditure are reduced.
In a preferred embodiment of the invention, the connecting element can be fixed to an outside, preferably to the top side, of the moveable part of the hinge. That permits particularly simple mounting and a lever arm which is as large as possible for the hinge lever, by way of which the connecting element is moveable. After the hinge is fitted on the fixing device, for example with the hinge arm, the connecting element is connected to the outside of the moveable hinge part, whereby coupling between the connecting element and the fixing device is implemented in a simple manner by way of the hinge lever. In general, the fixing device is arranged at the underside of the hinge so that the lever arm of the hinge lever amounts to the spacing between the top side of the moveable part of the hinge and the underside of the hinge if the connecting lever is fixed to the top side of the moveable part of the hinge, as is preferred.
In an embodiment of the invention, the fixing device which is moveable relative to the base plate by way of the hinge lever is moved relative to the base plate with a linear component when the hinge is opened or closed in the mounted condition. By virtue of a linear component, the fixing device can be moved outwardly for example in a furniture carcass, during the opening movement of the furniture door, with a linear motion component whereby the spacing of the furniture door relative to the closing edge of the furniture carcass is increased. In the reversed closing movement, that spacing is reduced by a linear movement of the fixing device into the interior of the furniture carcass.
In a preferred embodiment of the invention, the hinge arm can be clipped on to the fixing device. For that purpose, the fixing device has latching elements which are known in the state of the art and which can engage into holding elements or arresting elements corresponding thereto on the hinge arm, thereby affording a snap-action connection. A hinge which can be clipped on permits particularly simple fixing of the hinge to the mounting device. The latching or arresting elements can be resilient or spring-loaded. Preferably disposed in the hinge is a release device with which the snap-action connection can be released again so that the hinge can be easily removed from the mounting device. A release button with which the connection to a latching element can be released serves for example as the release device. For that purpose, the arresting element can be partially rotated about an axis with the release button. Releasable snap-action connections of that kind for fixing hinges to mounting plates are known in the state of the art.
In an embodiment of the invention, the connecting element can be clipped to the moveable part of the hinge. For that purpose, the hinge or the connecting element has latching elements which engage into arresting elements corresponding thereto on the respective other part and permit those parts to be connected. Once again, the latching elements and/or the arresting elements can be resilient or spring-loaded and there can be a release device. It can however also be provided that the connecting element is screwed to the moveable part of the hinge or fixed in some other fashion.
In an embodiment of the invention, the connecting element has a plate-shaped or a profile-shaped part or is at least in part of a plate-shaped or profile-shaped configuration to bear against the moveable part of the hinge in areal relationship. The profile-shaped part can at least partially embrace the moveable part of the hinge. That permits an efficient and simple way of fixing the connecting element. At the same time, the hinge movement can be transmitted uniformly to the connecting element.
In a further embodiment, the fixing device is substantially plate-shaped. Deviations from the plate shape are afforded for example by mounting lugs for moveably mounting the hinge lever, by way of which the connecting element is coupled to the fixing device, or the latching or arresting elements for fixing the hinge. The fixing device however can also have a receiving plate to which a fitment portion of the hinge can be fixed. The receiving plate can also be part of the fixing device which has a substantially plate-shaped configuration. In the case of fixing the hinge arm, the receiving plate preferably has an elongate shape adapted to the shape of the hinge arm.
In a preferred embodiment of the invention, the connecting element is in the form of a lever. Preferably in that respect, there is provided a two-part lever, thereby affording desirable kinematic relationships in conjunction with the hinge lever, by way of which the connecting element is connected to the fixing device.
In an embodiment, the fixing device is hingedly connected to the at least one hinge lever. For that purpose, there can be a mounting lug for the at least one hinge lever, with the hinge lever being mounted rotatably to the mounting lug. The connecting element is mounted pivotably relative to the fixing device by way of the hinge lever.
For moveably mounting the hinge lever to the base plate, a mounting lug to which the hinge lever is rotatably mounted can be provided.
A further method of moveably mounting the at least one hinge lever to the base plate involves a gear or a gear segment, by which the hinge lever is mounted rotatably to the base plate. In that case, the hinge lever is mounted both rotationally and also moveably with a translatory movement by way of the gear or the gear segment.
As a counterpart to the gear or gear segment arranged on the base plate, at least one toothed bar meshes with the gear or the gear segment, and also serves for moveably mounting the hinge lever to the base plate.
At least one further hinge lever can be provided for moveably mounting the fixing device to the base plate. Additionally or alternatively, a guide device can be arranged on the base plate, by which the movement of the fixing device is guided relative to the base plate.
For hinges in which the hinge arm is moved during the opening and closing movement in the mounted condition of the hinge, the mounting device can have such a configuration that the connecting element can be fixed to the hinge arm.
In addition, hinges are known in the state of the art, in which there is an intermediate portion which is mounted moveably on the hinge arm and which is preferably coupled to the hinge arm by at least two levers. In the mounted condition of the hinge, that intermediate portion is moved relative to the hinge arm which is fixedly joined to the furniture carcass. In that case, the mounting device has such a design that the connecting element can be connected to that intermediate portion which represents the moveable part of the hinge.
For that purpose, the dimensions of the at least one hinge lever and the connecting element are adapted to the dimensions of the hinge arm or to the dimensions and the arrangement of the intermediate portion mounted moveably to the hinge arm.
The invention also concerns an arrangement having a hinge, in particular a wide-angle hinge, and a mounting device as described above.
In an embodiment, the hinge has a hinge arm fixable to the fixing device. In addition, an intermediate portion can be mounted to the hinge arm and is preferably coupled to the hinge arm by at least two levers. In that case, the connecting element can be fixed to the intermediate portion.
The invention further concerns an article of furniture comprising a furniture carcass and a furniture door mounted moveably to the furniture carcass. A mounting device as described above is mounted to the furniture carcass, and a hinge, preferably a wide-angle hinge, for opening and closing the furniture door, is fixed to the mounting device.
BRIEF DESCRIPTION OF THE DRAWINGS
Further details and advantages of the present invention are described more fully hereinafter by the specific description with reference to the drawings, in which:
FIGS. 1 a through 1 d are plan views of a mounting device known in the state of the art with a fixed hinge in various open positions,
FIGS. 2 a through 2 c are perspective views of a hinge fixed to a mounting device according to the state of the art in two different open positions and a separate view of those components,
FIGS. 3 a through 3 d are plan views of a first embodiment of the mounting device according to the invention with fixed wide-angle hinge in various open positions,
FIGS. 4 a and 4 b are perspective views of the first embodiment of the mounting device according to the invention with fixed wide-angle hinge in various open positions,
FIG. 5 shows a mounting device of the first embodiment, mounted to a furniture carcass, with fixed wide-angle hinge and furniture door fixed thereto in the closed position,
FIGS. 6 a through 6 c are perspective views of the first embodiment of the mounting device according to the invention in various operating positions and a related exploded view,
FIGS. 7 a through 7 d are plan views of a second embodiment of the mounting device according to the invention with fixed wide-angle hinge in various open positions,
FIGS. 8 a and 8 b are perspective views of a second embodiment of the mounting device according to the invention with fixed wide-angle hinge in various open positions,
FIG. 9 shows a mounting device of the second embodiment, mounted to a furniture carcass, with fixed wide-angle hinge and furniture door fixed thereto in the closed position, and
FIGS. 10 a through 10 c are perspective views of the second embodiment of the mounting device according to the invention in various operating positions and a related exploded view.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 a shows a plan view of a mounting plate 4 in the state of the art, mounted to a side wall 2 of a furniture carcass. Fixed to the mounting plate 4 is a wide-angle hinge 1 , by which a furniture door 3 can be opened and closed. Like the adjacent furniture door 3 a the furniture door 3 is of a great thickness d. The hinge 1 is in the end position defined by the closed condition.
In this case the wide-angle hinge 1 is fixed to the mounting plate 4 with a first fitment portion—here the hinge arm 11 . With the second fitment portion—here the hinge cup 12 —the hinge is fixed to two pivotably mounted furniture doors 3 , relative to the side wall.
The intermediate portion 10 is moveable relative to the hinge arm 11 by two hinge arm levers 13 and is positively coupled to the hinge arm 11 by the levers 13 , wherein the levers 13 are mounted rotatably both on the intermediate portion 10 and also on the hinge arm by way of suitable spindles 14 . By that intermediate portion 10 , it is possible for the furniture parts 2 and 3 not only to be pivoted relative to each other but also for their spacing from each other to be increased in the pivotal movement, that is to say to afford an increased opening stroke movement. For that purpose, the intermediate portion 10 is pivoted by the levers 13 at the first end position shown in FIG. 1 a beyond the hinge arm 11 and prolongs same to the end position shown in FIG. 1 d , defined by the completely open position. That means that the two fitment portions 11 and 12 are moved away from each other to differing degrees in the two end positions. A hinge very similar to that hinge 1 , with the same functional principle, is disclosed in WO 2006/053364.
As can be seen from FIGS. 1 b and 1 d , the thickness d however is so great that, in spite of the increased opening stroke movement of the hinge 1 , a collision occurs between the adjacent furniture doors 3 and 3 a . If there were a wish to even further increase the opening stroke movement, the proportions of the hinge would have to be markedly increased, whereby valuable space inside the furniture carcass is lost.
FIGS. 1 a , 1 b , 1 c and 1 d represent the time sequence of the opening movement of the hinge 1 with fixed furniture door 3 . As a consequence of the collision diagrammatically shown in FIG. 1 d between the furniture doors 3 and 3 a , the theoretically possible maximum opening angle of about 170° of the hinge 1 cannot be reached.
FIG. 2 a shows a perspective view of the hinge 1 in the condition of being connected to the mounting plate 4 of the state of the art. The hinge 1 is in the closed position. The limbs 16 a and 16 b of the hinge cup lever 15 of the hinge are in the completely folded-together condition.
FIG. 2 b shows a perspective view of the hinge 1 in the second end position in which the hinge 1 is completely open. The limbs 16 a and 16 b of the hinge cup lever 15 are completely pivoted away from each other. The intermediate portion 10 is also in the end position defined by the hinge lever 13 , relative to the hinge arm 11 , whereby the maximum opening stroke movement is achieved.
FIG. 2 c shows the view of FIG. 2 b with the mounting plate 4 of the state of the art, separate from the hinge. In this case, the mounting plate 4 is of such a design configuration that the hinge arm 11 can be easily clipped on to the mounting plate 4 , thereby providing a snap-action connection. The mounting plate 4 itself is fixed to the furniture carcass with screws.
FIG. 3 a shows a plan view of a hinge 1 which substantially corresponds to the hinge 1 in FIGS. 1 and 2 . The hinge 1 is again fixed with a hinge cup 12 to a furniture door 3 and to a side wall 2 of a furniture carcass by a hinge arm 11 . In this case, the hinge arm 11 is again not fixed directly to the furniture carcass, but by way of a mounting device 9 according to the invention.
The hinge 1 itself has the increased opening stroke movement already described hereinbefore, which in regard to the prevailing factors, by virtue of the thickness d of the furniture doors 3 , 3 a , is not sufficient to avoid collisions during the opening movement. A connecting element 6 is fixed to the intermediate portion 10 mounted moveably relative to the hinge arm 11 by the hinge lever 13 , and the connecting element 6 in this embodiment is in the form of two-part lever comprising the lever arms 18 a and 18 b which are connected rotatably relative to each other by the spindle 19 . The hinge levers 7 a , 7 b are rotatably connected to the connecting element 6 by the spindle 17 . The hinge levers 7 a and 7 b are further mounted rotatably to the fixing device 5 by the spindle 20 . Mounting lugs 21 a , 21 b arranged on the fixing device 5 serve for that purpose.
In addition, the hinge levers 7 a , 7 b are mounted rotatably to the base plate 8 by the spindle 22 . Mounting lugs 23 a , 23 b are also arranged on the base plate 8 for that purpose. Also arranged on the fixing device 5 are further mounting lugs 24 a , 24 b , to which a respective further fixing device hinge lever 26 a , 26 b is mounted. The further hinge levers 26 a , 26 b are rotatably mounted at their other end to the base plate 8 , further mounting lugs 25 a , 25 b being provided for that purpose on the base plate 8 .
FIGS. 3 a , 3 b , 3 c and 3 d correspond to the time sequence of an opening movement of the hinge 1 . As can be seen in particular from FIGS. 3 b and 3 d , the opening stroke movement which is already increased by the hinge is further increased by the mounting device 9 so that no collision between the adjacent furniture doors 3 and 3 a occurs and the hinge 1 can be opened to its maximum opening angle, that is to say to its end position. The movement of the fixing device 5 relative to the base plate 8 can be particularly clearly seen by virtue of the movement of the mounting lugs 24 a , 24 b on the fixing device 5 , relative to the mounting lugs 25 a , 25 b on the base plate 8 .
FIG. 4 a shows the hinge 1 in the condition connected to the first embodiment of the mounting device 9 according to the invention, in its closed position. The connecting element 6 is in the form of a two-part lever comprising lever arms 18 a and 18 b . The lever arm 18 a of the connecting element 6 has a partially plate-shaped configuration, and in the condition of being connected to the hinge 1 bears flat against the top side of the intermediate portion 10 . The connecting element 6 has latching elements which are not visible in this Figure and which are in engagement with corresponding arresting or holding elements of the hinge 1 for fixing the connecting element 6 . In that respect, one or both openings 42 shown in FIGS. 2 b and 2 c in the intermediate portion 10 can serve as the arresting elements, which openings 42 are in latching engagement with latching elements which are arranged on the connecting element 6 and which can have a resilient nature or be spring-loaded, and they can thus form a snap-action connection. Alternatively, however, it is also possible to provide for fixing with a screw or screws which can be fitted into holes 45 in the connecting element 6 .
In addition thereto, the lever arm 18 a has two tongues 28 which are hingedly connected to the second lever arm 18 b and the hinge 1 by the spindle 19 . In that arrangement, the tongues 28 can be clipped on to slightly projecting pin portions 27 of the hinge 1 , thereby providing a simple and releasable snap-action connection.
FIG. 4 b shows the hinge 1 with mounting device 9 in the completely open position, utilizing the entire opening stroke movement of the hinge 1 and the mounting device 9 .
FIG. 5 shows a perspective view of the first embodiment of the mounting device 9 , fixed to a side wall 2 of the furniture carcass. The hinge 1 which is in the closed position is connected to the side wall 2 by the mounting device 9 and to the furniture door 3 a by the hinge cup 12 .
FIGS. 6 a and 6 b show the mounting device 9 without hinge 1 in the closed position ( FIG. 6 a ) and in the open position ( FIG. 6 b ). It can be seen that the fixing device 5 with the further hinge levers 26 a , 26 b forms a parallel lever assembly. The connecting element 6 can be fixed to the intermediate portion 10 which moves during the opening and closing movement of the hinge 1 . The fixing device 5 is operated by base plate hinge levers 7 a , 7 b , in which case the fixing device 5 is moved relative to the base plate 8 by the movement of the connecting element 6 , that is coupled to the hinge movement, during the opening and closing process of the hinge 1 . In the opening movement the fixing device 5 moves in the direction of the arrow A relative to the base plate 8 . The connecting element 6 is fixed to the hinge 1 by latching elements which are known in the state of the art and which are not visibly illustrated in FIGS. 6 a through 6 c , whereby the connecting element 6 can be clipped on to the intermediate portion 10 .
The hinge arm 11 of the hinge 1 is clipped on to the fixing device 4 , resilient latching elements 29 a , 29 b being provided for that purpose and engaging into corresponding arresting elements of the hinge arm. The hinge itself has a release device, by which the connection to the mounting device 9 can be released again.
When the furniture door 3 is opened, the fixing device 5 moves together with the hinge 1 and the furniture door 3 a fixed thereto in an arc out of the furniture carcass and passes around the adjacent door 3 a . That combination of stroke movement and linear movement can be particularly clearly seen in FIGS. 3 b through 3 d . In the end position shown in FIG. 6 b , the mounting lugs 24 a , 24 b arranged on the fixing device 5 have been moved forwardly relative to the mounting lugs 25 a , 25 b on the base plate 8 , in relation to the end position shown in FIG. 6 a.
FIG. 6 c shows an exploded view of the mounting device 9 and a perspective view of the hinge 1 to be fixed thereto. The base plate 8 comprises three plate-shaped elements 8 a , 8 b , 8 c and is fixed to the furniture carcass with screws (not shown) which are fitted into holes 44 provided for same. The part 8 b is fitted into openings 41 provided for same in the part 8 a so that the base plate 8 is of a compact structural height. The part 8 c is fitted under a bridge-shaped part of the fixing device 5 . Relative mobility of the fixing device 5 is limited by the leg of the part 8 c . The mounting lugs 25 a , 25 b are fitted into slot-shaped openings 40 a , 40 b in the base plate element 8 a.
The base plate 8 has an adjusting element for adjustment in respect of height and depth. Eccentrics 30 a and 30 b which are fitted into openings 43 a and 43 b respectively serve that purpose.
FIGS. 7 a through 7 d show plan views of a time sequence of the opening movement of a hinge 1 fixed to a second embodiment of the mounting device 9 according to the invention. It is possible once again to see the opening stroke movement which is increased in relation to the hinge 1 , whereby collisions with the adjacent furniture door 3 a can be avoided. In this embodiment, the connecting element 6 is fixed to the intermediate portion 10 with a screw 31 fitted into one of the openings 45 . The hinge levers 7 a and 7 b are again mounted rotatably to mounting lugs 21 a , 21 b of the fixing device 5 by way of a spindle 20 .
In this embodiment of the mounting device, the hinge levers 7 a , 7 b are however not connected to the base plate 8 by way of a fixed joint but at their ends have a respective gear segment 32 meshing with a corresponding toothed bar 33 of the base plate 8 . Consequently, the hinge levers 7 a , 7 b are not only rotated but also displaced with a translatory movement during the movement of the hinge 1 relative to the base plate, as can be clearly seen on the basis of the shift in position of the gear segment 32 relative to the toothed bar 33 in FIG. 7 a through 7 d.
FIG. 8 a shows the hinge 1 and the connected mounting device 9 in the closed position of the hinge 1 . The gear segments 32 of the hinge levers 7 a , 7 b are arranged at the end of the toothed bars 33 , that is at the inside of the carcass.
FIG. 8 b shows the completely open position of the hinge 1 and of the mounting device 9 . Now the gear segment 32 is arranged at the end of the toothed bar 33 , that is at the outside of the carcass, this corresponding to the maximum mobility of the fixing device 5 relative to the base plate 8 .
FIG. 9 shows the hinge 1 and the mounting device 9 of FIG. 8 a , wherein the mounting device 9 is mounted to the side wall 2 of the furniture carcass and the hinge 1 is mounted with the hinge cup to the furniture door 3 .
FIG. 10 a shows a perspective view of the second embodiment of the mounting device 9 . A part 8 c of the base plate 8 has a bridge-like connection 34 over an opening 35 , which serve as a guide device for the fixing device 5 . Instead of the parallel lever assembly of the first embodiment the hinge lever 7 a which is controlled by the gear segment has the advantage that the fixing device 5 is only moved linearly relative to the base plate 8 and does not require any additional stroke movement, as can also be seen from FIGS. 7 a through 7 d.
FIG. 10 b shows a perspective view of the mounting device 9 in the completely open position, thereby affording the maximum additional opening stroke movement in relation to the opening stroke movement by the hinge 1 .
It can be seen from an exploded view of the mounting device 9 and a perspective view of the hinge 1 in FIG. 10 c that the base plate 8 is again composed of three parts 8 a , 8 b , 8 c . Adjustment in respect of height and depth of the base plate 8 fixed to the furniture carcass is possible by eccentrics 30 a and 30 b and the openings 43 a and 43 b . While in the first embodiment the further hinge levers 26 a , 26 b prevented the fixing device from lifting off the base plate 8 , in this embodiment that purpose is served by the bridge-like connection 34 and a projecting pin portion 39 which can be fixed to the part 8 a of the base plate 8 and which is displaceably guided in a slot-shaped opening 38 in the fixing device 5 . The same purpose is served by a pin portion 37 which is fixed to the part 8 b and which is displaceably mounted in the slot 36 .
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The invention relates to a mounting device for fixing a furniture hinge, comprising a base plate, which is to be fixed to a furniture part, in particular a lateral wall of a furniture body, and comprising a fixing device for fixing the hinge to the mounting device, preferably in a removable manner. The fixing device is movably mounted on the base plate, said mounting device having a connecting element which is mounted on the base plate in a movable manner via at least one toggle lever and which can be fixed to a hinge part that can be moved during the opening and closing movement of the hinge, wherein the fixing device can be moved relative to the base plate via the toggle lever.
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[0001] This application is based on Japanese Patent Application No. 2005-025969 filed on Feb. 2, 2005, the contents of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to the structure of a test disc for the testing of an optical disc apparatus.
[0004] 2. Description of Related Art
[0005] In the production line of DVD recording/playback apparatuses, during the set assembly process for assembling together a pickup and a front-end system (the part that performs servo control), test recording to a DVD is performed when their assembly is complete. If recording fails here, the assembly is judged to be defective, but it is still necessary to find out which is responsible for the failure of recording, the pickup or the front-end system. This makes it desirable to evaluate the performance of the pickup, as a recording pickup on its own, prior to the set assembly process, that is, during the mass production process of the pickup.
[0006] As test discs for use for the evaluation of pickups, DVD/CD hybrid glass discs are commercially available. However, since these test discs have the formats of DVD- or CD-ROMs, they are not completely appropriate for the evaluation of recording pickups (for test discs for playback, see, for example, JP A H9-274740). With recordable DVDs (DVD-R, DVD-RW, DVD+R, and DVD+RW), it is necessary to additionally perform wobble signal evaluation and land prepit (LPP) signal evaluation.
[0007] Accordingly, in a case where the signal evaluation of a pickup with respect to recordable DVDs is incorporated in the mass production process of the pickup, one way of performing the signal evaluation is by using commercially available test discs that use polycarbonate as their substrate and that have formats complying with various recordable DVD standards. On the other hand, for example, JP A H7-93829 discloses, as a test disc, an optical disc in which preformat pits are formed at locations intentionally displaced from the center of a land or groove.
[0008] Inconveniently, when the commercially available test discs mentioned above are used to perform signal evaluation with respect to DVD- family discs (DVD-R and DVD-RW) and DVD+ family discs (DVD+R and DVD+RW), it takes much time to change the test discs. If, in addition, the tolerance of a pickup against low-quality discs, which have been an issue in the market of recordable DVDs, needs to be checked, it takes still more time to change discs. This lowers the efficiency of testing. On the other hand, when the optical disc disclosed in JP A H7-93829 mentioned above is used as a test disc, it is possible to check the tolerance of a pickup against low-quality DVD- family discs, which have land prepits, but it is not possible to perform signal evaluation with respect to DVD+ discs. Thus, this again lowers the efficiency of testing.
[0009] There also are the following inconveniences. Test discs using polycarbonate substrates tend to develop a warp. This makes them unreliable for use for signal evaluation. Test discs using polycarbonate substrates also tend to suffer scratches and thus have shorter lifetimes. This make them disadvantageous in terms of cost. Test discs that use organic colorant film in their recording layers, like append-only DVDs (DVD-R and DVD+R), are prone to secular changes in properties. This makes them unreliable for use for signal evaluation.
SUMMARY OF THE INVENTION
[0010] An object of the present invention is to provide a test disc that dramatically enhances the efficiency of the testing of a pickup for recording to a DVD.
[0011] To achieve the above object, according to the present invention, a test disc has: a first area in which a recorded region and an unrecorded region are provided; a second area in which a recorded region and an unrecorded region are provided; a third area in which at least one region is provided in which the wobble frequency is varied from 140 kHz; a fourth area in which at least one region is provided in which the wobble frequency is varied from 817 kHz; a fifth area in which at least one region is provided in which the wobble phase difference is varied from 180 degrees; a sixth area in which regions are provided between which the directions of the land prepits formed therein as observed within the land surface are mutually different; and a seventh area in which regions are provided between which the lengths of the land prepits formed therein as observed along the direction of the tracks are mutually different. Here, the first, third, sixth, and seventh areas are used for signal evaluation with respect to a DVD- family disc, and the second, fourth, and fifth areas are used for signal evaluation with respect to a DVD+ family disc.
[0012] With this structure, it is possible to perform, with a single disc, the signal evaluation of a pickup with respect to DVD- family discs and DVD+ family discs and the checking of the tolerance of the pickup against low-precision recordable DVDs such as low-quality discs. Thus, it is possible to dramatically enhance the efficiency of the testing of a pickup for recording to a DVD.
[0013] According to the present invention, preferably, the test disc structured as described above further has a substrate; moreover, the first, second, third, fourth, fifth, sixth, and seventh areas are formed on the substrate; and furthermore, the recorded regions are where pits are formed and the unrecorded regions are where no pits are formed.
[0014] With this structure, pits are formed on the substrate. This eliminates the need for a recording layer, and thus eliminates the concern about secular changes in properties as described previously.
[0015] According to the present invention, preferably, the substrate is formed of glass. This makes the disc free from a warp, reliable for use for signal evaluation, and resistant to scratches. Thus, the disc provides a longer lifetime, and proves advantageous in terms of cost.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 is a sectional view of part of the glass substrate provided in a test disc according to the present invention;
[0017] FIG. 2 is a diagram showing an example of the layout of different areas in the direction of the radius of the test disc according to the present invention;
[0018] FIG. 3 is a diagram showing an example of land prepits formed to point in different directions within the land surface;
[0019] FIG. 4 is a diagram showing an example of land prepits formed to be differently long in the direction of the tracks; and
[0020] FIG. 5 is a flow chart showing the procedure for testing a pickup by the use of the test disc according to the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0021] Hereinafter, an example of the structure of a test disc according to the present invention will be described. FIG. 1 is a sectional view of part of the glass substrate provided in the test disc according to the present invention. As shown in FIG. 1 , on a glass substrate, there are formed lands 1 , grooves 2 , pits 3 (formed in the grooves 2 ), and land prepits 4 (for DVD- family discs only). The grooves 2 meander slightly in the direction of the radius of the disc, producing wobbles. If the laser wavelength is λ, the grooves 2 are formed to have a depth of λ/8, the pits 3 a depth of λ/8, and the land prepits 4 a depth of λ/4. On top of the glass substrate, there are laid, though omitted from illustration, a reflective layer and a protective layer. Here, no recording layer is needed. Typically, the reflective layer is formed of gold, silver, or the like, and the protective layer is formed of polycarbonate or the like.
[0022] FIG. 2 shows an example of the layout of different areas in the direction of the radius of the test disc according to the present invention. From the clamp region located at the innermost edge of the disc toward the outer edge thereof, there are formed areas “a” to “i”. Area “a” has the format of a DVD-ROM, and has a trail of pits formed on the glass substrate.
[0023] Areas “b”, “d”, “g”, and “h” are regions used for signal evaluation with respect to DVD- family discs, and areas “c”, “e”, and “f” are regions used for signal evaluation with respect to DVD+ family discs.
[0024] In area “b”, there are provided a recorded region and an unrecorded region. In the DVD- family format, wobbles are formed in the grooves, and land prepits are formed on the lands. The land prepits form address information. In the recorded region, the pits 3 are formed in the grooves 2 ( FIG. 1 ). For example, from the inner edge of area “b”, there are formed a recorded region and then an unrecorded region. This makes it possible to perform signal evaluation in the land prepits and the wobbles with and without recording, and also to perform decoding evaluation in the land prepits.
[0025] In area “c”, there are provided a recorded region and an unrecorded region. In the DVD+ family format, wobbles are formed in the grooves (at a higher frequency than in the DVD- family format), and no land prepits are formed. The wobbles are formed in two types, 180 degrees out of phase with each other, and these two types of wobbles are combined to form address information called ADIP. In the recorded region, the pits 3 are formed in the grooves 2 ( FIG. 1 ). For example, from the inner edge of area “c”, there are formed a recorded region and then an unrecorded region. This makes it possible to perform signal evaluation in the wobbles, and also to perform decoding evaluation in the ADIP.
[0026] Area “d” is where there is provided at least one region where the wobble frequency is varied from 140 kHz, which is the DVD- family standard value. For example, from the center edge of area “d”, there are formed a region where the wobble frequency is 140+α kHz and then a region where the wobble frequency is 140−β kHz. The values of α and β are determined on the basis of the limit values of the wobble frequency within which a disc is evaluated as meeting its standard, and on the basis of information on low-quality discs, which have been an issue in the market. This makes it possible to check the tolerance of the decoding of land prepits.
[0027] Area “e” is where there is provided at least one region where the wobble frequency is varied from 817 kHz, which is the DVD+ family standard value. For example, from the center edge of area “e”, a region where the wobble frequency is 817+α kHz and a region where the wobble frequency is 817−β kHz are formed in this order. The values of α and β are determined on the basis of the limit values of the wobble frequency within which a disc is evaluated as meeting its standard, and on the basis of information on low-quality discs, which have been an issue in the market. This makes it possible to check the tolerance of the decoding of ADIP.
[0028] Area “f” is where there is provided at least one region where the wobble phase difference is varied from 180 degrees, which is the DVD+ family standard value. For example, from the center edge of area “f”, a region where the wobble phase difference is 180+θ degrees and a region where the wobble phase difference is 180−δ degrees are formed in this order. The values of θ and δ are determined on the basis of the limit values of the wobble phase difference within which a disc is evaluated as meeting its standard, and on the basis of information on low-quality discs, which have been an issue in the market. This makes it possible to check the tolerance of the decoding of ADIP.
[0029] Area “g” is where there are provided regions between which the directions of the land prepits formed therein as observed within the land surface are mutually different. For example, as shown in FIG. 3 , from the inner edge of area “g”, there are formed a region where the center line of land prepits is rotated so as to be inclined at θ degrees relative to the direction of tracks and then a region where the center line of land prepits is rotated so as to be inclined at −δ degrees relative to the direction of tracks. The values of θ and δ are determined on the basis of the limit values of the land prepit direction within which a disc is evaluated as meeting its standard, and on the basis of information on low-quality discs, which have been an issue in the market. This makes it possible to check the tolerance of the decoding of land prepits.
[0030] Area “h” is where there are provided regions between which the lengths of the land prepits formed therein as observed in the direction of the tracks are mutually different. For example, as shown in FIG. 4 , from the inner edge of area “h”, there are formed a region where the length of land prepits in the direction of the tracks equals L1 and then a region where the length of land prepits in the direction of the tracks equals L2 (>L1). The values of L1 and L2 are determined on the basis of the limit values of the track-direction land prepit length within which a disc is evaluated as meeting its standard, and on the basis of information on low-quality discs, which have been an issue in the market. This makes it possible to check the tolerance of the decoding of land prepits.
[0031] Area “i” has the format of a CD-ROM, and has a trail of pits formed on the glass substrate.
[0032] Now, the procedure for testing a pickup by the use of the test disc according to the present invention described above will be described with reference to the flow chart in FIG. 5 .
[0033] First, in step S 10 , the test disc is loaded in a test apparatus. The test apparatus may be any conventionally know one for use for the development of pickups. Then, in step S 20 , a pickup is mounted on the test apparatus.
[0034] In step S 30 , the test apparatus adjusts the power of laser, and then, in step S 40 , the pickup moves to area “a”. In step S 50 , the focus error is measured. Then, in step S 60 , the focus servo is turned on, and skew adjustment and the like are performed.
[0035] In step S 70 , the pickup moves to area “b”. In step S 80 , on the basis of the light reflected from the test disc, whether or not the levels of the amplitudes of the land prepit signal and of the wobble signal meet the standard is checked. In addition, the results of the decoding of land prepits are checked.
[0036] In step S 90 , the pickup moves to area “c”. In step S 100 , on the basis of the light reflected from the test disc, whether or not the level of the amplitude of the wobble signal meets the standard is checked. In addition, the results of the decoding of ADIP are checked.
[0037] Subsequently, in steps S 110 to S 200 , testing is performed in similar manners in areas “d” to “h”. Specifically, in the areas directed to DVD- family, the levels of the amplitudes of the land prepit signal and the wobble signal and the results of the decoding of land prepits are checked, and, in the areas directed to DVD+ family, the level of the amplitude of the wobble signal and results of the decoding of ADIP are checked.
[0038] Next, in step S 210 , the pickup moves to area “i”. In step S 220 , the focus error is measured. In step S 230 , the focus servo is turned on, and skew adjustment and the like are performed. Now, the testing is complete.
[0039] In the above description, the test disc according to the present invention has been described as having a substrate formed of glass and having no recording layer. It is, however, also possible to form one as a disc, like commercially available recordable DVDs, having a substrate formed of polycarbonate and having a recording layer of organic colorant film or phase change film. In that case, for example, in the recorded regions of areas “b” and “c”, if the recording layer is organic colorant film, recording marks are formed by deforming parts of the recording layer, the substrate, and the reflective layer, and, if the recording layer is phase change film, recording marks are formed by making parts of the recording layer amorphous. Also with the test disc so structured, it is possible to dramatically enhance the efficiency of the testing of a pickup.
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With conventional test discs, changing them takes much time when a pickup is subjected to signal evaluation with respect to DVD- family discs (DVD-R and DVD-RW) and DVD+ family discs (DVD+R and DVD+RW), leading to low testing efficiency. A test disc of the invention has, formed on a single glass substrate, areas where there are provided regions where pits or no pits are formed and areas where there are provided regions where wobbles and land prepits are formed with varying parameters.
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This application is a continuation-in-part of copending U.S. application Ser. No. 08/962,170, filed Oct. 31, 1997, and U.S. application Ser. No. 08/962,171, filed Oct. 31, 1997, now U.S. Pat. No. 5,835,231, the disclosures of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to matter identifying devices, and more particularly, to those that measure the optical absorption by matter within an evanescent wave field generated by total internal reflection within a low-loss optical cavity.
2. Related Art
Optical absorption spectroscopy is fundamentally important in chemical analysis, providing decisive quantitative and qualitative information. Such diagnostic capabilities find substantial utility in both research and industrial process environments. Therefore, an advancement in sensitivity, accuracy, or adaptability of the technique will have a significant impact.
Absorption is usually determined from measurement of a ratio of optical powers at a certain wavelength. Recently, a new technique, termed cavity ring-down spectroscopy (E. K. Wilson, C&E News, Feb. 19, 1996, p. 34, incorporated herein by reference), has been developed to determine absorption by gases, which utilizes a pulsed light source and an optical cavity. Typically, a light pulse from a laser source is injected into a cavity which is formed by two high-reflectivity mirrors. The lifetime of the pulse in the cavity is highly sensitive to cavity losses, including absorption by gases. Measurement of the pulse decay time or "ring-down" time in the cavity can thereby provide a direct measure of absorption. Cavity ring-down eliminates the adverse effects of light source fluctuation, since the measurement is acquired with a single pulse of light. The feasibility of this technique arises from recent technological advances in optical polishing, which permit the fabrication of extremely low-scatter-loss optics. If ordinary optics such as high-reflectivity mirrors (R˜99%)are used, the pulse lifetime in the cavity is too short for the cavity ring-down strategy to provide a significant improvement in sensitivity, as compared to conventional absorption methods. However, with the advent of superpolishing, such as that described in N. J. Brown, Ann. Rev. Mater. Sci. 16, p. 371 (1986), incorporated herein by reference, mirrors with 99.99% reflectivity or better can be fabricated to construct low-loss optical cavities, thereby permitting ultra-high sensitivity to be routinely realized. The cavity ring-down technique has thereby become a viable form of optical absorption metrology, with trace analysis capabilities that greatly exceed conventional absorption methods.
A stable optical cavity used to measure the optical absorption of a material, as disclosed in copending application Ser. No. 08/962,170, is shown in FIG. 1. A three element cavity 5 is formed by two high-reflectivity concave mirrors 10, 12 with equal radii of curvature, and a Pellin-Broca prism 14 in a right-angle configuration. A light source 15 for injecting light, described throughout as a laser, is positioned adjacent mirror 10, and a photomultiplier 19 is positioned adjacent mirror 12. The Pellin-Broca prism 14 provides a total internal reflection with very high internal transmission for a light beam 16a that is polarized in the plane formed by the three element cavity 5, since an incident beam 16b and an exiting beam 16c traverse the prism faces at the Brewster's angle N B . By properly mounting the Pellin-Broca prism 14, the light beam will traverse the Pellin-Broca prism 14 at minimum deviation, which minimizes aberrations and beam translation with rotation about Brewster's angle N B . Since the total internal reflection occurs at a hypotenuse surface 14a of the Pellin-Broca prism 14, an evanescent wave 18 decays exponentially into the region external to the hypotenuse surface 14a. Absorbing materials (not shown) placed within the decay length of the evanescent wave 18 can thereby be sensitively probed through the change in the decay time of a laser pulse injected into cavity 5. This decay time is detected by photomultiplier 19 which senses a very small portion of the injected light which escapes through mirror or reflector 12. Cavity losses for the configuration shown in FIG. 1 are largely determined by surface roughness induced scattering, although stress-birefringence of the Pellin-Broca prism 14 may induce polarization scrambling.
The optical cavity shown in FIG. 1 includes high-reflectivity concave mirrors 10 and 12 located a distance from the prism 14. The mirrors 10 and 12 must be properly aligned with each other and the prism 14 in order for the cavity to operate properly.
SUMMARY OF THE INVENTION
In accordance with the invention, a device is provided which permits the sensitive measurement of optical absorption by matter in any state with diffraction-limited spatial resolution through utilization of total internal reflection within a high-Q (high-quality, low-loss) optical cavity. The optical cavity consists of a single optical element. The use of a single optical element for the cavity eliminates the requirement of properly aligning the elements found in related optical cavities and results in a more rugged structure. Intra-cavity total reflection generates an evanescent wave that decays exponentially in space at a point external to the cavity, thereby providing a localized region where absorbing materials can be sensitively probed through alteration of the Q-factor of the otherwise-isolated cavity. When a light pulse is injected into the cavity and passes through the evanescent state, an amplitude loss resulting from absorption is incurred that reduces the lifetime of the pulse in the cavity. By monitoring the decay of the injected pulse, the absorption coefficient of matter within the evanescent wave region, is accurately obtained from the decay time measurement. In some embodiments of the invention, microsampling with high-spatial resolution is achieved through repeated refocussing of the light pulse at the sampling point, under diffraction-limited conditions.
In accordance with a first embodiment of the invention, an intra-cavity total reflection apparatus for high sensitivity measurement of the optical absorption of a test material is provided which comprises: an injecting means for producing light for a predetermined length of time; an optical cavity, comprising first, second and third reflecting surfaces integrally formed on a cavity medium, for receiving the light produced by the injecting means and for providing total internal reflection of the light within the cavity so as to generate an evanescent wave at the third reflecting surface which decays within a decay length outside of the cavity beyond the third reflecting surface, the test material being disposed outside of the cavity within the decay length, and the injected light oscillating between the first and second reflecting surfaces such that a portion of the injected light escapes from the cavity; and a measuring means disposed adjacent one of the first and the second reflecting surfaces for monitoring the portion of the injected light that escapes from the cavity to determine the amount of decay time the light takes to decay within the cavity.
Advantageously, the measuring means comprises a photomultiplier.
In one preferred implementation of this embodiment, the first and the second reflecting surfaces are orthogonal to one another.
The cavity medium is preferably formed of fused silica.
In another preferred implementation of this embodiment, the injecting means and the measuring means are optically coupled to the optical cavity with fiber-optic waveguides.
It is preferred that the third reflecting surface is a convex surface.
The injecting means preferably comprises a laser and more preferably comprises one of a pulsed dye laser, a picosecond pulsed laser, a femtosecond pulsed laser and a continuous wave laser. In another preferred embodiment, the laser comprises a diode laser.
Other features and advantages of the invention will be set forth in, or apparent from, the following detailed description of the preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic top elevational view of a multiple element optical cavity; and
FIG. 2 is a schematic top elevational view of a single optical element optical cavity in accordance with a preferred embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A further preliminary discussion is thought to be helpful at this point in fully understanding the invention. The measurement of optical absorption is fundamental to science and engineering, since an absorption spectrum provides a fingerprint which permits the qualitative and quantitative analysis of material composition. Absorption measurements are also frequently used to extract rates of chemical reactions and other processes. Key objectives in the development of a new technology for measurement of absorption are: 1) a reduction of the minimum detectable described in N. J. Brown, Ann. Rev. Mater. Sci. 16, p. 371 (1986), incorporated herein by concentration, 2) an increase in the spatial resolution of the measurement, and 3) the incorporation of tunable, powerful, and highly monochromatic laser sources. By reducing the detection limit, important chemical reactions and processes that involve trace quantities or very short path lengths will be, in some cases, detectable for the first time or examined with higher signal-to-noise ratio thereby allowing more reliable quantification.
Previous attempts to increase the limit of detection have typically increased the sampled path length, which inherently results in a decrease in spatial resolution. A few devices have been developed which permit multiple sampling of a specific region, but typically with a small number of passes and a large beam diameter. The device of the present invention which uses a multiple-pass geometry with refocussing, substantially improves sensitivity and spatial resolution. Furthermore, by using a laser source with the device of the invention, the spatially coherent nature of laser light permits greater spatial resolution, since a focal spot size limited only by diffraction can be readily achieved. The laser-based device also benefits from the high output power and broad wavelength range obtainable through the combination of tunable, pulsed dye lasers and harmonic generation. Considering the current technological trend toward the micro- and nanostructured domains, the development of a sensitive absorption device with high-spatial resolution will likely facilitate technological innovations. However, to obtain the advantages of a pulsed laser source, the device circumvents the complication of pulse-to-pulse fluctuation, which is characteristic of pulsed laser systems. These measurements of optical absorption by intra-cavity total reflection achieve high-sensitivity with high-spatial resolution.
In the case of Attenuated Total Reflection (ATR) developed extensively by Harrick, Internal Reflection Spectroscopy, by N. J. Harrick (Interscience Publishers, New York 1967), incorporated herein by reference, an evanescent wave is generated by internal reflection in an optical cavity such as a prism, plate or thin-film waveguide at an internal angle of incidence that exceeds the critical angle. In ATR spectroscopy, the evanescent wave generated by total internal reflection at the base of a prism is used for optical absorption measurements by the conventional optical power ratio method. Absorption is determined from the optical power loss incurred in the critically reflected beam relative to total reflection when no absorbing material is present in the evanescent wave region.
ATR can be used to measure absorption for samples in the solid, liquid or gas phases, but is also highly effective for probing powders, fibers, thin-films, and absorbed molecular monolayers. For studies of thin-films and monolayers, ATR benefits from the enhanced surface electric field which exists at the interface where total reflection occurs. The direction of the surface field can also be controlled through polarization selection to probe molecular orientation effects, which can be important in, for example, catalysis and adhesion.
In optical cavity ATR, a light beam is coupled into a mode of an optical cavity, which contains an evanescent wave component that decays exponentially outside of the waveguide. Absorbing material within the decay length is then probed by measuring a corresponding power loss in the out-coupled beam after traversing the waveguide for a predetermined distance.
Waveguide cavity ATR has the advantage over ordinary ATR of increased effective path length, since light rays coupled into the cavity experience a large number of internal reflections over a short distance. The effective path length is proportional to the product of the total number of reflections and the evanescent wave decay length. However, conventional waveguide cavity ATR still employs an optical power ratio measurement, which ultimately limits its utility in trace analysis.
Although optical cavities have been described in many patents and publications, this does not detract from the originality of novel applications of such technology. For example, laser resonators and spectrum analyzers are common implementations of optical cavities, which in some cases use identical cavity designs.
The sensitivity of the measurement can be increased by utilizing optical element geometries that permit multiple total internal reflections and/or multiple passes to occur. Multiple reflections increase sensitivity with a concomitant decrease in spatial resolution by sampling at multiple points to yield an increase in the effective path length. A multiple-pass strategy repeatedly samples a single region to provide moderate spatial resolution. However, multiple pass elements typically provide only a few passes and do not refocus the beam at the sampled region to increase spatial resolution. Therefore, the development of an absorption technique which incorporates the powerful diagnostic capabilities of ATR and multiple-pass sampling with diffraction limited refocussing would represent a fundamental advancement in absorption measurement technology.
Apart from ATR is the cavity ring-down spectroscopy (CRDS) technique described in A. O'Keefe and D. A. G. Deacon, Rev. Sci. Instrum. 59, p. 2544 (1988) incorporated herein by reference, which is used for measuring the optical absorption spectra of gases. This technique was originally applied to narrowband gas phase absorption spectroscopy. U.S. Pat. No. 5,313,270 to Fishman and Haar, incorporated herein by reference, describes essentially identical technology to that of the O'Keefe reference mentioned above, with an intended application to the measurement of mirror reflectivity.
In CRDS, a single laser pulse is injected into a high-Q optical cavity, typically comprising a pair of concave high-reflectivity mirrors. Since the cavity Q-factor is high, the pulse makes many round trips, incurring only a small loss in amplitude per pass due to small intrinsic cavity losses resulting from, for example, mirror surface roughness scattering. Typically, the cavity is enclosed in a chamber which is filled with a gas of interest. When the frequency of the injected pulse corresponds to a resonant transition of the gas, the pulse amplitude loss per pass directly reflects the magnitude of the absorption. The temporal decay of the injected pulse is determined by monitoring the weak transmission which escapes from the cavity through one of the high-reflectivity mirrors. The transmitted intensity decays exponentially at a rate which reflects the total cavity losses, including absorption losses. Measurement of absorption is thereby achieved through a measurement of decay time instead of through a ratio of optical intensities. This time based measurement is equivalent to a large number of power ratio measurements with the same laser pulse, which inherently improves the accuracy and precision of the measurement since use of a single pulse eliminates the adverse effects of pulse-to-pulse fluctuation.
CRDS has only been applied to gas phase measurements, since the use of condensed matter sampling schemes which are common to transmission measurements, result in substantial intrinsic cavity losses which degrade the system performance. However, by utilizing intra-cavity total reflection, the advantages of a time-based absorption measurement can be combined with the advantages of ATR. The net result is a novel strategy for measurement of optical absorption by all states of matter. This strategy is fundamentally different from ATR, since a measurement of time instead of a ratio of intensities, is utilized. This strategy is different from CRDS since condensed matter can be probed through generation of an evanescent wave. Furthermore, the highly-localized nature of the evanescent wave combined with the spatial coherence provided by a laser source permits diffraction-limited spatial resolution and provides a decisively defined sample path length, which is necessary for accurate quantitative measurements.
Turning now to the embodiment shown in the FIG. 2, this embodiment takes advantage of the strategy discussed in the preceding paragraph, and the illustrated device is an intra-cavity total reflection device comprising a high-Q optical cavity. Losses introduced by any element in the system must be extremely small to produce a high-Q cavity.
It is noted that the preferred embodiment illustrated in FIG. 2 uses narrowband, multilayer coatings or Brewster's angle to achieve low cavity losses. In all of the embodiments disclosed, it is preferred that the optical cavities are stable optical cavities. Stable optical cavities are described in Lasers, by A. G. Seigman (University Science Books, California 1986), incorporated herein by reference.
In FIG. 2, a single element cavity 20 is formed by two high-reflectivity coated surfaces 22 and 24 and a convex superpolished surface 26 on cavity medium 28. The reflective surfaces 22 and 24 are preferably orthogonal to one another and the cavity medium is preferably fused silica. A light source 29, described throughout as a laser, is positioned adjacent to reflective surface 22 and produces light indicated as 30. The laser is preferably a diode laser. In another preferred embodiment, the light source 29 is a pulsed, dye laser used with frequency scanning. A detector 34 is positioned adjacent to reflective surface 24. In one preferred embodiment, the detector 34 is a photomultiplier. The cavity medium 28 provides a total internal reflection with very high internal transmission for a light beam 30 at the convex superpolished surface 26.
Since the total internal reflection occurs at the convex surface 26 of the cavity medium 28, an evanescent wave 32 is produced which decays exponentially into the region external to the convex surface 26. Absorbing materials 33 placed within the decay length of the evanescent wave 32 can thereby be sensitively probed through the change in the decay time of a laser pulse injected into cavity 20. This decay time is detected by detector 34 which senses a very small portion of the injected light which escapes through reflective surface 24. Cavity losses for the configuration shown in FIG. 2 are minimized through the use of ultra-high transmission optical materials, ultra-high reflectivity coatings, superpolishing, and proper cavity design.
In a preferred embodiment, the detector 34 senses the intensity of the light passing through reflective surface 24 and feeds the resultant signal to a digitizing means (not shown). In one preferred embodiment, the digitizing means is a digital oscilloscope. The decay time τ(ω) of the digitized signal is approximated by:
τ(ω)=t.sub.r /(2(1-R)+ζ.sub.bulk ζ.sub.surf +ζ.sub.abs)
where t r is the round-trip time in the cavity, R is the reflectivity of the coated surfaces 22, 24 and 26, ζ bulk is the bulk attenuation by the cavity medium 28, ζ surf is the surface scattering loss at the total internal reflecting surface 26 and ζ abs is the optical absorption by the absorbing material 33.
All of the loss terms in the decay time formula are known and are constant for a given cavity design except the optical absorption of the absorbing material ζ abs . Therefore, a measurement of the actual photon decay time allows one to obtain the unknown quantity ζ abs .
The use of a single optical element for the optical cavity 20 results in a more rugged cavity as compared to other, multi-element cavities. In addition, the single element cavity 20 allows for remotely positioning the cavity 20 from the light source 29 and the detector 32 without the burden of aligning plural elements. The light source and detector may be optically coupled to the optical cavity with fiber optic materials (not shown).
In an alternative preferred embodiment, a picosecond or femtosecond pulsed laser with continuum generation is used as the light source and frequency analysis of the output signal is performed either by interferometry or dispersion methods.
In general, it is important to note that although the cavity design is quite simple, the surface quality required to produce a sufficiently high Q-factor necessitates the use of state-of-the-art polishing techniques, which can produce surfaces with <0.1 nm RMS surface roughness. Furthermore, these cavities form stable optical resonators, so that an injected light pulse will retrace its path in the cavity a large number of times. The beam waist associated with the stable mode of the cavity is located in the vicinity of the totally reflecting surface to optimize spatial resolution. In the embodiments of FIGS. 1 and 2, the sample is probed by the light pulse a number of times N, equal to the ratio of the decay time to one-half the round trip time. This value will typically be on the order of 1,000.
Anticipated commercial applications for the invention include:
1. Biosensor applications
2. Catalysis
3. Corrosion
4. Adhesion
5. Trace analysis for semiconductor processes
6. Chromatography detector
7. Process measurements
8. Optical constant determinations
9. Hostile environments
10. Trace analysis in general
11. Research tool for surface science research
Although the present invention has been described to specific exemplary embodiments thereof it will be understood by those skilled in the art that variations in modifications can be effected in these exemplary embodiments without departing from the scope and spirit of the invention.
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An optical cavity resonator device is provided for conducting sensitive murement of optical absorption by matter in any state with diffraction-limited spatial resolution through utilization of total internal reflection within a high-Q (high quality, low loss) optical cavity. Intracavity total reflection generates an evanescent wave that decays exponentially in space at a point external to the cavity, thereby providing a localized region where absorbing materials can be sensitively probed through alteration of the Q-factor of the otherwise isolated cavity. When a laser pulse is injected into the cavity and passes through the evanescent state, an amplitude loss resulting from absorption is incurred that reduces the lifetime of the pulse in the cavity. By monitoring the decay of the injected pulse, the absorption coefficient of manner within the evanescent wave region is accurately obtained from the decay time measurement.
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BACKGROUND OF THE INVENTION
The present invention relates generally to electronic musical instruments and particularly concerns improved automatic accompaniment systems for electronic musical instruments.
Electronic musical instruments, most notably of the keyboard variety, which are capable of automatically playing a musical pattern or rhythm to accompany a melody played by a performer are well known in the art. The automatic accompaniment can be created in a variety of different musical styles and the instrumentation, rhythm, and chord patterns can be changed by the performer to add variety to the accompaniment. U.S. Pat. No. 4,433,601 to Hall et al. is exemplary of an electronic keyboard musical instrument having such an automatic accompaniment capability.
To add further interest to the automatic accompaniment, various special effects may be provided, such as the interruption of a rhythm pattern to insert a rhythm break, for example, a drum roll or the like. In musical performances, this type of special effect is frequently used to provide a musical accent or transition between the different parts of a song. U.S. Pat. No. 3,764,722 to Southard discloses an electronic musical instrument capable of inserting such musical breaks (sometimes called fill patterns) in automatic rhythm patterns. In the Southard system, the break is initiated by the performer operating a push-button switch, with the original rhythm pattern starting again at the end of the break. That is, the same rhythm pattern is played after the break as was played before it. This characteristic of prior art systems imposes a limitation on the variety of musical patterns which can be achieved in the creation of automatic accompaniment arrangements, and is therefore considered undesirable.
It is therefore an object of the present invention to provide an improved automatic rhythm or accompaniment system for an electronic musical instrument.
It is a further object of the invention to provide for the insertion of musical break patterns in an automatic accompaniment arrangement in a manner more musically interesting than has heretofore been done.
It is yet another object of the invention to provide for the insertion of a musical break in a first automatic accompaniment pattern and subsequently resume playing a second different automatic accompaniment pattern following completion of the break.
It is still a further object of the invention to delay the playing of a musical break initiated near the end of a musical interval until the beginning of the next interval.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects and advantages of the invention will be apparent on reading the following description in conjunction with the drawings, in which:
FIG. 1 is a time line representing the generation of an automatic accompaniment arrangement in accordance with the invention;
FIG. 2 is a simplified block diagram illustrating an electronic keyboard musical instrument embodying the present invention; and
FIGS. 3 and 4 are flow charts illustrating the method of programming the electronic musical instrument of FIG. 2 in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings, FIG. 1 is a diagrammatic representation of the manner of operation of an electronic musical instrument in accordance with the invention. The diagram is in the form of a time line 10 comprising a plurality of musical bars or measures which represent a portion of a complete automatic accompaniment arrangement. The organization of a musical composition with which an automatic accompaniment may be desired is generally very well defined and typically includes an introduction, followed by a verse section (sometimes referred to as the first chorus), then a chorus section (sometimes referred to as the second chorus),which may then be followed by a repetition of any of the above before concluding with an ending. As indicated by the legend in the Figure, a solid line represents an automatic accompaniment pattern particularly suited for playing with the verse portion of a composition, a wavy line an automatic accompaniment pattern particularly suited for playing with the chorus pattern of the composition, a dotted line the playing of a verse break pattern and a series of addition signs the playing of a chorus break pattern. As mentioned previously, the break or fill patterns provide musical accents for transitions between the different parts of the accompaniment pattern.
With further reference to the time line 10, the exemplary automatic accompaniment arrangement begins at a start point 12 with two bars of a selected automatic accompaniment pattern suited for playing with the verse portion of a musical composition. The verse accompaniment pattern continues into the third bar where it is interrupted at a point 14 by a performer initiated "break to chorus" which may comprise, for example, a drum roll or the like. The break initiated at point 14 preferably comprises a variation of the accompaniment pattern and is referred as a "break to chorus" in that, following its completion at the end of the third bar, the automatic accompaniment resumes with a pattern suited for the chorus portion of the composition as shown. It should, in particular, be noted that in accordance with the invention the accompaniment pattern following the break pattern is different from the accompaniment pattern immediately preceding it.
Continuing along time line 10, the chorus accompaniment pattern following the break initiated at point 14 is played for the next two bars and into a third bar. A second break at a point 16, a "break to verse", is initiated by the performer in this bar,providing for the playing of a verse break pattern until the end of the bar. Since this break pattern leads into an automatic accompaniment pattern suited for playing with the verse portion of the composition, it is referred to as a "break to verse" pattern. It will, again be noted that the accompaniment patterns immediately preceding and following the break initiated at point 16 are different, with a chorus accompaniment pattern preceding the break and a different verse accompaniment pattern following it.
The verse accompaniment pattern is played for the next three bars until another "break to verse" is initiated by the performer at a point 18 coincident with the beginning of the next bar. This again interrupts the verse accompaniment pattern with a suitable verse break pattern which lasts for a complete bar. However, since the verse accompaniment pattern in this case was interrupted by a "break to verse" (in contrast to the "break to chorus" at point 14), the verse accompaniment pattern is resumed in the next bar following the break. The verse accompaniment pattern is played for two more bars and into a third bar when another "break to chorus" is initiated at a point 20 by the performer. As in the case of the "break to chorus" initiated at point 14, the verse accompaniment pattern is again interrupted and replaced with a suitable chorus break pattern, after which the chorus accompaniment pattern is resumed.
The initiation of a final "break to chorus" by the performer is illustrated as occurring at a point 22. It will be observed that this break is activated during the last 1/4 interval of a bar. In a further aspect of the invention, if a break is initiated during a predetermined interval from the end of a bar, such as during the last 1/4 of a bar as in the illustrated preferred embodiment, the change to the break pattern is delayed until the downbeat of the next bar to insure that the break is played even if keyed just slightly before the downbeat. Thus, the playing of the chorus break pattern is delayed until the downbeat of the next bar at point 24. The chorus break pattern is then played for the complete bar beginning at downbeat 24, after which the chorus pattern is resumed.
The verse and chorus break or fill patterns described above may be of a fixed nature or may be based on a sequential or random selection from groups of stored patterns. Thus, the precise nature of these patterns should not be considered as a limitation of the invention. Also, it will be understood that the musical arrangement represented by time line 10 is only exemplary of many automatic accompaniment arrangements which may be played in accordance with the invention. Finally, since time line 10 only represents a portion of an automatic accompaniment arrangement, the introduction and ending portions thereof have not been illustrated. However, according to another aspect of the invention, musical breaks initiated during such introduction and ending portions of a composition are ignored and not played.
FIG. 2 is a block diagram illustrating an electronic keyboard musical instrument embodying the present invention. The musical instrument is controlled by a microprocessor 30 which is connected by a bi-directional data bus 32 to a program ROM 34, a RAM 36 and a pattern ROM 38. Data bus 32 also couples microprocessor 30 to a switch and keyboard scanner 40 which has an output 42 connected to an interrupt input of microprocessor 30. Microprocessor 30 addresses program ROM 34, RAM 36 and pattern ROM 38 via an address bus 44.
Switch and keyboard scanner 40 is responsive to inputs received over data bus 32 for generating scanning signals on a bus 50. These scanning signals are used to scan the switches and keys of a control switch matrix 46 and a keyboard 48. Control signals identifying switch and key closures are coupled back to scanner 40 on a bus 52. Scanner 40 interrupts microprocessor 30 over line 42 and control signals identifying switch and key closures are applied to the microprocessor over data bus 32. Microprocessor 30, in response to switch and key closure control signals from switch matrix 46 and keyboard 48, suitably interacts with memories 34-38 over data and address buses 32 and 44 to formulate a digital representation of a desired musical performance. The techniques and methods for formulating this digital representation are well known in the art and therefore will not be described in detail herein. Suffice it to say that the digital signals representing the musical performance are applied by microprocessor 30 to a digital tone generator 54 over a serial interface line 56. Digital tone generator 54 is a well known circuit for transforming the digital signals from microprocessor 30 into analog signals capable of producing the desired musical performance. In particular, the analog signals from tone generator 54 are amplified by a pair of amplifiers 60 and 62 and then applied to a pair of speakers 64 and 66 for acoustically producing the musical performance.
In accordance with the invention, program ROM 34 includes a first subroutine entitled "break to chorus" as illustrated in FIG. 3 and a second subroutine entitled "break to verse" as illustrated in FIG. 4. Pattern ROM 38 includes a plurality of sections of memory locations each storing a respective one of the accompaniment and break patterns illustrated in FIG. 1. As previously described, each pattern type may include a group of stored patterns which are selected for playing in a desired manner in accordance with the system program stored in ROM 34.
In operation, a performer initiates the playing of an automatic rhythm or accompaniment pattern by closing a switch 70 labeled "AR" on control switch matrix 46. The closure of this switch is communicated to microprocessor 30 by a control signal from scanner 40. In response thereto, microprocessor 30 in conjunction with the system program stored in ROM 34, reads selected accompaniment patterns from pattern ROM 38 and applies the patterns to tone generator 54 where they are converted to appropriate analog signals capable of being acoustically reproduced by speakers 64 and 66. It will be understood that the accompaniment patterns read from pattern ROM 38 may be temporarily stored in RAM 36 before being applied to tone generator 54 by microprocessor 30.
Control switch matrix 46 includes two additional switches, a switch 72 labeled "BTV" (break to verse) and a switch 74 labeled "BTC" (break to chorus). Closure of either of these two switches causes microprocessor 30 to branch to the corresponding subroutine shown in either FIG. 3 or 4 for executing the break features of the invention.
For example, assume that an automatic accompaniment pattern is being played as illustrated by time line 10 of FIG. 1. At some time corresponding to points 14, 20 or 22, the performer closes switch 74 to initiate a "break to chorus". This causes microprocessor 30 to execute the subroutine illustrated in FIG. 3. The first step in this subroutine is a decision 80 to determine whether the automatic rhythm feature is on or off. If the automatic rhythm function is off, the break pattern is not played as represented by block 82. Since, however, the automatic rhythm function is on, the subroutine continues to a second decision 84 to determine whether the introduction or ending of the accompaniment pattern is being played. If either are in progress, the break is again not executed in accordance with block 82. Assuming that neither the introduction nor ending is in progress, the subroutine proceeds to decision block 86. At this time, a decision is made regarding whether BTC switch 74 was operated within 1/4 of the end of the bar. In the cases of both points 14 and 20 of the accompaniment pattern of FIG. 1, the breaks were initiated before the last 1/4 of the respective bar leading the subroutine to begin playing the chorus break pattern substantially immediately. Thus, a selected chorus break pattern is read from pattern ROM 38 and played until the end of the bar. Upon completion of the chorus break pattern, the subroutine executes block 90 calling for the playing of a chorus accompaniment variation.
In the case of point 20, BTC switch 74 was operated within the last 1/4 of the bar. The subroutine therefore proceeds from decision 86 to block 92 which causes the chorus break pattern to be delayed until the downbeat of the next bar (i.e. point 24 in FIG. 1). As before, the chorus accompaniment variation is played in accordance with instruction 90 upon completion of the chorus break pattern. It will be observed that in the cases of the breaks initiated at points 14 and 20, the chorus break patterns served as transitions between a verse accompaniment pattern and a chorus accompaniment pattern while, in the case of the break initiated at point 22 (but not actually begun until point 24), the chorus break pattern formed a transition between two chorus accompaniment patterns.
Operation of BTV switch 72 is very similar to that of BTC switch 74. For example, operating BTV switch 72 at points 16 and 18 of the accompaniment pattern illustrated in FIG. 1 causes causes microprocessor 30 to execute the break to verse subroutine stored in program ROM 34 and illustrated by the flowchart of FIG. 4. The subroutine illustrated in this flowchart is substantially identical to the break to chorus subroutine illustrated in FIG. 3. Thus, the status of AR switch 70 is checked at a decision 100 and a determination is made at decision 102 as to whether the introduction or ending of the accompaniment pattern is in progress. As before, as represented by block 104, a break pattern will not be played if either the AR switch is off or an introduction or ending is in progress.
Next, a decision is made at 106 regarding the relative timing of the break which is then either started substantially immediately per block 108 or is delayed until the beginning of the next bar per block 110. Finally, following completion of the verse break pattern, the subroutine proceeds to play a verse accompaniment pattern as indicated at block 112. It will be observed that the verse break pattern initiated at point 16 formed a musical transition between a chorus accompaniment pattern and a verse accompaniment pattern while the verse break pattern initiated at point 18 formed a transition between two verse accompaniment patterns.
With the invention, a much improved method of inserting beak patterns in an automatic accompaniment arrangement is made available. It is recognized that numerous changes and modifications in the described embodiment of the invention may be made without departure from its true spirit and scope. The invention is therefore to be limited only as defined in the claims appended hereto.
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An electronic musical instrument includes first and second control switches for initiating chorus and verse break patterns in an automatic accompaniment arrangement. A chorus accompaniment pattern is automatically generated following the chorus break pattern and a verse accompaniment pattern is automatically generated following the verse break pattern, regardless of the pattern types generated prior to the breaks. The generation of breaks are inhibited during the last 1/4 interval of a bar and during the generation of the introduction and ending portions of the accompaniment arrangement.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation-in-part of copending application Ser. No. 698,449 which was filed June 21, 1976, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the utilization of natural gas, having a relatively high content of carbon dioxide in admixture with methane, to produce liquid fuel. In its preferred embodiment, the invention is also concerned with supply of a product gas stream rich in carbon dioxide and having reduced methane content as compared with the natural gas processed. Such product gas stream is utilized in tertiary methods of recovery of liquid petroleum from underground reservoirs which have been depleted to the extent viable by primary and secondary recovery methods.
2. Description of the Prior Art
The natural gases of interest in the process of this invention have previously been regarded as having no significant commercial value. Natural gas containing mixtures of carbon dioxide and methane in substantially equal volumes, and those containing a major proportion of methane, have been processed to separate the methane from the carbon dioxide and thus provide fuel gas of pipeline quality. However, it has been considered economically unrealistic to produce natural gas from extensive known reservoirs in which the gas contains a major proportion of carbon dioxide. The cost of the separation of the methane content of the gas from these reservoirs is too great, in comparison with the value of the recovered methane, to justify the construction and operation of separation facilities. Assuming a use for the carbon dioxide in tertiary recovery at petroleum reservoirs within a distance which can justify transporting the gas, such mixtures are unsuitable because of their content of methane which is known to inhibit solubility of carbon dioxide in petroleum.
In providing a combination of process steps which yield valuable products from natural gas previously considered valueless, the invention described herein utilizes known technology for:
(1) GENERATING A SYNTHESIS GAS OF CARBON MONOXIDE AND HYDROGEN PRIMARILY FROM THE REACTION OF METHANE AND WATER;
(2) SYNTHESIS OF METHANOL OR LIQUID HYDROCARBONS BY REACTION OF CARBON OXIDES AND HYDROGEN; AND
(3) TERTIARY RECOVERY OF PETROLEUM BY INJECTION OF CARBON DIOXIDE, WHICH CONTAINS LITTLE METHANE, INTO AN UNDERGROUND RESERVOIR, IT BEING KNOWN THAT METHANE REDUCES THE SOLUBILITY OF CARBON DIOXIDE IN PETROLEUM.
SUMMARY OF THE INVENTION
This invention provides a technique for the commercially practicable utilization of the previously valueless natural gases which contain upwards of fifty volume percent of carbon dioxide by a combination of steps which separate the natural gas feed into two separate streams and provide commercially useful products from both streams.
The first stream, the carbon dioxide content of which has been reduced to a level which is approximately optimal for subsequent methanol synthesis, is subjected to a reaction with water wherein the carbon content of the methane contained therein is converted into carbon monoxide in admixture with hydrogen. The resultant mixture is subjected to a synthesis reaction for the generation of liquid fuels such as methanol or hydrocarbons. The second stream, which comprises a substantial portion of the carbon dioxide from the natural gas feed, is sufficiently low in methane to be of significant utility in tertiary recovery of petroleum.
BRIEF DESCRIPTION OF THE DRAWING
The single FIGURE depicts a flow sheet of a typical process configuration in accord with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As shown in the drawing, a stream of low BTU gas, produced from conventional wells, is supplied via line 10. Such a feed gas may contain, for example, 75% carbon dioxide and 25% methane by volume, usually admixed with small amounts of sulfur compounds, such compounds being primarily hydrogen sulfide. If this low BTU feed gas is sufficiently low in sulfur to meet environmental standards and to be within the sulfur tolerance limitation of the equipment, a portion may optionally be withdrawn by way of line 11 to serve as fuel for steam reformer 32.
The low BTU natural gas feed is passed via line 10 to acid gas removal means 12. Such acid gas removal means may be any conventional process for recovering hydrogen sulfide and carbon dioxide gases, such as the Rectisol process described by G. Ranke at pages 77-84 of Chemical Engineering World, Volume 9, Number 8, August, 1974. Essentially, the natural gas feed is brought into contact with a polar solvent (e.g. methanol) in a multiple-stage extraction process which removes substantially all of the sulfur-containing compounds (H 2 S, COS, mercaptans, etc.) and most of the CO 2 . The extraction parameters may be adjusted to control the amount of CO 2 and sulfur-containing compounds removed and thereby "tailor" the composition of the gas left behind to whatever CO 2 /CH 4 mix is desired.
The acid gas removal means 12 is operated in such a manner as to produce a reformer feed gas for steam reformer 32 which comprises carbon dioxide and methane in approximately optimal proportions for subsequent liquid fuel synthesis step 43. For making methanol such optimal feed for the steam reformer is 20 to 40 mol percent carbon dioxide and 60 to 80 mol percent methane (i.e., 1.5 to 4 moles of CH 4 per mole of CO 2 ). A portion of this reformer feed gas may optionally be withdrawn by line 13 as fuel for steam reformer 32 should a fuel having a lower sulfur content then the low BTU natural gas feed be required.
The reformer feed gas is passed from the acid gas removal means 12, through line 30, to steam reformer 32 where the methane content is reacted with water to form hydrogen and carbon monoxide. The steam reformer is operated under conventional conditions to achieve the general overall reaction scheme:
3CH.sub.4 + CO.sub.2 + 3H.sub.2 O → 3CO + CO.sub.2 + 9H.sub.2
which is composed of sub-reactions:
CH.sub.4 → C + 2H.sub.2 (a) C + H.sub.2 O → CO + H.sub.2 (b) CH.sub.4 + CO.sub.2 → 2CO + 2H.sub.2. (c)
Typical of steam reformer operations are temperatures of 650°-1010° C. (1200°-1850° F.) at pressures in the range of 14-42 kgs. per square centimeter (200-600 pounds per square inch) absolute. The reformer contains a catalyst suitable to promote such reaction (e.g. nickel oxide on alumina) and, in general, it is preferred to supply excess water to the reformer to protect the catalyst against coking. For the present purpose, it is suitable to provide a molar ratio of water to methane of about 1.2:1 to 2.4:1.
The product stream from reformer 32, which comprises CO, CO 2 , H 2 and H 2 O, passes via line 33 to cooler 34, where the mixture is reduced in temperature, and thence through line 35 to condenser 36. Water condensed in condenser 36 is removed in decanter 38 and recycled via line 39 for reuse in the process or is discharged from the system.
The gas phase from decanter 38 is transferred by line 40 to compressor 41, which may be of the multi-stage type with interstage cooling. Some water vapor in the effluent of decanter 38 may condense at interstage cooling and such condensate is preferably discharged for recycle or other disposition. The gas mixture (primarily CO, CO 2 and H 2 ) is compressed to a high pressure suitable to the synthesis reaction and passed by line 42 to liquid fuel synthesis reactor 43 for reaction of the carbon monoxide, carbon dioxide and hydrogen to produce methanol, hydrocarbons, or the like by known techniques. For example, methanol synthesis may be conducted at temperatures in the neighborhood of 200°-370° C (400°-700° F) and pressures of 28-105 kg/sq. cm. (400-1500 psia). Temperatures in the range of 218°-304° C (425°-580° F) are preferred.
The liquid fuel synthesis is carried out over a suitable catalyst, of which many are known in the art. Exemplary of such suitable catalysts would be partially reduced oxides of copper, zinc and chromium, zinc oxide and chromium oxide, zinc oxide and copper, copper and aluminum oxide or cerium oxide, zinc oxide and ferric hydroxide, zinc oxide and cupric oxide, a copper zinc alloy, and oxides of zinc, magnesium, cadmium, chromium, vanadium and/or tungsten with oxides of copper, silver, iron and/or cobalt, and the like. If the liquid fuel to be produced is methanol, the preferred catalyst is copper and zinc oxides on alumina. The reaction proceeds as follows:
CO + 2H.sub.2 → CH.sub.3 OH (a) CO.sub.2 + 3H.sub.2 → CH.sub.3 OH + H.sub.2 O (b) CO.sub.2 + H.sub.2 → CO + H.sub.2 O (c)
The Fischer-Tropsch synthesis is well known to reduce carbon monoxide with hydrogen to hydrocarbons over potassium promoted iron catalyst. Newer techniques involve the use of a carbon monoxide reduction catalyst in combination with a porous crystalline aluminosilicate such as zerolite ZSM-5.
The carbon monoxide reduction is highly exothermic and requires extraction of heat to maintain suitable reaction temperatures. One technique for achieving this result is introduction of cold reactant at spaced points along the path of the reactor 43. For the purposes of this invention, it is preferred to dispose the catalyst in tubes within a vessel for generation of steam from water about the exterior of the tubes. This permits close control of temperatures and two stages of reaction, with the second stage at a lower temperature, by allowing steam to evolve at a lower pressure from the second stage vessel and thus promote completion of the reaction.
Effluent of reactor 43 at line 44, which is largely depleted of carbon monoxide, carbon dioxide and hydrogen content, passes to cooler 45 for condensation of the liquid fuel product. From cooler 45 the product stream passes via line 46 to decanter 47, from which the liquid fuel is withdrawn by line 51 for distillation and such other finishing steps as may be appropriate.
The gas phase from decanter 47 is separately withdrawn through lines 48 and 49 and recycled to compressor 41 for conversion of unreacted CO, CO 2 and H 2 to additional liquid product in reactor 43. From time to time it will be necessary to withdraw a portion of the gas phase from the system to maintain the concentration of inert substances (e.g. methane) at an acceptable level. This is accomplished by means of valved line 50. This purge stream may, upon discharge via valved line 50, be burned for its fuel value.
There are two product streams which result from acid gas removal means 12, the first being the aforedescribed reformer feed gas. The second product stream, which is taken off at line 20, comprises a substantial portion of the carbon dioxide and essentially all of the sulfur compounds from the low BTU natural gas feed. It is preferred that this CO 2 -rich stream be further processed to provide a source of CO 2 valuable for use in tertiary methods of recovery of petroleum from subterranean oil-bearing formations and for other uses.
Should the sulfur compounds contained in the CO 2 -rich stream be at an objectionable concentration, they may be removed by any of several variations of the conventional acid gas scrubbing technologies, such as selective extraction with liquid solvents, sorption on solid bodies and so forth, and such technology is not intended to be limiting in any way. Most conventional scrubbing systems can operate to give a CO 2 -rich gas stream almost nil in H 2 S and a gas stream having a high concentration of the extracted sulfur compounds. When such sulfur removal is desired, the CO 2 -rich stream contained in line 20 is passed to conventional sulfur removal stage 21 and the sulfur-rich stream obtained therefrom is withdrawn from the system by line 22 for subsequent recovery of the sulfur in a Claus Plant or other suitable means.
From here the CO 2 -rich stream, the sulfur content of which is now reduced to an acceptable level, proceeds through line 23 and may take one of two directions. If further uses for the carbon dioxide are not economically attractive because of the location of the plant or other reason, the stream is discharged from the system through valved line 24. Preferably, the plant will be located within a reasonable distance of a subterranean petroleum-bearing formation and therefore the CO 2 -rich stream becomes valuable for use in tertiary methods of recovery of the petroleum. In such case, the CO 2 -rich stream is compressed at compressor 25 and continues through line 26 for use in tertiary recovery by techniques long known in the production art. See, for instance, U.S. Pat. No. 2,623,596, Whorton et al., Dec. 30, 1952.
A typical operation according to the invention is set forth in the Example below, based on computer calculations simulating the several reactions at equilibrium conditions. It will be recognized that any specific plant may vary somewhat from these results, depending largely on kinetic considerations.
EXAMPLE
The natural gas processed by computer simulation was that found in a field in Texas. The analysis of the gas is 75% carbon dioxide, 25% methane, with 50 ppm hydrogen sulfide. The gas is washed in a suitable absorption column (acid gas removal means 12) to remove 85% of the CO 2 content and all of the H 2 S content, to leave a reformer feed gas which is 31% CO 2 and 69% CH 4 by volume. This mixture of methane and carbon dioxide is reacted with water, over nickel oxide on alumina, at 850° C (1560° F) and 15.5 kg/sq. cm. (220 psi) absolute pressure. The compositions of the feed gas and product are shown in Table I.
TABLE I______________________________________Composition of Feed and Products in Steam Reforming Reformer Feed Reformer Product Gas Moles Moles______________________________________H.sub.2 249.93CO 81.11CO.sub.2 45 46.65H.sub.2 O 240 155.59CH.sub.4 100 17.24______________________________________
The product from the steam reformer is cooled and the water content thereof removed. The remaining product is then converted to methanol at 260° C (500° F) and 52.7 kg/sq. cm. (750 psi), absolute pressure, over copper and zinc oxides on alumina at a recycle ratio of 4.8 volumes of gas effluent (stream 49) from decanter 47 per volume of fresh feed to the methanol synthesis reactor. Utilization of synthesis gas is 92.5% at a conversion per pass of 28.7%. Composition of the various streams is shown in Table II in moles. For convenience the reference numeral of the drawing at which each stream is found is noted in parenthesis on each column of the Table.
TABLE II__________________________________________________________________________Composition of Streams in MolesFresh Liquid Purge Recycle Combined ReactorFeed (40) Product (51) (50) (49) Feed (42) Exit (44)__________________________________________________________________________CO 81.11 0.12 4.75 153.67 234.78 159.00CO.sub.246.65 3.71 15.20 491.60 538.25 511.71H.sub.2249.93 0.28 18.11 585.47 835.40 604.24H.sub.2 O0.00 26.51 0.02 0.62 0.62 27.15CH.sub.3 OH0.00 102.03 0.26 8.48 8.48 110.79CH.sub.417.24 0.34 15.10 488.17 505.41 505.41__________________________________________________________________________
The CO 2 which is removed from the low BTU natural gas feed in the acid gas removal step is recovered from the wash liquid by subjecting the solution of CO 2 and sulfur compounds to reduced pressure and drawing off the overhead gas. The CO 2 -rich stream obtained thereby, which comprises approximately 90-99% CO 2 , 1-10% methane and 60 ppm H 2 S, is then compressed and, having such drastically reduced methane content relative to the low BTU natural gas feed, is well-suited for tertiary recovery operations.
The foregoing is meant to be exemplary of the invention disclosed herein and is in no way limiting thereon. As one skilled in the art can readily appreciate, modifications and changes may be made in the embodiments herein described without departing from the scope and spirit of the invention.
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Natural gas having a high CO 2 content and low heating value is converted to useful and valuable products by the extensive removal of CO 2 followed by conversion of the residue to a liquid product useful as fuel (e.g. methanol) through a process combining steam reforming and conversion of the resultant reformer stream, which contains CO, CO 2 and H 2 to liquid products. The CO 2 removed from the natural gas feed is used, in a preferred embodiment, in tertiary methods of recovery of petroleum from natural reservoirs in which primary and secondary methods are no longer viable.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 09/779,437, filed Feb. 9, 2001, now abandoned the contents of which are incorporated by reference in their entirety.
FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
This invention was made with government support under Grant No. DE-FG02-02ER45974, awarded by the Department of Energy, and Grant No. DMR-0213282, awarded by the National Science Foundation. The government has certain rights in the invention.
TECHNICAL FIELD
This invention relates to a temperature-sensing composition.
BACKGROUND
Specialty compositions, which can contain luminescent probes that are sensitive to environmental parameters such as, for example, temperature and pressure, have a variety of analytical applications. For example, specialty compositions can form coatings used to remotely determine the surface temperature of an object in a non-invasive manner.
Objects can be coated with films containing the sensing compositions which emit light of varying intensities, depending on temperature and oxygen pressure. In a specific example, temperature-sensing compositions can be used in combination with compositions for measuring the pressure of an oxygen-containing gas on an aerodynamic surface by oxygen-quenching of luminescent pressure sensing compositions. These compositions can be used to provide convenient and inexpensive methods for determining pressure or temperature maps at surfaces. An example of a pressure-sensing composition includes a phosphorescent porphyrin which has an emission that is quenched by oxygen. This quenching can be used to quantitatively measure the static pressure on the surface of the object. In certain circumstances, the emission of the pressure-sensing composition can have temperature dependence in addition to pressure dependence. Accordingly, pressure measurements containing a temperature-sensing composition can be corrected by sensing fluctuations in the temperature in addition to pressure.
SUMMARY
Temperature-sensing compositions can include an inorganic material, such as a semiconductor nanocrystal. The nanocrystal can be a dependable and accurate indicator of temperature. The intensity of emission of the nanocrystal varies with temperature and can be highly sensitive to surface temperature. The nanocrystals can be processed with a binder to form a matrix, which can be varied by altering the chemical nature of the surface of the nanocrystal. A nanocrystal with a compatibilizing outer layer can be incorporated into a coating formulation and retain its temperature sensitive emissive properties.
In one aspect, a method of sensing temperature includes providing a temperature sensor including a matrix on a surface of a substrate, the matrix comprising a semiconductor nanocrystal in a binder, irradiating a portion of the sensor with an excitation wavelength of light, detecting emission of light from the sensor, and determining the temperature from the emission of light from the sensor.
In another aspect, a temperature sensor includes a matrix containing a semiconductor nanocrystal. The matrix can be formed from a semiconductor nanocrystal and a binder.
In another aspect, a temperature-sensing coating includes a matrix on a surface of a substrate. The matrix can include a semiconductor nanocrystal in a binder.
In another aspect, a temperature-sensing paint includes a semiconductor nanocrystal in a binder and a deposition solvent. The semiconductor nanocrystal can emit light independent of oxygen pressure and dependent upon temperature upon irradiation by an excitation wavelength of light. The emission intensity can change by 1.1-1.6% per degree centigrade. The paint can include a pressure-sensitive composition, the pressure-sensitive composition emitting light dependent upon oxygen pressure upon irradiation by an excitation wavelength of light. The pressure-sensitive composition can include a porphyrin, such as a platinum porphyrin. The deposition solvent can include an alcohol.
In another aspect, a method of manufacturing a temperature-sensing paint includes combining a semiconductor nanocrystal, a binder, and a deposition solvent to form a paint. The paint can be used to manufacture a temperature sensor by depositing a temperature-sensing paint on a surface of a substrate.
The semiconductor nanocrystal can include a group II-VI semiconductor, a group III-V semiconductor, or group IV semiconductor, for example, ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgSe, HgTe, AlN, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, InN, InP, InAs, InSb, TlN, TlP, TlAs, TlSb, PbS, PbSe, PbTe, or mixtures thereof. The semiconductor nanocrystal can be overcoated with a second semiconductor material. The semiconductor nanocrystal can include an organic or organometallic overlayer, the overlayer making the nanocrystal dispersible in the binder. The overlayer can include a hydrolyzable moiety, such as a metal alkoxide.
The nanocrystal can be a member of a substantially monodisperse core population, such as a population exhibiting less than a 15% rms deviation in diameter of the nanocrystal, which can emit light in a spectral range of no greater than about 75 nm full width at half max (FWHM). The nanocrystal can photoluminesce with a quantum efficiency of at least 10% and can have a particle size in the range of about 15 Å to about 125 Å.
The binder can include an organic polymer or inorganic matrix.
The details of one or more embodiments are set forth in the accompanying drawings and the description below. Other features and advantages will be apparent from the description and drawings, and from the claims.
DESCRIPTION OF DRAWINGS
FIG. 1 is a graph depicting emission spectra of ZnS-capped CdSe nanocrystals in a poly(lauryl methacrylate) matrix irradiated at 480 nm at various temperatures.
FIG. 2 is a graph depicting integrated emission intensity of the ZnS-capped CdSe nanocrystals dispersed in a matrix over a range of temperatures.
DETAILED DESCRIPTION
A temperature-sensing composition can include a semiconductor nanocrystal. Nanocrystals composed of semiconductor material can be illuminated with a light source at an absorption wavelength to cause an emission at an emission wavelength, the emission having a frequency that corresponds to the band gap of the quantum confined semiconductor material. The band gap is a function of the size of the nanocrystal. Nanocrystals having small diameters can have properties intermediate between molecular and bulk forms of matter. For example, nanocrystals based on semiconductor materials having small diameters can exhibit quantum confinement of both the electron and hole in all three dimensions, which leads to an increase in the effective band gap of the material with decreasing crystallite size. Consequently, both the optical absorption and emission of nanocrystals shift to the blue (i.e., to higher energies) as the size of the crystallites decreases.
The emission from the nanocrystal can be a narrow Gaussian emission band that can be tuned through the complete wavelength range of the ultraviolet, visible, or infrared regions of the spectrum by varying the size of the nanocrystal, the composition of the nanocrystal, or both. For example, CdSe can be tuned in the visible region and InAs can be tuned in the infrared region. The narrow size distribution of a population of nanocrystals can result in emission of light in a narrow spectral range. The population can exhibit less than a 15% rms deviation in diameter of the nanocrystals, preferably less than 10%, more preferably less than 5%. Spectral emissions in a narrow range of no greater than about 75 nm, preferably 60 nm, more preferably 40 nm, and most preferably 30 nm full width at half max (FWHM) can be observed. The breadth of the emission decreases as the dispersity of nanocrystal diameters decreases. Semiconductor nanocrystals can have high emission quantum efficiencies such as greater than 10%, 20%, 30%, 40%, 50%, 60%, 70%, or 80%.
The narrow emission band of the nanocrystal can improve the performance and reliability of the temperature-sensing composition relative to compositions that include conventional molecular probes that have broad, fixed wavelength emission bands. In addition, the excitation profile of the nanocrystal can be broad and intense, which can allow efficient excitation of the nanocrystals across a range of wavelengths in the visible spectrum. These factors together offer flexibility in the design of optical detection systems for temperature-sensing applications.
The nanocrystal can be chemically stable when illuminated. The nanocrystal can be relatively unreactive with other materials, which can permit it to be used as a temperature probe in a wide variety of environments. For example, the emission of the nanocrystal can be independent of gas pressure, such as oxygen pressure, or resistant to degradation in the presence of oxygen. Conventional organic temperature probes can degrade rapidly when illuminated, decreasing the useful lifespan of the coatings that contain them. A variety of applications can be envisioned for temperature-sensing compositions that contain nanocrystals on the well-defined temperature dependent emission properties of the nanocrystal. For example, in aerospace engineering, nanocrystal-based temperature indicators can be used as the active component in temperature sensitive paints or as an internal temperature calibrant for two-component pressure sensitive paints.
Methods of preparing monodisperse semiconductor nanocrystals include pyrolysis of organometallic reagents, such as dimethyl cadmium, injected into a hot, coordinating solvent. This permits discrete nucleation and results in the controlled growth of macroscopicquantities of nanocrystals. Preparation and manipulation of nanocrystals are described, for example, in U.S. Pat. No. 6,322,901, incorporated herein by reference in its entirety. The method of manufacturing a nanocrystal is a colloidal growth process. Colloidal growth occurs by rapidly injecting an M donor and an X donor into a hot coordinating solvent. The injection produces a nucleus that can be grown in a controlled manner to form a nanocrystal. The reaction mixture can be gently heated to grow and anneal the nanocrystal. Both the average size and the size distribution of the nanocrystals in a sample are dependent on the growth temperature. The growth temperature necessary to maintain steady growth increases with increasing average crystal size. The nanocrystal is a member of a population of nanocrystals. As a result of the discrete nucleation and controlled growth, the population of nanocrystals obtained has a narrow, monodisperse distribution of diameters. The monodisperse distribution of diameters can also be referred to as a size. The process of controlled growth and annealing of the nanocrystals in the coordinating solvent that follows nucleation can also result in uniform surface derivatization and regular core structures. As the size distribution sharpens, the temperature can be raised to maintain steady growth. By adding more M donor or X donor, the growth period can be shortened.
The M donor can be an inorganic compound, an organometallic compound, or elemental metal. M is cadmium, zinc, magnesium, mercury, aluminum, gallium, indium or thallium. The X donor is a compound capable of reacting with the M donor to form a material with the general formula MX. Typically, the X donor is a chalcogenide donor or a pnictide donor, such as a phosphine chalcogenide, a bis(silyl) chalcogenide, dioxygen, an ammonium salt, or a tris(silyl) pnictide. Suitable X donors include dioxygen, bis(trimethylsilyl) selenide ((TMS) 2 Se), trialkyl phosphine selenides such as (tri-n-octylphosphine) selenide (TOPSe) or (tri-n-butylphosphine) selenide (TBPSe), trialkyl phosphine tellurides such as (tri-n-octylphosphine) telluride (TOPTe) or hexapropylphosphorustriamide telluride (HPPTTe), bis(trimethylsilyl)telluride ((TMS) 2 Te), bis(trimethylsilyl)sulfide ((TMS) 2 S), a trialkyl phosphine sulfide such as (tri-n-octylphosphine) sulfide (TOPS), an ammonium salt such as an ammonium halide (e.g., NH 4 Cl), tris(trimethylsilyl) phosphide ((TMS) 3 P), tris(trimethylsilyl) arsenide ((TMS) 3 As), or tris(trimethylsilyl) antimonide ((TMS) 3 Sb). In certain embodiments, the M donor and the X donor can be moieties within the same molecule.
A coordinating solvent can help control the growth of the nanocrystal. The coordinating solvent is a compound having a donor lone pair that, for example, has a lone electron pair available to coordinate to a surface of the growing nanocrystal. Solvent coordination can stabilize the growing nanocrystal. Typical coordinating solvents include alkyl phosphines, alkyl phosphine oxides, alkyl phosphonic acids, or alkyl phosphinic acids, however, other coordinating solvents, such as pyridines, furans, and amines may also be suitable for the nanocrystal production. Examples of suitable coordinating solvents include tri-n-octyl phosphine (TOP) and tri-n-octyl phosphine oxide (TOPO). Technical grade TOPO can be used.
Size distribution during the growth stage of the reaction can be estimated by monitoring the absorption line widths of the particles. Modification of the reaction temperature in response to changes in the absorption spectrum of the particles allows the maintenance of a sharp particle size distribution during growth. Reactants can be added to the nucleation solution during crystal growth to grow larger crystals. By stopping growth at a particular nanocrystal average diameter and choosing the proper composition of the semiconducting material, the emission spectra of the nanocrystals can be tuned continuously over the wavelength range of 400 nm to 800 nm. The nanocrystal has a diameter of less than 150 Å. A population of nanocrystals has average diameters in the range of 15 Å to 125 Å.
The nanocrystal can be a member of a population of nanocrystals having a narrow size distribution. The nanocrystal can be a sphere, rod, disk, or other shape. The nanocrystal can include a core of a semiconductor material. The nanocrystal can include a core having the formula MX, where M is cadmium, zinc, magnesium, mercury, aluminum, gallium, indium, thallium, or mixtures thereof, and X is oxygen, sulfur, selenium, tellurium, nitrogen, phosphorus, arsenic, antimony, or mixtures thereof.
The core can have an overcoating on a surface of the core. The overcoating can be a semiconductor material having a composition different from the composition of the core. The overcoat of a semiconductor material on a surface of the nanocrystal can include a group II-VI, III-V or IV semiconductor, such as, for example, ZnO, ZnS, ZnSe, ZnTe, CdO, CdS, CdSe, CdTe, MgO, MgS, MgSe, MgTe, HgO, HgS, HgSe, HgTe, AlN, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, InN, InP, InAs, InSb, TlN, TlP, TlAs, TlSb, PbS, PbSe, PbTe, or mixtures thereof. For example, ZnS, ZnSe or CdS overcoatings can be grown on CdSe or CdTe nanocrystals. An overcoating process is described, for example, in U.S. Pat. No. 6,322,901, incorporated herein by reference in its entirety. By adjusting the temperature of the reaction mixture during overcoating and monitoring the absorption spectrum of the core, over coated materials having high emission quantum efficiencies and narrow size distributions can be obtained.
The particle size distribution can be further refined by size selective precipitation with a poor solvent for the nanocrystals, such as methanol/butanol as described in U.S. Pat. No. 6,322,901, incorporated herein by reference. For example, nanocrystals can be dispersed in a solution of 10% butanol in hexane. Methanol can be added dropwise to this stirring solution until opalescence persists. Separation of supernatant and flocculate by centrifugation produces a precipitate enriched with the largest crystallites in the sample. This procedure can be repeated until no further sharpening of the optical absorption spectrum is noted. Size-selective precipitation can be carried out in a variety of solvent/nonsolvent pairs, including pyridine/hexane and chloroform/methanol. The size-selected nanocrystal population can have no more than a 15% RMS deviation from mean diameter, preferably 10% RMS deviation or less, and more preferably 5% RMS deviation or less.
Transmission electron microscopy (TEM) can provide information about the size, shape, and distribution of the nanocrystal population. Powder x-ray diffraction (XRD) patterns can provided the most complete information regarding the type and quality of the crystal structure of the nanocrystals. Estimates of size are also possible since particle diameter is inversely related, via the X-ray coherence length, to the peak width. For example, the diameter of the nanocrystal can be measured directly by transmission electron microscopy or estimated from x-ray diffraction data using, for example, the Scherrer equation. It also can be estimated from the UV/Vis absorption spectrum.
The outer surface of the nanocrystal can include layer of compounds derived from the coordinating solvent used during the growth process. The surface can be modified by repeated exposure to an excess of a competing coordinating group to form an overlayer. For example, a dispersion of the capped nanocrystal can be treated with a coordinating organic compound, such as pyridine, to produce crystallites which disperse readily in pyridine, methanol, and aromatics but no longer disperse in aliphatic solvents. Such a surface exchange process can be carried out with any compound capable of coordinating to or bonding with the outer surface of the nanocrystal, including, for example, phosphines, thiols, amines and phosphates. The nanocrystal can be exposed to short chain polymers which exhibit an affinity for the surface and which terminate in a moiety having an affinity for a suspension or dispersion medium. Such affinity improves the stability of the suspension and discourages flocculation of the nanocrystal.
The compound forming the overlayer can have a reactive group that can react with another compound to bond the nanocrystal to the binder. The binder can form a matrix. The matrix can be an organic polymer matrix, such as a polyacrylate matrix, or an inorganic matrix, such as a sol-gel-derived matrix.
The reactive group can be a polymerizable moiety, such as an acrylate moiety, a stryryl moiety, or a hydrolyzable moiety, for example, silicon alkoxide, titanium alkoxide, zirconium alkoxide, or other metal alkoxide, metal amide, metal carboxylate, or metal halide groups. The reactive groups can react with each other, or with reactive groups of other compounds or monomers, to form a solid matrix containing the nanocrystals. In this manner, the nanocrystal can be incorporated into a solid matrix formed in part by reaction of the reactive groups. Alternatively, the reactive group can be a functionality, such as an amino or hydroxyl group, that can react with a multifunctional component, such as a dicarboxylic acid, or reactive derivative thereof, or a diisocyanate, to form a solid matrix containing the nanocrystals.
The temperature-sensing composition can be applied to a substrate as a paint. The paint can include a binder and a deposition solvent. The binder can produce a film on a surface of an object upon evaporation of solvent. The binder can include an organic or inorganic polymer or prepolymer, for example, a polymer or prepolymer typically used in a paint composition. The binder can form a film by chemical reaction with atmospheric moisture, a heat or light induced reaction, a chemical interaction with other components within the paint, such as the nanocrystal overlayer, or combinations thereof. The binder can include a silicone polymer, for example, a thermoplastic silicone copolymer or dimethyl polysiloxane, a silicone co-polymers such as silicone-polyurethane or silicone-polyester co-polymers, an acrylate or urethane polymer or prepolymer, or a hydrolyzable composition including a silicon alkoxide, a titanium alkoxide, a zirconium alkoxide, an aluminum alkoxide, or other metal alkoxide that can form an inorganic matrix. The deposition solvent is a solvent that dissolves the nanocrystal and binder and can be sufficiently volatile to produce a smooth film. The deposition solvent can include 1,1,1-trichloroethane, dichloromethane, ethyl alcohol, butyl alcohol, isopropyl alcohol, cyclohexane, or mixtures thereof.
The paint can be applied to a substrate to form a film. A white substrate can improve the performance of the sensor by reflecting the emitted light more completely. The film can be thin, for example, 1-100, 2-50, 3-20, or 5-10 microns in thickness. Film thickness can be determined using an ultraviolet/visible spectrometer by measuring the optical absorption of the nanocrystal and applying Beer's law. The nanocrystal can be uniformly distributed in the film. The coated surface can be irradiated with the excitation wavelength. While the coated object is irradiated, the emission wavelength can be monitored, for example, with a photomultiplier tube. The intensity of the emission can be compared with predetermined calibration values to produce measurements of the temperature on the surface. By distributing nanocrystals over a surface and monitoring emission at particular regions on the surface, a quantitative map of temperature on the surface can be obtained.
The temperature-sensing composition can be used in the preparation of pressure sensitive paints, such as those described in Gouterman et al., U.S. Pat. No. 5,186,046, incorporated by reference in its entirety. The pressure sensitive paint includes a pressure-sensing composition that produces an emission that is dependent on pressure. Any temperature dependence can be corrected by including the temperature-sensing composition in the pressure sensitive paint. A pressure-sensing composition can include a porphyrin, such as a platinum porphyrin, in particular, platinum octaethylporphyrin. For porphyrins, the individual molecules should be separated by at least about 50 Å to prevent triplet-triplet deactivation. This intermolecular separation corresponds to a porphyrin concentration of about 10 −2 molar. The excitation spectrum for platinum octaethylporphyrin displays a strong excitation band in the near ultraviolet region of the visible spectrum at approximately 380 nm and a weaker band in the green region at approximately 540 nm and an emission in the red region of the visible spectrum at approximately 650 nm. Platinum octaethylporphyrin has an emission quantum yield of approximately 90%.
In a pressure sensitive paint, either the excitation wavelength or the emission wavelength of the pressure-sensing composition and the temperature-sensing composition are different. When a common excitation wavelength is present, the emission wavelength maxima can be separated by 10 nm or more, or 20 nm or more, so that the data for each composition can be measured separately. One advantage of a temperature-sensing composition including a nanocrystal is that the emission wavelength of the nanocrystal can be selected so that the emission does not interfere with the emission from the pressure-sensing composition. The excitation wavelength can be selected so that the nanocrystal and the pressure-sensing composition are excited at the same wavelength.
When different emission wavelengths are generated, the intensities can be measured by rotating different interference filters in front of a detection device, such as a video camera, or a photomultiplier tube, during irradiation with the excitation wavelength. Alternatively, a diode array detector can be used to monitor emissions.
EXAMPLES
Semiconductor Nanocrystals were Shown to be Emissive Temperature Probes in Solution and in Polymer Matrices
Highly emissive nanocrystals of cadmium selenide (CdSe) were synthesized by colloidal growth, such as, for example, the method described in U.S. Pat. No. 6,322,109, incorporated herein by reference in its entirety. The CdSe nanocrystals were overcoated with zinc sulfide (ZnS). Semiconductor nanocrystals with average diameters in the range 4 to 5 nm were size selected by precipitation, reducing the distribution of sizes about the average diameter. The size-selected nanocrystals provide indicators with an emission maximum at 600 nm at ambient temperature. The absorption profile of the size-selected ZnS-capped CdSe nanocrystals was intense, having an onset of absorbance that began at approximately 600 nm and extended into the ultraviolet spectral region.
The nanocrystals are well-suited for use as luminescent temperature probes. ZnS-capped CdSe nanocrystals dispersed in a poly(lauryl methacrylate) polymer matrix provided a material for optical measurements. A polymer rod containing nanocrystals was prepared by redispersing synthesized nanocrystals into laurylmethacrylate monomer containing TOP (5% v/v). Then, ethyleneglycol dimethacrylate crosslinker was added to the nanocrystal-monomer solution with 1:4 volume ratio of cross-linker to monomer. After azobisisobutyronitrile radical initiator (<1% (w/w)) was added, the final solution was transferred to a 60 mm×5 mm (length×diameter) glass tube and polymerized in an oven at 70-75° C. for 2 hours. The high-clarity nanocrystal-polymer composite rod was then removed from the glass mold.
A thin disk of the polymer-supported nanocrystals was cut from the rod with a single edge razor blade. The disk had a diameter of 5 mm and a thickness of approximately 1 mm. The disk was mounted flat on a surface of a temperature-controlled stage using thermal grease (CRY-CON thermal conductive grease available from Lake Shore Cryotonics). The stage was a flat surface temperature controlled with a water bath. Temperatures were maintained within ±0.5 per degree Centigrade. The disk was irradiated with monochromatic blue-green light having a wavelength of 480 nm. The emission intensity of the nanocrystals in the disk was measured at various temperatures. The temperature dependent emission spectrum of the polymer-supported nanocrystals was measured using a steady-state emission spectrophotometer. The flat disk of nanocrystals mounted on a thermostatically controlled black flat plate was orientated at a 45° angle to an incident monochromatic excitation beam. Monochromatic excitation was achieved using a 200 W Hg—Xe arc lamp equipped with a Spex Model 1680B monochromator and a chopper. The emitted light intensity was measured normal to the incident excitation beam using a dry-ice cooled photomultiplier tube (Hamamatsu Type R943-02) after dispersal with a Spex Model 1870B monochromator. The background spectrum was subtracted using a Stanford Scientific Instruments photon counter. Specifically, the temperature of the stage was varied from 25 to 40, 40 to 25, 25 to 15, 15 to 5, and 5 to 25 degrees centigrade. FIG. 1 depicts the emission intensity of the disk at each temperature.
The decrease in emission intensity with temperature is linear. As depicted in FIG. 2 , the change in emission intensity was 1.3% per degree centigrade. The temperature dependence of the emission intensity is not dependent on the characteristics of the sample to any great degree. The slope of the temperature dependent emission intensity does not vary greatly from sample to sample. Generally, the slope varies from 1.1 to 1.6% per degree centigrade. The emission intensity also can be independent of excitation wavelength in the visible spectrum and is not dependent on the initial quantum yield of the sample or the supporting matrix. Furthermore, the change in emission intensity with temperature is fully reversible as indicated by the superposition of spectra obtained at 25 degrees centigrade at the beginning, middle, and end of the experiment after heating and cooling the disk. There is no hysterisis, which could indicate decomposition of the nanocrystals. Similar effects have been noted for nanocrystals dispersed in other matrices. For example, the nanocrystals can be dispersed in a sol-gel matrix. 40-50 mg of CdSe nanocrystal, either overcoated with ZnS or bare, which were washed repeatedly to remove any excess TOPO cap, are pumped dry under a vacuum and transferred into an inert atmosphere glove box. The nanocrystals were then redissolved in a solvent mixture consisting of 150 mg of tetrahydrofuran, 600 mg ethyl alcohol and 60 mg of tris-hydroxylpropyl phosphine. After stirring this solution for 10 minutes at approximately 50° C., 60-70 mg of tetrabutoxy (IV) titanate was added dropwise to this solution. The solution was then further stirred for 3 hours under the inert nitrogen atmosphere of the glove box. The films were finally prepared by spin-coating a freshly filtered nanocrystal precursor solution onto freshly cleaned microscope slides for 1 minute and then annealing for 2 minutes at 160-200° C. The spinning speed was between 3000 and 7500 rpm and decided by the desired thickness of the film. Thicker films were generated at slower spin speeds. It is necessary to eliminate exposure of the precursor solution to water prior to spin-coating, hence all the solvents used were anhydrous and the solution was allowed to pre-polymerize in the glove box.
In another example, a dispersion of nanocrystals in a binder of Dow C734, a silicone polymer was prepared. The CdSe nanocrystals were dissolved in dichloromethane at a concentration of at least 1 mM to form a nanocrystal solution. A 5:1 or 10:1 ratio of the nanocrystal solution to binder was combined and thoroughly mixed until uniform. The binder-nanocrystal solution was deposited on a glass slide or a quartz slide to form a film. Various concentrations of nanocrystal in binder were prepared such that color of the films ranged from white (low concentration of nanocrystals, ˜0.1 mM) to pale in color as determined by naked eye in room light. The films were excited using with monochromatic blue-green light having a wavelength of 480 nm. The lower concentration films produced emission that were very difficult to detect by eye, but could be easily seen with a photomultiplier tube detector. Emission from the more concentrated films was visible by eye. The emission from the higher concentration films could also be observed by eye using a hand held Hg lamp for excitation. The maximum wavelength of emission and band width of the emission are similar for nanocrystals in binder and nanocrystals in solution.
Other embodiments are within the scope of the following claims.
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Temperature-sensing compositions can include an inorganic material, such as a semiconductor nanocrystal. The nanocrystal can be a dependable and accurate indicator of temperature. The intensity of emission of the nanocrystal varies with temperature and can be highly sensitive to surface temperature. The nanocrystals can be processed with a binder to form a matrix, which can be varied by altering the chemical nature of the surface of the nanocrystal. A nanocrystal with a compatibilizing outer layer can be incorporated into a coating formulation and retain its temperature sensitive emissive properties.
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FIELD OF THE INVENTION
The following invention relates generally to the application of an artificial nail tip to a finger nail. More specifically, this invention relates to methods of applying an artificial nail tip using cyanoacrylate, methacrylate, polymerization inhibitors and accelerants, and opaquing agents with a goal of reducing appreciably the time required for applying artificial nails.
Finger nail augmentation has become a growth industry relying on professional manicurists who practice time consuming methods. Curing times in nail processing have limited productivity.
BACKGROUND OF THE INVENTION
The use of cyanoacrylates and methacrylates to apply artificial nails to nail tips is not new. Various method have been developed to try to make the application of an artificial nail tip to a finger nail safer, easier, quicker and more economical and effective. They have been met with varying degrees of success, but still each suffer from differing types of problems or difficulties.
Some examples are disclosed in U.S. Pat. No. 5,824,180 to Mikuni, et al. The Mikuni patent discloses the prior art method of: (i) bonding an artificial nail tip to a finger nail with an adhesive; (ii) then applying a polymerizing resin to fill in the recessed part of the junction between the artificial nail tip and finger nail; (iii) then applying a polymerization accelerator; (iv) filing the resulting polymerized surface; and (v) coating the resulting nail surface with a lacquer or resin. This method requires the user to engage in the substantial, time-consuming effort of filing the polymerized resin surface. In addition, the Mikuni reference teaches that use of polymerization accelerators involves use of a solvent, which generates an odor that is unpleasant, and creates a troublesome working environment.
The Mikuni patent is directed toward trying to overcome these types of difficulties by use of photocurable adhesive. Photocurable adhesives have not proven satisfactory for a variety of reasons such as expense, lengthy curing times, and difficulty of controlling the timing of the curing process once the photocurable adhesive is exposed to light.
Other prior art methods are disclosed in U.S. Pat. No. 4,626,428 to Weisberg, et al. For example, the Weisberg, et al. patent describes the following prior art nail sculpting process: (i) cleaning, roughening and treating a finger nail with bromide; (ii) coating the nail with an adhesive such as cyanoacrylate ester, or a primer container methacrylic acid that binds the acrylic to the nail; (iii) wetting a brush with liquid methacrylate esters and a promoter, such as toluidine, to induce the decomposition of benzoyl peroxide applied in the next step; (iv) dipping the brush in powered methacrylate containing benzoyl peroxide to act as a polymerization catalyst, causing the methacrylate esters and powder to polymerize sufficiently to provide a dough-like substance; (v) brushing the dough on the nail; and (vi) after the dough has cured and hardened in place on the finger nail, sculpting the artificial nail surface on the surface of the hardened dough.
The Weisberg, et al. patent explains that this sculpting method is very difficult to perform. This sculpting method requires substantial dexterity, time, and experience to properly apply and sculpt the polymer dough, including substantial filing of the dough after it has cured. The sculpting method also ruins the brush since a substantial quantity of the dough often hardens in place on the brush.
The Weisberg, et al. patent describes other variants of the nail sculpting method in which the nail is first wetted and then dipped into a powder, rather than applying a dough, and then covered with other seal and fill coats. The Weisberg patent notes that the prior art methods do not induce sufficient cross-linking of the monomers in the various components, so the resulting nail is not sufficiently strong and durable.
The method of the Weisberg, et al. patent seeks to solve these problems by first applying a solvent to the brush prior to exposure of the brush to the liquid. The solvent helps prevent polymerization and bonding to the brush. In addition, the Weisberg method teaches dipping of the wetted nail in a resin powder of polymethacrylate esters and benzoyl peroxide, which is then again coated with liquid methacrylate ester monomers for curing and cross-linking of the liquids and powder in air. This prior art method, however, requires use of solvents of the type that prevent polymerization, and as noted by the Mikuni patent, these types of solvents present significant working environment issues.
U.S. Pat. No. 4,687,827 to Russo also discloses a method of applying nail tips by use of polymerization accelerators to achieve shortened curing time. The Russo patent also discloses extension of shelf life of cyanoacrylate adhesive, prior to application of the adhesive, by addition of polymerization inhibitors such as hydroquinone. The Russo patent also suggests inclusion of silica to build up the nail surface. Like the Weisberg patent, however, the Russo patent does so in the context of teaching use of pre-wetting solvent to keep the liquid adhesive cyanoacrylates from curing too soon.
U.S. Pat. No. 4,844,102 to Repensek discloses use of a dryer sprayed on cyanoacrylate to encourage faster polymerization during application of an artificial finger nail tip. The Repensek method, however, also involves use of a polymer solvent (and the attendant problems and issues noted above). In the Repensek method, the solvent is applied after application of the applied monomers and polymers in order to dissolve, spread, and shape them and, by the endothermic evaporation of the solvent, reduce the amount of heat otherwise imparted to the finger nail by the exothermic reaction of the polymerizing components.
U.S. Pat. No. 5,770,184 to Keller teaches the application of a nail tip by applying one or (optionally when used to apply a prefabricated nail) two coats of cyanoacrylate adhesive followed by immediate application of a nail tip. The Keller patent teaches that the user should then wait for the cyanoacrylate adhesive to dry and secure the nail tip to the finger nail, and then add additional coats of cyanoacrylate followed by spraying the cyanoacrylate coats with a mixture of pink acrylic powder and sodium bicarbonate to accelerate polymerization. The Keller patent also suggests use of benzoyl peroxide in the powder, to accelerate polymerization, and the use of opaquing agents such as silicon dioxide. The Keller method requires a substantial amount of time waiting for the first and, if applied, second coat of cyanoacrylate adhesive to dry under the applied vinyl nail tip. The applicant also believes that the nail resulting from the Keller patent is not as strong as is desirable.
SUMMARY OF THE INVENTION
The applicant has invented a method of applying an artificial nail to a finger nail and composition. One hallmark involves reducing the time required to install artificial nails. The method includes the steps of applying a first base resin coat of cyanoacrylate to the finger nail and quickly curing the base resin with a dryer, and then applying the same base resin for application of the artificial nail over the first coating. Next, apply one coat of finish resin to the exposed artificial nail surface, and dip the finger nail and nail tip into a powder resin mixture of poly methyl methacrylate and a polymerization catalyst. Then apply a further coat of finish resin to the finger nail and nail tip. Finally, spray the finger nail and nail tip with an aromatic dryer to accelerate polymerization.
Preferably, the nail tip is secured in place without use of any solvents such as those for dissolving polymers, and without the need for any grinding or filing and with only a relatively light buffing of the nail. Preferably, the base resin mixture includes a polymerization inhibitor, and the powder resin mixture includes both a polymerization catalyst and an opaquing and filling agent such as silica.
Most preferably, the polymerization dryer comprises ethyl acetate and aromatic amines.
Although this is a brief summary of the invention, it is to be understood that the scope of the invention is determined by reference to the accompanying claims and not by whether a given embodiment includes the features briefly stated herein.
OBJECTS OF THE INVENTION
It is an object of the present invention to provide an easy, quick, and relatively safe and reliable method of applying an artificial nail to a finger nail and composition.
It is an advantage of the present invention that it is very economical because artificial nails can be installed in a fraction of the time heretofore experienced.
It is yet another advantage of the present invention that it provides a nail tip that is very securely mounted on the finger nail.
It is a further advantage of the present invention that it can secure an aesthetically pleasing nail tip to a finger nail without use of harmful solvents and without the need for grinding or filing of the natural nail tip or other components applied with the method.
A still further advantage of the present invention is that it utilizes relatively readily available and economical components and compositions.
Yet another advantage is that the present invention can provide components having a long shelf life and yet allows the nail tip to be secured in position on the finger nail quickly and without a long polymerization or curing time.
An additional advantage is that the present method can include use of opaquing and filling agents that makes the resulting nail appear more natural while also providing a more effective and quick method of filling in any cracks, depressions, or joints when finishing the nail and nail tip.
These and other objects will be made manifest when considering the following detailed specification when taken in conjunction with the appended drawing figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a chart showing the main steps and order of the steps in the preferred method.
FIG. 2 is a perspective view showing applying a base resin.
FIG. 3 is a perspective view showing applying a dryer.
FIG. 4 is a perspective view showing filing the nail.
FIG. 5 is a perspective view showing applying the base resin.
FIG. 6 is a perspective view showing applying the nail.
FIG. 7 is a perspective view showing the nail applied.
FIG. 8 is a perspective view showing applying a finish resin.
FIG. 9 is a perspective view showing dipping the nail in a powder glaze.
FIG. 10 is a perspective view showing applying the finish resin.
FIG. 11 is a perspective view showing applying the dryer.
FIG. 12 is a perspective view showing filing the nail.
FIG. 13 is a perspective view showing applying the sealer.
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring now to FIG. 1, the applicant's preferred embodiment consists of twelve easy steps, with no mandatory nail brushing, no mandatory nail filing, and no mandatory use of polymer solvents. Before commencing the twelve steps of FIG. 1, however, the applicant generally prefers to engage in certain limited nail preparation steps as follows:
1. Remove any pre-existing nail polish from the finger nail with a nail polish stripper in a fashion well known to those of skill in the art.
2. Cleanse the hands, including the finger nails, with a hygienic soap; rinse the hands and nails with warm water, and let dry thoroughly. It is important that this cleaning step should not involve use of any primers or dehydrators.
3. Push back the cuticles on each finger nail with a rubber tipped cuticle pusher such as are commonly available on the market.
4. Trim and shape each finger nail, leaving approximately {fraction (1/16)}″ of free outer edge on the exposed end of the finger nail. Smooth the free edge using a file, preferably of 240 grit (medium grit).
5. Remove any shine from the natural nail with a file, preferably of 600 grit (fine grit). Wipe away any nail dust.
The preferred method shown in FIG. 1 then proceeds immediately thereafter as follows:
1. Size the artificial nail tip to the desirable length.
2. Using a nail brush (such as those that are commonly available in the trade and are provided commonly inside a bottle downwardly extending from the bottle cap), brush a first coating of a base adhesive resin mixture smoothly onto the entire natural nail surface. Preferably, the brush is included in the cap of the bottle for the base adhesive resin mixture.
3. Spray the entire exposed part of the nail, including the nail sides, with an aromatic dryer (to accelerate polymerization) from 4-5″ away from the nail.
This step causes the base resin mixture to polymerize or cure and harden.
4. Using preferably a 240 (medium) grit file, remove the surface shine from the portion of the finger nail on which the artificial nail is to be mounted. The artificial nail should preferably be mounted on at least {fraction (1/16)}″ of natural nail free edge as per FIG. 7 . Remove any filing dust.
5. Brush a second coating of the base adhesive resin mixture onto the portion of the outer nail surface on which the artificial nail tip is to be mounted (at least {fraction (1/16)}″ of the free edge and away from the cuticle).
6. Apply the artificial nail tip to the area on the finger nail coated with the second coating of the base adhesive resin mixture. The preferred nail tip is the Nouveau Tip available from Backscratchers®.
7. Brush a first coating of the finish adhesive resin mixture over the entire artificial nail tip and any exposed underlying portion of the finger nail, but not on the ⅛″ portion extending from the cuticle. As noted above, that portion of the nail should not be coated or covered and should remain exposed to the open air.
8. Dip the finger nail/artificial nail tip into a container of a powder glaze resin mixture. Remove the finger nail/artificial nail tip from the container and lightly tap off any excess powder glaze resin mixture back into the container or onto a piece of paper for later return of the unused powder resin glaze mixture back into its container.
9. Brush a second coating of the finish adhesive resin mixture over the entire artificial nail tip and any exposed underlying portion of the finger nail, but not on the {fraction (1/16)}″ portion of the finger nail extending from the cuticle. At this point, the applicant prefers to wipe any base or powder glaze resin off of the brush and return the brush to the resin container.
10. Spray the entire exposed part of the finger nail and nail tip with an aromatic dryer from 4-5″ away from the nail.
11. Buff the finger nail and tip to smooth out the exposed nail and nail tip surface. Using preferably 600 grit (fine), then white and gray buffers. The applicant prefers to buff the nail tip in three successive stages using first the 600, then the white, then the gray. The applicant also prefers to buff around the cuticles to make sure to remove any resin that has cured in that area, to prevent early lifting of the nail tip from the finger nail.
12. Optionally, the operator may then apply, to the exposed portions of the nail tip only, a sealer such as Extreme Glaze Sealer™ available from Backscratchers®. Optionally, the preferred method may also include applying a polish or a cuticle treatment to the cuticle and underside of the nail, such as Nail Radiance® also available from Backscratchers®.
In the applicant's preferred method, the base adhesive resin mixture consists of 70-100% of ethyl cyanoacrylate, 10-30% poly methyl methacrylate, and 0-1% hydroquinone. The aromatic dryer consists of 80-100% ethyl acetate and 0-20% aromatic amines. The finish adhesive resin mixture consists of 70-100% of ethyl cyanoacrylate, 10-30% of poly methyl methacrylate, and 0-1% of hydroquinone. The powder glaze mixture consists of 90-100% poly (ethyl or ethyl/methyl) methacrylate, 0-5% benzoyl peroxide, and 0-5% silica. The silica serves as an opaquing agent, to render the resulting nail more natural in appearance, and as a filler, to aid in filling any cracks or gaps in the nail and nail tip surface. The powder glaze mixture has a white to pink (blush) hue.
The resulting nail/nail tip is very strong and natural in appearance. The nail tip will often remain in position on the finger nail for at least four weeks, until the finger nail grows so far that the artificial nail grows away from the cuticle.
The above method can be varied depending on the circumstances. For example, the operator may apply additional coatings of the base resin and, optionally, additional dips of the powder glaze may be interspersed between the additional coatings of the finish resin, in order to build up the artificial nail surface or to fill in cracks or gaps on the nail/nail tip surface. In addition, the operator may also spray repeated, additional coats as desired to enhance polymerization of the coatings and intermittent dips. In other words, steps seven (7) through ten (10) above may be repeated a number of times if desired. If necessary, in these circumstances (although generally not preferred and not necessary to securely mounted nail tip in a natural-looking fashion on a finger nail), filing and/or buffing steps then may be added prior to a final buff in order to smooth out and shape the nail surface. While the spray shown is an aerosol, a pump spray could be used.
Moreover, having thus described the invention, it should be apparent that numerous structural modifications and adaptations may be resorted to without departing from the scope and fair meaning of the instant invention as set forth hereinabove and as described hereinbelow by the claims.
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This patent specification discloses a method and compositions for applying an artificial finger nail tip to a natural finger nail. The method applies: (i) multiple brush-on coatings of a mixture of ethyl-2-cyanoacrylate, poly methyl methacrylate, and hydroquinone; (ii) several spray coatings of an aromatic dryer of ethyl acetate and aromatic amines; and (iii) at least one dip of glaze powder of poly (ethyl or ethyl/methyl) methacrylate, benzoyl peroxide, and silica as an opaquing agent. The preferred method is very easy to perform and does not require any use of polymer solvents or grinding or filing steps.
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This application is a continuation-in-part of pending U.S. application Ser. No. 08/444,548 filed on May 19, 1995 in the name of Patrick J. O'Neil which is hereby fully incorporated herein by this reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to an airfoil management device and more particularly to the use of passive porosity in combination with (controlled transference and seepage of air through the skin of various regions of airfoils for use as lift and drag management devices.
2. Description of the Prior Art
Conventional non-porous airfoils typically utilize various mechanical structures, such as spoilers and associated structural and actuation hardware, in order to alter, vary and control the lift on an airfoil. Spoilers are typically comprised of at least one structural member which is movably connected to an airfoil, with various types of mechanical hardware, such that the structural member may be hydraulically, pneumatically, or otherwise mechanically raised into the airstream on at least one side of an airfoil in order to interrupt the air flow over the respective surface of the airfoil. Such devices are used to achieve a variety of objectives including, for example, to provide roll control, direct lift control, increased drag to facilitate greater engine power requirements (some engines have improved performance characteristics when operated at increased power levels), a reduction in altitude gain during aircraft landing (sometimes referred to as flap anti-ballooning), and to increase drag and reduce velocity (sometimes referred to as "air brakes").
Conventional hydraulic, pneumatic, and other mechanical devices (such as spoilers), including the structural and actuation hardware related thereto, utilized to alter, vary and control lift are subjected to various static and dynamic forces, loads, pressures, stresses, strain, wear, and fatigue which result in reducing the life and accelerated failure of the various components. Of course, as the structural and actuation hardware are fastened or otherwise affixed to the airfoil itself, the static and dynamic forces, loads, pressures, stresses, and strains which occur in or upon the structural components and actuation hardware are transferred or otherwise transmitted to portions of the airfoil itself resulting in wear, fatigue and a reduction in the useful life of the wing structure itself. Reducing or eliminating such forces and wear upon such components, and upon wings in general, would serve to increase the reliability, useful life, and safety of any aircraft, vehicles, or other devices which utilize conventional lift control mechanisms.
Conventional mechanical lift control mechanisms, such as spoilers, and their related structural components and actuation hardware, utilize a substantial amount of beneficial area and mass. The mass attributable to conventional mechanical lift control mechanisms result in decreased usable space, heavier crafts, decreased fuel efficiency, and increased loads. In airfoil applications, the efficient utilization of useable area and mass is extremely important. If the amount of area and mass required to employ lift control mechanisms, such as spoilers, could be partially or totally eliminated, such area and mass could be employed for other useful purposes such as, for example, additional or increased passenger or cargo capacity, fuel storage, instrumentation, or armament storage.
Through the use of passive porosity and the controlled seepage and transference of air through one or more surfaces on various regions of an airfoil, the present invention partially or completely eliminates the need for conventional mechanical lift and drag control mechanisms, such as spoilers, and most of the associated structures, actuation devices, support hardware, hydraulic systems, and other related components thereto, thereby increasing the amount of usable area and space on and in an airfoil, decreasing the number of required moving parts, decreasing the amount of mass necessary to achieve the results previously only performed by mechanical structures such as spoilers, and eliminating the various static and dynamic forces, loads, pressures, stresses, strain, wear, and fatigue which result from conventional mechanical lift control mechanisms. Additionally, as the present invention will partially or completely eliminate the mechanical disruption of airflow as accomplished by conventional spoilers, thereby partially or completely eliminating the need to physically maneuver mechanical spoiler structures into an airstream, the present invention will result in substantially improved acoustic signatures and decreased reflective surfaces.
The general use of porous skin regions on airfoils is disclosed in U.S. Pat. Nos. 5,167,387, 4,575,030, and 4,726,548. In an attempt to improve lift and drag characteristics at subcritical and supercritical conditions, U.S. Pat. No. 5,167,387 uses porous airfoil skin surfaces to vent air pressure from the leading edge region to the trailing edge region of an airfoil in order to alter the effective airfoil thickness. U.S. Pat. No. 4,575,030 uses active suction mechanisms in connection with porous airfoil skin surfaces in an attempt to control the laminar flow over an aircraft wing. U.S. Pat. No. 4,726,548 uses porous airfoil skin surfaces in an effort to draw boundary layer air into an airfoil and then evacuate such air at the end of the airfoil in order to improve drag characteristics. U.S. Pat. No. 2,077,071 discloses a boundary layer control mechanism for airfoils.
The disadvantages of the prior art are overcome by the present invention which uses passive porosity in combination with controlled seepage and transference of air through the skin on various regions of an airfoil for use as a lift and drag management device thereby partially or completely eliminating conventional mechanical components and systems for altering, varying and controlling lift and drag or enhancing the capabilities of the airfoil. Additionally, unlike the prior art, the present invention does not require that the air be vented from one plenum chamber to another, rather, the present invention has the unique ability to effect and control lift and drag on an airfoil by controlling the seepage and transference of air through one or more porous skin regions into and out of one or more corresponding plenum cavities. The present invention does not require that the air in one plenum cavity which is associated with a porous region be able to fluidly communicate with the air or air pressure in any other plenum cavity or any other porous region. The present lift management invention has the unexpected result of allowing for a decreased amount of moving parts, improved airfoil acoustic signatures, improved efficiency and reliability, increased performance characteristics, a decrease in the amount of mass necessary to achieve lift and drag management, and the elimination or reduction of separate control surfaces and related hardware required to achieve lift and drag management by conventional means. Further advantages of the present invention will be recognized by those skilled in the art.
SUMMARY OF THE INVENTION
The present invention is a lift and drag management device and process for an airfoil which provides a mechanism and method for controlling and modifying the lift and drag on an airfoil through the controlled seepage and transference of air utilizing passive porosity on one or more regions of an airfoil. The present invention preferably has one or more outer porous skin regions on the surface of one or more regions of an airfoil. The porous skin regions preferably have a plurality of perforations therethrough. Each of the porous skin regions are preferably capable of being in fluid communication with at least one corresponding upper plenum cavity disposed in the interior portion of the airfoil. In a preferred embodiment, air on one or more outer surfaces of the outer porous skin regions on the leading edge region of the airfoil will preferably cause, through the passive seepage and transmission of air through all or a portion of the perforations in the porous skin regions, certain air pressures and flow fields to develop in corresponding plenum cavities and on the outer surface of the airfoil. A portion of the air which enters the plenum cavities will exit the plenum cavities through all or a portion of the perforations in the corresponding porous skin regions.
The passive seepage and transmission of air in and out of the perforations in one or more porous skin regions on the surfaces of the airfoil, and in and out of corresponding plenum cavities, is preferably controlled so that: (i) the amount of seepage of air through the respective porous skin regions, or portions thereof; (ii) the flow field caused by the passive transmission of air in the corresponding plenum cavities; (iii) the flow fields and disturbances caused on the outside surfaces of the airfoil; may be regulated.
In one presently preferred embodiment of the present invention, a means for permitting and stopping the passive seepage and transference of air through the porous skin regions is preferably used. For example, in a preferred embodiment, one or more impermeable panels which are each connected to corresponding linear actuators are preferably employed inside the airfoil adjacent corresponding porous skin regions. In said preferred embodiment, when a linear actuator is extended, the impermeable panel preferably physically contacts the corresponding porous skin region on the interior surface of the airfoil thereby precluding air seepage and transference through the corresponding perforations and in and out of the corresponding plenum cavity. Similarly, when a linear actuator is retracted, the impermeable panel is not in physical contact with the corresponding porous skin region on the interior surface of the airfoil thereby permitting air seepage and transference through the corresponding perforations and in and out of the corresponding plenum cavity. In another preferred embodiment, one or more bladders are preferably employed inside the airfoil adjacent corresponding porous skin regions. When a bladder is inflated, the bladder preferably physically contacts the corresponding porous skin region on the interior surface of the airfoil thereby preferably precluding air seepage and transference through the corresponding perforations and in and out of the corresponding plenum cavity. Similarly, when a bladder is deflated, the bladder preferably is no longer in physical contact with the corresponding porous skin region on the interior surface of the airfoil thereby preferably permitting air seepage and transference through the corresponding perforations and in and out of the corresponding plenum cavity.
Other preferred embodiments of a means for permitting and stopping the passive seepage and transference of air through the porous skin regions include, for example, employing the use of moveable pins, plates, and/or membranes which are aligned with corresponding perforations in the porous skin region of the airfoil and which may be moved to preclude or permit air seepage and transference through said perforations. Another preferred embodiment employs the use of a material which, when actuated or de-actuated, itself opens and closes the perforations in the porous skin region. As is described more fully herein, and as will be appreciated by persons of ordinary skill in the art, there are innumerable embodiments and variations of the present invention for permitting or precluding air from entering or exiting through the perforations, or opening or closing the perforations, of corresponding porous skin regions. Additionally, the present invention is not limited to only permitting or precluding air from entering or exiting an entire porous skin region, but, rather, also encompasses the flexibility of permitting air to enter and exit one or more portions of a porous skin region, or specific perforations, while precluding air from entering or exiting one or more other areas of the porous skin region or other perforations.
The present invention preferably further comprises a means for controllably monitoring and regulating the passive seepage and transference of air through selective airfoil surface regions, perforations in the porous skin surfaces, and in and out of corresponding plenum cavities, in order to preferably control, reduce, modify, vary or otherwise effect flow fields, air disturbances, and the lift and drag on an airfoil.
BRIEF DESCRIPTION OF THE DRAWINGS
To facilitate further description of the invention, the following drawings are provided in which:
FIG. 1 is a perspective view of the upper surfaces of a conventional prior art aircraft wing;
FIG. 2 is a cutaway perspective view of a prior art spoiler used on a conventional aircraft wing;
FIG. 3 is a perspective view similar to FIG. 1, of the upper surfaces of an aircraft wing incorporating a preferred embodiment of the present invention;
FIG. 4 is a cut-away cross-sectional view of the aircraft wing of FIG. 3 utilizing a preferred embodiment of the present invention;
FIG. 5 is a cut-away cross-sectional view of the aircraft wing of FIG. 3 utilizing a preferred embodiment of the present invention;
FIG. 6 is a cross sectional view an aircraft wing utilizing a preferred embodiment of the present invention; and
FIG. 7 is a blow-up of the leading edge portion of the aircraft wing of FIG. 6 utilizing a preferred embodiment of the present invention;
FIG. 8 is a cross-sectional view of the aircraft wing of FIG. 6 utilizing a preferred embodiment of the present invention;
FIG. 9 is a blow-up of the trailing edge port ion of the aircraft wing of FIG. 8 utilizing a preferred embodiment of the present invention;
FIG. 10 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 11 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 12 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 13 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 14 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 15 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 16 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil;
FIG. 17 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil; and
FIG. 18 is cut-away cross-sectional view of a preferred embodiment of a means for permitting and stopping the passive seepage and transference of air through a porous skin regions of an airfoil.
These drawings are provided for illustrative purposes only and should not be used to unduly limit the scope of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, and more particularly to FIGS. 1 and 2, a conventional airfoil 1, such as those used on aircraft, is composed of three primary regions, a leading edge region 2 which extends chordwise from the leading edge 19 of the airfoil 1 to the front spar 16, a trailing edge region 3 which extends chordwise from the aft spar 10 to the trailing edge 20 of the airfoil 1, and a wing box region 18 which extends chordwise from the front spar 16 to the aft spar 10 of the airfoil 1.
Conventional airfoils, such as aircraft typically employ, utilize at least one mechanical structure, such as spoilers 6 (FIG. 2), in order to alter, vary and control the airflow on the upper surface 4 of the airfoil 1. As shown in FIGS. 1 and 2, spoilers 6 are commonly employed on the trailing edge region 3 of an airfoil 1. Such devices are used to achieve a variety of objectives including, for example, to provide roll control, direct lift control, increased drag to facilitate greater engine power requirements (some engines provide improved performance characteristics when operated at increased power levels), a reduction in altitude gain during aircraft landing (sometimes referred to as flap anti-ballooning), and to increase drag and reduce velocity (sometimes referred to as "air brakes"). When employed, spoilers 6 are typically pivotally raised into the airstream over the upper surface 4 of an airfoil 1 thereby disrupting the airflow over the upper surface 4 of an airfoil 1 causing an increase in the air pressure on the upper surface 4 relative to the lower surface 5 of an airfoil 1, resulting in a reduction in lift. At all other times, when not employed, spoilers 6 typically remain in relative linear alignment with the upper surface 4 of an airfoil 1. Spoilers 6 are movably connected to the airfoil 1 with various types of mechanical hardware such that the spoilers 6 may be mechanically/electrically, hydraulically, or pneumatically raised into the airstream on the upper surface 4 in order to interrupt the air flow over the upper surface 4 of an airfoil 1. As shown in FIG. 2, in order to movably connect spoilers 6 to an airfoil, for example, spoiler support brackets 7, actuators 9, spoiler actuator supports, bracing structures, pivot components, operational controls, fastening hardware, and additional hardware must be utilized. Additionally, where hydraulic or pneumatic actuation systems are employed, hydraulic hoses, fluids, couplings, valves, monitors, and instrumentation are required. Likewise, if a mechanical/electrical actuation system is used, in addition to the mechanical components, electrical circuitry, wiring, and instrumentation would be required. When employed, conventional spoilers 6, including the related structural, mechanical, and actuation hardware, as well as the structural portions of the airfoil 1 itself to which such components are fastened, are subjected to various static and dynamic forces, loads, pressures, stresses, strain, wear, and fatigue which result in reducing the life of the various components and accelerated failure.
The present invention uses passive porosity in combination with controlled seepage and transference of air through the skin of an airfoil 1 on one or more regions of an airfoil 1 for use as a lift, drag and air flow management device thereby partially or completely eliminating conventional mechanical components and systems for altering, varying and controlling lift, drag and roll, or enhancing the capabilities of the airfoil, and to improve airfoil acoustic signatures, improve airfoil efficiency and reliability, increase performance characteristics, decrease the amount of mass necessary to achieve lift, drag and roll management, and eliminate or reduce the need for separate control surfaces and related hardware required to achieve lift, drag and roll management by conventional means.
In a presently preferred embodiment of the invention, as shown in FIGS. 4-5, preferably, a plurality of outer porous skin regions 17 are employed on the upper surface 4 and lower surface 5 of the airfoil 1 and said outer porous skin regions 17 preferably having a plurality of perforations 8 therethrough. The corresponding interior portions of the airfoil 1, of a preferred embodiment of the invention, preferably have at least one plenum cavity 11 corresponding to respective outer porous skin regions 17 on the upper surface 4 and lower surface 5 of the airfoil 1. In a presently preferred embodiment, a plurality of either, or both, upper and lower outer porous skin regions 17 are preferably located, as shown in FIGS. 4 and 5, forward of the front spar 16 on the upper surface 4 and lower surface 5 on the leading edge region 2 of the airfoil 1. Similarly, in a preferred embodiment, a plurality of either, or both, upper and lower outer porous skin regions 17 are preferably located, as shown in FIGS. 4 and 5, behind the front spar 16 on either or both the upper surface 4 and lower surface 5 on the wing box region 18 of the airfoil 1. Additionally, in a preferred embodiment, a plurality of either, or both, upper and lower outer porous skin regions 17 are preferably located, as shown in FIGS. 4 and 5, on either or both the upper surface 4 and lower surface 5 in the trailing edge region of the airfoil 1. As will be appreciated by those skilled in the art, the present invention may employ any combination or number of upper and lower outer porous skin regions 17 located on any or all of the regions, including the leading edge region 2, wing box region 18, and the trailing edge region 3, of an airfoil 1.
In a preferred embodiment, air outside of the airfoil 1 on a portion or all of an outer porous skin region 17 will preferably cause, through the passive seepage and transmission of air through all or a portion of the perforations 8 in the outer porous skin region 17, air pressures and flow fields to develop and change in a corresponding plenum cavity 11. Air which enters the plenum cavity 11 through perforations 8 will cause air to exit the plenum cavity 11 through all or a portion of the perforations 8 in the corresponding outer porous skin region 17. Preferably, the passive seepage and transmission of air through one or more outer porous skin regions 17, and into and out of the corresponding plenum cavities 11, will result and cause certain flow fields and flow disruptions to occur on the outer surface of the airfoil in, and in some cases beyond, the boundary layer of the outer porous skin region 17 and on certain areas adjacent to the outer porous skin region 17. Depending upon the location and shape of an outer porous skin region 17 on an airfoil 1, the resulting flow fields and flow disruptions caused by the passive seepage and transmission of air through the outer porous skin region 17 and into and out of a corresponding plenum cavity 11 results in either an increase or decrease in lift and/or drag on the applicable segment of the airfoil 1.
The passive seepage and transmission of air in and out of the perforations 8 in one or more outer porous skin regions 17 on the surfaces of the airfoil 1, and in and out of corresponding plenum cavities 11, is preferably controlled so that: (i) the amount of seepage of air through the respective outer porous skin regions 17, or portions thereof; (ii) the flow field caused by the passive transmission of air in the corresponding plenum cavities 11; (iii) the flow fields and disturbances caused on the outer porous skin regions 17 and on adjacent areas of the outer surface of the airfoil 1; may be regulated thereby facilitating the ability to control the effect upon lift and drag caused by the passive porosity system of the present invention.
In one presently preferred embodiment of the present invention, a means for permitting and stopping the passive seepage and transference of air through an outer porous skin region 17 is preferably used. In one preferred embodiment, as shown in FIGS. 4-9, one or more impermeable panels 22 are each connected to a link 24 which link 24 is then connected to a linear actuator 23. The linear actuators 23 are preferably employed inside the airfoil 1 adjacent corresponding impermeable panels 22. In a preferred embodiment, when a linear actuator 23 is extended, as shown in FIG. 4, the impermeable panel 22 preferably physically contacts the corresponding porous skin region on the interior surface of the airfoil 1 thereby precluding air seepage and transference through the corresponding perforations 8 and in and out of the corresponding plenum cavity 11. The perforations 8 are thereby closed off at the site of the perforations 8. Similarly, when a linear actuator 23 is retracted, as shown in FIG. 5, the impermeable panel 22 is preferably pulled away from the porous skin region and is no longer in physical contact with the corresponding porous skin region and perforations 8 on the interior surface of the airfoil 1 thereby permitting air seepage and transference through the corresponding perforations 8 and in and out of the corresponding plenum cavity 11. Of course, the linkage and linear actuator 23 may be configured such that the impermeable panel 22 will stop the seepage of airflow through the corresponding porous skin region when the linear actuator 23 is retracted and, accordingly, permit the seepage of airflow when the linear actuator 23 is extended. An alternative embodiment of an impermeable panel 22 of the present invention is shown in FIG. 12(a) and (b). In this arrangement, the impermeable panel 22 may be actuated from a flow state, as shown in FIG. 12(a), to a non-flow state, as shown in FIG. 12(b).
In another preferred embodiment, as shown in FIG. 10(a) and (b), one or more internal bladders 30 are preferably employed inside the airfoil 1 adjacent corresponding porous skin regions. The bladder is preferably connected to a hose 31 which is connected to a pump 32, such that said pump 32 may inflate or deflate the bladder 30. Preferably, when a bladder 30 is inflated, as shown in FIG. 10(a), the bladder 30 preferably physically contacts the corresponding porous skin region and applicable perforations 8 on the interior surface of the airfoil 8 thereby preferably precluding air seepage and transference through the corresponding perforations 8 and in and out of the corresponding plenum cavity 11. Similarly, when the bladder 30 is deflated, as shown in FIG. 10(b), the bladder 30 preferably moves away from the porous skin region such that it is no longer in physical contact with the corresponding porous skin region on the interior surface of the airfoil 1 thereby preferably permitting air seepage and transference through the corresponding perforations 8 and in and out of the corresponding plenum cavity 11.
In another preferred embodiment, as shown in FIG. 11, pins 34 are affixed to a plate 33 which may be activated to move towards or away from the corresponding porous skin region. The pins 34 are preferably aligned with corresponding perforations 8 in the porous skin region such that when the plate 33 is activated to move towards the porous skin region, the pins 34 either plug or cover the corresponding perforations 8 thereby preferably precluding air seepage and transference through the corresponding perforations 8 and in and out of the corresponding plenum cavity 11. It will also be appreciated by those skilled in the art that the present invention may be employed to control the seepage and transference of air through a single perforation 8, any combination of perforations 8, or any specific area of a porous skin region.
Another preferred embodiment of the present invention is shown in FIG. 16 which shows the use of a material 40 which itself has perforations 8 which, when actuated or deactuated, itself opens and closes its perforations 8. Said material 40 may be actuated or deactuated through activation means known by those skilled in the art including, for example, energized by electricity, magnetism, heat, cold, or the another energy source.
Additional preferred embodiments for controlling passive seepage and transference of air through the porous skin regions are shown in FIGS. 13, 14, and 17. FIG. 13 shows the employment of the use of a sliding sub-skin 36 of the present invention below the surface of the outer porous skin region. When the sliding sub-skin 36 is shifted, the perforations 8 are preferably opened and permit the seepage and transference of air through the perforations and into and out of the plenum cavity 11. Similarly, FIG. 14 shows the employment of an outer sliding skin 37 which works in the same manner as the sub-skin 36, however, the sliding skin is on the outer surface of the airfoil 1. FIG. 17 shows the use of a rotating surface 44 of the present invention which may be employed when a porous skin region of the present invention is located on a surface having a radius. The rotating surface 44, as shown in FIG. 17, may be rotatably moved to cover the perforations 8 of the porous skin region to preclude the seepage and transference of air through the perforations 8, or, alternatively, rotated such that seepage and transference may occur. FIG. 18 reflects the use of a sliding segmented sub-skin 42 of the present invention which, when shifted, the perforations 8 are preferably opened and permit the seepage and transference of air through the perforations and into and out of the plenum cavity 11. As will be appreciated by persons of ordinary skill in the art, there are innumerable embodiments and variations of the present invention for permitting or precluding air from entering or exiting through the perforations 8, or opening or closing the perforations 8, in corresponding porous skin regions.
The present invention preferably further comprises a means for monitoring and controllably regulating the passive seepage and transference of air through selective airfoil surface regions, perforations in the porous skin surfaces, and in and out of corresponding plenum cavities, in order to preferably control, reduce, modify, vary or otherwise effect flow fields, air disturbances, and the lift and drag on an airfoil 1.
Pressure and/or flow monitoring sensors in plenum cavities 11 or on respective upper surface 4 and lower surface 5 regions, are preferably connected to a microprocessor, artificial intelligence, or similar device, in order to accurately monitor air pressures, velocities and/or flows, and control the passive transfer of air through perforations 8 and in and out of plenum cavities 11. The air pressures, velocities and/or flow developed in respective plenum cavities 11 and on the outer surface of the airfoil 1 may preferably be determined by sensors producing outputs or signals which may be correlated by the microprocessor, artificial intelligence, or similar device, to determine, track and control the desired effect on the upper and lower surfaces 4 and 5.
In the present invention, the types of airfoils utilized and the desired applications and objectives will be useful in determining the quantity and location of upper and lower plenum cavities 11 utilized and the locations on the upper surface 4 and lower surface 5 upon which outer porous skin regions 17 should be located. Additionally, such factors will also effect the manipulation and manner of actuating and modulating the passive seepage and transference of air in a particular embodiment to achieve the advantages and results desired of the present invention.
As will be further appreciated by those skilled in the art, depending upon the application and desired effect upon the lift, drag, roll, and control of a particular airfoil, numerous variations, combinations, and locations of a plurality of porous skin regions 17 and upper and lower plenum cavities 11 of the present invention may be utilized to achieve a variety of varying results. For example, depending upon the application, if a desired result of the present invention is to control roll, it may be preferable to locate the outer porous skin regions 17 closer to the tip of the leading edge 19 of the wing. If a spoiler effect is desired, depending upon the type and magnitude of spoiler effect desired, it may be preferable to incorporate outer porous skin regions 17 over a larger portion of the upper and lower surfaces, 4 and 5, of the leading edge region 2. It may also be desirable to correspond a plurality of porous skin regions 17 on the upper surface 4 with a lesser number of porous skin regions 17 on the lower surface 5, or the reverse. Furthermore, it may be preferable to vary the sizes, locations, types and combinations of porous skin regions 17 and upper and lower plenum cavities 11.
As will be appreciated by those skilled in the art, in such a preferred embodiment, any combination of perforations 8 and/or porous skin regions may preferably be opened, closed, or modulated at any one time in a multiplicity of combinations in order to control lift or drag by, for example, influencing the air flow over an area of the outer porous skin regions 17 on the upper surface 4 in a uniform manner, influencing the air flow over an area in a predefined inharmonic manner, interrupting flow in a serial manner, or manipulating the lift and drag characteristics to reduce or increase altitude gain and/or speed. Of course, the variations that may be obtained with respect to the actuation of independent perforations or porous skin regions, or portions thereof, the configuration and location of corresponding outer porous skin regions 17, the configuration and location of corresponding plenum cavities 11, and the duration of actuation or modulation of such features, are relatively limitless. Additional examples of uses and variations of the present invention include, for example, (a) the actuation of only a single outer porous skin region independently in order to achieve certain roll or pitch control characteristics by altering the flow characteristics on a specific portion of the leading edge region 2 of an airfoil 1, (b) the actuation of a selected set of perforations 8 or outer porous skin regions in order to achieve certain desired roll, pitch or yaw control, (c) the actuation and modulation perforations 8 or outer porous skin regions in a selected order and duration in order to obtain roll, pitch, yaw, or other desired characteristics through lift and/or drag control, (d) the actuation of certain or all perforations or outer porous skin regions based upon predetermined specific parameters relating to air flow changes experienced on the upper 4 and lower 5 surfaces of an airfoil 1, (e) the actuation of certain or all perforations or outer porous skin regions based upon such variables as velocity, flow, altitude, temperature, density, pressure, time, humidity, mass, or other variables, which may effect the characteristics desired, and (f) the actuation of certain all perforations or outer porous skin regions in order to decrease lift, increase drag, or to facilitate greater engine power requirements.
As will be appreciated by those skilled in the art, the present invention is applicable to most applications where it is desirable to control, reduce, modify, vary or otherwise effect lift or drag on an airfoil including, by way of example, commercial aircraft, military aircraft, personal aircraft, high performance automobiles, high performance water craft, helicopters, and hydrofoils.
Variations and modifications of the present invention will be apparent to those skilled in the art and the claims are intended to cover any variations and modifications falling within the true spirit and scope of the invention.
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A passive porosity management device and process for an airfoil which provides a mechanism and method for controlling and modifying the lift, drag and flow field characteristics on an airfoil through the controlled seepage and transference of air utilizing passive porosity through one or more regions of an airfoil and into, and out of, one or more plenum cavities disposed in the interior portion of the airfoil.
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FIELD OF THE INVENTION
This invention relates to a process for producing a polyphenylene oxide. More particularly, it relates to a process for producing a polyphenylene oxide by oxidative polymerization of a nucleus-substituted phenol in the presence of a catalyst containing a manganese compound, a basic compound, an alkanolamine, and a primary and/or secondary amine.
BACKGROUND OF THE INVENTION
Polyphenylene oxides obtained by oxidative polymerization of nucleus-substituted phenols are known to be useful resins. In particular, a polymer alloy or polyblend comprising polyphenylene oxide and polystyrene or polyamide possesses excellent thermal, mechanical, and electrical properties and has recently broadened its application as a molding material in various fields.
Many processes for producing polyphenylene oxides by oxidative polymerization of nucleus-substituted phenols are known in the art. The oxidative polymerization is commonly carried out using a catalyst system comprising a combination of a copper, manganese or cobalt compound and a ligand selected from various amines and bases, and many proposals have so far been made on such a catalyst system. Of these, a catalyst system comprising a manganese compound combined with a basic compound such as sodium hydroxide, as described in Japanese Patent Publication No. 30354/70, is noteworthy because of not only good economy but also its high activity. However, this catalyst system has problems such that the molecular weight of the resulting polyphenylene oxide cannot be controlled and the resulting polyphenylene oxide is gelled on heat melting.
In order to solve these problems, the inventors previously proposed a catalyst system comprising monoethanolamine and/or diethanolamine, a manganese compound, and a basic compound as disclosed in Japanese Patent Application (OPI) No. 44625/82 (the term "OPI" as used herein means an "unexamined published application"). It has also been proposed recently to use an N-alkylalkanolamine in place of the monoethanolamine and/or diethanolamine as disclosed in Japannese Patent Application (OPI) No. 8318/85.
According to these techniques, the problem of molecular weight control and gelation on heat melting can be settled. However, the resulting polyphenylene oxide turned out to be still unsatisfactory as a starting resin of a polymer alloy with polystyrene or polyamide. For example, molded articles obtained by injection molding of the aforesaid polymer alloy are of inferior quality, e.g., in planar impact resistance.
SUMMARY OF THE INVENTION
An object of this invention is to provide a process for producing a polyphenylene oxide suitable for producing a polyphenylene oxide-based polymer alloy having improved planar impact characteristics.
In the light of the above object, the inventors conducted extensive investigations on a process for producing a polyphenylene oxide in the presence of a catalyst system comprising a combination of a manganese compound and a basic compound which is of great benefit in economy. As a result, it has now been found that a polyphenylene oxide of superior quality meeting the purpose of the present invention can be obtained by using a catalyst system comprising a manganese compound and a basic compound combined with a specific alkanolamine and a specific amine as compared with those combined with either one of the alkanolamine or the amine alone, the latter having been disclosed in Japanese Patent Publication No. 30355/70 and Japanese Patent Application (OPI) No. 79993/78. The present invention has been completed based on this finding.
The present invention relates to a process for producing a polyphenylene oxide which comprises oxidative polymerization of a nucleus-substituted phenol with an oxygen-containing gas in an organic solvent in the presence of a catalyst system comprising a manganese compound containing at least one divalent manganese salt, at least one basic compound selected from hydroxides, alkoxides or phenoxides of the group IA metals of the Periodic Table and hydroxides or oxides of the group IIA metals of the Periodic Table, an alkanolamine represented by formula (I) shown below, and an amine represented by formula (II) shown below.
Formula (I) is represented by formula
R.sup. --NH--R.sup.2 --OH (I)
wherein R 1 represents a hydrogen atom, an alkyl group having from 1 to 12 carbon atoms, or a hydroxyl-substituted alkyl group having from 1 to 12 carbon atoms; and R 2 represents an alkylene group having from 2 to 12 carbon atoms.
Formula (II) is represented by formula
R.sup.3 R.sup.4 NH (II)
wherein R 3 and R 4 each represents a hydrogen atom, an alkyl group having from 1 to 24 carbon atoms, or an aralkyl group having from 7 to 24 carbon atoms, with proviso that R 3 and R 4 do not simultaneously represent a hydrogen atom, or R 3 and R 4 may be taken together to form a ring.
DETAILED DESCRIPTION OF THE INVENTION
The nucleus-substituted phenol which can be used in the present invention is represented by formula (III) ##STR1## wherein R 1 , R 2 , R 3 , R 4 , and R 5 each represents a hydrogen atom, a halogen atom, a hydrocarbon group, a cyano group, a hydrocarbonoxy group, or a substitued hydrocarbonoxy group, with at least one of them being a hydrogen atom and at least one of the rest being other group than a hydrogen atom.
Specific examples of the nucleus-substituted phenol represented by formula (III) include 2-methylphenol, 3-methylphenol, 2-ethylphenol, 2-methyl-6-benzylphenol, 2,6-dimethylphenol, 2-methyl-6-ethylphenol, 3-methyl-6-t-butylphenol, 2,6-diallylphenol, 2,6-diphenylphenol, 2,6-dichlorophenol, 2,6-dibromophenol, 2,6-dimethoxyphenol, 4-cyanophenol, 2,3,6-trimethylphenol, 2,4-dimethyl-3-chlorophenol, etc. These compounds may be used either individually or in combination of two or more thereof.
The manganese compound which can be used in the present invention includes manganese halides, e.g., manganese chloride, manganese bromide, etc.; manganese salts with organic or inorganic acids, e.g., manganese nitrate, manganese sulfate, manganese carbonate, manganese formate, manganese acetate, manganese oxalate, manganese naphthenate, etc.; manganates, e.g., sodium manganate; permanganates, e.g., potassium permanganate, calcium permanganate, etc.; manganese hydroxide; and manganese oxide.
These manganese compounds may be either anhydrous or hydrated. Of these, preferred are manganese chloride, manganese bromide, and manganese acetate.
One of advantages characteristic of the present invention resides in that oxidative polymerization proceeds with an extremely small amount of the manganese compound. In carrying out the present invention, the above-described manganese compound is used in an amount of 0.00001 mol or more, preferably 0.0001 mol or more, per mol of the nucleus-substituted phenol. If the amount of the manganese compound to be used is less than 0.00001 mol, progress of the oxidative polymerization is insubstantial or, if any, very slow. There is no particular upper limit of the amount to be used.
The basic compound which can be used in the present invention includes hydroxides of the group IA metals of the Periodic Table, e.g., lithium hydroxide, sodium hydroxide, potassium hydroxide, etc.; hydroxides or oxides of the group IIA metals of the Periodic Table, e.g., calcium hydroxide, magnesium hydroxide, calcium oxide, etc.; alkoxides of the group IA metals of the Periodic Table, e.g., sodium methoxide, potassium methoxide, sodium ethoxide, sodium n-propoxide, sodium isopropoxide, potassium t-butoxide, etc.; and phenoxides of the group IA metals of the Periodic Table, e.g., sodium phenoxide, potassium phenoxide, etc. Preferred of them are sodium hydroxide and potassium hydroxide. These basic compounds are fed to the reaction system either as they are or as dissolved in a polar solvent such as alcohols.
The amount of the basic compound to be added ranges from 10 to 10,000 mols, preferably from 50 to 1,000 mols, per mol of the manganese compound. If it is less than 10 mols, the rate of polymerization attained is extremely low. Amounts exceeding 10,000 mols produce no further effects and are thus uneconomical.
The purpose of producing a polyphenylene oxide having excellent qualities can first be accomplished by using both a specific alkanolamine and a specific amine in combination with the aforesaid manganese compound and basic compound. The specific alkanolamine herein referred to is an alkanolamine having a primary or secondary amino group moiety and is represented by formula (I). In formula (I), specific examples of R 1 include a hydrogen atom, a methyl group, an ethyl group, a propyl group, a butyl group, a 2-hydroxyethyl group, etc.; and specific examples of R 2 include an ethylene group, a propylene group, a butylene group, etc. Specific examples of the alkanolamine represented by formula (I) are monoethanolamine, N-methylethanolamine, N-ethylethanolamine, isopropanolamine, isobutanolamine, di-n-propanolamine, diisopropanolamine, diethanolamine, diisobutanolamine, etc. Preferred among them are monoethanolamine, diisopropanolamine, and diethanolamine, with diethanolamine being more preferred.
The alkanolamine of formula (I), when used in an amount of a specific range based on the nucleus-substituted phenol, exhibits an activity to accelerate oxidative polymerization and plays an essential role in catalytic action. The amount of the alkanolamine to be used ranges from 0.001 to 0.3 mol, preferably from 0.005 to 0.1 mol, per mol of the nucleus-substituted phenol. The alkanolamine in an amount less than 0.001 mol or more than 0.3 mol per mol of the nucleus-substituted phenol fails to obtain polyphenylene oxides having practically useful molecular weights.
The amine which can be used in the present invention is a primary or secondary amine represented by formula (II). Specific examples of R 3 and R 4 in formula (II) include a hydrogen atom, a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group, an octyl group, a decyl group, a dodecyl group, a benzyl group, etc. Specific examples of the amines of formula (II) are primary amines, e.g., n-propylamine, isopropylamine, n-butylamine, isobutylamine, sec-butylamine, n-hexylamine, n-octylamine, 2-ethylhexylamine, cyclohexylamine, laurylamine, benzylamine, etc.; and secondary amines, e.g., diethylamine, di-n-propylamine, diisopropylamine, di-n-butylamine, diisobutylamine, di-n-octylamine, piperidine, 2-pipecoline, etc. Polyamines that can be regarded to contain a moiety represented by formula (II) as a repeating unit are equivalent to the amines of formula (II) and are, therefore, embraced in the scope of the present invention. Examples of such polyamines are ethylenediamine, piperazine, and 1,3-dipiperidylpropane. Of these amines including polyamines, preferred are primary amines, e.g., n-butylamine and isobutylamine; and secondary amines, e.g., diethylamine, di-n-propylamine, di-n-butylamine, diisobutylamine, piperidine, and 2-pipecoline, with secondary amines, e.g., di-n-butylamine and piperidine, being more preferred.
The above-described amine is used in an amount of from 0.001 to 0.2 mol, preferably from 0.005 to 0.05 mol, per mol of the nucleus-substituted phenol. If its amount is less than 0.001 mol, substantial effects of obtaining a high-quality polyphenylene oxide cannot be achieved. If it is more than 0.2 mol, a polyphenylene oxide having a practically useful molecular weight cannot be produced.
The organic solvent which can be used in the present invention is not particularly limited as far as it is inert to the nucleus-substituted phenol and is liquid at the reaction temperature. Suitable organic solvents include aromatic hydrocarbons, e.g., benzene, toluene, xylene, etc.; cyclic or acyclic aliphatic hydrocarbons, e.g., heptane, cyclohexane, etc.; halogenated hydrocarbons, e.g., chlorobenzene, dichlorobenzene, dichloromethane, etc.; ethers, e.g., dioxane, diethyl ether, etc.; ketones, e.g., cyclohexanone, acetophenone, etc.; esters, e.g., ethyl acetate, propiolactone, etc.; nitriles, e.g., acetonitrile, benzonitrile, etc.; alcohols, e.g., methanol, ethanol, n-propanol, isopropanol, n-butanol, sec-butanol, etc.; nitrobenzene; sulfolane; and so on. These organic solvents may be used either individually or in combination thereof. Preferred organic solvents are mixed solvents of aromatic hydrocarbons and alcohols. More preferred are a mixed solvent of toluene with methanol, ethanol, n-propanol, or isopropanol; and a mixed solvent of xylene with methanol, ethanol, n-propanol, or isopropanol.
In carrying out the present invention, the aforesaid organic solvent is used in an amount so that the nucleus-substituted phenol solution has a concentration of from 5 to 35% by weight, preferably from 10 to 25% by weight. In concentrations out of this range, polyphenylene oxides having practically useful molecular weights cannot be obtained.
The oxygen-containing gas to be used in the oxidative polymerization includes pure oxygen and a mixed gas such as air.
In carrying out the present invention, the nucleus-substituted phenol, the manganese compound, the basic compound, the alkanolamine, the amine, and the solvent are supplied to a reactor either separately or in admixture of all or some of them and contacted with the oxygen-containing gas under predetermined temperature and pressure conditions. The feed rate of the oxygen-containing gas to the reaction system is selected arbitrarily while taking into consideration heat removal, etc., and is usually 10 Nm1/min or more as pure oxygen per mol of the nucleus-substituted phenol charged. It is necessary to sufficiently contact the reaction mixture with oxygen by, for example, a commonly employed gas-liquid contact means such as blowing of an oxygen-containing gas into the reaction mixture under vigorous stirring. The reaction can be conducted in either a batch system or a continuous system. The reaction temperature is selected from a range within which the reaction smoothly proceeds while maintaining the reaction system in a liquid phase, usually a range of from 0° to 100° C. and preferably of from 10° to 60° C. At temperatures lower than 0° C., the rate of polymerization is too low, whereas at temperatures higher than 100° C., the polymerization does not substantially proceed. The reaction pressure is not particularly restricted and can be selected arbitrarily. A preferred pressure is from atmospheric pressure to about 20 atms. The reaction time varies depending on the amount of the catalyst, the concentration of the nucleus-substituted phenol, the feed rate of the oxygen-containing gas, and the like and preferably ranges from 0.5 to 20 hours.
After reacting for a predetermined period of time, the produced polyphenylene oxide is obtained in the form of a solution in a polymerization solvent or in the form of a slurry of solid particles. The polyphenylene oxide can be isolated from the reaction mixture as a final product by various working-up techniques. For example, the reaction mixture is treated with an acid, e.g., hydrochloric acid and acetic acid, to deactivate the catalyst in the system and then contacted with a non-solvent for the polyphenylene oxide, e.g., alcohols, to obtain a slurry which is then subjected to solid-liquid separation, followed by washing and drying the resulting solid. Otherwise, the reaction mixture is washed with water and then subjected to liquid-liquid partition, and the organic solvent in the separated organic phase is removed by steam stripping to obtain an aqueous slurry which is then subjected to solid-liquid separation and drying. The solid-liquid separation can be effected by the use of commonly employed means, e.g., a centrifugal separator, a decanter, a vacuum filter, etc. The drying can be performed by means of ordinary devices, e.g., a vacuum drier, a rotary drier, a paddle drier, a flow drier, etc.
The present invention will now be illustrated in greater detail by way of the following examples, but it should be understood that the present invention is not limited thereto. In these examples, physical properties of the produced polyphenylene oxide were determined according to the following methods.
Reduced Viscosity (ηsp/c):
Determined in a 0.5 g/dl solution in chloroform at 25° C.
Du Pont Impact Strength (kg·cm):
Ten sheets of specimens each having a thickness of 1.6 mm and a diameter of100 mm are horizontally mounted on a cylinder having an inner diameter of 25 mm with its radial being in a horizontal direction. A metal rod having a semispherical tip of 10 mm in curvature radius is set on the specimen sothat the semispherical tip contacts with the specimen, and a weight of 2.5 kg is fallen onto the metal rod from a prescribed height. The Du Pont impact strength which is a measure for planar impact characteristics is calculated by multiplying 2.5 kg by the height at which a half of the specimens (5 sheets) are broken.
Heat Distortion Temperature (HDT):
Measured in accordance with ASTM D648.
Tensile Strength:
Measured in accordance with ASTM D638 using an ASTM dumbbell specimen.
Elongation:
Measured in accordance with ASTM D638 using an ASTM dumbbell secimen.
Notched Izod Impact Strength (N I ):
Measured in accordance with ASTM D256 using a specimen having a thickness of 3.2 mm.
EXAMPLE 1
In a 10 l-volume jacketed autoclave equipped with a stirrer, a thermometer,a condenser, and a tube for introducing air which reached the bottom of theautoclave were charged 3420 g of xylene, 1366 g of methanol, 1222 g (10 mols) of 2,6-dimethylphenol, and 24 g (0.6 mol) of sodium hydroxide to form a uniform solution. To the solution was added a solution of 31.5 g (0.3 mol) of diethanolamine, 19.4 g (0.15 mol) of di-n-butylamine, and 0.99 g (0.005 mol) of manganese chloride tetrahydrate in 100 g of methanol. Air was then bubbled through the solution at a rate of 5 l/min while vigorously stirring. While continuing the bubbling, the reaction temperature and pressure were maintained at 35° C. and 9 kg/cm 2 , respectively. After the elapse of 7 hours from the start of bubbling, the air feed was stopped, and the reaction mixture was poured into a mixture of 66 g (1.15 mols) of acetic acid and 4900 g of methanol. The resulting slurry was filtered under reduced pressure to isolate a polyphenylene oxide in a wet state. The isolated polyphenylene oxide was washed with 7200 g of methanol and dried under reduced pressure overnight at 150° C. to obtain 1179 g of a polyphenylene oxide in a dry statehaving a reduced viscosity of 0.562 dl/g.
A compound comprising 45 parts (by weight, hereinafter the same) of the resulting polyphenylene oxide, 55 parts of a high-impact rubber-modified styrene resin ("Estyrene® H63" produced by Nippon Steel Chemical Co., Ltd.), and 1 part of polyethylene ("Sumikathene® E-210" produced by Sumitomo Chemical Company, Limited) was extruded in an extruder set at 260° C. to obtain pellets of a resin compound. The pellets were injection molded at 280° C. to produce test specimens for measurement of physical properties. The results obtained are shown in Table 1.
EXAMPLES 2 TO 12 AND COMPARATIVE EXAMPLES 1 AND 2
Polyphenylene oxides were produced in the same manner as in Example 1 except for changing the kinds and amounts of the alkanolamine and amine asshown in Table 1. The reduced viscosity of each of the resulting polyphenylene oxides is shown in Table 1. Test specimens were prepared in the same manner as in Example 1, and the results of measurement of physical properties are also shown in Table 1.
TABLE 1__________________________________________________________________________ DuPont Alkanolamine Amine Tensile Elong- ImpactExample Amount Amount ηsp/C HDT Strength ation N.sub.I StengthNo. Kind (mol) Kind (mol) (dl/g) (°C.) (kg/cm.sup.2) (%) (kg · cm/cm) (kg · cm)__________________________________________________________________________Example 1 diethanolamine 0.3 di-n-butylamine 0.15 0.562 122 550 140 21.7 280Example 2 " " diethylamine " 0.528 121 520 120 20.5 260Example 3 " " di-n-propylamine " 0.556 122 545 135 21.2 265Example 4 " " diisobutylamine " 0.556 123 550 140 21.0 265Example 5 " " piperidine " 0.534 121 540 150 20.2 270Example 6 " " 2-pipecoline " 0.541 122 540 140 20.8 270Example 7 " " n-propylamine " 0.575 123 525 125 21.0 185Example 8 " " n-butylamine " 0.571 123 520 125 20.5 190Example 9 " " isobutylamine " 0.541 122 535 100 20.3 225Example 10 monoethanol- 0.5 di-n-butylamine 0.4 0.518 121 550 135 21.0 255 amineExample 11 N--methyl- " " 0.08 0.524 121 530 110 19.5 180 ethanolamineExample 12 diisopropanol- 0.3 " 0.015 0.546 122 545 120 20.2 260 amineComparative diethanolamine 0.3 -- -- 0.702 120 540 105 20.3 115Example 1Example 2 -- -- di-n-butylamine 0.15 0.165 96 180 35 6.8 35__________________________________________________________________________
EXAMPLE 13
In the same autoclave as in Example 1 were charged 3,567 g of xylene, 1,219g of methanol, 1,222 g (10 mols) of 2,6-dimethylphenol, and 33.7 g (0.6 mol) of potassium hydroxide to form a uniform solution. To the solution was added a solution of 9.5 g (0.09 mol) of diethanolamine, 12.9 g (0.1 mol) of di-n-butylamine, and 0.44 g (0.0018 mol) of manganese acetate in 100 g of methanol. Air was then bubbled through the solution at a rate of 1.5 l/min while vigorous stirring. While continuing the bubbling, the reaction temperature and pressure were maintained at 40° C. and 9 kg/cm 2 , respectively. After the elapse of 15 hours from the start of bubbling, the air feed was stopped. The obtained reaction mixture was subjected to the same treatment as in Example 1, and consequently 1,172 g of a polyphenylene oxide having a reduced viscosity of 0.526 dl/g was obtained. Test specimens were prepared in the same manner as in Example 1.The test specimens were measured to have a Du Pont impact strength of 210 kg·cm.
As described above, in the production of a polyphenylene oxide using a catalyst system basically composed of a manganese compound and a basic compound, the present invention characterized by combining the above catalyst system with a specific alkanolamine and a specific amine makes itpossible to obtain a polyphenylene oxide suitable for the production of polyphenylene oxide-based polymer alloys. As is demonstrated in the Comparative Examples, the known catalyst system in which a combination of a manganese compound and a basic compound is further combined with an alkanolamine alone or an amine alone fails to produce a polyphenylene oxide suitable for preparing a polyphenylene oxide-based polymer alloy having excellent planar impact characteristics. To the contrary, the polyphenylene oxides obtaind in the Examples exhibit markedly improved planar impact characteristics while retaining other physical properties. Therefore, the process using the catalyst system according to the present invention provides a high-quality polyphenylene oxide suitable as a starting material for the production of polyphenylene oxide-based polymer alloys, having considerable use value in industry.
While the invention has been described in detail and with reference to specific embodiments 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.
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A process for producing a plyphenylene oxide is disclosed, comprising oxidative polymerization of a nucleus-substituted phenol with an oxygen-containing gas in an organic solvent in the presence of a catalyst system comprising a manganese compound containing at least one divalent manganese salt, at least one basic compound selected from hydroxides, alkoxides or phenoxides of the group IA metals of the Periodic Table and hydroxides or oxides of the group IIA metals of the Periodic Table, an alkanolamine represented by formula (I)
R.sup.1 --NH--R.sup.2 --OH (I)
wherein R 1 represents a hydrogen atom, an alkyl group having from 1 to 12 carbon atoms, or a hydroxyl-substituted alkyl group having from 1 to 12 carbon atoms; and R 2 represents an alkylene group having from 2 to 12 carbon atoms, and an amine represented by formula (II)
R.sup.3 R.sup.4 NH (II)
wherein R 3 and R 3 each represents a hydrogen atom, an alkyl group having from 1 to 24 carbon atoms, or an aralkyl group having from 7 to 24 carbon atoms, with proviso that R 3 and R 4 do not simultaneously represent a hydrogen atom, or R 3 and R 4 may be taken together to form a ring. The polyphenylene oxide produced has improved planar impact characteristics without failure in other properties and is, therefore, suitable as a starting material for the production of polyphenylene oxide-based polymer alloy.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] A terminal block connecting apparatus includes first and second support members displaceable from a disengaged condition toward an engaged condition in which corresponding main terminal blocks are brought into electrical engagement, characterized by the provision of first and second test terminal blocks connected with the support members for electrical engagement when the first and second support members are in an intermediate condition between the disengaged and engaged conditions. Carrier means support one of the test terminal blocks for displacement relative to the associated support member, whereby the test terminal blocks remain in electrical engagement during displacement of the support members between the intermediate test condition and the final connected condition. Friction retaining means serve to resist displacement of the carrier member relative to its associated support member.
[0003] 2. Description of Related Art
[0004] It is known in the patented prior art to provide electrical switching and connecting arrangements, such as in the field of emergency power supplies, to connect and disconnect electrical power contacts. In this operation, an additional equipment segment with corresponding power contacts is pushed upon a basic equipment segment with first power contacts. It is known that along with the power contacts, one can connect additional contacts with each other on the equipment segments, which already contact each other in a test position before there is any pushing of the equipment segment into the final engaged position in which the power contacts are also connected with each other. In this way, before reaching the final engaged position, one can already perform tests, for example, to check functions of the equipment segments that are to be connected with each other. In the broadest sense, the invention relates to the area of connecting the additional contacts upon equipment segments that are to be connected with each other by means of suitable switch gears. It is, for example, conceivable that one of the contacts to be connected with each other is fashioned in the form of a sliding contact in which the other contact can be moved out of a first position—the test position—in a sliding manner all the way into the final engaged position (in which the power contacts are connected with each other).
[0005] Such switch gears are known from the state of the art. But their structure is often relatively complicated. Besides, the known designs are not always fully functionally reliable.
[0006] Against this background, the present invention was developed to provide a switch gear that has a simple design and nevertheless a particularly stable structure by means of which, also in case of strong forces to be included in the wiring, one can reliably and easily attain the required test position as well as the final connected position.
[0007] Accordingly, the switch gear has at least one separable locking device for the purpose of locking the switch gear in the first position on the support collar of the electrical appliance, which is so designed that the locked position can be separated only by the shifting of the switch gear by overcoming a friction force between elements of the locking device.
[0008] The switch gear of the present invention has a simple structure and can therefore be made at reasonable cost. The locking device is so structured that, first of all, one attains a clearly recognizable locking position. Either in this position or shortly thereafter, one reaches the test position to perform tests. The engaged or “connect position” can be attained only by further insertion with a stronger insertion force. The switch gear can also absorb very strong forces without any further trouble.
SUMMARY OF THE INVENTION
[0009] Accordingly, a primary object of the present invention is to provide a connector arrangement in which a pair of test terminal blocks are initially brought into electrical engagement when a pair of support means are displaced from a disconnected condition toward an intermediate test condition, and a pair of main terminal blocks are brought into electrical engagement when the support means are displaced from the intermediate test position toward the final connected condition, one of the test terminal blocks being supported on a carrier member that is displaceable relative to the associated support means, thereby to maintain the test terminal blocks in engagement as the support means are displaced to effect engagement of the main terminal blocks.
[0010] According to a more specific object of the invention, friction retaining means serve to maintain the carrier member in one of its first and second positions during the assembly and disassembly of the terminal blocks. The friction retaining means includes a pair of parallel locking levers that are pivoted outwardly by a control member into locking engagement with respective locking recesses contained in the associated support member. The control member is axially displaced relative to a guide sleeve as the main support means are displaced toward one of the test and final engaged conditions.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Other objects and advantages of the invention will become apparent from a study of the following specification, when viewed in the light of the accompanying drawing, in which:
[0012] FIG. 1 a is a perspective left-hand view, with certain parts broken away, of the terminal block connecting apparatus in the initial disconnect condition, and FIGS. 1 b and 1 c are corresponding right-hand sectional views of the test connector block arrangement and the frictional retaining means, respectively, of the apparatus of FIG. 1 a;
[0013] FIG. 2 a is a left-hand perspective view of the apparatus of FIG. 1 a when in the intermediate test position, and FIGS. 2 b and 2 c are corresponding right-hand sectional views of the test connector block arrangement and the friction retaining means, respectively, of the apparatus of FIG. 2 a;
[0014] FIG. 3 a is a left-hand perspective view of the apparatus of FIG. 1 a when in the fully connected condition, and FIGS. 3 b and 3 c are right-hand sectional views of the test connector block arrangement and the friction retaining means, respectively, of the apparatus of FIG. 3 a;
[0015] FIG. 4 is a right-hand perspective view of the apparatus of FIG. 2 a;
[0016] FIG. 5 is a right-hand perspective view of the apparatus of FIG. 3 a;
[0017] FIG. 6 is an exploded bottom perspective view of the carrier means that support the friction retaining means of FIG. 1 a, and FIG. 7 illustrates the apparatus of FIG. 6 when in the assembled condition;
[0018] FIGS. 8 a - 8 f are schematic views illustrating the operation of the friction retaining means of FIG. 6 ;
[0019] FIG. 9 a is a left hand perspective view of a modification of the apparatus of FIG. 2 a when in the test condition; and
[0020] FIG. 10 a is a detailed perspective view of the friction retaining means of FIG. 1 , and FIGS. 10 b and 10 c are perspective and side views, respectively, of a modification of the friction retaining means of FIG. 10 a.
DETAILED DESCRIPTION OF THE INVENTION
[0021] Referring first more particularly to FIGS. 1 a - 1 c, the connecting apparatus of the present invention is operable to connect a main terminal block assembly 1 electrically with a corresponding main terminal block assembly 1 ′ as shown in FIG. 1 b. The main terminal block assembly 1 includes a plurality of terminal blocks 2 that are supported by a moveable support means 6 for displacement toward a stationary support means 3 that is connected with a standard electrical installation, system or appliance, not shown. The contacts of the two terminal block assemblies 1 and 1 ′ are of the corresponding pin and socket contact type, whereby displacement of the components together is shown by the arrow x in FIG. 1 c, effects engagement of the two main block assemblies.
[0022] The terminal block assembly 1 includes a pair of parallel rows of contacts 5 a and 5 b that are arranged above the horizontal support plate 6 a. Arranged below the support plate 6 a is a test terminal block 9 that is adapted for connection with a corresponding test terminal block 8 that is supported by the carrier means 4 for displacement relative to the stationary support means 3 . The test terminal block 8 is so supported by the carrier means 4 that as the support means 6 and 3 are brought together as shown by the arrow x in FIG. 1 c, the contacts 9 a of the test terminal block 9 carried by the movable support means 6 are brought into electrical engagement with corresponding contacts 8 a of the test terminal block 8 that is carried by the stationary support means 3 .
[0023] Upon continued displacement of the movable support means 6 toward the intermediate test position shown in FIGS. 2 a - 2 c, the test contacts 9 a are brought into electrical contact with the corresponding test contacts 8 a of FIG. 2 b, thereby to energize the test circuitry associated with the test terminal blocks, which circuitry is energized from the power supply 40 of FIG. 1 b. When the support members 3 and 6 are in this intermediate test position, the electrical contacts of the main terminal blocks 1 and 1 ′ have not yet been brought into electrical contact with each other. Upon further displacement of the moveable support means 6 toward the final contact position of FIGS. 3 a - 3 c, the contacts of the main terminal assembly 1 are brought into electrical engagement with the corresponding contacts of the associated main terminal block 1 ′, as shown in FIG. 3 b.
[0024] In accordance with a characterizing feature of the present invention, friction retaining means 10 ( FIG. 1 a ) are provided for locking the carrier means 4 in one of its end positions of travel. The carrier means 4 includes a generally U-shaped frame 11 ( FIG. 6 ) having a central panel portion 11 a, and a pair of orthogonally-arranged side walls 11 b. Similarly, the stationary support means 3 comprises a collar element having a central panel portion 3 a, and a pair of orthogonally-arranged side walls 3 b. Guide means 18 support the carrier member 11 for linear displacement in the given direction x relative to the stationary support means 3 . When in the assembled condition of FIG. 7 , the side walls 11 b are parallel with and in spaced relation from the corresponding side walls 3 b of the stationary support member 3 , thereby to define a pair of spaces for receiving respectively on of the the friction retaining means 10 of the present invention.
[0025] As best shown in FIGS. 6 and 10 a, the friction retaining means 10 includes a pair of locking levers 14 that are pivotally connected at one end by pivot pins 15 with the outer surface of one side wall 11 b of the carrier member 11 . The other ends 14 a of the locking levers are bifurcated to define a pair of outwardly directed detent portions. Arranged between the locking levers 14 is a control member 19 that is supported for axial displacement in a direction parallel with said given direction x. The opposed sides at one end of the control member 9 contain a pair of recesses 23 that cooperate to define an enlarged head portion 19 a that is joined with the body portion of the control member by a neck portion 19 b. The enlarged head portion 19 a engages the adjacent surfaces of the inner detent portions at the bifurcated ends 14 a of the two locking levers 14 , as shown in FIG. 10 a. The control member 19 is slidably displaceable within a through bore contained in a guide sleeve member 20 that is fastened to the outer surface of a side wall 11 b of the carrier member 11 .
[0026] Referring again to FIGS. 1 a - 1 c, the moveable support means 6 , which may be formed of metal or a suitable synthetic plastic material, includes a pair of parallel spaced resilient arm portions 6 b that extend toward the stationary support means 3 . The support arms 6 b are provided at their free extremities with hook-like extensions, and cooperate with the transverse wall portion 6 c of the integral base portion 6 d of the movable support means 6 to define a chamber 42 for receiving the guide sleeve 20 associated with the control member 19 . Compression spring 22 is mounted within a bore contained in the base of the body portion of the control member 19 for reaction with the transverse wall 6 c, as will described in greater detail below. Thus, when the moveable support means 6 is displaced toward the stationary support means 3 in the direction illustrated by the arrow x in FIG. 2 c, the resilient arm portion 6 b of the support member 6 engage external projections 20 a contained on the outer surface of the guide member 20 , thereby to connect by a snap fit the support member 6 into engagement with the shoulder portions 20 a on the outer surfaces of the guide sleeves 20 that are fastened to the side walls 11 of the carrier member 11 . As shown in FIG. 2 c, the compression spring 22 cooperates with the transverse wall 6 c to bias the control member 19 to the left toward the stop position defined by the guide sleeve 20 , as shown in FIG. 2 c. As shown in FIG. 2 b, the pin and socket contacts 9 a and 8 b of the two test terminal blocks are now in engagement to control test circuits supplied with power from the power supply 40 . Upon further displacement of the moveable support means 6 toward the final connected position of FIGS. 3 a - 3 c, the extremities of the resilient arm portion 6 b engage the bifurcated ends 14 a of the locking levers 14 , thereby to pivot the same inwardly toward the unlocked position shown in FIG. 3 c. As shown in FIG. 3 b, the carrier member 11 is displaced in such a manner as to maintain the contacts of the two test terminal blocks 8 and 9 in continued engagement as the main terminal blocks 1 and 1 ′ are displaced toward the connected condition of FIG. 3 b. FIG. 4 illustrates the apparatus when in the test condition of FIGS. 2 a - 2 c, and FIG. 5 illustrates the apparatus when in the finally assembled contact position of FIGS. 3 a - 3 c.
[0027] Referring now to FIGS. 8 a - 8 f, the operation of the friction retaining means 10 is illustrated schematically. More particularly, as shown in FIG. 8 a, when the moveable support member 6 is displaced toward the stationary support member 3 , the resilient actuating arms 6 b are shifted to the right over the lateral projections 20 a on the side walls of the guide sleeve 20 , whereupon the bottom wall 6 c of the recess 42 engages the spring 22 mounted in a bore contained at the lower extremity of the control member 19 . As the actuating portion 6 d is shifted to the right in FIG. 8 b, the locking levers 14 are pivoted inwardly to remove the outer detents from the locking recesses 17 contained in the stationary guide member 3 . Thus, the carrier member 11 is released for travel to the second position illustrated in FIG. 8 c, which is the final connected position in which the main terminal blocks 1 and 1 ′ are electrically connected as shown in FIG. 3 b.
[0028] To disconnect the main terminal blocks 1 and 1 ′, the moveable element 6 is displaced in the opposite direction as shown by the arrow in FIG. 8 d, whereupon the hook portions at the ends of the resilient actuating arms 8 b engage the shoulder surface of the guide sleeve 20 , thereby to initiate displacement of the carrier member 11 to the left. When the outer detents on the locking levers reach the locking recesses 17 , the levers are separated by the enlarge head portion 19 a of the control member, thereby to lock the levers 14 to the recesses 17 . Upon further displacement of the operating member 6 d to the left, the enlarged head portion 19 a of the control member is wedged into frictional engagement with the inner detents at the bifurcated end portions of the locking levers. If desired, the member 6 d can be further displaced to the left to totally disengage the member 6 from the support member 3 , whereby the components are in the initial disengaged condition of FIGS. 1 a - 1 c.
[0029] In the modified embodiment of FIGS. 9 a - 9 c, the design is such that the control member 19 in the test position is already inserted so far that its head portion 19 a no longer precisely engages between the inner detent portions of the locking levers 14 . This locking position is thus, so to speak, left again for the attainment of the test position according to FIG. 2 , which offers the advantage that the mechanical components in the test position are further relieved of forces when the test position is retained, for example, for a longer period of time.
[0030] Referring now to the modification of FIGS. 10 b and 10 c, the resilient arm portions 106 b of the moveable support member 106 are provided with ribbed inner surfaces 106 f on the resilient arm portions 106 b that engage corresponding external rib surfaces 120 f on the outer surface guide sleeve 120 . This design is particularly stable and thus insensitive to variations in force.
[0031] Of course, it is contemplated that the elements might be reversed so that the friction retaining means are mounted on the stationary support means 3 rather that the moveable support means 6 .
[0032] While in accordance with the provisions of the Patent Statutes the preferred forms and embodiments of the invention have been illustrated and described, it will be apparent to those skilled in the art that changes may be made without deviating from the invention described above.
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A terminal block connecting apparatus includes first and second support members displaceable from a disengaged condition toward an engaged condition in which corresponding main terminal blocks are brought into electrical engagement, characterized by the provision of first and second test terminal blocks connected with the support members for electrical engagement when the first and second support members are in an intermediate condition between the disengaged and engaged conditions. One of the test terminal blocks is supported by a carrier member for movement relative to the associated support member, whereby the test terminal blocks will remain in electrical engagement during displacement of the support members between the test and connected conditions. A friction retaining arrangement serves to resist displacement of the carrier member relative to its associated support member.
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BACKGROUND OF THE INVENTION
1. Field of the Invention:
This invention relates to improved cardboard furniture. More specifically, the invention relates to the use of snap-in-place cardboard surface members in combination with a honeycomb like cardboard egg crate divider core to make structurally sound and anatomically correct furniture.
2. Description of the Prior Art:
The basic concept of manufacturing and selling light weight furniture is generally known, particularly in regards to contemporary aluminum lawn chairs and the like. Likewise, the concept of providing either a pattern or kit for the do-it-yourselfer to make light weight furniture is generally known, for example, in making PVC pipe furniture. And, at least one academic institution has studied the possibility of designing light weight furniture from cardboard including the use of the so-called "egg crate divider" structural system involving a cardboard honeycomb made from a criss-cross pattern of interlocking, cut sheets or strips of cardboard. However, in the case of using cardboard as the structural material, very little commercial success or consumer acceptance has been achieved primarily because of the lack of dimensional rigidity and/or structural stability. Also, most light weight furniture has failed to achieve an acceptable level of comfort associated with an anatomically contoured seat, chair, or the like.
SUMMARY OF THE INVENTION
The present invention provides an inexpensive, light weight, structurally sound system for manufacturing anatomically correct furniture out of nothing but cardboard. According to the present invention, the cardboard furniture can be made out of pre-cut sheets of cardboard and assembled without the use of special tools, fasteners, adhesives or the like. As such, the piece of furniture can be sold as a kit and assembled by merely compressively snapping or folding the individual pieces together. Because of the use of external cardboard surface panels in combination with an internal "egg crate divider" core, the resulting furniture is rigid and dimensionally stable.
Thus, the present invention provides a cardboard furniture kit comprising in combination:
(a) a plurality of sheets of cardboard forming a first sequential set wherein each sheet of cardboard of the first sequential set is pre-cut such that the lower edge of each sheet is adapted to rest flat on a floor and at least one other edge is pre-cut to conform anatomically to the contour of the human body in a first direction parallel to a corresponding anatomically contoured portion of each other sheet of the first sequential set when sequentially positioned parallel and equal distance to each other and wherein the relative position of each anatomically contoured portion of each sheet of the first sequential set when sequentially positioned parallel and equal distance to each other correspond to the contour of the human body in a second direction perpendicular to the first direction and wherein each of the sheets of cardboard forming the first sequential set are periodically slotted such as to structurally engage to compatible periodical slots in a plurality of sheets of cardboard forming a second sequential set;
(b) a plurality of sheets of cardboard forming a second sequential set wherein each sheet of cardboard of the second sequential set is pre-cut such that the lower edge of each sheet is adapted to rest flat on a floor and at least one other edge is pre-cut to conform anatomically to the contour of the human body in a second direction perpendicular to the first direction and parallel to a corresponding anatomically contoured portion of each other sheet of the second sequential set when sequentially positioned parallel and equal distance to each other and wherein the relative position of each anatomically contoured position of each sheet of the second sequential set when sequentially positioned parallel and equal distance to each other corresponds to the contour of the human body in the first direction and wherein each of the sheets of cardboard forming the second sequential set is periodically slotted such as to structurally engage to the compatible periodical slots in the plurality of sheets of cardboard forming the first sequential set, thus being adapted to form simultaneously a flat surface of intersecting lower edges and at least one anatomically contoured surface of intersecting anatomically contoured other edges; and
(c) at least one cardboard sheet wherein the perimeter of the sheet is periodically slotted such as to be adapted to form tabs that fold, insert, and engage around the perimeter of the anatomically contoured surface of intersecting anatomically contoured other edges.
It is an object of the present invention to provide cardboard furniture that is anatomically correct and structurally sound. It is a further object of the present invention to provide cardboard furniture in a kit form that is extremely inexpensive in that nothing other than cardboard is employed and no special tools or other equipment is necessary to hand assemble the kit. Fulfillment of these objects and the presence and fulfillment of other objects will become apparent upon complete reading of the specification and claims taken in conjunction with the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 a partial cut-away perspective view of a typical cardboard studio chair according to the present invention.
FIG. 2 is a bottom view of the cardboard studio chair of FIG. 1.
FIGS. 3 and 4 are side plan views of the vertical combined seat and back rest cardboard structural elements of the studio chair of FIG. 1.
FIG. 5 is a side profile view of the cardboard structural elements of the studio chair of FIG. 1 that are part of the seat and the back rest but lie perpendicular to the structural elements of FIGS. 3 and 4.
FIG. 6 is a top plan view of the surface panel for the seat and the back rest of the studio chair of FIG. 1 before assembly of the chair.
FIG. 7 is a top plan view of the base support element of the studio chair of FIG. 1 again before being folded and assembled to the chair.
FIG. 8 is a perspective view of a studio sofa according to the present invention.
FIG. 9 is a perspective view of an ottoman according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The improved cardboard furniture according to the present invention, how it can be provided and hand assembled in a kit form, and how it differs from previously known cardboard furniture can perhaps be best explained and understood by reference to the drawings. FIG. 1 illustrates a typical studio chair (generally designated by the numeral 10) according to the present invention. As illustrated in this specific embodiment, the studio chair 10 is made up entirely of pre-cut sheets of cardboard which are slotted periodically to either slide together forming a central structural core forming a so-called egg crate divider type criss-crossing pattern 12 or the sheets are periodically slotted to form tabs that bend, insert and engage to openings created by the egg crate divider structure.
As illustrated in FIGS. 1 and 2, the egg crate divider structure of the core of the studio chair 10 involves a sequential set of five vertical sheets of cardboard, three corresponding to sheet 14 of FIG. 3 and two corresponding to sheet 16 of FIG. 4. As seen in FIG. 1, sheets 14 are positioned at the outer sides and directly in the middle of the seat and back rest of chair 10, while the larger sheets 16 are positioned between sheets 14, thus producing a slight arch with a center depression in the seat and back rest. Perpendicular to sheets 14 and 16 are ten sheets 18 as shown in FIG. 5. Five of the sheets 18 criss-cross with the sheets 14 and 16 in the seat area of the chair 10 and the other five criss-cross with the sheets 14 and 16 in the back rest portion of the chair. As further seen in FIGS. 3, 4 and 5, the cardboard sheets 14, 16 and 18 are provided with interlocking slots 20, 22 and 24 periodically positioned along the back rest and seat edges of sheets 14 and 16 and along the flat bottom edge of sheet 18. The length and width of the slots are sufficient to allow the respective sheets to interlock with each other forming the egg crate divider type core structure of the chair 10.
As further seen in FIG. 1, both the seat area and the back rest area of the studio chair 10 are covered with a cardboard surface 26. As shown in FIG. 6, the cardboard surface 26 in the unassembled form is made from a single flat sheet of cardboard with the perimeter of the sheet 26 periodically slotted and scored, thus forming a series of adjacent flaps 28 and folding lines 29. The flaps 28 are intended to be bent during assembly of the chair 10 such that they insert and wedge into the opening formed between successive criss-crossed sheets 14, 16 and 18; i.e., between the square opening in the egg crate divider structure. In this manner, the cardboard surfaces 26 bends at the score lines 29 such as to conform to the geometry and curvature in the seat and back rest areas of the chair. In a similar manner, the under side and back side of the chair 10 are provided with an additional stabilizing cardboard sheet or surface 30, see FIG. 2. As shown in FIG. 7, the stabilizing sheet 30 involves an upper edge 32 and a lower edge 34, each having a series of periodical slots 36 and 38 that when folded about dashed lines 40 and 42 will insert into slots 44 and 46 of the cardboard sheets 14 and 16 (see FIGS. 3 and 4) making up the combined back rest and seat of chair 10. In order to engage slots 36 and 38 with slots 44 and 46, the entire sheet 30 is further folded about the central line 48, see FIGS. 2 and 7. Because of the presence of the exterior cardboard surfaces 26 and particularly the stabilizing cardboard surface 30, the entire chair 10 after assembly is extremely rigid, yet virtually no tools or adhesives need be employed during assembly. Because of the use of cardboard, the chair is extremely light weight and the respective edges of the structural elements can be readily contoured to anatomically conform to the contours of the human body.
As illustrated in FIGS. 8 and 9, the basic concept of the present invention can be readily incorporated into other pieces of furniture; including by way of example, but not limited thereto, a studio sofa as shown in FIG. 8, an ottoman as shown in FIG. 9 or the like. As suggested in FIG. 8 by extending the structural pieces corresponding to FIGS. 5, 6 and 7 to a greater length and by simultaneously providing a greater number of pieces of FIG. 3, a studio sofa can be readily produced. Similarly, by eliminating the back rest portion, an ottoman can be produced. It should be appreciated that other pieces of furniture could also be readily produced using the combination of surface stabilizing cardboard sheet and criss-crossing structural cardboard sheet honeycomb like core. It should also be appreciated that various other anatomically correct designs can be readily incorporated into the present invention, including a complete line of corresponding children's furniture.
More explicitly, in the case of the above illustrated studio chair, a back rest of approximately 327/8 inches, and seat of 25 inches as measured along the bottom and back of the piece shown in FIGS. 3 and 4 with a seat height of approximately 12 11/16 inches, FIG. 3, (13 13/16 inches for FIG. 4) and a spacing of about 4 inches between slots will produce an anatomically correct studio chair for an average size adult. The corresponding measurements for a child's studio chair would be approximately 19.73 inches, 15 inches, 7.61 inches (8.29 inch for FIG. 4) and 2.40 inches, respectively. Typically, the width of the adult studio chair would be 28 inches while the child version would be 16.8 inches.
In order to facilitate the ease of assembly of the cardboard furniture according to the present invention and to insure structure integrity of the assembled piece of furniture, the respective slots in the individual cardboard sheet can preferably be slightly tapered such as to insure ease of initial alignment of a slot with another engaging slot and upon deep penetration create a firm wedge affect. Also, the length of the tabs positioned around the perimeter or along the outer edges of the surface forming cardboard sheets can preferably be staggered, as suggested in FIG. 6. This allows the slightly longer tab to be inserted first and systematically advanced deeper as the adjacent relatively shorter tab is folded and inserted into the next opening in the egg crate divided type structure. Furthermore, the surface forming sheets of cardboard can preferably be prescored, perforated or prefolded to facilitate conforming with the surface curvature of the underlying criss-crossed support members.
The actual manufacturing of the elements making up the cardboard furniture according to the present invention can be out of any of the common cardboard structural materials and by any of the well known fabrication techniques as generally known in the art. Preferably, the individual pieces are die cut to shape. Most preferably, the pieces are fabricated out of conventional cardboard box type material.
Having thus described the invention with a certain degree of particularity, it is to be understood that the invention is not limited to the embodiments set forth herein for purposes of exemplification, but is to be limited only by the scope of the attached claims, including a full range of equivalents to which each element thereof is entitled.
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Improved cardboard furniture (e.g., chair, sofa, ottoman or the like) comprising a structural core of periodically slotted cardboard sheets interlocked in a criss-crossing, egg crate divider type assembly with external stabilizing cardboard surfaces made from cardboard sheets having their perimeter periodically slotted such as to form tabs that fold, insert and engage in the openings of the egg crate divider type assembly. Such cardboard furniture can be provided in a kit form that is readily hand assembled, without special tools, adhesives or other fasteners into structurally stable and anatomically correct light weight furniture.
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This is a continuation of U.S. application Ser. No. 08/882,395, filed on Jul. 10, 1997, now U.S. Pat. No. 5,915,585.
TECHNICAL FIELD
The present invention relates generally to promotional closures for containers configured for use in connection with a sales promotion or game, and more particularly to a promotion-receiving compartment for a closure which is configured to facilitate easy-opening by consumers for removal of a promotional element from within the compartment.
BACKGROUND OF THE INVENTION
Promotions and games which are associated with the sale of products have shown enduring popularity with consumers. A wide variety of such promotions and games are known, and may include gaming systems where game elements are collected to receive an award, or receipt by a consumer of a promotional element which can be redeemed for an award, or which may have intrinsic value for the consumer.
Promotional systems for use with container closures have heretofore taken various forms. For example, it has been known to provide the liner portion of a closure in the form of a gaming piece, whereby collection of certain ones of the liners permits prize redemption, or the liners themselves can be individually redeemed for cash or other awards. It has also been known to provide container closures with a compartment element positionable generally within the closure so that a promotional element can be positioned within the compartment for removal upon opening of the container. Closure/compartment arrangements of this nature are disclosed in U.S. Pat. No. 5,056,659, to Howes et al., hereby incorporated by reference.
The present invention is directed to an easy-open promotion-receiving member for a promotional closure which is configured to facilitate convenient manipulation and opening by consumers for use in a promotional or gaming system.
SUMMARY OF THE INVENTION
A promotional closure with which the present invention is particularly suited for use includes an outer plastic closure cap having a circular top wall portion and a depending annular skirt portion. The closure is adapted for application to an associated container, typically by the provision of interengaging threads. In accordance with the present invention, the promotion-receiving member of the closure includes a cup-shaped promotion compartment positionable generally beneath the top wall portion of the outer closure cap. Notably, the promotion compartment includes a frangible side wall strip. A promotional element positioned within the compartment can be easily removed as the side wall strip is at least partially separated from the side wall portion of the compartment to gain access into the compartment, all of which can be accomplished without resort to tools or other implements.
As noted, the promotion compartment of the present invention is positionable beneath the top wall portion of the outer closure cap, and inwardly of the annular skirt portion of the cap for disposition generally within an associated container. The cup-shaped promotion compartment includes a circular bottom wall, and an upstanding, generally cylindrical side wall extending upwardly therefrom. In the preferred form, the compartment includes an annular flange extending outwardly from the side wall. The cap includes a seal covering an inside of the top wall thereof and having an annular radially inwardly extending flange or lip. The annular flange of the compartment is captured between the top wall and the lip to be held within the cap. When the cap is removed from the bottle, the compartment can be removed from the cap by manipulating the compartment to cause the flange to disengage from the lip.
In accordance with the illustrated embodiment, the side wall of the compartment comprises a frangible portion which can be opened after the closure is removed from the associated container and the promotion compartment is removed from within the closure cap. Opening of the frangible portion of the compartment facilitates removal of a promotional element, such as a coupon, currency, or other promotional item, from within the promotion compartment.
In the preferred form, the frangible portion of the side wall comprises a side wall with a circumferentially extending band which extends at least partially about the circumference of the side wall and is defined by tear lines of weakened side wall, e.g., molded relatively thin wall sections, score lines, perforations, etc. Fracture along the weakened lines permits opening of the compartment such as by a hinging movement of the circular bottom wall about a remaining side wall portion which joins the bottom wall to the remainder of the compartment.
The annular flange acts in the nature of a finger grip to facilitate opening of the compartment. Also, in some embodiments, a bottom flange is also included which provides a finger grip for removing the compartment from the cap and for manipulating the compartment during opening thereof. The bottom flange also protects the pull tab affixed to the frangible portion during handling, assembly, and high speed application of closures to containers. The promotion compartment is thus split or opened circumferentially from its cup-shaped configuration, facilitating convenient access to a promotional element carried within the compartment.
A preferred fabrication of the compartment from low density polyethylene further facilitates convenient opening of the compartment.
The promotional closure embodying the principles of the present invention thus provides a method for accessing a prize or like promotional piece from a bottle. The method comprises the steps of removing a closure from the associated bottle, and thereafter removing a prize-container compartment from within the closure. The prize is accessed from within the compartment by tearing open the compartment by at least partially separating a frangible portion of the compartment, which extends at least partially circumferentially of the compartment. By this opening of the compartment, the prize can thereafter be accessed by removing the prize from within the compartment.
Other features and advantages of the present invention will become readily apparent from the following detailed description, the accompanying drawings, and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-sectional view of a promotional closure having an easy-open promotion-receiving member embodying the principles of the present invention;
FIG. 1a is an enlarged cross-sectional view of a portion of the closure of FIG. 1;
FIG. 2 is a top perspective view of the promotion-receiving member of the present invention;
FIG. 3 is a bottom perspective view of the promotion-receiving member of the present invention;
FIG. 4 is a bottom perspective view of the promotion-receiving member of FIG. 3 from a different viewing angle;
FIG. 5 is a bottom perspective view illustrating opening of the promotion-receiving member of the present invention;
FIG. 6 is a bottom perspective view of an alternate promotion-receiving member of the present invention; and
FIG. 7 is a bottom perspective view of the alternate promotion-receiving member of FIG. 6 from a different viewing angle;
FIG. 8 is a bottom perspective view of a further alternate embodiment of the present invention;
FIG. 9 is a bottom perspective view of a further alternate embodiment of the present invention; and
FIG. 10 is a bottom perspective view of the embodiment of FIG. 9 from a different viewing angle.
DETAILED DESCRIPTION
While the present invention is susceptible of embodiment in various forms, there is shown in the drawings and will hereinafter be described presently preferred embodiments, with the understanding that the present disclosure is to be considered as an exemplification of the invention, and is not intended to limit the invention to the specific embodiments illustrated.
With reference first to FIG. 1, therein is illustrated a promotional closure 10 including an easy-open promotion-receiving member embodying the principles of the present invention. Promotional closure 10 is particularly configured for use with an associated container, a portion of which is illustrated and is designated C shown in FIG. 1a. The container, such as a bottle, can be closed by the closure such as by threaded application to a neck portion of the container. Closures of the type illustrated in FIG. 1 can be formed in accordance with the teachings of U.S. Pat. No. 4,497,795, hereby incorporated by reference.
Closure 10 is in the form of an assembly that includes a molded plastic outer closure cap 12 having a circular top wall portion 14 and a depending annular skirt portion 16. The annular skirt portion 16 includes an internal helical thread formation 18 configured for cooperating threaded engagement with the associated container C. A sealing liner 20 positioned adjacent the top wall portion 14 of the closure facilitates sealing engagement of the closure with an associated container, and permits the closure to be configured for use with containers having carbonated contents.
The illustrated closure 10 is of the so-called tamper-indicating type, and includes a detachable pilfer band 22 depending from the annular skirt portion 16. The pilfer band 22 is distinguished from the upper closure cap 12 by a circumferentially extending score line 24, with a plurality of circumferentially spaced frangible ribs 26 extending between the inside surfaces of the closure cap and the pilfer band. A plurality of circumferentially spaced container-engaging flexible projections 28 extend inwardly of the pilfer band, for cooperating engagement with the locking portion of the associated container. By such cooperating engagement, the frangible ribs 26 split and fracture during removal of the closure from the container, thereby separating the pilfer band from the skirt portion 16 of the closure cap for the desired tamper-evidence. The illustrated embodiment of the pilfer band is configured in accordance with U.S. Pat. No. 4,938,370, hereby incorporated by reference, but may alternately be configured in accordance with the teachings of U.S. Pat. No. 4,418,828, hereby incorporated by reference.
The closure 10 is intended for use in connection with consumer promotions or games, and to this end, the closure includes a promotion-receiving member positioned generally within the closure cap 12. As illustrated in FIGS. 2 through 4, the promotion-receiving member is provided in the form of a promotion compartment 30 having a generally cup-shaped configuration including a circular bottom wall 32, and a generally cylindrical upstanding side wall 34 extending upwardly from the bottom wall 32. In the preferred form, the promotion compartment 30 includes a depending annular bottom flange 36 which facilitates finger grasping for removal of the compartment from within the closure cap 12. The bottom flange 36 also desirably protects the pull tab (as will be described) of the compartment 30.
The compartment 30 is preferably of unitary construction apart from its cover member, and preferably molded from low density polyethylene plastic material which, as will be further described, facilitates tearing, opening, or splitting of the compartment so that a promotional element positioned within the compartment can be easily removed by consumers. Positioning of the compartment 30 within the closure cap 12 is facilitated by the provision of an annular compartment flange 38 which extends generally outwardly from the upper edge of the side wall 34. The annular compartment flange 38 is interengaged with a portion of the sealing liner 20 of closure 10, by the provision of an annular liner flange or lip 39 on the liner which fits between the container C and the compartment flange 38. The flange 39 extends from an annular liner bead 20b. As will be observed in FIGS. 1A and 2, the compartment flange 38 is preferably held in generally captive relationship between the liner flange 39 and the liner bead 20b within closure cap 12.
However, a closure prize compartment embodying the principles of the present invention can be otherwise retained within the associated outer closure cap. The closure assembly can be configured such that the upper annular flange 38 of the compartment effects sealing engagement with the associated container, with the closure liner 20 having no lip 39 or the like. In such an arrangement, a preformed disc liner can be provided in the outer cap (rather than the illustrated molded in place liner 20) to provide a so-called secondary seal, that is, an arrangement for sealing the container after removal of the compartment 30 from within the outer cap. In such an alternative construction, the compartment may be configured for self-venting. Such venting can be desirable in view of the elevated gas pressure which can exist within the compartment from use of the closure assembly on a container having carbonated contents. Normal migration of gas pressure into the compartment occurs after application of the closure assembly to the container after filling. Attendant to closure removal, gas pressure is released from within the container, but the sealed compartment 30 remains slightly pressurized. If the compartment is not retained within the closure cap (such as by the provision of lip 36 on liner 20), self-venting of the gas pressure within the compartment avoids outward expansion of the compartment which expansion can result in inadvertent dislodgement of the compartment from within the cap. A self-venting compartment can be provided by configuring the seal of cover member 40 to delaminate or open in a predetermined fashion. A suitable self-venting seal arrangement is described in commonly assigned U.S. patent application Ser. No. 08/746,710, filed Nov. 15, 1996.
The installation of the compartment 30 into the cap 12 includes the bending of the compartment flange 38 upwardly into a cone shape for passing an outer edge of the compartment flange between the lip 39 and the liner bead 20b. The bending is done by a tool which then releases the compartment flange 38 allowing the compartment flange to snap back to its planar configuration fully inserted between the lip 39 and the bead 20b.
FIG. 1 also illustrates that in the preferred form, the tab 48 extends radially outwardly no further than the bottom flange 36, and the top flange 38. This protects the tab 48 from damage during handling and assembly, and facilitates high-speed application of closures to containers.
A suitable promotional element (not shown) can be positioned within the interior of the compartment 30. Such a promotional element can be provided in the form of a coupon redeemable for an award or the like, folded currency (i.e., cash), or some other suitable promotional article. Retention of the promotional element within the compartment is desirably enhanced by the optional provision of a cover member 40 in the form of a membrane fitted to the flange 38, which cover member 40 can be provided in the form of a suitable plastic film or the like heat-sealed or otherwise secured to the flange 38 of the compartment. The cover 40 acts to desirably isolate the contents of the compartment from the contents of the associated container C, and to desirably enhance the structural integrity of the compartment 30 without impairing easy-opening of the compartment. The cover member can be a laminate of low density polyethylene with PET (polyethylene terephthalate) with a polyurethane bonding agent.
When the closure/container combination is used to contain carbonated beverages, the contents of the compartment 30 eventually become pressurized by the CO 2 within the container. When the closure is removed, the pressure inside the compartment has a tendency to "dome" or push out the film cover member 40 against the inside surface 20a of the seal 20. This can cause the compartment, particularly the compartment flange 38, to inadvertently release or "pop off" from above the liner flange 39. To prevent this occurrence, a substantially rigid reinforcing disc 41 is carried in a recessed annular step 42 (see FIG. 1) of the flange 38 and is sealed to the cover member 40. The disc 41 is sufficiently thick to substantially prevent "doming" which prevents pressing of a top of the cover member 40 to the inside surface 20a. The disc 41 is preferably composed of high density polyethylene. As an alternative arrangement the disc 41 can have a snap engagement to positively lock to the annular step 42. The disc can also be provided with a vent hole beneath the cover member for venting if the cover member is peeled off, or if a removable membrane-like cover member is contemplated.
One size of closure commonly used for containers for carbonated beverages has a diameter of 28 millimeters, with a promotion compartment embodying the principles of the present invention sized for disposition within an associated container when a closure of this size is applied thereto. While a promotion compartment in accordance with this invention can be configured for use with closures of many different sizes, use in connection with a 28 millimeter closure necessarily requires that the promotion compartment be relatively small in size. As such, removal of a promotional element from within the compartment should be as easy as possible to permit removal by consumers without resort to use of a tool or other implement.
Accordingly, the promotion compartment 30 in accordance with the present invention is configured for easy-opening, that is, is configured to split or open in a fashion which permits the contents of the compartment to be easily removed without the use of an associated implement. Thus, even when the promotion compartment 30 is sized for use with 28 millimeter closures, consumers can very easily gain access to the contents of the compartment.
As illustrated in FIGS. 3 and 4, the sidewall has an upper annular L-shaped (in cross-section) rim 44 which provides the stepped recess 42 for holding the disc 41. The depending annular bottom flange 36 is also L-shaped in cross-section, forming a bottom recess 45. The flange 36 can be used for finger gripping to remove the compartment from the cap. Within the bottom recess 45, an outer surface 32a of the bottom wall 32 is exposed. The outer surface 32a can carry indicia such as advertising, game information, or an announcement of a winning compartment, i.e., that the compartment contains a prize.
A handle or tab 46 is provided having an elongate body 48 with finger-gripping ribs 50 provided thereon on a front side and ribs 52 optionally provided on a back side. The elongate body 48 is connected to a pull portion 54 which is molded to a side wall region 58 having a reduced thickness. The pull portion 54 has a height in a direction parallel to an axis of the cylindrical wall 34. Two sets of intermittently weakened lines, preferably formed by molding relatively thin regions in the sidewall 34, are arranged in parallel around a partial circumference of the wall 34, spaced apart a distance approximating the height of the pull portion. The circumferentially extending tear lines preferably extend 270°-300° around the circumference, in substantially parallel relationship to each other.
A top weakened or tear line 60 has intermittent bridges or residual regions 62. A lower weakened or tear line 64 has residual regions 66. The upper and lower tear lines 60, 64 are spaced apart to define a frangible band-shaped portion 68 therebetween extending from the pull portion 54 around a partial circumference of the wall 34. The upper tear line 60 terminates in a first substantially circular recess 70 while the lower tear line 64 terminates in a second substantially circular recess 72. Additionally, a last region 74 of the tear line 60 which is contiguous with the recess 70, has a depth decreasing into the recess 70. Similarly, a last region 76 of the tear line 64 contiguous with the second recess 72 has a depth decreasing into the circular recess 72. The decreasing depth of the tear lines and the circular recesses tend to slow down and terminate ripping of the side wall at the recesses.
The first circular recess 70 terminates around the circumference of the wall 34 at a position A, while the second circular recess 72 extends further and terminates at the position B. The difference C between these two positions tends to cause the frangible portion 68, if ripped past the recesses 70, 72, to be removed along offset paths 80, 82 shown dashed, which are offset at an end region thereof toward the rim 44 rather than to continue across the side wall circumferentially. Thus, when the frangible portion 68 is forcibly removed, a region 90 substantially remains intact to retain the flange 38 connected to the wall 34 at this position. It should be noted that the residuals 62, 66 can be formed by relatively thick regions of the thinly molded tear lines 60, 64 or by using overlying bridge pieces similar to the bridge pieces 26 spanning across the score line 24 of the pilfer band.
FIG. 5 illustrates the promotion compartment 30 removed from the cap and in a partial stage of opening. The tab or handle 46 has been pulled from the region of reduced thickness 58 along a tear line 92 and the tear lines 60, 64. The residuals 62, 66 have been broken into half pieces or fragmentary pieces 62a, 62b and 66a, 66b. When the frangible portion or band 68 is sufficiently opened, the promotion piece held within the container 30 can be removed. If the frangible band-shaped portion 68 is continuously torn from the wall 34, the offset terminations A and B will cause an angular rip toward the flange 38 preventing a complete circumferential rip of the band and separation of the compartment 30 into top and bottom pieces. It is preferable to retain the entire opened compartment 30 as a single piece, or to allow only the band 68 to be removed while retaining the remainder of the container 30 as a single piece.
FIGS. 6 and 7 illustrates an alternate embodiment promotion-receiving compartment 100 having a wide band 102 across its side wall 106 defined by two continuous tear lines 108, 110. A tangentially extending handle 116 connects to the band 102 at a rectangular depression 118 which form a reduced thickness wall region. When the handle 116 is forcibly pulled away from the wall 106, the vertical line 120 at the inner face between the handle 116 and the recess 118 separates and the band 102 can be peeled open along the tear lines 108, 110 circumferentially around the wall 106 to terminations A, B shown in FIG. 7. In this embodiment, no circular enlarged recesses are used at the termination positions A, B, and the termination positions are not offset circumferentially. However, the depth of the tear lines 108, 110 decreases gradually throughout the regions 126, 128 which are adjacent the terminal positions A, B. This decrease in depth at the terminal regions effectively slows the speed of peeling or tearing of the panel 102 from the wall 106 to prevent unwanted tearing throughout the wall region 130 between the terminal positions A, B and the recess 118.
FIG. 8 illustrates a further alternate promotion-receiving compartment 200. In this illustrated embodiment, stepped annular top and bottom flanges, as in the previous embodiments, are not used but optionally could be used. Instead, a reinforced planar annular flange 201 and a recessed bottom 202 are used. A frangible portion in the form of a band 204 is formed by a first tear line 206 and a second tear line 208 formed into an annular side wall 210 of the container 200. The tear lines 206, 208 extend substantially circumferentially around a portion of the circumference of the side wall 210 and turn down arcuately at positions 212, 214 into axially arranged tear line portions 216, 218 which extend to a bottom edge 220 of the wall 210. Additionally, an overhang portion 224 is provided contiguous with the band 204 and which extends outwardly of the edge 220 to provide a finger grip or pull tab. The tear lines 206, 208 wrap around the circumference of the wall 210 and terminate at positions A, B which can, for example, be configured and shaped as positions A, B shown in FIG. 7 with decreasing depth contiguous to the positions A, B; or configured and shaped as the terminations A, B shown in FIG. 3 with offset circular recesses and decreasing depth. Although no residuals are shown in the tear lines 206, 208 in the embodiment of FIG. 8, it is also possible to use residuals to strengthen the container.
FIG. 9 shows a still further alternate embodiment promotion-receiving compartment 300, somewhat similar to the compartment shown in FIG. 8. A frangible portion comprising band 304 defined by a first tear line 306 and a tear line 308 formed into an annular wall 310 of the container, extends circumferentially around the annular wall 310. At positions 312,314, the tear lines are arcuately turned down toward a bottom edge 320 of the wall 310. A recessed bottom wall 346 is provided. The tear lines 306, 308 extend downwardly into expanded tear lines 322, 324 diverging from each other. The tear lines 322, 324 then are turned downwardly into tear lines 326, 328 to the bottom edge 320 of the wall 310. The band 304 extends further outwardly of the bottom edge 320 with an overhanging portion 330. Thus, the overhanging portion 330 as well as the tear lines 322, 324, 326, 328 define a pull tab, easily gripped and manipulated for removing the band along the tear lines 326, 328, 322, 324, 306 and 304 around the partial circumference of the wall 310. The tear lines 306, 308 terminate at positions A, B, (not shown) in a fashion such as that shown in FIG. 3 or FIG. 7, or combination of the two methods. As with the other embodiments, residuals can be used optionally to increase the strength of the container 300, spaced intermittently along the tear lines.
FIG. 10 illustrates in a bottom view the tab 330 having on a back side thereof reinforcing gussets 340, 342, which are molded into a recess region 344 of the bottom wall 346.
From the foregoing, it will be observed that numerous modifications and variations can be effected without departing from the spirit and scope of the novel concept of the present invention. It is to be understood that no limitation with respect to the specific embodiments disclosed herein is intended or should be inferred. The disclosure is intended to cover by the appended claims all such modifications as fall within the scope of the claim.
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A closure includes a promotion piece holding container within a cap to be installed onto a container such as a bottle. The promotion piece receiving container includes a top flange captured by a lip of a seal installed within the cap. The promotion piece receiving container includes a frangible band extending circumferentially around a substantial circumference of the container. The container can include a bottom flange arranged for convenience gripping and removing of the container from the cap, and a pull tab attached to the frangible band to assist in removing the frangible band to open the container for removal of the promotion piece.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a manufacturing method of semiconductor devices. It is especially suitable for manufacturing non-volatile semiconductor memory devices.
2. Description of the Related Art
A memory cell transistor in a non-volatile semiconductor memory device (EPROM) hitherto has such a structure as shown in FIG. 1, for instance. A gate electrode portion 25 having a two-layer gate structure is formed on each of element regions of a semiconductor substrate (silicon substrate) 1. The gate electrode portion 25 has a first gate insulating film 3, a floating gate electrode 4, a second gate insulating film 5, a control gate electrode 6, and an insulating film 7, all of which are formed on a main surface of the semiconductor substrate 1. These elements are formed by successively placing one over another. The side walls of gate electrode portion 25 are covered with the insulating film 7. Those portions of the insulating film 7 that cover the side walls are formed by the side walls of the electrode 6 and the side walls of the electrode 4 being oxidized when the insulating film 7 is formed on the control gate electrode 6 by thermal oxidation. Impurity diffusion regions 14 and 16, which are respectively to be a source region and a drain region of a floating gate type MOS transistor, are formed in that portion of the substrate 1 that is below the gate electrode portion 25 with a channel region interposed between them. In the structure shown in FIG. 1, the impurity diffusion region 16 is commonly used by any two adjacent floating gate type MOS transistors (memory cell transistors). On the resultant structure an interlevel insulating film 21 is formed. The interlevel insulating film 21 has a plurality of contact holes 26 each at that portion that is above one of the impurity diffusion regions (the drain region 16, for instance). Metal wiring layers (aluminum wiring layers, for instance) 24 functioning as bit lines are formed over the interlevel insulating film 21 such that they contact through the contact holes 26 with the drain regions 16.
Note that, when manufacturing the above-mentioned EPROM, a field oxide film (not shown in the drawings) for element isolation is used as a reference for mask alignment. Therefore, a certain amount of margin must be allowed when mask alignment is performed to form contact holes, when the margin is not allowed, those portions of the insulating film 7 that cover the side walls of the gate electrode portion 25 may be removed by etching, and the aluminum wiring layers 24 and the control gate electrode 6, or the floating gate electrode 4, of the memory cell transistor may be short-circuited in a worst case.
Therefore, the above-mentioned conventional EPROM requires a margin between the gate electrode portion and the contact hole when mask alignment is performed. The amount of the margin is determined by the exposure system, etc. Therefore, the reduction of the space between memory cell transistors has a limit, which hinders cell miniaturization.
To solve the above problem, the present inventors had already proposed a semiconductor integrated circuit device and its manufacturing method, which realize reduction of the margin between the control gate electrode, or the floating gate electrode, and the contact hole when performing a mask alignment to make the contact hole, and promote miniaturization (Japanese Unexamined Publication No. 1-251761 corresponding to Japanese Patent Application No. 63-78980). One example of a semiconductor integrated circuit device in accordance with the above-identified application is shown in FIGS. 2A and 2B. FIG. 2A is a plan view showing a pattern, and FIG. 2B is a sectional view taken along an X-X' line of FIG. 2A for showing the sectional structure.
This semiconductor integrated circuit device comprises memory cell arrays, each having floating gate type MOS transistors. In each of the MOS transistors, a source region 14 and a drain region 16 are self-align formed with respect to a multilayer-structured pattern which is made of a floating gate electrode 4 and a control gate electrode 6. A gate electrode portion 25 has an insulating film 7 on its upper surface and an insulating film 11 on its side walls. A low concentration impurity diffusion region 15 is formed at that portion of the drain region 16 that is near the channel region. A conductive layer 19 made up of a low resistance material covers the surface of the drain region 16 and the surface of at least those portions of the insulating film 11 that are on the side walls of the gate electrode portions 25 and are located at the end of the region 16. An interlevel insulating film 21 is formed on the resultant structure. A contact hole 26 is formed in that portion of the interlevel insulating film 21 that is above the conductive layer 19. Metal wiring layers 24 are formed on the interlevel insulating film 21 and the conductive layer 19 within the contact hole 26, and the metal wiring layers 24 are electrically connected with the drain region 16.
The characteristic feature of the structure shown in FIGS. 2A and 2B is that the conductive layer 19 is interposed between the drain region 16 and the metal wiring layers 24. Namely, the conductive layer 19 protects the side walls of each gate electrode portion 25 when making the contact hole 26, so that the margin between the gate electrode portion 25 and the contact hole 26 can be made as small as possible. Therefore, miniaturization of the device can be promoted.
In the above structure, the field oxide film 2 for element isolation is discretely formed, as shown in FIG. 2A, so that the distance d between the end of the gate electrode portion 25 (the insulating films 7 and 11) and the end of the field oxide film 2 must be set carefully in consideration of the margin for mask alignment, or the width of the source region 14 will be narrow, when divergence in mask alignment occurs, and thus the element characteristics will be degraded.
As explained above, in the conventional semiconductor device manufacturing method, the margin between the gate electrode portion and the contact hole for the source or drain must be sufficiently allowed for mask alignment, so that the space between the memory cell transistors cannot be made narrow. If it is made narrow, the element characteristics will be degraded.
SUMMARY OF THE INVENTION
Therefore, the object of the present invention is to provide a semiconductor device manufacturing method which realizes a high integration without causing degradation in element characteristics.
Another object of the present invention is to provide a semiconductor device manufacturing method which realizes simplification in manufacturing steps.
These objects are achieved by a semiconductor device manufacturing method comprising:
a step of forming strip shaped first insulating films separately extending in parallel with each other over a surface of a semiconductor substrate of a first conductivity type;
a step of forming over the semiconductor substrate and the strip shaped first insulating films a plurality of stacked gate structures extending in parallel with each other and in perpendicular to the strip shaped first insulating films, each stacked gate structure including a second insulating film, a floating gate electrode, a third insulating film, a control gate electrode, a fourth insulating film, and an etching stop film having a slower etching speed than the fourth insulating film;
a step of self-align removing those portions of each of the first insulating films that are located between any two of the adjacent stacked gate structures extending in parallel with each other and are located above source forming regions with using one end side of each of the stacked gate structures as a part of a mask, so as to expose those portions of the semiconductor substrate that are located at the source forming regions;
a step of self-align introducing impurities of a second conductivity type into each of the source forming regions using the one end side of each of the stacked gate structures as a mask;
a step of forming fifth insulating films on the side wall portions of each of the stacked gate structures;
a step of self-align introducing impurities of the second conductivity type into each of drain forming regions using the other end side of each of the stacked gate structures;
a step of self-align exposing those portions of the semiconductor substrate that are located at the drain forming regions with using as parts of a mask the fifth insulating films each formed on the other end side of each of the stacked gate structures;
a step of forming conductive layers which contact with surfaces of the exposed drain regions and cover at least those parts of the fifth insulating films that are laid on the walls of the drain region side of each of any two adjacent stacked gate structures with one of the exposed drain regions being interposed between them;
a step of forming sixth insulating films on the resultant structure;
a step of making contact holes by selectively removing the sixth insulating films with using the conductive layers as stoppers; and
a step of forming wiring patterns on those portions of the sixth insulating films that include the contact holes.
The provision of the fourth insulating films and the etching stop films having much slower etching speeds than the fourth insulating films on the two layer gate structures makes it possible to simultaneously perform the step of selective removal of the first insulating films (the field oxide films) for the formation of the source regions and the step of self adjusted treatment for the formation of the drain contact portions. Therefore, the margins for mask alignment can be reduced without increasing manufacturing steps. As a result, both miniaturization and high integration can be easily achieved. In addition, since the field oxide films are formed as parallel strips, there is no fear that the width of each of the source regions becomes narrow to degrade the element characteristics due to the occurrence of divergence when mask alignment. Therefore, a semiconductor device manufacturing method is provided which realizes a high integration without incurring degradation in element characteristics, and simplifies manufacturing steps.
Additional objects and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate presently preferred embodiments of the invention, and together with the general description given above and the detailed description of the preferred embodiments given below, serve to explain the principles of the invention.
FIG. 1 is a sectional view showing the structure of a memory cell transistor of a conventional EPROM;
FIG. 2A is a plan view of the pattern showing the structure of the memory cell transistor of the conventional EPROM modified by the present inventors;
FIG. 2B is a sectional view taken along the X-X' line of the pattern shown in FIG. 2A;
FIGS. 3A to 3I are plan views showing patterns arranged in manufacturing step order for explaining a semiconductor device manufacturing method in accordance with a first embodiment of the present invention;
FIGS. 4A to 4I are respectively sectional views taken along the Z-Z' lines in the patterns shown in FIGS. 3A to 3I;
FIGS. 5A to 5H are respectively sectional views g taken along the Y-Y' lines in the patterns shown in FIGS. 3A to 3I;
FIGS. 6A to 6J and FIGS. 7A to 7I are sectional views arranged in manufacturing step order for explaining a semiconductor device manufacturing method in accordance with a second embodiment of the present invention; and
FIGS. 8A to 8I and FIGS. 9A to 9H are sectional views arranged in manufacturing step order for explaining a semiconductor device manufacturing method in accordance with a third embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Each set of FIGS. 3A to 3I, FIGS. 4A to 4I, and FIGS. 5A to 5H shows a series of EPROM manufacturing steps in order for explaining the semiconductor device manufacturing method in accordance with a first embodiment of the present invention. FIGS. 3A to 3I are plan views showing patterns obtained at the respective manufacturing steps. The next two sets of FIGS. 4A to 4I and FIGS. 5A to 5H respectively show sectional views taken along Z-Z' lines and sectional views taken along Y-Y' lines in the corresponding patterns in FIGS. 3A to 3I.
First of all, element isolation is performed, for instance, by forming on a surface of a P-type silicon substrate 1 a plurality of strip shaped field oxide films 2, as shown in FIG. 3A, using a known technique. Then, first gate insulating films 3 each having a thickness of about 200 Å are formed on the surface of the silicon substrate 1 using a thermal oxidation method, such that the field oxide films 2 and the first gate insulating films 3 are alternately arranged. After that, a first polycrystalline silicon layer 4 having a thickness of about 200 Å is deposited over the entire surface of the resultant structure using a vapor phase growing method. Impurities such as phosphorous are doped into the polycrystalline silicon layer 4 by an ion-implantation or thermal diffusion method with using POCl 3 as a diffusion source. Then, the polycrystalline silicon layer 4 is selectively removed for floating gate isolation using photoresists (FIG. 3B), and a second gate insulating film 5 having a thickness of about 300 Å is formed over the entire surface of the resultant structure. Then, a second polycrystalline silicon layer 6 is deposited on the second gate insulating film 5 using the vapor phase growing method, and phosphorous is doped into the second polycrystalline silicon layer 6 as an impurity material. A first insulating film 7 is deposited on the polycrystalline silicon layer 6, and a third polycrystalline silicon layer 8 having a thickness of about 100 Å is deposited over the entire surface of the insulating film 7 using the vapor phase growing method (FIGS. 4A and 5A).
As shown in FIGS. 3C, 4B and 5B, the third polycrystalline silicon layer 8, the first insulating film 7, the second polycrystalline silicon layer 6, the second gate insulating film 5, the remained first polycrystalline silicon layers 4, and the first gate insulating films 3 are selectively etched in succession by an anisotropic etching method using the resist patterns 9 as masks so as to form cell transistor regions and gate electrode regions.
Those portions of each of the strip shaped field oxide films 2 that are located at the source forming regions are selectively removed by a reactive ion etching method, which uses photoresist mask 10 which is aligned with reference to the patterns of the stacked gate structure, and thus those portions of the substrate 1 that are located at the source forming regions are exposed (FIGS. 3D, 4C and 5C).
Arsenic, for instance, is ion-implanted as an impurity into the source forming regions under a condition of 40 KeV in acceleration energy and 2×10 15 cm -2 in dose, while the drain forming regions are being covered with the photoresist mask 10. After the photoresist mask 10 is removed, the source forming regions are covered with photoresist mask not shown in the drawings, and then phosphorous, for instance, is ion-implanted as an impurity into the drain forming regions under a condition of 40 KeV in acceleration energy and 5×10 14 cm -2 to form low concentration impurity diffusion regions at the drain forming regions.
Then, a first CVD-SiO 2 film 11, for instance, is deposited on the resultant structure, and then is selectively etched by the reactive ion etching method, so that some portions of the SiO 2 film are left out on the side walls of each gate electrode portion, as shown in FIGS. 3E, 4D and 5D. After that, arsenic, for instance, is ion implanted-into the substrate 1 under the condition of 40 KeV in acceleration energy and 2×10 15 cm -2 in dose. Furthermore, silicon oxide films 12 and 13 are respectively formed on the surface of the source regions and that of the drain regions of the substrate 1. Note that both the ion implanted arsenic and phosphorous are diffused in this process, and high concentration impurity regions 14 are formed for the source regions, and low concentration impurity regions 15 and high concentration impurity regions 16 are formed for the drain regions. Thus, an LDD (Lightly Doped Drain) structure is obtained. Furthermore, the polycrystalline silicon layers 8 are oxidized to be silicon oxidation films 17 (FIGS. 4E and 5E).
The silicon oxide films 13 on the surfaces of the drain regions 16 are etched using a photoresist mask 18 (the obliquely lined portion in FIG. 3F) which is aligned with reference to the field oxide films 2. A fourth polycrystalline silicon layer 19 having a thickness of about 100 Å is deposited on the resultant structure by the vapor phase growing method as shown in FIGS. 4F and 5F. Then, impurities are doped into the fourth polycrystalline silicon layer 19, and each resist is made to have a pattern with making use of each gate electrode region as a reference of mask alignment so as to form each resist pattern 20 (obliquely lined portions), as shown in FIG. 3G. The fourth polycrystalline silicon layer 19 is etched with using the resist pattern 20 as a mask, so that each of the remained portions of the fourth polycrystalline silicon layer 19 covers both the surface of corresponding one of the drain regions 16 and the surfaces of corresponding two SiO 2 films 11 attached on the facing side walls of adjacent two gate electrodes with interposing the corresponding one of the drain regions 16 in between.
A second CVD-SiO 2 film 21, from which interlevel insulator is formed, is deposited on the resultant structure by a low pressure CVD (LPCVD) method. Then, a resist is made to have a pattern with using the gate electrodes as a reference of mask alignment so as to form a resist pattern 22 (obliquely lined portion in FIG. 3H). The resist pattern 22 is used as a mask while the remained portions of the fourth polycrystalline silicon layer 19 are used as a stopper to etch the SiO 2 film 21 as shown in FIGS. 4H and 5H. An aluminum layer, for instance, is deposited on the resultant structure by a spattering method, and a pattern of a resist is made with using a pattern of contact openings (namely, the etched pattern of the SiO 2 film 21) as a reference of alignment. The aluminum layer is etched with using resist pattern 23 (obliquely lined portion in FIG. 3I) as a mask so as to form a wiring pattern 24 as shown in FIG. 4I.
Now, the manufacturing process of drain-contact portions has just been explained, but source-contact portions are formed by a self-align contact hole forming method in the same manner. After both portions have been formed, passivation films and bonding pads are formed on the wiring pattern 24 by a known MOS integrated circuit manufacturing method, and a complete EPROM is made.
In the above manufacturing method, the polycrystalline silicon layer 8 is deposited, with the insulating film 7 interposed in between, on the two layer gate structure comprising the first gate oxide film 3, the floating gate electrode 4, the second gate insulating film 5, and the control gate electrode 6, so that the self-align etching process of the field oxide films 2 for the formation of the source regions and the self-align process for the formation of the drain-contact portions are simultaneously performed. Therefore, the margin for mask alignment can be made as narrow as possible without increasing manufacturing steps, and the miniaturization and the high integration become easy. Furthermore, since the field oxide films 2 are each formed to have a strip shape and are arranged in parallel with each other, the source forming regions will not be narrow even when the mask is misaligned, so that there is no fear that the circuit characteristics are degraded.
Note that the polycrystalline silicon layer 8, the upper most layer of each stacked gate structure, is completely made to be the silicon oxide film 17 by thermal oxidation in the first embodiment, as shown in FIGS. 4E and 5E. However, the polycrystalline silicon layer 8 need not be completely oxidized, but it may be possible to partially remain the polycrystalline silicon layer 8. Any material may be used as the layer 8, if only it has an etching selective ratio with respect to the side walls of the gate (in the above embodiment CVD-SiO 2 films 11), and there is no need to oxidize the material by the thermal oxidation.
The polycrystalline silicon is used as a low resistant conductive material for self-align forming the contact holes in the embodiment, but it is needless to say that the same effect can also be obtained by the other suitable conductive material.
In the above first embodiment, the introduction of high impurities into the drain regions 16 and the doping of impurities into the conductive layer 19 are performed in separate steps, but they can be performed at the same step.
Now, a second embodiment will be explained below with reference to FIGS. 6A to 6J and FIGS. 7A to 7I. The set of FIGS. 6A to 6J and the set of FIGS. 7A to 7I respectively show the sectional structure portions of the patterns shown in FIGS. 3A to 3I in manufacturing order, and they respectively correspond to the set of 4A to 4I and the set of FIGS. 5A to 5I.
First of all, element isolation is performed. Then, stacked gate structures, each comprising a first gate insulating film 3, a first polycrystalline silicon layer 4, a second gate insulating film 5, a second polycrystalline silicon layer 6, a first insulating film 7, and a third polycrystalline silicon layer 8, are formed within the element regions which are formed on a silicon substrate 1 by the element isolation. After that, those portions of each of strip shaped field oxide films 2 that are located at source forming regions are selectively removed by a reactive ion etching method so as to expose those portions of a silicon substrate 1 that are located at the source forming regions. Then, ion-implantation is performed, and insulating films 11 are formed on the side walls of each stacked gate structure (FIGS. 6A to 6D and FIGS. 7A to 7D). The second embodiment is the same as the first embodiment until this step.
The third polycrystalline silicon layer 8 formed on the upper most layer of each stacked gate structure is removed by etching, and arsenic, for instance, is ion-implanted into the substrate 1 under a condition of 40 KeV in acceleration energy and 2×10 15 cm -2 in dose, as shown in FIGS. 6E and 7E. When the polycrystalline silicon layers 8 are removed by etching, the surface of each source region and that of each drain region may be slightly etched, but diffusion layers having a good shape can be formed by the following ion-implantation.
Then, silicon oxide films 12 and 13 are respectively formed on the surface of each source forming region and the surface of each drain forming region of the substrate 1 by thermal oxidation. In this process, arsenic and phosphorous, which were implanted in the preceding ion-implantation steps, are diffused, and thus high concentration impurity regions 14 are formed for the source regions, and low concentration impurity regions 15 and high concentration impurity regions 16 are formed for the drain regions. In this manner, an LDD structure is formed.
Then, a fourth polycrystalline silicon layer 19 is formed and selectively removed to cover the drain-contact regions, an interlevel insulating film 21 is deposited and selectively removed to form contact holes, and a wiring pattern 24 is formed (FIGS. 6G to 6J and FIGS. 7G to 7I). These steps are the same as those of the first embodiment. The source-contact portions are formed in the same way. Then, passivation film and bonding pads are formed on the wiring pattern 24 to form an EPROM integrate circuit in accordance with the common MOS integrated circuit manufacturing method. These steps are also the same as those of the first embodiment.
The second embodiment also realizes that a self-align etching for the formation of the source regions and a self-align process for the formation of the drain-contact portions are easily performed with the use of two layers, i.e., the polycrystalline silicon layer 8 and the first insulating film 7.
Now, a third embodiment will be explained bellow with reference to FIGS. 8A to 8I and FIGS. 9A to 9H. The set of FIGS. 8A to 8I and the set of FIGS. 9A to 9H are sectional views corresponding to the set of FIGS. 4A to 4I and the set of FIGS. 5A to 5I, respectively.
The steps from element isolation till the formation of a stacked gate structure on each element region of a silicon substrate 1 (FIGS. 8A and 8B and FIGS. 9A and 9B) are the same as those of the first embodiment (FIGS. 4A and 4B and FIGS. 5A and 5B). Then, arsenic, for instance, is ion-implanted into drain forming regions under a condition of 40 KeV in acceleration energy and 5×10 14 cm -2 in dose. Then, the CVD-SiO 2 film 11 is deposited on the resultant structure, and is selectively etched by a reactive ion etching method so that portions of the SiO 2 film 11 are left on the side walls of each gate electrode portion, as shown in FIGS. 8C and 9C.
Then, a fourth polycrystalline silicon layer 19 having a thickness of about 100 Å is deposited on the resultant structure by a vapor phase growing method, as shown in FIGS. 8D and 9D. Impurities are doped into the fourth polycrystalline silicon layer 19. Then, the same patterns as those shown in FIG. 3G of the first embodiment are used with making use of the gate electrode portions as a reference for mask alignment to form resist patterns 20. The fourth polycrystalline silicon layer 19 is etched with making use of the resist patterns 20 (obliquely lined portion in FIG. 3G) as a mask. As a result, as shown in FIGS. 8E and 9E, each portion of the polycrystalline silicon layer 19 that covers both the surface of corresponding drain region and the surfaces of corresponding SiO 2 films attached on the facing side walls of the adjacent two gate electrodes with interposing the drain region in between. The polycrystalline silicon layer 8, or the upper most layer of each stacked gate structure, is also selectively etched for each cell.
With the use of photoresist mask 10, which is formed with using the gate electrode portions as a reference of mask alignment, the strip shaped field oxide films 2 are selectively removed by a reactive ion etching method in the same way as the first embodiment to expose those portions of the silicon substrate 1 that are located at the source forming regions. Note that, while this etching process is performed, those SiO 2 films 11 that are located at the source regions are removed from the side walls of the stacked gate structures (FIGS. 8F and 9F).
In the next step, arsenic, for instance, is ion-implanted into the exposed portions of the substrate 1 under a condition of 60 KeV in acceleration energy and 2×10 15 cm -2 in dose. A silicon oxide film 12 is formed on the surface of each source region of the substrate 1 by thermal oxidation, and a thermal oxide film 17 is formed on the surface of each stacked gate structure and the surface of each polycrystalline silicon layer 19 at the same time. Note that arsenic and phosphorous, both having been ion-implanted when the ion-implantation was performed, are diffused in this step so as to form highly concentrated impurity regions 14 for the source regions and low concentrated impurity regions 15 and highly concentrated impurity regions 16 for the drain regions. In this way, an LDD structure is obtained (FIGS. 8G and 9G).
The CVD-SiO 2 film 21, from which interlevel insulating films are formed, is deposited on the resultant structure by, for instance, an LPCVD method. Then, a resist is made to have a pattern with the use of the gate electrode portions as a reference of mask alignment, so as to form a resist pattern 22, in the same way as what is shown in FIG. 3H of the first embodiment (obliquely lined portion in FIG. 3H). With using the resist pattern 22 as a mask and the remaining portions of the fourth polycrystalline silicon layer 19 as a stopper, the SiO 2 film 21 is etched as shown in FIGS. 8H and 9H. Then, an aluminum layer is deposited on the resultant structure by a sputtering method, and a resist is made to have a pattern with making the contact hole pattern (namely, the etching pattern of the SiO 2 film 21) as the alignment reference. With the use of the resist pattern as a mask, the aluminum layer is etched to form a wiring pattern 24 as shown in FIG. 8I.
Then, source-contact portions are also formed by a self-align contact forming method, and passivation film and bonding pads are formed on the wiring pattern 24 by the known MOS integrated circuit manufacturing method, thereby forming an EPROM, which is the same as the first and second embodiments.
The manufacturing method in the third embodiment also realizes that the self-align etching for the formation of the source regions and the self-align process for the formation of the drain-contact portions are simultaneously performed, since the two layer films, consisting of an insulating film and a polycrystalline silicon film, are formed on the two layer gate structure. Therefore, the margin for mask alignment can be made narrow without increasing manufacturing steps, and miniaturization and high integration can be easily accomplished.
Note that, in the third embodiment, the remaining portions of the polycrystalline silicon layer 8 that are located just under the corresponding portions of the polycrystalline silicon layer 19 are partially etched out when the polycrystalline silicon layer 19 is selectively etched in a step shown in FIGS. 8E and 9E. However, the partially etched out region of each layer 8 may be completely removed when the polycrystalline silicon layer 19 is selectively etched. In such a case, the exposed portion of each insulating film 7 is removed by such an etching step that each strip shaped field oxide film 2 is selectively removed to expose the source regions (FIGS. 8F and 9F), and thus each polycrystalline silicon layer 6, which is to be a control electrode, will be partly exposed. However, the exposed portion of each layer 6 is covered through the steps of thermal oxidation and the deposition of the interlevel insulating film 21, so that insulation ability will be maintained.
The explanation was given to the examples of a manufacturing method of two layer structure memory transistor cell, but it is needless to say that the present invention can be applied to a manufacture of a MOS transistor having a one layer gate electrode.
As explained above, the present invention realizes that the step of selective removal of the field oxide film and the step of self-align process for the formation of the drain-contact portions are simultaneously performed due to the fact that two layer film, consisting of the insulating film and the polycrystalline silicon film, is formed on the two layer gate structure. Therefore, margin for mask alignment can be made as narrow as possible without increasing manufacturing steps, resulting in the ease in miniaturization and high integration. In addition, the provision of the parallel arranged strip shaped field oxide films prevents the source forming regions from being narrow in width even when masks are misaligned. Therefore, there is no fear of degradation in element characteristics.
Therefore, the present invention makes it possible to obtain a method of manufacturing a semiconductor which can be highly integrated without causing degradation in element characteristics and complexity in manufacturing steps.
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There is formed on a surface of a first conductivity type semiconductor substrate strip shaped first insulator separately extending in parallel with one another. A plurality of stacked gate structures, each comprising a second insulator, a floating gate, a third insulator, a control gate, a fourth insulator and an etching stopper having a slower etching speed than the fourth insulator, are formed on the substrate and the first insulator. Those portions of each first insulator that are located between the parallel extending gate structures and are present at prospective source regions are self-aligningly removed with using one end side of each gate structure as a part of a mask, so as to expose those portions of the substrate that are located at the prospective source regions. Impurities of a second conductivity type are self-aligningly introduced into each prospective source region with using one end side of each gate structure as a part of a mask to form a fifth insulator on a side wall of each gate structure. Impurities of the second conductivity type are self-aligningly introduced into each of prospective drain regions with using a drain side end of each gate structure as a part of a mask. Conductive layers are formed to contact with surfaces of the exposed drain regions and cover at least those parts of the fifth insulator that are laid on the walls at the drain regions of any two adjacent gate structures with corresponding one of the exposed drain regions between them. Sixth insulator is deposited on the resultant structure and are selectively removed with using the conductive layers as stoppers to make contact holes.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to position sensitive radial bypass damper (RBD) components that regulate gas/oil flow of an off road vehicle shock absorber. Such components may include a radial bypass damper housing, an anti-cavitation valve (ACV), and an incremental flow metering valve (IFMV).
[0002] Vehicle suspension undergoes dynamic movements as it negotiates obstacles generally found in off-road racing venues. Shocks are provided to control wheel movement by resistance in off-road vehicles with such suspension. Such resistance arises from pressure forming on the compression side of the working piston during the compression stroke and on the rebound side of the piston during the rebound stroke. The nitrogen chamber, separated from the hydraulic oil by a floating dividing piston, provides an opposing force on the said oil during the dynamic functions of the damper. Oil displacement and directional forces compress and expand the nitrogen chamber but can induce cavitation of the oil within the damper itself if the transient response of the dividing piston from positive force to negative force is delayed (hysteresis).
[0003] The radial bypass damper of a vehicle shock absorber uses hydraulic oil transfer to deflect valving shims that are located on both sides of the working piston. Foaming of the hydraulic oil, or cavitation, is inherent to the dynamics inside the radial bypass damper, but may be avoided with a nitrogen gas chamber of the reservoir. The life of the radial bypass damper is dependent on the longevity of the seals, wear bands, and the hydraulic oil itself. Preventing the damper from overheating is critical to avoid the break down of the hydraulic fluid and seals from excessive heat buildup caused by energy dissipation of the damper. However, conventional steel housings that typically have smooth tubing do not optimize their surface area for cooling and therefore the air flow past the damper is not utilized as well for dissipating the extreme heat generated from damping an off road vehicle's suspension movements.
[0004] It would be desirable to provide components for an off road vehicle shock absorber that are suited to promote improved thermal management, weight savings, adjustability, durability, and adaptability to changing conditions.
BRIEF SUMMARY OF THE INVENTION
[0005] One aspect of the invention is to provide a radial bypass damper useful in providing a shock absorption function that achieves a substantial reduction (1) in heat build up due to the use of a finned aluminum alloy housing, (2) in weight by as much as 25% over a conventional steel housing because of the aluminum alloy construction, and (3) in adverse wear characteristics on piston wear bands from distortions in the housing that arise due to welding external bypass tubes onto the housing. Such welding is avoided with the invention.
[0006] Such a radial bypass damper comprises an elongated housing with a main hole; at least one auxiliary hole spaced from the main hole, the main hole and the at least one auxiliary hole being elongated in a direction of elongation of the housing and being free from intersecting each other, the housing having an intervening housing material that is continuous and unbroken and arranged to space the main hole from the at least one auxiliary hole, the housing having an intersecting passageway extending between the main hole and the at least one auxiliary hole and not beyond the at least one auxiliary hole.
[0007] Another aspect of the invention resides in valving shims in the working piston and in an ACV that have continuous, inclined passages for hydraulic oil flow to prevent cavitation during sudden changes of directional travel of the working piston and to maintain positive pressure at the working piston. The ACV with such valving shims permits lower nitrogen gas pressure to prevent cavitation of the oil over that of conventional shock absorbers not equipped with a like ACV, yet reduces pressure generated at its piston rod. This effectively improves the performance of the shock absorber and increases positive feed back to the driver by reducing the harshness incurred by sharp increases in force when the shock absorber compresses over rough surfaces.
[0008] A further aspect resides in an IFMV that permits adjustments to the bypass of fluid at different points of up and down travel. Accurate adjustment is available without the need to visually see the index points, because of a detent ball assembly providing an audible “click” and feel at each setting.
[0009] Such an IFMV, comprises a valve housing having a passage for fluid flow through the valve housing, a piston configured to move in response to application of fluid forces toward and away from a position that closes the passage; and a flow regulating mechanism including a regulator arranged to regulate flow of fluid through the passage, the flow regulating mechanism including a plurality of selectable settings that are accessible from outside the valve housing and including a regulator movable to vary a dimension of at least a portion of the passage in accordance with a selected one of the selectable settings so as to provide a substantially linear variation in the flow of fluid through the passage as the regulator moves to a position corresponding to the selected one of the selectable settings, the flow regulating mechanism providing regulation of the flow of fluid through the passage substantially independent of movement of the piston as long as the piston is away from a position that closes the passage.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] For a better understanding of the present invention, reference is made to the following description and accompanying drawings, while the scope of the invention is set forth in the appended claims.
[0011] FIG. 1 is an isometric view of the shock absorber in accordance with the invention.
[0012] FIG. 2 is an isometric view of the radial damper housing of the shock absorber of FIG. 1 .
[0013] FIG. 3 is a schematic representation of the compression stroke of the working piston within the radial bypass damper, showing the relative flow within the correlating bypass.
[0014] FIG. 4 is a schematic representation of the compression stroke of the working piston within the radial bypass damper, showing the point at which the bypass function is no longer actuated.
[0015] FIG. 5 is an end view of the radial damper housing of FIG. 3 .
[0016] FIG. 6 is a transverse cross section midway along the radial damper housing of FIG. 3 .
[0017] FIGS. 7-10 are longitudinal cross sections of the radial damper housing of FIG. 2 across the main hole and respective ones of the auxiliary holes.
[0018] FIG. 11 is an end view as in FIG. 5 , but marked with notation for indicating the manufacturing procedure.
[0019] FIG. 12 is a longitudinal view taken across 12 - 12 of FIG. 11 and marked with notation for indicating the manufacturing procedure.
[0020] FIG. 13 is a schematic representation of a drilling procedure to form an interconnecting passageway in between main and auxiliary holes of the radial damper of FIG. 2 .
[0021] FIG. 14 is an isometric view of a drilling tool used in the drilling procedure of FIG. 13 .
[0022] FIG. 15 is a schematic representation of the shock absorber of FIG. 1 showing the flow direction during the compression (bump) stroke of the working piston, between the working piston, the hose and the ACV.
[0023] FIG. 16 is a schematic representation of the shock absorber of FIG. 1 showing the flow directions during the extension (rebound) stroke of the working piston, between the working piston, the hose and the ACV.
[0024] FIG. 17 is an isometric view of the ACV assembly installed in the reservoir end cap.
[0025] FIG. 18 is an isometric cutaway view midway across the ACV of FIG. 17 .
[0026] FIG. 19 is an isometric view of the rebound face of the ACV and washer of the valving shims of FIG. 17 .
[0027] FIG. 20 is an exploded view of the components of the working piston including valving shims.
[0028] FIG. 21 is a schematic representation of flow direction through the IFMV in place in an auxiliary hole of the radial damper housing.
[0029] FIG. 22 is a cross-section of a portion of an auxiliary hole of the radial damper housing into which is to be fitted the IFMV.
[0030] FIG. 23 is a side view of the IFMV that is represented schematically in FIG. 21 .
[0031] FIG. 24 is an isometric view of the IFMV of FIG. 23 .
[0032] FIG. 25 is a side view of the IFMV of FIG. 23 but with portions shown transparent that otherwise block portions underneath from view.
[0033] FIG. 26 is an exploded view of the components of the IFMV of FIG. 25 .
[0034] FIG. 27 is a graph of the force/velocity change at each of the settings of the IFMV of FIG. 23 .
DETAILED DESCRIPTION OF THE INVENTION
[0035] Off-road racing vehicles include those in a truck-race, buggy-race, lifted truck recreational, sand car-recreational, monster truck and military specialty vehicles. The function of the shock absorber 20 ( FIG. 1 ) of the invention is to permit such off road racing vehicles to pass over extremely rough terrain at high speeds with improved control and stability.
[0036] The shock absorber 20 includes a radial bypass damper housing 22 having a chamber in which moves a working piston and shaft 24 to effect compression and rebound strokes. A hose 26 connects the opposite end of the chamber with an oil gas reservoir 28 .
[0037] Turning to FIG. 2 , the radial bypass damper housing 22 is made of aluminum alloy and formed without welds. The housing of the radial bypass damper housing 22 may be formed from extruded 6061-T6 aluminum alloy that is manufactured in solid profile in fixed lengths. The profile of the radial bypass damper housing 22 incorporates cooling fins, which in turn offer substantially more surface area and material to disperse the heat during operation and direct airflow than smooth, un-finned surfaces.
[0038] When the invention was tested in operation, temperature indicators showed that the operating temperatures that are experienced are lower than when steel dampers are used. Also, higher vehicle speeds were attained than for other damper types installed on test vehicles on the same course. Inspection of components that are susceptible to wear showed improvement in reduced wear and reduced failure in long-term service over conventional dampers tested. Such performance gains signify the realization of serviceability and cost savings in operation during the life of the damper.
[0039] The fixed lengths are cut to suit installation for an off-road vehicle. The different lengths for longitudinal auxiliary holes (bypass passageways) 30 are cut to the appropriate dimensions. The longitudinal auxiliary holes 30 are machined into the solid parts by a gun-drilling procedure. The main hole (cylinder) 32 is precision bored.
[0040] FIGS. 3 and 4 show respectively the compression strokes of the working piston 24 within the main hole 32 of the radial bypass damper housing 22 . As best seen in FIGS. 5-10 , there are two longitudinal auxiliary holes (bypass passageways) 30 that allow the oil to bypass through the two longitudinal auxiliary holes depending upon the position of the working piston during the compression stroke with respect to the intersecting ports 34 . There is no bypass function performed by these two longitudinal auxiliary holes (bypass passageways) 30 during the rebound stroke. However, there are two other longitudinal auxiliary holes (bypass passageways) that provide bypass function during the rebound stroke depending upon the position of the working piston 24 during the rebound stroke with respect to the intersecting ports 34 . The longitudinal auxiliary holes 30 widen into a chamber 36 at an end and into which is to be inserted an IFMV.
[0041] As the working piston 24 travels towards the open intersecting ports 34 , the oil flows in the opposite direction, deflecting the piston of the IFMV 38 . The oil then flows through the IFMV 38 at a preset position and to the backside of the working piston 24 . This is the bypass function of the radial bypass damper housing 22 during the compression stroke. The location of the open intersecting ports varies and is reliant on the total stroke length of the working piston 24 within the radial bypass damper housing 22 .
[0042] When the working piston 24 covers the open-intersecting bypass port 34 , the bypass function becomes disengaged entirely. This is also true as the working piston 24 travels beyond the bypass port 34 . This same dynamic function is observed during the rebound stroke of the working piston 24 with the incremental metering flow valve 38 located at the opposite end of the bypass port, thereby governing the flow in the opposite direction from what is viewed in FIG. 4 .
[0043] During the rebound stroke, the incremental metering flow valve 38 sees equal pressure on both sides of its piston and will remain closed, or inactive. When the working piston 24 is beyond the bypass ports in its compression stroke, the valving found in the working piston 24 and the ACV 40 is governing flow/resistance in its entirety, thus no additional bypass is in use.
[0044] The radial bypass damper housing 22 of the invention preferably has no welds and the longitudinal auxiliary holes 30 and main hole 32 are manufactured precisely straight and true to provide longer wear band service life, less frictional resistance and reduced heat build up as compared to having external bypass tubes welded onto the housing. Such welding gives rise to unwanted distortions that create adverse wear characteristics on piston wear bands. After machining, the housing of the damper is preferably hard anodized to specification MIL-A-8625F Class 1, type III for corrosion and wear resistance.
[0045] The radial bypass damper housing 22 acts as a heat sink. It dissipates the heat built up from damping energy by transferring it outward through the surface area of the profile provided by the cooling fins 42 and external profile. Analogous to a radiator, airflow over the damper housing improves the cooling performance and stabilizes the temperature at a lower level for the duration of a race with the off-road vehicle. The rate of cooling has been tested and found to reduce peak temperatures by as much as 100 degrees F., which constitutes as much as a 33% reduction in temperature. Steel shock tubes under the same test conditions often reach peak temperatures of 325 degrees F. and above.
[0046] FIGS. 11 and 12 illustrate the steps in the manufacturing procedure for the radial bypass damper housing 22 . An aluminum alloy extrusion process is used, the steps of which are conventional for extruding aluminum alloy housings, albeit unique as it applied to the damper housing of the invention. A tool-die is made with the parts cross-sectional profile machined in its center. The outer features of the damper housing are incorporated in to the tool-die. The die is placed in a conventional extrusion apparatus and semi-molten aluminum alloy is forced through the die at high pressure and cooled upon exit to maintain the shape with minimal distortion over a 12′ length. The steps of manufacture are: 1. Initially solid profile of aluminum alloy is extruded, such as in 12 foot lengths. 2. The solid profile is cut to desired lengths, e.g., four different lengths. 3. The main hole (cylinder) is located, e.g., 3 inch diameter. 4. Radial bypass bosses are milled to length. 5. The longitudinal auxiliary hole centers are located. 6. The longitudinal auxiliary holes are gun drilled. 7. The main hole is precision bored and honed to specification. 8. Bypass counter bores and threading is made. 9. Main hole counter bores and threading is made. 10. Intersecting bypass ports are drilled. 11. Surface finish and cleanup are performed. 12. Hard anodized clear, MIL-A-86256, Class 1-Type III is conducted. 13. Logo is milled onto housing.
[0047] A drilling process ( FIG. 13 ) is performed from the inside of the radial bypass damper housing 22 outward through intervening walls 44 ( FIGS. 7-10 ). An appropriate drilling tool 52 ( FIG. 14 ) is used to perform a drilling process for forming intersecting passageways 34 between the main hole 32 and respective ones of the longitudinal auxiliary holes 30 . This drilling process is not from the outside inward through the exterior of the longitudinal auxiliary holes and thus eliminates the need for external plugs and potential seal failures that otherwise are present conventionally with steel tubes where the exterior of the longitudinal auxiliary holes are drilled into from the outside. Counter bores are made at the ends of the auxiliary holes and main hole to accommodate the insertion of further components, such as IFMVs.
[0048] Turning to FIGS. 15 and 16 , compression and rebound strokes of the working piston 24 and their effect on flow through valving shims of the ACV 40 ( FIG. 17 ) are depicted. Deflective disks (or valving shims) ( FIGS. 17, 18 ) that form a valve stack are used to tune the amount of flow/resistance in both compression and rebound strokes of a mono-tube damper. The shims are found primarily on the active/working piston 24 within the damper housing 22 ( FIG. 24 ), but may also be used in conjunction with a base valve/ACV ( FIGS. 15, 17 ). The greatest diameter shim found directly on the surface of the piston/base valve is called a cover disc and jointly acts as a check valve, governing oil flow in the opposite direction during the rebound or compression stroke of the damper.
[0049] Referring to FIGS. 17 and 18 , the ACV 40 is a tuning tool that permits far less gas pressure to achieve the task of preventing oil cavitation (foaming). An ACV 40 is more commonly associated with twin-tube shock design because it is fixed toward the base of the internal shock tube and generally is without a gas chamber. In mono-tube shock design, the location is much the same but with the option of moving it into a remote reservoir with the gas chamber and dividing piston.
[0050] The ACV 40 is stationary and located in the reservoir end cap between the floating piston, which separates a nitrogen gas chamber from the oil, and the working piston. Its function is not affected by either of the aforementioned locations. The base valve 40 enhances the effects of a damper's nitrogen chamber. The nitrogen gas chamber provides a reactive force on the hydraulic oil, and prevents cavitation of the oil. This is an inherent byproduct of flowing fluid past solid objects at high velocity, i.e. the working piston and valve shims. Cavitation is the sudden formation and collapse of low-pressure bubbles in liquids by means of mechanical forces, such as those resulting from propeller rotation.
[0051] The dividing piston will move relative to oil displacement caused by the piston rod plunging in or out of the damper, while maintaining force on the oil due to the nitrogen chambers ability to compress and expand. The side effect is that the gas pressure rises significantly as the chamber is reduced in size. This creates force on the piston rod effectively adding “spring rate”. In other words, the gas force wants to push the piston rod back out of the damper. This force is like a spring on a vehicle and can increase the resistance put upon the vehicles “sprung weight” and change the dynamics of the vehicles handling and feel. A sudden ramp-up of gas force when the piston rod displaces the oil can make a vehicle feel very harsh over rough terrain, effectively losing traction and “detaching” the driver from feedback through vehicle.
[0052] The ACV 40 is tuned to maintain pressure between the working piston and reservoir when the shock is in transition from compression to rebound strokes. It works with the nitrogen chamber to reduce the chance of cavitation during sudden changes of directional travel of the piston but with upwards of 175% less psi. Without the ACV 40 , the gas pressure must be set to 200-250 psi static to help the piston respond quickly to the rebound stroke. However, the inherent lag in transient response, or hysteresis, can cause an air pocket to form at the head of the working piston. Hysteresis is the lagging of a physical effect on a body behind its cause (as behind changed forces and conditions).
[0053] When the working piston 24 goes into its rebound stroke, the dividing piston must respond by changing direction as well. In other words, the gas pressure expands when the force changes from compression to extension. This is the dynamic point of action that can induce cavitation at the working piston. Without a quick response, an air pocket can form in the main damper cylinder, directly affecting the performance of the damper throughout the duration of a race or hard use. This air pocket is found in between the hose inlet and the working piston. With each stroke, the air pocket would continue to disperse to both sides of the working piston and bypass ports, causing what is called “fade”. The working piston 24 will lose its ability to generate the needed resistance to the dynamic motions of the vehicle and its suspension, allowing the tires to lose contact or allow the vehicle to bottom out it's suspension travel.
[0054] The ACV 40 is fixed in place by an internal retaining ring and permits easy servicing and tuning. The remote reservoir housing contains the gas chamber, which is separated from the hydraulic oil with a floating dividing piston. The ACV 40 reduces the required gas pressure by as much as 130-175% as compared to conventional products. As in the working piston 24 of the shock absorber, the ACV 40 uses valving shims to govern the flow of oil and maintain positive pressure at the working piston. Charge pressures are reduced from as much as 250 psi to a minimum of 50 psi, effectively reducing the gas spring force on the piston rod and therefore reducing measurable spring rate. The rod force of a shock absorber not equipped with the ACV 40 , charged to 200 psi, was measured at 338.32 lbf (1504.83 N) when compressed. The rod force of the same shock absorber equipped with the ACV 40 and charged to 60 psi was measured at 101.49 lbf (451.45 N). No performance lag (indicating cavitation) was observed when tested on a dynamometer.
[0055] Turning to FIG. 19 , the cover plate valving shim 58 has three compression ports 54 that are angled into a tuned valve stack, which is located on opposite side, as viewed. The cover plate valving shim 58 has six rebound ports 56 that allow the reverse flow through the ACV 40 to occur, only having to actuate a single lightly rated deflective shim. This shim 58 acts as a directional valve with minimal resistance to the flow of oil on rebound. The heavy washer 60 is shimmed a particular distance away from the cover shim and acts as a stop plate. A fastener 62 through the center of the valving shims keeps the valving shim assembly together. Only the required amount of deflection to allow maximum flow is needed and limiting the cover shim at that point reduces cycle fatigue.
[0056] Opposite from that of the working piston, the greater number of ports in the ACV 40 are utilized for the rebound stroke, and the lesser for compression. The ACV 40 must permit the dividing piston to react as quickly as possible during its rebound travel and therefore rebound force must be relieved effectively. In contrast, the compression ports of the ACV 40 are fewer and are restricted with a tuned valving stack, much like the working piston within the radial bypass damper. The intent being to prolong a built up force under compression stroke between the working piston and the ACV 40 .
[0057] Conventionally bypass dampers that are position sensitive include variable flow metering check valve assemblies. The off-road industry has used several variations of bullet style check valve pistons with contoured valve seat that are adjusted by a threaded stop-pin that limits the distance the piston can travel. The amount of flow is governed at this piston and its mating/sealing surface.
[0058] FIG. 20 shows some exemplary components of the working piston 24 , such as a nut 64 , washer 66 , valving shims 68 , wear band 70 , O-ring 72 , piston 74 , washer 76 , piston rod 78 , bearing spacer 80 , bearing cup seal 82 , internal retaining ring 84 , spherical bearing 86 and rod end 88 . The valving shims 68 may include the cover plate valving shim 58 of FIGS. 18-19 , except arranged in a reverse orientation in that more flow is needed during the compression stroke for regulation but flow may be restricted during the rebound stroke.
[0059] Turning to FIGS. 21 , 23 - 26 , the present invention encompasses an IFMV 38 for whose piston travel is not limited until maximum flow through the valve occurs. That is, its piston does not limit the regulation of flow at all. Instead, a flow regulating mechanism 90 is provided that includes a triangular port assembly located at one end of the bypass port to govern the flow bypass adjustments. The IFMV 38 is positioned within the cavity 36 ( FIG. 22 ) at an end of each of the longitudinal auxiliary holes 30 .
[0060] The triangular port assembly includes an opening 92 that is shaped like an isosceles triangle to allow for precise monitoring of the bypass. Two opposed triangular ports are machined into the valve housing, position diametrically across from each other. The flow regulating mechanism includes a flow regulator 94 that is rectangular in shape to sweep past the triangular shaped ports to create a linear change in the rate of flow, i.e. increase or decrease as applicable depending upon the unobstructed dimension through the triangular ports.
[0061] The actuation of the IFMV 38 is adjusted externally and has sure-indexing features 96 . The valve is a one-piece unit sealed with Buna O-rings that prevent oil from escaping and prevent dirt and water from entering. A spring-loaded detent ball 98 is arranged to provide and audible click and feel as it is moved along each of the selectable settings. The valve cannot be rotated beyond a ninety-two degree range due to internal features and each selectable setting is marked on the valve housing.
[0062] The valve has a hex head 100 that may be readily accessed with a wrench or socket to turn as desired. The regulator 92 moves in unison with the turning of the hex head 100 . Likewise, either the spring-loaded detent ball 98 or the selectable settings 96 move in unison with the turning of the hex head 100 as well. Thus, turning of the hex head 100 is accomplished with a single tool, even when the valve is not easily visible. Preferably, the valves are color coded for both bump (compression) and rebound (extension).
[0063] The check valve piston 102 has a contoured face that seats against a machined tapered surface and provides smooth, uninhibited flow of the hydraulic oil. All of the edges of the piston are rounded, thereby reducing cavitation as the oil flows past them. A linear coil spring 104 assists in returning the piston to its position against the sealing surface when flow changes direction. The pressure generated by the working piston governs how far the IFMV must travel to permit the flow of oil to bypass it without restriction. Bleed ports 106 are provided in the piston head to allow oil to flow out of the cavity between the internal bore of the IFMV piston 108 and the guide pin 110 , preventing hydraulic lock. This in turn allows the piston to reciprocate quickly and without delay.
[0064] Also shown in FIG. 25 are O-rings 112 , the valve housing 114 , and the socket head cap screw used to secure the IFMV into a pair of receiving screw holes 116 at the end of the longitudinal auxiliary holes 30 ( FIG. 5 )
[0065] Each radial bypass damper has four IFMV assemblies, two for bump (compression) and two for rebound (extension). The position of the assembly is dependent on the travel length of the radial bypass damper.
[0066] Each setting of the IFMV 38 changes the force/velocity, either positively or negatively, in a linear fashion. FIG. 27 shows a graph of the force/velocity change, which is indicative of the separation achieved with each setting on the rebound/bump stroke of the shock absorber.
[0067] While the foregoing description and drawings represent the preferred embodiments of the present invention, it will be understood that various changes and modifications may be made without departing from the scope of the present invention.
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Shock absorber components, such as a radial bypass damper, an anti-cavitation valve (ACV) and an incremental flow metering valve IFMV. The damper is of a continuous, unitary construction with a main hole and auxiliary holes interconnected by passageways. The ACV has openings that angle obliquely relative to entry surfaces of valving shims and extend at an incline continuously through the valving shims. The metering valve linearly regulates flow, substantially independent of piston displacement.
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BACKGROUND OF THE INVENTION
The invention is based on a fuel injection pump having a pump piston, an adjusting member the position of which determines the duration of the fuel variation effected by the pump piston, and a connecting line leading from the pump work chamber to a fuel withdrawal chamber, the cross section of the connecting line being adjustable by means of a throttle device in order to determine the injection quantity. In a known pump of this kind, the duration of fuel supply is determined by the adjusting member embodied as a governor slide, while the injection quantity is varied by an adjustable bypass throttle parallel to the injection nozzle. The supply duration is thus freely selectable, independently of the injection quantity. The variation of the injection quantity, at a predetermined supply duration, is brought about by the variable cross section of the bypass throttle, which is adjusted in turn, via a hydraulic servomotor and a differential-pressure regulating valve, until such time as the injection quantity per unit of time corresponds to the prespecified value of the differential-pressure valve. The supply duration is arbitrarily varied in accordance with the position of the gas pedal by varying the position of the slide. However, the entire quantity of fuel pumped over the duration of supply does not reach the injection valve. Some of it flows out via the adjustable bypass throttle. In this known fuel injection pump, however, there is no particular provision made for regulating the injection quantity during idling operation.
OBJECT AND SUMMARY OF THE INVENTION
The fuel injection pump according to the invention as further described hereinafter and finally claimed has the advantage over the prior art that, using simple means, it is possible to effect an rpm-dependent regulation of the injection quantity for idling given a long, freely selectable injection duration, in order to attain smooth and knock-free combustion during idling. Since during idling the rpm can be used as a standard for the injection quantity, then regulation of the injection quantity can be effected by detecting only the rpm and the position of the driving pedal; these two values together produce a signal of an electronic control unit for a pressure control device. The pressure control device, in turn, adjusts the throttle device in order to determine the injection quantity. The dependent claims disclose further developments of the fuel injection pump disclosed in the main claim.
The invention will be better understood and further objects and advantages thereof will become more apparent from the ensuing detailed description of a preferred embodiment take in conjunction with the drawing.
BRIEF DESCRIPTION OF THE DRAWING
The single FIGURE of the drawing illustrates an embodiment of the invention which is described in greater detail below.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the drawing, an internal combustion engine engine 1 is illustrated in simplified form. It is supplied with fuel in the conventional manner via injection valves 2 and injection lines 3 leading to these valves from an injection pump 4. In each of the injection lines 3, there is a relief valve 5 opening in the direction toward the injection valve 2. The injection pump 4, in the illustrated example, is a distributor injection pump having a pump piston 6, which in a manner known per se is caused by means not shown to reciprocate and simultaneously rotate counter to the force of a restoring spring. The pump piston 6 moves within a closed cylinder 7 and with one end face it defines a pump work chamber 8. During the supply stroke of the pump piston 6, the pump work chamber 8 communicates via a longitudinal conduit 9 in the pump piston 6 and via a radial bore 10 branching off from the longitudinal groove 9 and having an adjacent longitudinal distributor groove 11, with one of the injection lines 3 leading away from the cylinder 7. The injection lines 3 are distributed at a uniform distance from one another about the cylinder 7, corresponding in number to the number of engine cylinders to be supplied with fuel, and as a result of the rotational movement of the pump piston 6 they are connected one after another with the longitudinal distributor groove 11 in the coarse of the supply stroke.
During the intake stroke, the pump work chamber 8 of the pump 4 is supplied with fuel via longitudinal grooves disposed in the jacket face of the pump piston 6 and via a bore 14 formed in the pump housing.
The longitudinal conduit 9 of the pump piston 6 is embodied as a blind bore. It communicates with a relief conduit 15 in the form of a radial bore of the pump piston 6. The opening of the relief conduit is controlled by means of the upper edge of an annular slide 16 displaceably disposed on the pump piston 6. The position of the annular slide 16 is determined via a lever 17, which is capable of assuming a substantially constant position but can also be adjusted in accordance with selected operating parameters. For this purpose, there is a servomotor 18, which in the exemplary embodiment can be influenced by the signals of an electronic control unit 19. Depending upon the position of the annular slide 16, the relief conduit 15 may remain closed during the entire supply stroke of the pump piston 6. If on the other hand the annular slide 16 is set at a lower position, then the relief conduit 15 is opened up toward the end of the supply stroke, and the supply pressure in the pump work chamber 8 is reduced abruptly, because from this instant on the entire quantity of fuel then being pumped can flow out into a relief chamber 20, which in this case is the suction chamber of the pump.
From the relief chamber 20, the pump work chamber 8 is supplied with fuel via the bore 14. A connecting line 21 which cannot be closed by the pump piston 6 also begins at the pump work chamber 8 and discharges into a fuel supply container 36. A throttle device embodied as a piston slide 22 is provided in the connecting line 21 following its outlet from the pump work chamber 8. The piston slide 22 is disposed in a cylinder 23, and with one end face 24 it defines a control chamber 25. The other end face 26 is engaged by a compression spring 27, which is supported in a relief chamber 28 of the cylinder 23. The piston slide 22 has an annular groove 29, which overlaps the outlet opening 30 of the connecting line 21 from the cylinder 23, while the inlet opening 31 of the connecting line 21 into the cylinder 23 can be sealed off from the outlet opening 30 by a control edge 32 of the annular groove 29. Depending upon the position of the piston slide 22, the inlet opening 31 is closed by the piston slide 22, or else a cross section of greater or lesser size is opened up between the inlet opening 31 and the annular groove 29. In the section between the outlet opening 30 and the fuel supply container 36 of the connecting line 21, there is a check valve 33 opening toward the fuel supply container 36. The relieved side of the check valve 33 is connected with the relief chamber 28 of the cylinder 23. The piston slide 22 has a longitudinal bore 34 passing all the way through it, and a first throttle restriction 35 is embodied in the longitudinal bore 34 near its point of discharge into the control chamber 25.
The injection pump 4 is supplied with fuel from the fuel supply container 36 via a fuel supply line 37 in which a fuel supply pump 38 is disposed. To this end, the fuel supply line 37 discharges into the suction chamber 20 of the injection pump 4. A fuel filter 39 is disposed if needed in the fuel supply line 37, between the fuel supply pump 38 and the suction chamber 20. A line 41 provided with an overflow throttle 40 leads back to the fuel supply container 36 from the suction chamber 20 of the injection pump 4. With the overflow throttle 40, it is possible to attain a desired, substantially constant, fuel supply pressure in the suction chamber 20 of the injection pump 4; this pressure can also be further influenced in accordance with selected operating parameters, such as the air pressure or the temperature.
A control line 42 leads from the suction chamber 20 to the control chamber 25 on the piston slide 22. A second throttle restriction 43 is embodied in the control line 42. The suction chamber 20, which is under substantially constant pressure, and the second throttle restriction 43 represent the pressure source for a subsequent pressure control device 44, by which in turn the piston slide 22 of the throttle device in the connecting line 21 between the pump work chamber 8 and the fuel supply container 36 can be adjusted, and by which the injection quantity can thus also be determined by regulating the throttle cross sections 29, 31, 32 in the connecting line 21.
The pressure control device is embodied, in the exemplary embodiment, as a magnetic valve 44, the adjusting member 45 of which is controllable by means of signals of the electronic control unit 19. Serving as a feedback signal for the correct supply quantity during idling is the idling rpm n, which reaches the electronic control unit 19 from a transducer 46. The electronic control unit 19 is also influenced by the position of the gas pedal 47, so as to make the influence of rpm on the control unit 19 effective only during idling.
The piston slide 22 of the throttle device is also provided with a transverse bore 48, which discharges into a leakage groove 49 on the circumference of the piston slide 22. Fuel flowing into the cylinder 23 between the annular groove 29 and the control chamber 25 can thus pass from the circumference of the control slide 22 via the longitudinal bore 34 to the relief chamber 28, without undesirably affecting the pressure of the fuel in the control chamber 25.
For starting of the engine, it must be assured that the entire quantity of fuel pumped into the pump work chamber 8 will reach the injection valves 2 via the associated injection lines 3. The annular slide 16 is kept by the servomotor 18 in the full-load position, in which the relief conduit 15 is closed. The inlet and outlet openings 31 and 30, respectively, in the cylinder 23 of the throttle device and the annular groove 29 of the piston slide 22 having the control edge 32 are furthermore so embodied that upon engine starting, the inlet opening 31 is closed by the piston slide 22, and thus the second outlet of the pump work chamber 8, that is, the connecting line 21, is also closed.
Since in the described fuel injection pump the duration of injection is determined by the position of the annular slide 16, the maximum prolongation of the duration of injection is attained by positioning the annular slide 16 in the full-load position. This position of the annular slide is also maintained during idling. The injection quantity is then determined by the rpm. The transducer 46 detects the idling rpm, as a result of which a corresponding signal is emitted by the electronic control unit 19 to the pressure control device embodied as a magnetic valve 44, 45. From the suction chamber 20, which is under substantially constant pressure, and through the second throttle restriction 43 inserted into the control line 42, fuel flows at a predetermined pressure to the magnetic valve 44, 45. In accordance with the signals at the magnetic valve 44, 45, which are derived from the idling rpm, the pressure in the portion of the control line 42 leading downstream of the magnetic valve 44, 45 to the control chamber 24 is adjusted. A control pressure for the piston slide 22 thus builds up in the control chamber 25 and thus ahead of the first throttle restriction 35. The piston slide 22, acting as a bypass, opens the connecting line 21 from the pump work chamber 8 to the fuel supply container 36. As a result, a portion of the fuel quantity pumped into the pump work chamber 8 is diverted. Only the injection quantity required for the idling rpm still flows from the pump work chamber 8 via the longitudinal conduit 9, the radial bores 10 having the longitudinal distributor grooves 11, and the associated injection lines 3 to reach the respective injection valves 2.
In order to keep the injection quantity required for idling constant, the piston slide 22 and thus the throttle cross section between the inlet opening 31 of the connecting line 21 in the cylinder 23 and the annular groove 29 of the piston slide 22 having the control edge 32 are variable. This is effected by means of feedback signals of the idling rpm via the control unit 19 and the pressure control device 44 and by means of corresponding pressure forces which are exerted, counter to the force of the compression spring 27 in the control chamber 28, upon the piston slide 22.
To this end, the opening time of the magnetic valves 44, 45 is designed such that with a slight quantity of fuel diverted from the suction chamber 20, in accordance with the two throttle restrictions 43 and 35 and the force of the compression spring 27, the pressure required for positioning the piston slide 22 is built up in the control chamber 25, this position of the piston slide 22 being that at which the throttle slit 31, 29, 32 has the cross section necessary for the "bypass quantity" to be diverted from the pump work chamber 8, and in which only the injection quantity sufficient for idling reaches the injection valves 2.
In the unbalanced state, i.e. non-equal pressures, of the quantity regulating device which comprises the pressure control device 44, 45 and the adjusting piston 22 as a throttle device, the adjusting piston 22 is adjusted, because of a pressure change in the control chamber 25 dictated by the rpm-dependent control of the magnetic valve 44, 45 until such time as the quantity of fuel corresponding to the desired idling rpm flows out via the throttle opening 31, 29, 32 into the connecting line 21, and the idling rpm thus corresponds to the prespecified value.
The two throttle restrictions 35 and 43 are designed such that the pressure buildup and pressure reduction are effected in the same length of time. The check valve 33 disposed in the connecting line 21 between the throttle device 22 and the fuel supply container 36 assures that a shift in injection onset is prevented. Its valve spring exerts a sufficiently great force in the closing direction, as a result of which a high pressure level is established between the throttle restriction 31, 29, 32 and the check valve 33. As a result, fuel is not capable of escaping continuously from the pump work chamber 8 through the connecting line 21 during the supply stroke, which would otherwise result in the undesired shift in injection onset.
In order to obtain the most compact possible apparatus, with short pressure lines, the throttle device 22 and the magnetic valve 44, 45 are disposed by way of example on the top of the housing of the injection pump 4. The throttle device 22 is screwed into the top, while the magnetic valve 44, 45 is seated in a flange secured to the top.
The substantial advantages of the fuel injection pump operated in the manner described above is that a constant supply stroke can be maintained, and thus despite minimal injection quantities--that is, such quantities of fuel as are sufficient for idling--a very long duration of injection is attained. As a result, a substantial reduction in combustion noise in Diesel engines during idling is also attained.
The foregoing relates to a preferred exemplary embodiment of the invention, it being understood that other embodiments and variants thereof are possible within the spirit and scope of the invention, the latter being defined by the appended claims.
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A fuel injection pump is proposed, based on a fuel injection pump of a known type, which has an adjusting member for determining the injection duration and is provided with a throttle device for determining the effective supply stroke of the pump piston. In accordance with the invention it is proposed that the position of the throttle device be varied by means of a pressure control device, which is controllable by signals of an rpm-dependent electronic control unit. The position of the adjusting member determining the duration of injection remains as constant as possible, while the throttle device adjusts the flowthrough cross section of a connecting line leading from the pump work chamber to a fuel withdrawal chamber in accordance with rpm. Thus it is possible, in particular given the small injection quantities required during idling, to effect a uniformly small injection quantity per unit of time during a relatively long injection duration; this results in a substantial reduction in noise.
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TECHNICAL FIELD
[0001] The present invention relates to the automated processing of images, in particular to the scanning and processing of images of mail pieces to decode address and other information.
BACKGROUND OF THE INVENTION
[0002] Current state-of-the art postal address processing normally acquires address information appearing on mail pieces in electronically captured binary form. This information is then used by automated mail sorting equipment and processing systems to sort the mail based upon the captured destination information. In these systems, scanners of various types are used to capture an image of one or more surfaces of a mail piece. The image is then analyzed using automated or human-aided systems such as optical character recognition (OCR), a bar code reader (BCR), specialized video processing systems, image processing systems, forms readers, forms video processing, and video coding systems. Allen et al. U.S. Pat. No. 5,422,821 describes one such system wherein mail piece addresses and bar codes are scanned and checked against a forwarding address database so that forwarding to the new address can occur without first sending the mail piece to the old address. Other systems only use bar code readers, acquiring destination information from bar codes previously applied to the mail pieces.
[0003] U.S. Pat. No. 5,311,999 describes a tunnel scanner for packages wherein image data for different sides of the parcel is taken in a rough scan, and then a fine scan is made of one of the sides based on operator recognition of a split screen display of all the scanned images, e.g., the one with the writing on it is chosen. The operator, using a touch screen, mouse or similar device, chooses the partial image. In an alternative automated embodiment, six images obtained from the rough scan are examined for regions, which coincide in a selection of features with the model of an address sticker, or an address region on a package. Features of this type are, for example, the color contrast of an area compared to its surroundings, the gray value contrast of an area compared to its surroundings, the shape of this area, the type and number of dark regions within the area, its location with respect to other distinct objects and with respect to the outline of the package.
[0004] According to known image recognition methods, the image most likely containing an address region is selected automatically from the images obtained by rough scanning, whereupon this region is subjected to fine scanning. The images may also already be supplied to an automatic character recognition device. Fine scan processing then takes place only if the images obtained by rough scanning are selected by the region of interest selection device. Rough scanning may be also be done by extracting a down sampled rough image from a fine (high resolution) scan.
[0005] Conventional scanning methods rely on a number of techniques for identifying and decoding possible regions of interest on a scanned mail piece. According to one such system, the overall image is subdivided into a 3-by-3 array of nine areas. Each area has a predetermined probability associated with it that any written matter found within the area will be an address. The center area may be assigned the highest probability. Current software also checks written matter in each region to determine whether it forms lines, is text justified, uses a single (common) font, and whether the matter is a bar code. All of these factors are considered in determining whether an address or other specific type of identification has been found. For purposes of performing several different kinds of analysis (e.g., OCR) simultaneously, it is preferred to send the initial scan results to more than one computer or processor.
[0006] Scanning systems of the kind used to read mail can also be used to read forms, such as postal change of address forms. According to current United States Postal Service (USPS) procedures, a person wishing to have the USPS forward mail to a new address submits a Change of Address (COA) Order Form (Form 3575) that requests mail forwarding. This form is normally completed by hand-printing the requested information including name, old address, new address, whether the move is for a family or individual, effective date and duration of the change on the form and submitting the form to a local post office. Commonly-assigned U.S. patent application Ser. No. 09/534,182, filed Mar. 24, 2000, the contents of which are hereby incorporated by reference herein for all purposes, provides a process for handling such forms wherein it is necessary to transmit the image from the computer associated with the scanner to a second computer which is used to analyze (decode) the image. The images are generally transmitted through a network or other data communication line.
[0007] For purposes of both mail pieces and form processing, the read rate of the scanning system should be as high as possible. Systems such as MLOCR (multiline optical character readers) and bar code scanners are incorporated into postal sorting machines now in use such as DIOSS (delivery bar code sorter/optical character reader/input subsystem/output subsystem) machines and DBCS (delivery bar code sorter) machines. These systems achieve read rates as high as 80%. However, the unreadable mail must be diverted and sent to video coding, where a human operator reviews an image of the mail piece and keys in the corrected address so that the corresponding zip+4 postal bar code can be printed on the mail piece. This manual review process is laborious and expensive, and it has been estimated that a 1% improvement in read rate corresponds to a savings of 9.5 million dollars per day. The present invention provides a system and method that can significantly improve the OCR and bar code scanning success rate in postal operations and potentially in other environments.
SUMMARY OF THE INVENTION
[0008] The invention provides a method of processing an image containing written information include the steps of:
[0009] (a) scanning a surface of an object to obtain an image of the surface represented by first image data;
[0010] (b) creating second image data of the image of the surface, the second image data having a lower data density than the first image data;
[0011] (c) analyzing the second image data with first image analysis logic to decode the written information; and
[0012] (d) if the written information cannot be decoded to a desired extent from the second image data, analyzing the first image data with second image analysis logic different from the first image analysis logic to decode the written information. As used herein the term “written information” includes alphanumeric characters, bar codes and other machine readable indicia including handwritten information, printed information, and information encoded onto the surface of an article such as a mail piece using similar techniques. Steps (a) and (b) preferably use a single scanning device to create the high data density image (e.g., color or grayscale) from which the lower data density image (e.g., binary or black and white) can then be created. However, in a variant of this method, the two images could be created from separate scans. “Data density” in this case refers to the well-known differences in total bytes per unit size between like images saved in different graphics formats.
[0013] The method of the invention is typically practiced on mail pieces such as letters or flats that are passing through a postal sorting machine at a high feed rate. Thus, steps (a)-(d) are typically carried out for a succession of images, and a buffer is maintained containing the second image data for a number of consecutive images so that the second image data is maintained in the buffer during step (c). The computer memory buffer is then accessed when necessary to obtain the image for processing in step (d). The postal sorting machine may use a bar code scanner (BCS), an optical character recognition (OCR) scanner, or both, and the method of the invention can be adapted to the scan type and the make-up of the incoming mail in a number of ways.
[0014] In the case of mail pieces, the goal is to determine the destination address of the mail piece so that the mail piece can be sorted or otherwise processed accordingly. The preferred destination reflected in the postal bar code is a zip+4 postal bar code, although other levels of specificity could be chosen, e.g., just the basic 5 digit zip code. For a sorter equipped with bar code scanning capability only, the scanned image is analyzed to read the bar code, and if a valid destination address is identified, the mail piece passes through the system with no further processing and is sorted based on the result. If the mail piece has a postal bar code thereon which cannot be decoded, the first image data is then analyzed to make a second attempt at decoding. If the first image data is successfully decoded before the mail piece reaches an essential decision point downstream, usually the first diverter gate, then the mail piece is sorted based on the second decoding attempt. However, many bar code sorting machines provide a relatively short conveyor path distance between the scanner and the first diverter gate, allowing insufficient time for the second decoding attempt to run to completion. In such a case, the mail piece is sorted to a reject bin. Later, the correct zip code is determined either by re-feeding the mail piece to a machine capable of applying an ID tag and associating it with a video image, or through video coding by a human operator. An ID labeled mail piece can be fed into an input/output subsystem that reads the ID tag, finds the result and labels the mail piece with the correct bar code, so that it can be sorted in a normal manner when re-fed into a sorting machine. In the alternative, a sorter can be programmed to read the ID tag, obtain the result of offline processing such as video coding, and sort the mail piece by reference to the result without need for relabeling the mail piece with the correct bar code.
[0015] The method of the invention proceeds along similar lines when the machine uses optical character recognition to read mail pieces lacking bar codes, except that the first and second image data represent alphanumeric characters. In this instance, the items being processed may be something other than mail pieces, for example, forms that are being scanned such as change of address forms as mentioned in Allen et al. U.S. Pat. No. 5,422,821 and Bruce et al. U.S. Patent Publication 2002/0168090, Nov. 14, 2002. OCR-based sorters are often provided with bar code printers and have a greater transport path length that BCR machines. As a result, upon successful resolution of the address by means of optical character recognition, a postal bar code can be applied to the mail piece before it is sorted. This bar code will often be used in later, downstream sorting processes.
[0016] The method of the invention can also be applied to mail processing machines such as DIOSS having both bar code and OCR capabilities. The mail incoming to such a machine may be entirely pre-bar coded, or may be a mix of bar coded and un-bar coded mail pieces. According to a preferred method of the invention, where the mail pieces include both mail pieces with both alphanumeric address and postal bar code information thereon, and mail pieces with alphanumeric address information lacking a postal bar code, steps (c) and (d) preferably further comprise:
[0017] determining if a mail piece has a postal bar code thereon;
[0018] if the mail piece has a postal bar code thereon, analyzing the second image data to decode the postal bar code;
[0019] if the decoded bar code identifies a destination address, ending the method as to such mail piece;
[0020] if the decoded postal bar code does not identify a destination address, analyzing the first image data to decode the postal bar code;
[0021] if the mail piece lacks a postal bar code that identifies a destination address, or has a postal bar code thereon which cannot be decoded from either the first or second image data, then analyzing the second image data to read a postal address from alphanumeric address data using optical character recognition;
[0022] if the decoded alphanumeric address data identifies a destination address, ending the method as to such mail piece;
[0023] if the decoded alphanumeric address data does not identify a destination address, analyzing the first image data to decode the destination address; and
[0024] if the mail piece has alphanumeric address data that cannot be decoded from either the first or second image data, then optionally diverting the mail piece for human review.
[0025] According to this aspect of the invention, four computer-implemented attempts may be made at decoding either the bar code and the written address on the mail piece. As in the OCR embodiment discussed above, it may be possible to complete secondary processing using the first image data on the bar code or address or both before the associated mail piece reaches the first downstream decision point in a sorting process. In such a case, the mail piece may be sorted based on the decoded bar code, the decoded address, or an arbitrated result. Such an arbitrated result is determined by software comparing the results obtained from the decoded bar code and the decoded address and deciding which to base the sorting decision on, or whether a result derived in part from each represents the correct destination. If the bar code is only readable to five digits, for example, the hand written address may provide enough information to derive the remaining digits from a computerized table of 9-digit zip codes. In another case, the bar code may be readable but in conflict with the written address, in which case a decision is made, based on past experience, whether to sort on the basis of the zip code or the written address.
[0026] At each stage where decoding is attempted, the computer-implemented method must be programmed to decide whether it will end the method based on an apparent successful result, or continue processing. Normally a bar code than scans on the first try (based on the second data, typically binary) is highly reliable, and therefore upon a successful first attempt at decoding the bar code, all other decoding for that mail piece is terminated. On the other hand, as to a bar code that failed to decode on the first try but was decoded on a second attempt using the first data (e.g., grayscale), it may be preferred to await the outcome of OCR processing and compare the results before reaching a decision.
[0027] The decoding of bar code and address results above may be carried out either in series or in parallel, in any desired order. The specific procedure will depend in part on the length of the sorter path (if the method is being used on a sorter) and the computing resources available, which will determine how rapidly a result can obtained. For example, bar code processing and OCR processing may be initiated at the same time and carried out in parallel as described in U.S. Provisional Application No. 60/436,339, filed Dec. 24, 2002, the entire contents of which are incorporated by reference herein. In the alternative, it may be desired to complete bar code processing before OCR processing commences, since it the case of pre-bar coded mail, the decision will most often be made based on the bar code.
[0028] If no destination address can be determined from either a postal bar code or a postal address read using the second image data, the mail piece is diverted for video coding. This preferably involves saving at least one of the first and second image data, marking the mail piece with an identification code, and then diverting the mail piece for holding until video coding is completed. The data saved is preferably the first data, e.g. grayscale or color, which will give the operator the best chance to see the address image.
[0029] The invention further provides computerized systems for implementing the foregoing methods, as described hereafter. These and other aspects of the invention are further described and discussed in the detailed description, which follows.
BRIEF DESCRIPTION OF THE DRAWING
[0030] In the accompanying drawing, wherein like numerals represent the same or similar elements throughout:
[0031] [0031]FIG. 1 is a schematic diagram of a prior art system for scanning mail pieces; and
[0032] [0032]FIG. 2 is a schematic diagram of a system for scanning mail pieces according to the invention; and
[0033] [0033]FIG. 3 is a flow chart of logic according to one embodiment of the invention.
DETAILED DESCRIPTION
[0034] This invention provides a novel method to improve the determination of addresses and other information contained on mail items and documents where multiple recognition processes (OCR and bar code) are being performed in parallel or in sequence and are unable to completely resolve the data on the mail item or document. The invention does so by adding an image buffering system that holds the image until traditional image processing techniques run to completion. As the following example shows, the invention enables the performance of existing mail processing systems to be improved without requiring major changes to the existing processes. This is especially important where disruption causes loss of productivity and has economic impact.
[0035] As shown in FIG. 1, the current state-of-the art deployed postal address processing system 1 (DIOSS, DBCS-OCR, or MLOCR) either decodes a pre-printed bar code or performs OCR image processing (limited to a binarized image), depending upon the mode in which the machine is operating. In the OCR mode of operation, a gray scale or color image may be captured by the imaging camera system of system 1 . Often bandwidth limitations or the speed of hardware deployed a number of years ago require that the image be binarized prior to being processed by system 1 , by itself or in parallel with additional computers 2 and 3 known in the art as USPS coprocessor 2 and remote computer reader (RCR) 3 .
[0036] These binarized images are then processed. A certain fraction of the images cannot be resolved due to the quality of the binarized image. Whenever the binarized image is not resolved to the finest level required to process the mail item through the automated processes, the resultant reject image from the automated system 1 is sent to an image storage and transfer processor 4 , then transferred to an image processing sub-system 5 , and then sent to a video coding station at which a human operator reviews the binarized image and can often resolve it and determine a zip code. The rejected mail is then re-run on an output sub-system (OSS) 7 to apply the correct bar code for the determined zip code.
[0037] Another method of operation for this equipment is to operate in a bar code only mode. In this method of operation, the OCR functions and image lifter are turned off (or not present), and only a bar code reader is used to determine the address zip code and the resultant sorting of mail. Alternatively, the OCR and image lift function may be optimized to process only bar coded mail items. When the bar code recognition function does not successfully determine a bar code from the pre-printed bar code, the item is rejected and the physical item must then be re-run on an OCR capable mail processing system as discussed above.
[0038] This invention provides a cost effective method to process the full gray scale or color image by adding an image buffering computer or other device to the camera output which buffers sufficient images to permit the traditional automated recognition process to continue until the process or multiple processes (e.g., OCR or BCR) have run to completion. At the completion of the automated recognition process, but before the binarized image is transmitted to the human operator for keying, feedback is sent to the image buffering computer that a specific process has not resulted in a bar code or address recognition. The full gray scale or color image is then conveyed to an appropriate automated recognition process where more robust algorithms are invoked to resolve the image. This intermediate process provides enhanced image processing which resolves many more mail items that cannot be finalized by the traditional binarized process, and permits other data on the mail item to be processed for value added purposes. Data routinely placed on mail items such as the return address, postal and non-postal bar codes indicating special services, such as certified or registered mail, tracking codes and other corporate endorsements such as internal distribution codes, or indicia patterns can be detected by special software routines loaded into this single process. This provides a postal service or commercial mail processor with a simple method to process these codes and markings without changing all the other OCR processes that they may have.
[0039] Any images for which processing of the gray scale or color image cannot make the final determination are released for viewing by a human operator in any of the various binary, grayscale or color methods that are readily available. In this manner, selective use of grayscale or color images stored in a rolling buffer to increase the number of successful machine decodes reduces the cost of image processing as well as maximizes the opportunity for an automated solution thru the use of optical character recognition (OCR), bar code readers (BCR), specialized video processing systems, image processing systems, forms readers, forms video processing, video coding systems and/or any combination thereof.
[0040] Turning to FIG. 2, an embodiment of a system of the invention includes a Delivery Bar Code Sorter Input Output Subsystem (DIOSS) 1 through which a stream of mail pieces is processed for sorting. DIOSS has both bar code and optical character readers and a printer for applying a POSTNET bar code identifier to mail pieces. The incoming mail to DIOSS 1 may be one of several types. Some mail pieces will have mailer-prepared delivery point bar codes on them. In such a case, the bar code is scanned by the bar code scanner of the system, and if successfully read, the mail piece is sorted according to the bar code. If the bar code is missing or unreadable, then an image of the address taken by the OCR scanner is used to determine the destination address, and if successful, the mail piece is sorted according to the result.
[0041] Prior to sorting, a POSTNET bar code is most often applied to the scanned mail piece. As is known in the art, when the machine is running in OCR mode, the OCR image is read, an address determined, a POSTNET code determined and then, before the mail gets to the bar code reader, a POSTNET code is sprayed onto the mail piece. The bar code reader reads the bar coded zip code, and then a sort decision is made. The mail piece can then be run on any other machine anywhere and be sorted properly. A second printer is provided to spray on the reverse side of a mail piece an identification tag code. The ID tag is printed when no address can be determined by an OCR machine. The image associated with this tag is sent off for video coding or further processing, then the ZIP code results are linked to the ID tag in a database. At a later time when this mail piece is run, the ID tag is read, and the results are looked up, sent to the machine in real time and the mail piece is then sorted. In some cases, no POSTNET code is printed from this lookup, but in others a POSTNET code is sprayed before it is sorted. In general, when a POSTNET code is sprayed by a postal processing machine it is almost always used for processing by other machines down the line in the distribution process that do not have the capability to print POSTNET codes.
[0042] In current DIOSS machines, the image acquired is in grayscale format and is immediately converted to a binary format for OCR and bar code recognition processing as illustrated in FIG. 1. If neither a bar code nor a recognizable address is found, the mail piece is assigned an ID code and diverted for video coding (human review of the mail piece image to determine, if possible, the correct delivery point address.) Transit time for a mail piece through a DIOSS sorting machine is in the range of approximately 3 to 5 seconds. If image data for a mail piece cannot be resolved during that period, the mail piece must be sorted as a reject or as a 5-digit (if only the first 5 digits of the zip code can be determined.)
[0043] According to the invention, a copy of each gray scale image is transmitted from DIOSS 1 to a gray scale image server 8 at the time of creation. Server 8 stores the image in a memory buffer containing a predetermined number of the most recently taken images in the order received. OCR image data is analyzed by OCR software of the DIOSS 1 itself and is also transmitted to a coprocessor 2 and a remote character reader (RCR) 3 . DIOSS 1 , coprocessor 2 and RCR 3 each analyze the image using different OCR logic. The results from DIOSS 1 and RCR 3 are each transmitted to coprocessor 2 , which arbitrates the result by methods known in the art.
[0044] The arbitrated result is sent back to DIOSS 1 . If the image was read successfully and a ZIP+4 delivery point identified, DIOSS 1 sends a signal to image server 8 instructing it to discard or archive the grayscale image saved for that mail piece. Information obtained from the image data, typically a header including destination information and a copy of the binary image data, is transmitted to a storage and transfer processor (STP) 4 . In the majority of cases, image data for mail pieces will be resolved and a sorting decision made at DIOSS 1 , and a POSTNET bar code label will be printed on the mail piece in DIOSS 1 in real time.
[0045] The ability to archive the grayscale image may become increasingly important for forensic reasons in the event of a bio-terrorist attack. According to a further aspect of the invention, all of the sorter machines used by the USPS forward their archived image data (binary, grayscale/color, or both) to a central database which stores the image for a period of time, along with identifying information (destination address or ID number), the date and time of processing, and the identity and location of the sorting machine that handled the mail piece. This data, extremely large in volume, would be saved for a period of time before being discarded, anywhere from several days, a month, or a year or more depending on storage capacity available. Law enforcement officials working on a case wherein contaminated letters were sent through the mail could thereby determine accurately where the mail piece was processed so that decontamination can be carried out and any patterns of mailing used by the perpetrator can be analyzed.
[0046] If the binary image cannot be resolved, DIOSS 1 signals image server 8 to transmit the gray scale image data to gray scale processor 9 . Gray scale processor 9 , such as a Siemens R1000 system, is tuned for decoding the gray scale image data. If gray scale processor 9 is provided with multiple processors for applying different algorithms to the image data, an additional processor or processors may be provided to arbitrate the results obtained using the different algorithms. The results of the image processing by image processor 9 are transmitted back to image server 8 . If the gray scale image was likewise unreadable or readable only to 5 digits, then the initial result remains unchanged.
[0047] Image server 8 can also send a copy of the image or a differently processed binary image to the remote computer reading (RCR) system 3 . Results returned from RCR 3 can be compared with those from gray scale processor 9 to obtain the highest quality result.
[0048] Time permitting, a sorting decision can then be made using the result of the secondary decoding process, reducing the overall number of mail pieces that are rejected. In such a case, server 8 transmits the result back to DIOSS 1 and action is taken to mark the mail piece with the correct bar code and sort it accordingly. If a successful result is obtained after the point of no return for the mail pieces in the conveyor pathway, it can be sorted to a separate batch of rejects not requiring manual review (video coding). When an ID number is applied as described above, the mail pieces in this batch must be re-fed through the sorter, but the time associated with video coding is saved. For this purpose, if processor 9 succeeds in reading the gray scale image but corrective action must be taken after the initial sort is completed, such result is transmitted to STP 10 from image server 8 , and header information for that binary image is revised to include the result of the gray scale process.
[0049] According a preferred form of the invention, STP 10 comprises an image and data storage buffer and forwarding device that maintains a queue of images and results received from DIOSS 1 and gray scale image server 8 . In the known system shown in FIG. 1, by contrast, the original gray scale image data is discarded and STP 4 receives only the black and white data from DIOSS 1 . Header and unresolved image data are transmitted from STP 10 to an image processing sub-system (IPSS) 11 that provides image and result management functions. IPSS 11 routes image data that cannot be resolved without operator intervention to a video display terminal (VDT) of video coding system 15 where the image is reconstructed on a video screen, allowing an operator to visually decipher the image and key in the address information from the image. In the known system of FIG. 1, this image is the black and white (binary) one; according to the invention, it becomes possible to provide the VDT operator with the grayscale or color image from image server 8 .
[0050] STP 10 according to the invention is modified as compared to the STP 4 currently in use in that it delays sending results to IPSS 5 until finalized results are received from image server 8 and processor 9 . The STP image header is revised to reflect the correct destination point code when server 8 informs STP 10 that an image previously identified as a reject or 5-digit has been fully decoded. Similarly, IPSS software 11 is revised to accommodate the revised image header. As a result, substantially fewer images are sent to video coding as compared to the prior process.
[0051] Results from the above-described image processing functions are transmitted from IPSS 11 to DSU 12 for storage. These comprise include results returned to IPSS 11 from video coding, or gray scale processing for items that have missed the first processing run and must be re-run in a second pass. These second pass mail piece results are fed from DSU 12 into output subsystem 7 , which operates in a conventional manner, except that some of the corrected results it receives are from the gray scale processor, not video coding. Output subsystem 7 reads the ID code previously applied (as by printing) to a mail piece that could not be identified, checks DSU 12 for a corrected result, and then applies the corresponding POSTNET bar code to corrected items.
[0052] An example of control logic for a system having both OCR and BCR capabilities is shown in FIG. 3. After an initial scan 31 , a first attempt 32 is made to read a bar code using the binary data. If this read is successful (decision 33 ), as it is in most cases, the process then terminates and the grayscale data in the buffer is discarded or archived. If it fails, then an attempt 34 is made to read the binary address information by an OCR process. If this second read is successful (decision 36 ), the process then terminates, and the grayscale data in the buffer is discarded or archived. If both attempts to read the binary data have failed, then the grayscale data held in the buffer is processed, in this case in parallel steps 37 , 38 , in an attempt to determine a grayscale BCR result and a grayscale OCR result. Of these two attempts, if neither is successful (decision 39 ) then the mail piece is rejected and may then be labeled with an ID number and sorted to a reject bin for video coding. If one attempt succeeds but the other fails (decision 41 ), then the process terminates, resulting in sorting of the mail piece according to the successful result if time permits, or labeling with an ID tag and subsequent relabeling with a postal bar code as described above. If both attempts were successful, then arbitration logic is applied (step 42 ) and the mail piece is sorted according to the result or, more likely, labeled with an ID tag and reprocessed for relabeling with a postal bar code.
[0053] It will be evident to one of skill in the art that these steps could be rearranged or varied in accordance with desired performance parameters. For example, the binary read steps 32 - 36 can be executed in parallel rather than in series as shown, and a separate scan can be initiated for each if the sorting system has separate bar code and OCR scanners. The end result of such first stage processing can be arbitrated in the same manner as in step 42 . However, for most efficient processing, a successful bar code read in steps 32 - 33 will normally end the process. Each of the various decoding steps may be executed by several different software systems and the result arbitrated in each case before comparison to the other results from other steps.
[0054] The invention thereby provides a means of increasing the machine-based resolution rate of image data scanned from flat objects such as mail pieces without substantially increasing processing time. This result is achieved though the use of a data intensive image format and processing such as gray scale or color image processing that is utilized only when the resolution of the less data intensive black and white image data fails. In this manner, operator intervention in image processing is minimized, throughput and efficiency is increased and processing costs reduced.
[0055] Although various embodiments of the invention have been illustrated in the accompanying drawings and described in the foregoing detailed description, it will be understood that the invention is not limited to the embodiments disclosed but, as will be appreciated by those skilled in the art, is susceptible to numerous modifications and variations without departing from the spirit and scope of the invention as hereinafter claimed. For example, while various functions have been described as performed on different computers or processors, it is specifically contemplated that a greater or lesser number of computers or processors may be used to perform the various functions described herein, depending upon the specific, design, application and system configuration. The described system process is not limited to mail pieces, and is applicable to any information bearing item wherein the information is to be scanned and an action taken based on the result, such as sorting or printing with a coded label.
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The invention provides a method of processing an image containing written information include the steps of (a) scanning a surface of an object to obtain an image of the surface represented by first image data, (b) creating second image data from the first image data, the second image data having a lower data density than the first image data, (c) analyzing the second image data with first image analysis logic to decode the written information, and (d) if the written information cannot be decoded to a desired extent from the second image data, analyzing the first image data with second image analysis logic different from the first image analysis logic to decode the written information. Steps (a) and (b) preferably use a single scanning device to create the high data density image (e.g., color or grayscale) from which the lower data density image (e.g., binary or black and white) can then be created. The resulting two-stage image analysis provides a significant improvement in OCR results. Further, when a pre-printed bar code is present but does not result in a destination bar code, using the methods of step 7, determining the destination address zip code using OCR techniques, printing the resultant ZIP Code and sorting the mail based on the new OCR derived data.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention is in the field of retractors typically used for seat belts and child safety seats.
2. Description of the Prior Art
Many patents have been granted that disclose automatic belt retracting devices having a spring biased spool to normally withdraw the belt into the retractor, but yieldable to allow the belt to be withdrawn therefrom and attached at the opposite end to a buckle or tongue. Typically, the prior art spools include a ratchet configured end plate that is lockingly engaged by a spring biased locking bar pivotally mounted to the retractor frame. Many of the prior art retractors have means for automatically holding the locking bar out of the locking position until a sufficient amount of belt has been withdrawn from the retractor. One such approach has been to provide a belt follower engaged with the bar that will hold the bar out of position until a sufficient amount of belt has unwrapped from the spool. Another approach is to provide a gearing mechanism or cam plate that holds the bar away from the locking position until the spool has rotated to a predetermined angle. The various mechanisms, including the cam plate, hold the locking bar out of the locking position until the retractor spool is slightly rewound. Once the locking bar is allowed to pivot into a locking position, the retractor is operable to prevent further withdrawal of the belt from the retractor. Thus, if the desired or necessary amount of belt is not withdrawn from the retractor prior to attaching the opposite end of the belt to a tongue or a buckle, and if the spool is allowed to slightly rewind, the retractor will automatically lock, preventing further belt withdrawal and possibly attachment of the belt to the tongue or buckle. In such a case, the belt must be completely rewound onto the retractor spool, resulting in considerable inconvenience to the user.
Disclosed in U.S. Pat. No. 4,720,148 is a mechanism for deactivating the cam plate and locking bar of a child seat retractor until the tongue attached to the opposite end of the belt is inserted into a buckle, whereupon the cam plate is released, allowing the locking bar to lockingly engage the retractor spool. It is also known to provide a locking bar which engages the ratchet spool only when the tongue and buckle are interengaged, such as shown in U.S. Pat. No. 3,915,402, or to provide a mechanism to contact and normally hold the locking bar in the removed position until the tongue is inserted into the buckle. Alternative design approaches have been suggested that include rotating the cam plate or to provide a non-automatic manual actuator for independent operation of the cam plate.
It is also known to provide a child seat for mounting atop an automobile seat with the child seat having a harness for securing a child therein, such as shown in U.S. Pat. Nos. 5,380,066; 4,679,852; and 4,720,148. It is also known to provide on a child seat a retractor with the aforementioned mechanism for directly contacting and holding the locking bar for the controlled withdrawal of the child seat harness. Pat. No. 5,380,066 issued to Wiseman et al., discloses a manual pushbutton control that causes movement of the locking bar away from the ratchet shaped end plates allowing withdrawal of the belt harness from the spool until the pushbutton is released. Upon release of the pushbutton, the locking bar pivots to its normal position in locking engagement with the ratchet shaped end plates preventing further withdrawal of the belt harness from the spool. One disadvantage of this system is that the user must use one hand to disengage the locking bar while using the other hand to adjust the web harness. A further disadvantage is that the actuator assembly between the push button and locking bar requires several components, thus increasing manufacturing time and costs. Despite the prior products, there remains a need for a retractor having a simple release mechanism allowing the user to easily lock and unlock the retractor web spool.
The retractor of the present invention, disclosed herein, incorporates a locking bar extension connected directly to the locking bar and actuated by either a pivoting release lever mounted directly to the child seat or the interengagement of the buckle and tongue.
SUMMARY OF THE INVENTION
One embodiment of the present invention is a retractor for mounting to a child seat having a harness, an interengaged combination of a tongue and seat belt buckle comprising a frame, a spool to wrappingly receive a portion of the harness and having an axle and end walls at least one of which is configured as a ratchet wheel with the spool rotatably mounted to the frame, a first spring mounted to the frame and normally urging the spool to rotate to a retracted position whereat a portion of the harness is wrapped thereon, a locking bar mounted to the frame to be moveable between a removed position whereat the locking bar is located apart from the ratchet wheel and a locking position whereat the locking bar lockingly engages the ratchet wheel limiting movement of the spool, and a release lever pivotally mounted to the child seat and controlling the locking bar between the removed position and the locking position.
Another embodiment of the present invention is a retractor for use with a harness and interengaged combination of a tongue and seat belt buckle having a slot for receiving the tongue, comprising a frame, a spool to wrappingly receive a portion of the harness and having an axle and end walls at least one of which is configured as a ratchet wheel with the spool rotatably mounted to the frame, a first spring mounted to the frame and normally urging the spool to rotate to a retracted position whereat a portion of the harness is wrapped thereon, a locking bar mounted to the frame to be movable between a removed position whereat the locking bar is located apart from the ratchet wheel and a locking position whereat the locking bar lockingly engages the ratchet wheel limiting movement of the spool, a second spring mounted to the frame and normally urging the locking bar to the removed position apart from the ratchet wheel, a locking bar extension having a first and a second end, the first end attached to the locking bar, and the locking bar extension second end extending into the seat belt buckle slot, wherein upon insertion of the tongue into the slot, the locking bar extension urges the locking bar into the locking position.
It is an object of the present invention to provide a new and improved means for deactivating a belt retractor's locking bar.
A further object of the present invention is to provide a new and improved child seat with harness incorporating a belt retractor with means for manually and selectively deactivating the locking bar of the retractor while the harness is being adjusted but which will inhibit further adjustment once the tongue and buckle are interengaged.
Yet another object of the present invention is to provide a retractor for mounting to a child seat having a harness with tongue and buckle with the retractor deactivated by rotating a lever on the child seat.
Still a further object of the present invention is to provide a retractor with a locking bar extension for use with a harness having a tongue and buckle with the retractor deactivated by force transmitted through the locking bar extension upon interengagement of the the buckle and tongue.
Related objects and advantages of the present invention will be apparent from the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front view of a child seat incorporating an alternative embodiment of the new and improved retractor disclosed herein.
FIG. 2 is a fragmentary rear view of the seat of FIG. 1.
FIG. 3 is a fragmentary side view of the seat of FIG. 1.
FIG. 4 is an enlarged perspective view of a first preferred embodiment of the new and improved retractor disclosed herein.
FIG. 5 is an enlarged right-side view of the retractor of FIG. 4.
FIG. 6 is an enlarged perspective view of a second preferred embodiment of the new and improved retractor disclosed herein attached to a buckle assembly.
FIG. 7 is an enlarged fragmentary left-side view of the retractor of FIG. 6 and showing the ratchet wheel and spring biased locking bar in the normal locking position, limiting withdrawal of belt material from the retractor spool.
FIG. 8 is the same view as FIG. 7, only showing the spring-biased locking bar in the removed position, freeing the retractor spool to allow withdrawal of belt material.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
For the purposes of promoting an understanding of the principles of the invention, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended, such alterations and further modifications in the illustrated device, and such further applications of the principles of the invention as illustrated therein being contemplated as would normally occur to one skilled in the art to which the invention relates.
Referring now to the drawings, in FIG. 1 there is shown a child seat 10, which includes an outer frame 11 having a pair of downwardly extending arms 12 and 13, with a cushioned seat area 14 and a cushioned back supporting area 15 located therebetween. A plurality of conventional tubing 35 forms a rear frame 36, which is adjustable to support the child seat 10 at a proper angle upon an automobile seat. Tubing 35 may be utilized to secure the child seat 10 to an automobile seat by any suitable means such as by extending the automobile seat belt securely around tubing 35. In the seat area 14, there is provided a seat belt buckle 17 of conventional construction. A pushbutton 18 of buckle 17 faces outwardly allowing the child seat user to depress the same to release tongue 19. Tongue 19 is mounted on a cushioned arm 28 which receives web portions 23 and 24, each of which extends through the back supporting area 15 of seat 10 and down the rear side of seat 10 (FIG. 2) to a belt connector 25. Cushioned arm 28 is pivotally mounted to the child seat by bolts 38 and 39. Multiple pairs of slots 26 and 27A and 27B are provided in back supporting area 15 of seat 10. Belts 23 and 24 are extended through the upper pair of slots 26 if a large child is to be supported, or through either of the lower pair of slots 27A or 27B if a smaller child is to be supported.
Referring now to FIG. 2, a third web portion 32 has a distal end 33 fixedly secured to belt connector 25, with the proximal end of web portion 32 being wrappingly mounted on a spool 44 (FIG. 4) of a belt retractor 22 of the present invention.
The child seat and harness system disclosed in FIGS. 1-3 is illustrative of conventional child seat harness restraint systems and is not intended to limit the invention disclosed, it being understood that there are many alternative child seat harness systems available in the marketplace which can be readily adapted to utilized the present invention. As discussed further, the present invention relates to the improved retractor and actuating mechanism disclosed herein. Referring now to FIG. 3, the child seat of FIGS. 1 and 2 is shown in a left side view in a fragmentary, diagrammatic view. Retractor 22 is mounted below seat area 14 and is further provided with a locking bar extension 31 which extends beyond retractor cover 37.
Crotch stalk 21 is positioned to extend between the legs of a child seated in the child seat and cooperates with the harness system to restrain the child in the child seat. Crotch stalk 21 extends through oblong opening 20 and is pivotally mounted by pin 34 to the child seat. The upper portion of crotch stalk 21 includes buckle 17. Interengagement of tongue 19 and buckle 17 securely fasten the pivoting crotch stalk 21 to the harness system restraining the child in seat 10. The lower portion of crotch stalk 21 extends below pivot pin 34 to form a crotch stalk extension 30. As shown, crotch stalk 21 is positioned such that crotch stalk extension 30 is spaced from locking bar extension 31. It being understood that crotch stalk 21 pivots about pivot pin 34 through opening 20 in the direction of arrow 16 such that crotch stalk extension 30 engages locking bar extension 31. Movement of crotch stalk 21 thereby controls the locking bar of retractor 22 to disengage the ratchet wheels and allow withdrawal of web portion 32.
Referring now to FIG. 4, retractor 22 of the present invention includes a U-shaped frame 40 having a pair of spaced apart sidewalls 41 and 42 that are integrally joined together by a bottom wall 43. An additional cross-member 54 extends between and secures the sidewalls 41 and 42 of the retractor frame together. Bottom wall 43 is further provided with attachment holes 61 and 62, as well as clearance hole 60. A retractor spool 44 is rotatably mounted to and between sidewalls 41 and 42, and includes an axle 45 (FIG. 5) extending through sidewalls 41 and 42. One end 48 of axle 45 extends through sidewall 42 and is attached to a helical spring 49 provided within cover 50. The helical spring is operable to urge axle 45 to rotate and withdraw web portion 32 onto spool 44 of retractor 22, but is yieldable to allow for the withdrawal of web portion 32 from spool 44.
A pair of ratchet shaped end plates 51 and 52 form ratchet wheels which are fixedly attached to axle 45 immediately inward of sidewalls 41 and 42. Plates 51 and 52 rotate with spool 44 as web portion 32 is pulled from or withdrawn onto the spool. A spring biased locking bar 55 has opposite ends which extend through sidewalls 41 and 42 and is pivotal in slot 63 from a locking position in which locking bar 55 engages ratchet shaped end plates 51 and 52 of spool 44, thereby restricting the movement of spool 44, to a removed position in which the locking bar is freed from its locking engagement with ratchet end plates 51 and 52, allowing spool 44 to rotate to permit web portion 32 to be withdrawn from spool 44. A wire spring 56 has one end 57 attached to locking bar 55 and an opposite end 58 attached to cross-member 54. The wire spring 56 is operable to normally urge locking bar 55 into the locking position and thus into engagement with ratchet shaped end plates 51 and 52, such that ends 65 of locking bar 55 may enter into contact with the ratchet shaped end plate and block further withdrawal of web portion 32 from spool 44.
A retractor with a locking bar and ratchet shaped end plates associated with the retractor spool, is conventional in nature and is similar to the retractor disclosed in the commonly owned U.S. Pat. No. 5,511,856 which is incorporated herein by reference. The improvement of the present invention includes fixedly mounting a locking bar extension 31 by rivets 46 and 47 to locking bar 55. Locking bar extension 31 provides an effective means to control the position of locking bar 55, as well as simplifying manufacture and assembly of the retractor.
Retractor 22 is mounted to a child seat frame or in certain cases, a child seat may be originally installed with the vehicle main seat, in which case the retractor is not mounted to the child seat frame but instead is mounted to the vehicle main frame or the vehicle main frame seat frame.
Crotch stalk 21 is pivotally mounted to child seat 10 such that when pivoted outwardly to the adjustment position in the direction of arrow 16, crotch stalk extension 30 engages locking bar extension 31 to overcome the force of spring 56 and moves locking bar extension 31 in the direction of arrow 72 (FIG. 5), thereby moving locking bar 55 out of engagement with ratchet shaped end plates 51 and 52. With crotch stalk 21 in the adjustment position, spool 44 is free to rotate and web portion 32 may be withdrawn as desired. As shown in FIG. 3, cushioned arm 28 may be pivoted in the direction of arrow 70 to permit a child seat occupant to be placed or removed from the child seat. Upon pivoting crotch stalk 21 inwardly to the restraining position in a direction opposite arrow 16, crotch stalk extension 30 disengages locking bar extension 31 and spring 56 normally urges locking bar 55 into engagement with ratchet shaped end plates 51 and 52. Cushioned arm 28 may be pivoted in a direction opposite arrow 70 to interengage tongue 19 and buckle 17, thereby restraining the child seat occupant and inhibiting movement of crotch stalk 21.
Many variations are contemplated and included in the present invention. For example, crotch stalk 21 may contain a tongue and cushioned arm 28 may contain a buckle. Moreover, various harness configurations are presently available on the market, many of which may be adapted to utilize the present invention. Further, instead of utilizing a release lever which is an integral part of the harness restraint system, a separate lever may be pivotally mounted to the car seat frame to provide an alternative means to control locking bar 55.
An alternative design of the retractor of the present invention is shown in FIG. 6. Similar to the embodiment shown in FIG. 4, retractor 88 includes a U-shaped frame 40 having a pair of spaced apart sidewalls 41 and 42 that are integrally joined together by a bottom wall 43. A retractor spool 44 is rotatably mounted to and between sidewalls 41 and 42 and includes a pair of ratchet shaped end plates 51 and 52. As with the embodiment shown in FIG. 4, a helical spring 49 provided within cover 50 is operable to urge spool 44 to rotate and withdraw web portion 32 onto spool 44, but is yieldable to allow for withdrawal of web portion 32 from spool 44. The embodiment of FIG. 6 further includes wire spring 80 having a first end 81 attached to sidewall 41 and a second end 82 attached to locking bar 55, such that spring 80 normally urges locking bar 55 out of engagement with ratchet shaped end plates 51 and 52.
In this embodiment, retractor 88 is mounted on buckle assembly 90 by bolts 92 and 93. The buckle assembly is of conventional nature and includes a slot 91 for receiving tongue 99 and as shown in FIGS. 7 and 8, spring biased locking member 98 engages tongue opening 96 to secure tongue 99 in slot 91 until released. As is well known in the art, pushbutton 97 moves within buckle assembly body 95 to overcome the spring force normally urging locking member 98 into tongue opening 96 and to withdraw locking member 98 from tongue opening 96 and out of engagement with tongue 99. With locking member 98 removed, tongue 99 may be readily withdrawn from slot 91.
The present embodiment includes a locking bar extension 85 having a first end 86 fixedly attached to locking bar 55 by rivets 83 and 84, and a second end 87 of locking bar extension 85 extending into the rear end 76 of slot 91. As a result of the arrangement of the components in the illustrated embodiment, locking bar extension 85 is formed of a relatively flexible material, i.e. spring steel, to conform to the curvatures required, yet sufficiently rigid to transmit force applied at the second end 87 to the first end 86, thereby controlling locking bar 55.
Referring now to FIGS. 7 and 8, upon insertion of tongue 99 into the front end 77 of slot 91, leading edge 94 of tongue 99 engages locking bar extension 85 at curled edge 89 thereby forcing locking bar extension 85 to move within slot 91 away from locking member 98. This force is transmitted along locking bar extension 85 to overcome the spring force of spring 80 and thereby urge locking bar 55 into engagement with ratchet shaped end plates 51 and 52. Engagement of locking bar 55 with ratchet end plates 51 and 52 prevents rotation of spool 44 about axis 45 and therefore prevents withdrawal of web portion 32 in the direction of arrow 100. In the absence of tongue 99 in slot 91, wire spring 80 urges locking bar 55 out of engagement with end plates 51 and 52 and urges locking bar extension 85 to extend further into slot 91. In this position, spool 44 is free to rotate about axle 45 and thus web portion 32 may be withdrawn in the direction of arrow 100.
For this embodiment of the present invention, buckle assembly may be mounted to a child seat or to a vehicle main seat frame such that tongue 99 may be readily inserted into slot 91 and the user has access to pushbutton 97. Alternatively, a buckle assembly of conventional construction may be located on a child seat or vehicle main seat frame adjacent the retractor disclosed herein, with the locking bar extension extending into the slot of the buckle.
While the invention has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character, it being understood that only the preferred embodiments have been shown and described and that all changes and modifications that come within the spirit of the invention are desired to be protected.
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A retractor for controlling the withdrawal of a belt therefrom actuated by movement of a locking bar extension. The retractor frame having a spring biased rotatably mounted spool wrappingly receives one end of the belt harness, the opposite end of the belt harness having fixed thereto either a buckle or a buckle tongue. Attached to a seat is a pivoting crotch stalk including either a buckle or a buckle tongue that receives the corresponding mating part of the buckle tongue combination which is attached to the buckle harness. A locking bar with attached extension is engageable with the ratchet shaped end plates of the spool to prevent further withdrawal of the belt harness. The pivoting crotch stalk engages the extension causing movement of the locking bar into contact with the ratchet shaped end placed, thereby preventing the spool from rotating to allow any further withdrawal of the belt harness. In an alternative embodiment, the locking bar extension extends into the slot of the buckle and upon insertion of the tongue causes movement of the locking bar into the ratchet wheel.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to universal turret milling machines and more particularly, to an insert designed for horizontal insertion in, or mounted on a plate inserted in, a Bridgeport-type milling machine, to facilitate horizontal milling and drilling operations, in addition to conventional vertical machine operation. In a preferred embodiment tire horizontal insert is characterized by a generally cylindrical quill housing, the bottom surface of which is formed with a circular male pilot for insertion in a female pilot provided in the upper surface of the column element of the milling machine. The quill housing is bolted to the upper surface of the column element and the upper surface of the quill housing is shaped with a female pilot and a circular T-slot for receiving T-nuts and bolts which extend through the turret element of the milling machine. A standard or conventional quill assembly is horizontally slidably extendible from a quill bore provided in the quill housing and includes a rotatable spindle on the extendible end for mounting a milling tool or a drill. The splined end of the spindle is engaged by a standard or conventional electric milling machine motor mounted on the rear surface of the quill housing and rotates the spindle and an associated wormed power coupling, responsive to operation of the motor. Manipulation of a power feed control located on the quill housing exterior couples the wormed power coupling to a gear drive which is located in the quill housing and advances the quill assembly a predetermined distance from the quill bore by means of a rack and feed pinion gear. The wormed power coupling can thus be uncoupled from the gear drive train and the quill assembly manually advanced toward the workpiece by rotating a hand feed wheel selectively attached to a course hand feed shaft or a fine hand feed shaft, both of which extend from the quill housing and are each geared to the feed pinion gear. Manipulation of a speed control on the quill housing facilitates powered retraction and extension of the quill assembly into or from the quill bore at a selected speed and the advancing or retracting mode of the quill assembly can be controlled by means of a forward/reverse control. A spring-loaded and axially-shiftable feed stop adjusting screw, having a micrometer nut and a lock nut threadably mounted thereon, is horizontally mounted on the quill housing exterior adjacently parallel to a graduated scale. A toothed quill feed stop rack, mounted horizontally on a feed stop rack pinion gear located inside the quill housing, moves in concert with the quill assembly and is attached to a quill stop knob which extends outside the quill housing and encircles the feed stop adjusting screw. The lock nut and micrometer nut are positioned on the feed stop adjusting screw at a location corresponding to a selected location on the scale, to automatically halt advancement of the quill assembly from the quill bore. When the quill assembly advances a predetermined distance from the quill bore, either automatically by means of the motor or manually, by rotating the hand feed wheel, the quill stop knob extending from the stop rack engages the micrometer nut, causing the feed stop adjusting screw to shift against a spring and disengage a power feed handle provided on the housing which, in turn, disengages a toothed clutch in the gear train and automatically halts advancement of the quill assembly from the quill bore.
A Bridgeport-type universal milling machine is a machining tool commonly used, both in the United States and around the world, to perform a variety of machining operations, including drilling, tapping, reeming, milling and boring. The Bridgeport-type universal milling machine is very popular because it is extremely useful in performing smaller machining jobs, which usually make up the majority of work performed at a typical machine shop during any given year. However, one of the problems associated with conventional Bridgeport milling machines lies in the fact that these milling machines can only be used to perform machining operations in a vertical plane, or 45° with respect to the vertical plane. The horizontal insert of this invention is designed to be inserted horizontally between the bottom column and upper turret portions of a universal turret milling machine, particularly a Bridgeport-type milling machine, or on a plate so inserted, to facilitate performing machining operations on a workpiece in a horizontal plane and at various selected angles with respect to the horizontal plane, in addition to performing machining operations on a workpiece in a vertical plane. In addition, the horizontal insert of this invention is designed to bring the cutting tool mounted on the quill assembly into closer proximity to the workpiece and the rigidity of the machine column, than is presently possible, and will allow heavier cuts and feeds in all machining operations.
2. Description of the Prior Art
Various milling machines and milling machine attachments are known in the art for facilitating various machining operations such as drilling, on a workpiece. U.S. Pat. No. 943,845, dated Dec. 21, 1909, to G. G. Porter and F. E. Cable, details a "Universal Milling Attachment" for use with standard milling machines. The universal milling attachment is characterized by a frame having an arbor rotatably mounted therein and provided at one end with a mechanism to connect it to the spindle of a milling machine. An adjustable member is attached to the frame for securing the frame to the overhanging arm of the milling machine. A tool holder having a driving mechanism is carried by the frame. U.S. Pat. No. 988,231, dated Mar. 28, 1911, to Arthur Vernet, describes a "Multiple Milling Machine", including a turret having a work table with multiple lateral arms connected to the turret and a tool holder carried by each arm. The turret is rotatable relative to the table, to bring any one of the tool holders in operative position with respect to the table. Some of the tool holders are each provided with multiple milling tools and are rotatable independently of the turret to bring any one of the milling tools into operative position. U.S. Pat. No. 1,004,620, dated Oct. 3, 1911, to Charles E. Berold, discloses a "Milling Attachment For Planing Machines". Disclosed is a universal milling head for attachment to the cross rail of a planing machine, such that the milling tools may be presented to the work piece at any desired angle with respect to the horizontal or vertical planes of the planing machine. U.S. Pat. No. 2,055,783, dated Sep. 29, 1936, to Arthur F. Bennett, details a "Machine Tool Structure" including an upright, rigid stand having an abutment, through which a rotatable spindle extends. An attachment is mounted on the abutment for cooperation with the spindle and the upright stand has a second abutment spaced from the first abutment for mounting the attachment in operative position. U.S. Pat. No. 2,519,206, dated Aug. 15, 1950, to Carl Van Ausdall, describes a "Milling Machine Attachment" for use with standard vertical milling machines. The milling machine attachment enlarges the scope of vertical milling machines by converting vertical milling operations such as sawing, slab milling and straddle milling into horizontal milling operations. U.S. Pat. No. 291,885, dated Nov. 10, 1959, to M. P. Budney, et al, discloses a "Milling Adaptor Head" for use with conventional milling machines and enabling milling machines to cut slots or grooves in concave surfaces of hollow objects such as cylinder tubes, rings and the like. U.S. Pat. No. 2,945,402, dated Jul. 19, 1960, to Fred G. Burg, discloses a "Movable Mounting For Machine Tool", which is capable of adequately supporting a heat and complex tool structure, such as a multiple spindle drill. The movable mounting for machine tool is characterized by a support for a rectilinear guide, a tool member provided in the guide for rectilinear movement therein, with the guide including a pair of opposed surfaces, between which the members are movable. A mechanism for clamping and preventing movement of the tool members is provided. U.S. Pat. No. 2,955,515, dated Oct. 11, 1960, to C. W. Berthiez, details "Machine Tools" for enabling a milling machine to effect both horizontal and vertical milling operations. The machine tools are characterized by an auxiliary head which is adapted for connection to the conventional head-stock of a horizontal boring machine. The auxiliary head has a mechanism for rotatably supporting at least one auxiliary horizontal tool spindle provided in the form of a hollow sleeve which coaxially surrounds the conventional boring spindle of the machine. U.S. Pat. No. 3,163,081, dated Dec. 29, 1964, to Stanley E. Vickers, discloses a "Right Angle Milling Head" adapted to be mounted on and powered drilling machines and the like. The milling head greatly increases the utility of drilling units by permitting them to be used for many types of milling operations. U.S. Pat. No. 4,709,465, dated Dec. 1, 1987, to Henry Lewis, et al, describes an "Interchangeable Spindle-Head Milling System", characterized by a master milling head capable of providing spindle driving power and up to a five axis movement to a wide range of individual spindle heads, each designed for a specific machining function and each selectively, interchangeably and automatically matable to the master head.
It is an object of this invention to provide an insert designed for horizontal insertion in a universal turret milling machine to facilitate performance of horizontal milling operations on a workpiece.
Another object of this invention is to provide an insert designed for horizontal insertion between the bottom column element and top turret of a Bridgeport-type milling machine, or on a plate so inserted, with a rotatable spindle to facilitate performance of horizontal milling operations on a workpiece.
Still another object of this invention is to provide a horizontal insert for universal turret milling machines, which insert is characterized by a generally cylindrical quill housing, including a horizontally-extendible quill assembly which is rotated by a motor mounted on the posterior surface of the quill housing and can be selectively advanced from or retracted into the quill housing, either manually or by means of the motor. The insert housing may be mounted between the bottom column element and top turret element of the machine or it may be mounted on a plate so mounted on the machine.
Yet another object of this invention is to provide a horizontal insert for universal turret milling machines, which horizontal insert is characterized by a generally cylindrical quill housing for mounting between the bottom column element and top turret element of a Bridgeport-type turret milling machine or on a plate so mounted, and includes a quill assembly which rotatably receives a spindle for mounting a milling tool and is selectively advanced in concert with the spindle a predetermined distance from a horizontal quill bore provided in the housing, by means of an electric quill drive motor mounted on the housing, or by means of a hand feed wheel provided on the housing.
A still further object of this invention is to provide a horizontal insert for universal turret milling machines, which insert is characterized by a quill assembly that is horizontally-extendible from a quill housing mounted in or on a Bridgeport-type milling machine. A spindle in the quill assembly receives cutting and milling tools and is rotated by splines shaped in one end thereof, powered by a motor mounted on the quill housing and the spindle is selectively coupled to a gear drive train located in the quill housing for advancing the quill assembly a predetermined distance from the quill housing to a workpiece. The quill assembly is selectively uncoupled from the gear drive train by means of a clutch for manually advancing the quill assembly from the quill housing by rotating a hand feed wheel provided on the housing.
Yet another object of this invention is to provide a horizontal insert for mounting between the turret and column of universal turret milling machines, or side-mounted on a plate so attached to the universal turret milling machine, which horizontal insert is characterized by a horizontally-extendible quill assembly that is selectively advanced from or retracted into a quill housing, either manually or by means of a drive motor attached to the housing, the advancement of which quill assembly may be automatically halted after advancing a predetermined distance from the housing, by means of a gear drive train uncoupling mechanism.
SUMMARY OF THE INVENTION
These and other objects of the invention are provided in a horizontal insert for direct or side-mounting on universal turret milling machines, which horizontal insert is characterized by a generally cylindrical quill housing designed for horizontal mounting between the bottom column element and top turret element of a Bridgeport-type universal milling machine or attachment to a plate so mounted. A quill assembly, provided with a rotatable spindle having one end adapted for mounting a milling tool, chuck, drill bit and tap and like tools, is automatically or manually slidably extendible from a horizontal quill bore included in the quill housing and a splined end of the spindle is powered by an electric motor mounted on the quill housing exterior. The spindle is selectively coupled to a gear drive train located in the quill housing for motorized advancement of the quill assembly from the quill bore to the workpiece, or uncoupled by a power engage and disengage control from the gear drive train, to facilitate manual advancement of the quill assembly from the quill bore. Motorized advancement of the quill assembly at a selected speed may be automatically effected by means of a speed control mechanism and in a selected direction by a forward/reverse control. Automatic termination of advancement of the quill assembly after the quill assembly has advanced a predetermined distance from the quill housing is effected by a gear train uncoupling mechanism.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood by reference to the accompanying drawings, wherein:
FIG. 1 is a side view of a standard or conventional Bridgeport-type universal milling machine;
FIG. 1A is a side exploded view of the universal milling machine illustrated in FIG. 1, with the horizontal insert of this invention mounted thereon;
FIG. 2 is a perspective view, partially in section, of a preferred embodiment of the horizontal insert for universal turret milling machines of this invention;
FIG. 3 is an enlarged perspective view, partially in section, of the horizontal insert illustrated in FIG. 2;
FIG. 3A is an enlarged perspective view, further partially in section, of the horizontal insert illustrated in FIG. 2;
FIG. 4 is a left side view of the horizontal insert illustrated in FIGS. 1A-3A;
FIG. 4A is an enlarged front view of the power feed handle element of the horizontal insert;
FIG. 5 is a rear view, partially in section, of the power feed handle operating linkage and the horizontal insert;
FIG. 6 is a right side view of the horizontal insert;
FIG. 7 is a top view of the horizontal insert;
FIG. 8 is a bottom view of the horizontal insert;
FIG. 9 is a side view of the power feed handle element of the horizontal insert illustrated in FIGS. 1A-8;
FIG. 10 is a side sectional view of the horizontal insert, more particularly detailing the components of a gear train contained in the horizontal insert housing;
FIG. 11 is a side view of the hand feed gear train of the horizontal insert;
FIG. 12 is a top view of the hand feed gear train illustrated in FIG. 11;
FIG. 13 is a top view of the motorized gear train of the horizontal insert of this invention;
FIG. 14 is a side view of the universal milling machine illustrated in FIG. 1, with an alternative embodiment of the horizontal insert side-mounted thereon;
FIG. 15 is a front view of the horizontal milling machine and alternative horizontal insert side-mount illustrated in FIG. 14; and
FIG. 16 is a plan view of an assembly mount plate element of the alternative embodiment.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring initially to FIGS. 1-8 of the drawings, in a preferred embodiment of the invention the horizontal insert for universal turret milling machines, hereinafter referred to as the horizontal insert, of this invention, is generally illustrated by reference numeral 1. The horizontal insert 1 is designed to fit on a universal turret milling machine 106, typically characterized by a vertical base or column 103, a ram 102 mounted on a turret 107, which is mounted on the column 103, a vertical quill housing assembly 101 provided on the front end of the ram 102 and a top housing 2, including an electric motor 100 mounted on the vertical quill housing assembly 101, as illustrated in FIG. 1. A knee 104 extends horizontally from the front surface of the column 103 and a work table 105 is provided on the upper surface of the knee 104.
The horizontal insert 1 of this invention is mounted between the turret 107 and column 103 by means of bolts 109 and studs 110, threaded into fixed T-nuts 108, as illustrated in FIG. 1A. The bottom threaded ends of the studs 110 are threaded into a stud seat 112 of a stud mount spider 111. The horizontal insert 1 is characterized by a horizontal quill housing 4, as illustrated in FIGS. 1A-8. As illustrated in FIGS. 2-3A, the flat upper top plate 4a surface of the horizontal quill housing 4 is circumscribed by a circular T-slot 38, aligned vertically with a top female pilot 63, which receives the male turret pilot 83 of the turret 107. Similarly, the flat bottom plate 4b surface of the horizontal quill housing 4 is provided with a bottom male pilot 64, as illustrated in FIG. 8, which seats in a female turret pilot 85 of the column 103. As further illustrated in FIG. 3, a quill cavity 3a extends through the horizontal quill housing 4 between the top plate 4a and bottom plate 4b. A generally elongated, cylindrical quill assembly 3, having a rack 58 machined on the surface thereof, is horizontally slidably accommodated and selectively manually or automatically extendible from and retracted into the quill cavity 3a, as hereinafter described. A conventional spindle 79, extending from the ends of the quill assembly 3, facilitates attachment of a milling tool, drill tap or other tool (not illustrated) at one end thereof. The quill assembly 3 includes a central splined quill cavity (not illustrated) located inside a wormed power coupling 5, which receives a splined end of the spindle 79, protruding from the rear of the horizontal quill housing 4, as illustrated in FIGS. 2 and 3. As further illustrated in FIG. 3, in a preferred embodiment the spindle 79 is encircled by the wormed powered coupling 5 where the spindle 79 exits the horizontal quill housing 4. A swinging worm gear shaft 7 is mounted in a swinging worm gear housing 9 (illustrated in FIG. 5) in the horizontal quill housing 4 in perpendicular relationship with respect to the spindle 79 and a swinging worm gear 6 is mounted on the swinging worm gear shaft 7. The swinging worm gear 6 normally meshes with a power coupling worm 5a on the wormed power coupling 5. The swinging worm gear shaft 7 terminates in a first bevel gear 8, which meshes with a second bevel gear 10, mounted on the end of a cluster gear shaft 11, in turn mounted in the horizontal quill housing 4 in perpendicular relationship with respect to the swinging worm gear shaft 7. A set of three cluster gears 12 is fixed to the cluster gear shaft 11 in spaced relationship with respect to each other and the second bevel gear 10. A sliding cluster gear shaft 14 is mounted in the horizontal quill housing 4 in parallel, adjacent relationship with respect to the cluster gear shaft 11 and terminates in a forward-reverse shift shaft 16, located adjacent to the second bevel gear 10. A pair of adjacent sliding cluster gears 13 of varying size are slidably mounted on the fixed sliding cluster gear shaft 14 for alternatively meshing with the variously sized cluster gears 12, provided on the cluster gear shaft 11, thereby providing 3 rates of rotational speed of the sliding cluster gear shaft 14 by meshing the respective sliding cluster gears 13 with the corresponding cluster gears 12. The sliding cluster gear shaft 14 terminates in a third bevel gear 15, that meshes with vertically-oriented upper and lower forward and reverse bevel gears 19, freely rotatably mounted on a forward-reverse shaft 18, which is mounted vertically in the horizontal quill housing 4 in perpendicular relationship with respect to the horizontal sliding cluster gear shaft 14. As illustrated in FIGS. 3, 3A and 10, a forward-reverse, top and bottom castlelated shift dog 20 is slidably mounted on the forward-reverse shaft 18 between the upper and lower forward and reverse bevel gears 19. A companion forward-reverse, curved shift yoke 17 is provided at the end of the third bevel gear 15 and engages the shift dog 20. Accordingly, the shift dog teeth 20a on the shift dog 20 are shifted into engagement with the shift teeth 19a on the respective forward and reverse bevel gears 19, by rotation of the forward-reverse shift shaft 16, as follows: As illustrated in FIG. 10 the shift dog 20 is slidably keyed to the forward-reverse shaft 18 and selectively engages the shift teeth 19a of the upper forward and reverse bevel gear 19 or the lower forward and reverse bevel gear 19, to drive the upper or lower forward and reverse bevel gears 19, as hereinafter further described. As illustrated in FIGS. 3A and 10, the forward-reverse shift yoke 17 is moved up and down to shift the shift dog 20 by rotation of a shift disc 45b, having a disc pin 45c, engaging a yoke slot 17a in the forward-reverse shift yoke 17. The forward/reverse shift shaft 16 is connected to the shift disc 45b and a forward/reverse feed handle 45 is attached to the forward/reverse shift shaft 16, as further illustrated in FIG. 3A. A worm 21 is mounted on the forward-reverse shaft 18 below the lower, or bottom forward and reverse bevel gear 19 and meshes with a worm gear 22, provided on a worm gear shaft extension 89, mounted for horizontal rotation in the horizontal quill housing 4, as further illustrated in FIGS. 3A and 11. As illustrated in FIGS. 3 and 11, a spring-loaded, toothed clutch, defined by engaged clutch engaging members 23, is also provided on the worm gear shaft extension 89 adjacent to the worm gear 22 and as illustrated in FIG. 3, a first transfer gear 24 is slidably mounted on the worm gear shaft extension 89 adjacent to the toothed clutch 23. Referring again to FIG. 11, one of the clutch engaging members 23 is positioned adjacent and attached to the worm gear 22, fixed to the worm gear shaft 27, while the corresponding clutch member 23 is fixed to the first transfer gear 24, which slides on the worm gear shaft 27. A thrust bearing 86 is located between the rotating transfer gear 24 and a non-rotating shaft mount 87, which is slidably mounted on the worm gear shaft extension 89. A clutch spring 25 is interposed on the worm gear shaft extension 89 between the shaft mount 87 and the spring tension nut 26, threaded on the end of worm gear shaft extension 89. A shaft mount shoulder 88 on the shaft mount 87 engages a corresponding shaft flange 89a on the worm gear shaft extension 89, as further illustrated in FIG. 11. The purpose of the worm gear shaft extension 89, shaft mount 87 and clutch spring 25 is to allow the clutch engaging members 23 to separate in case of an overload in the geared feed system, as hereinafter described. As further illustrated in FIGS. 3, 10 and 11, the first transfer gear 24, slidably mounted on the worm gear shaft 27, normally meshes with a second transfer gear 29, provided on a transfer shaft 28, positioned parallel to the worm gear shaft 27, one end of which transfer shaft 28 is mounted in a transfer shaft bearing block 36, provided in the horizontal quill housing 4, and the other end of which transfer shaft 28 extends through the horizontal quill housing 4, as illustrated in FIGS. 11 and 12. Referring again to FIG. 11, a feed engage yoke 49 is pivotally attached to the spring tension nut 26 by means of a yoke pivot pin 90. The feed engaging yoke 49 is also pivotally attached to the feed-engage cover 55, (illustrated in FIG. 2) by means of a stationary pivot pin 92. This arrangement facilitates pivoting of the feed engage yoke 49, both on the yoke pivot pin 90 and the stationary pivot pin 92, corresponding displacement of the worm gear shaft extension 89 and shaft mount 87 on the worm gear shaft 27 and separation of the toothed clutch engaging members 23, as hereinafter further described.
As further illustrated in FIG. 3 of the drawings, a hand wheel dentation 30 is shaped in the transfer shaft 28 adjacent to the extending end thereof. A feed stop rack pinion gear 31, having a diameter slightly less than that of thee second transfer gear 29, is mounted on the transfer shaft 28 adjacent to the second transfer gear 29. A third transfer gear 32 is also mounted on the transfer shaft 28 adjacent to the transfer shaft bearing block 36 and meshes with a fourth transfer gear 33, provided on a feed pinion gear shaft 34, which extends through the transfer shaft bearing block 36, across the quill cavity 3a and is rotatably mounted in a bearing block 37, mounted in the horizontal quill housing 4. A feed pinion gear 35 is also mounted on the feed pinion gear shaft 34 and meshes with the rack 58, machined on the surface of the quill assembly 3.
Referring now to FIGS. 2-13, a threaded feed stop adjusting screw 51 has one end mounted in a first screw socket and cover 56, mounted on the horizontal quill housing 4 and an opposite end mounted in a second screw socket and cover 57, also mounted on the horizontal quill housing 4 in spaced relationship with respect to the first screw socket and cover 56. A micrometer nut 54 and lock nut 53 are threaded on the feed stop adjusting screw 51, as illustrated in FIGS. 2 and 7, and a graduated scale 59 spans the first screw socket and cover 56 and the second screw socket and cover 57, in parallel, adjacent relationship with respect to the feed stop adjusting screw 51. As illustrated in FIGS. 2, 3A and 11-13, a quill feed stop rack 71, having rack teeth 78 (illustrated in FIGS. 2 and 3A) along the bottom edge thereof, is mounted horizontally in the horizontal quill housing 4, with the rack teeth 78 meshing with the feed stop rack pinion gear 31 (mounted on the transverse shaft 28, as illustrated in FIG. 3). A stop knob support 52a extends perpendicularly from the quill feed stop rack 71 and a cylindrical quill stop knob 52, having a stop knob opening 52b, as illustrated in FIG. 3A, is mounted on the stop knob support 52a, and extends from the quill feed stop rack 71, as illustrated in FIGS. 3A and 12. The stop knob opening 52b slidably accommodates the feed stop adjusting screw 51. A feed trip plunger 69, pivotally mounted in the first screw socket and cover 56 by means of a plunger pivot pin 69b, is biased by a plunger spring 69a, into a socket shaped in the feed engage lever 50, as illustrated in FIG. 4A. Accordingly, referring to FIGS. 3A, 4A and 13, the feed stop adjusting screw 51 extends through the stop knob opening 52b of the quill stop knob 52 to facilitate traversal of the quill stop knob 52 with respect to the feed stop adjusting screw 51 responsive to movement of the quill feed stop rack 71. Adjustment of the extent of travel of the quill assembly 3 from the horizontal quill housing 4 by operation of the drive train in the horizontal insert 1 can thus be effected by threadably releasing the lock nut 53 from contact with the adjacent micrometer nut 54 and then threadably repositioning the micrometer nut 54 in a desired location along the length of the feed stop adjusting screw 51 according to the markings on the fixed scale 59. The lock nut 53 is then again tightened against the micrometer nut 54 to allow linear movement of the sliding quill stop knob 52, mounted on the quill feed stop rack 71. Upon contact of the quill stop knob 52 with the fixed and repositioned micrometer nut 54, the feed stop adjusting screw 51 is displaced in the first screw socket and cover 56 and second screw socket and cover 57 against the feed trip plunger 69, illustrated in FIG. 4A, to overcome the bias of the plunger spring 69a and release the feed trip plunger 69 from the feed-engaging lever 50 of the power feed handle 47, disengage the power train and thus prevent further extension of the quill assembly 3 from the horizontal quill housing 4. It will be appreciated that the same disengagement may be effected by manual pivoting of the power feed handle 47 and the feed engaging lever 50 away from the feed trip plunger 69, responsive to grasping and manipulation of the power feed handle 47, extending from the feed engaging lever 50. This action is made possible by a pivot pin 72, which extends through the feed-engaging lever 50, seats in the first screw and socket cover 56 and facilitates pivoting of the feed-engaging lever 50 with respect to the first screw socket and cover 56 by manipulation of the power feed handle 47.
Referring now to FIGS. 3, 3A, 5 and 10 of the drawings, power may be applied to and disengaged from the first bevel gear 8, second bevel gear 10 and the associated power train inside the horizontal insert 1 by engagement and disengagement of the swinging worm gear 6 with the underlying power coupling worm 5a, mounted on the wormed power coupling 5. This engagement/disengagement is made possible by operation of a swinging worm gear cradle 9, having at one end an upper swing pin 75, pivotally attached to a swing arm 73, as illustrated in FIGS. 5 and 10 and pivoted at the opposite end on the cluster ear shaft 11, (illustrated in FIG. 3A) which mounts the second bevel gear 10. The swing arm 73 is, in turn, pivotally connected to a swing arm link 77 by means of a lower swing pin 74, as illustrated in FIG. 10 and the swing arm link 77 is likewise connected to a swing lever shaft 40. Rotation of the swing lever shaft 40 by means of a feed disengage handle 46 attached thereto as illustrated in FIG. 2, forces the swing arm 73 upwardly to lift the swinging worm cradle 9 and remove the underslung, attached swinging worm gear 6 from engagement with the underlying power coupling worm 5A. Rotation of the feed disengage handle 46 in the opposite direction moves the swing arm link 77 and the swing arm 73 downwardly and lowers the swinging worm gear cradle 9, thus again engaging the swinging worm gear 6 with the underlying power coupling worm 5A.
Referring now to FIGS. 2, 3a and 13 of the drawings, the hand feed wheel 42 may be selectively mounted on either the transfer shaft 28 or the fine hand feed shaft 48, both of which are connected to the power train inside the horizontal insert 1, as heretofore described. As illustrated in FIGS. 2 and 3, the hand feed wheel 42 is removably mounted on the transfer shaft 28 and is seated in position by operation of a hand wheel dentation 30, provided in the transfer shaft 28. A corresponding rod (not illustrated) located in the hand feed wheel 42 removably seats in the hand wheel dentation 30 by manipulation of a feed wheel mount knob 43, provided on the hand feed wheel 42, to removably seat the hand feed wheel 42 in position. Accordingly, the hand feed wheel 42 can be utilized to hand feed the quill assembly 3 into and from the horizontal quill housing 4 at a relatively fast rate by rotation of the respective third transfer gear 32 and meshed fourth transfer gear 33, mounted on the feed pinion gear shaft 34, which, in turn, rotates the feed pinion gear 35 that meshes with the corresponding rack 58, machined on the quill assembly 3 as heretofore described. Use of the hand feed wheel 42 with regard to the coarse feed described above is possible only when the toothed clutch engaging members 23 are disengaged as heretofore described. The finer adjustment of the quill assembly 3 into and from the horizontal quill housing 4 can be effected by removing the hand feed wheel 42 from the transfer shaft 28 and replacing it on the fine hand feed shaft 48, also fitted with a hand wheel dentation 30 to receive the hand feed wheel 42. Rotation of the fine hand feed shaft 48 by means of the hand feed wheel 42 thus rotates the hand feed bevel gear 68, mounted on the fine hand feed shaft 48, which hand feed bevel gear 68 engages the top and bottom forward and reverse bevel gear 19 that transmits power to the connected worm 21 and associated worm gear 22, mounted on the worm gear shaft 27. Power is thus transmitted from the first transfer gear 24, also Located on the worm gear shaft 27, to the meshing feed stop rack pinion gear 31 mounted on the transfer shaft 28, in order to transmit power to the feed pinion gear 35 in the same manner as described above with respect to the power feed operation. Hand extension and retraction of the quill assembly 3 by use of the hand feed wheel 42 with respect to the fine hand feed shaft 48, is possible only where the swinging worm gear 6 is disengaged, as hereinafter described.
Referring now to FIGS. 2 and 13 of the drawings, the operational speed of the gear train located inside the horizontal insert 1, and thus, the speed of extension and retraction of the quill assembly 3 to and from the horizontal quill housing 4, can be controlled by a feed rate change handle 44, connected to a shift crank shaft 65b, which mounts a shift crank 65, fitted with a crank pin 65a. The crank pin 65a engages a shift shoe 67, which slides on a slide pin 66 and engages the largest of the three sliding cluster gears 13, mounted on the sliding cluster gear shaft 14. Accordingly, manipulation of the feed rate change handle 44 shifts the shift shoe 67 and the sliding cluster gears 13 on the sliding cluster gear shaft 14 into various engagement with the facing cluster gears 12, for speed control of the drive train.
Referring now to FIGS. 14-16 of the drawings, in an alternative preferred embodiment of the invention a side mount quill assembly 80 is mounted between the turret 107 and the column 103 of the universal turret milling machine 106 in the same manner as the horizontal insert 1 illustrated in FIG. 2. The side mount quill assembly 80 includes a horizontal insert 1 which is characterized by a side mount quill housing 81, bolted or otherwise attached to an assembly mount plate 82 that is sandwiched between the turret 107 and the column 103, as described above. Mount plate openings 82a serve to secure the side mount quill housing 81 to the assembly mount plate 82 by means of plate mount bolts 82b. A pilot opening 84 in the assembly mount plate 82 receives the male turret pilot 83 of the turret 107, as illustrated in FIGS. 14-16 to securely seat the assembly mount plate 82 and thus the attached side mount quill housing 81, to the universal turret milling machine 106. It will be appreciated by those skilled in the art that the electric motor 100 provided in the top housing 2 and bolted to the side mount quill housing 81 may be identical to the corresponding top housing 2 and motor 100 which is mounted on top of the vertical quill housing assembly 101. It will be further appreciated from a consideration of FIG. 15 that the side mount quill assembly 80 may be bolted to the assembly mount plate 82 using the mount plate bolts 82b either on the bottom or top side of the assembly mount plate 82, as illustrated in phantom in FIG. 15. It will be still further appreciated by those skilled in the art that the side mount quill assembly 80 may be identical in construction and have identical features to the horizontal insert 1 illustrated in FIGS. 1-13 or it may be less sophisticated, in that it may be provided with fewer drive train gears and accessories, as desired.
In operation, and referring again to the drawings, the horizontal insert 1 of this invention is used to facilitate horizontal milling, drilling, tapping and other machine operations, as follows. When it is desired to automatically extend the quill assembly 3 from the horizontal quill housing 4 in order to place a cutting tool, bit or other tool in the receiving end of the spindle 79, power is transmitted as hereinafter described from the rotating wormed power coupling 5, connected to the splined end of the spindle 79 and operated by an electric motor 100, located in the corresponding top housing 2. The feed disengage handle 46 is manipulated to pivot the swing arm link 77 and swing arm 73 and drop the swinging worm gear cradle 9 to mesh the attached swinging worm gear 6 with the underlying power coupling worm 5a and transmit power from the wormed power coupling 5 to the power feed system in association with the first bevel gear 8 and second bevel gear 10, as illustrated in FIGS. 5 and 10. This power transmission causes the cluster gear shaft 11 to rotate, along with the three cluster gears 12, which mesh with the corresponding sliding cluster gears 13 in a drive sequence determined by manipulation of the feed rate change handle 44 and adjustment of the sliding cluster gears 13 on the sliding cluster gear shaft 14, as heretofore described with respect to FIG. 13. Power is thus transmitted to the third bevel gear 15, located on the end of the horizontal sliding cluster gear shaft 14. As illustrated in FIG. 3A, the forward-reverse shift shaft 16, attached to the forward-reverse feed handle 45 and extending through the sliding cluster gear shaft 14, is rotated to operate the forward-reverse shift yoke 17 either upwardly or downwardly. This action shifts the forward-reverse reverse shift dog 20 into driving engagement with the shift teeth 19a of either the top or bottom forward and reverse bevel gear 19, to rotate the vertical forward-reverse shaft 18 in a selected direction, as illustrated in FIG. 10. Meshing of the corresponding worm 21, also mounted on the forward-reverse shaft 18, with the adjacent worm gear 22, mounted on the horizontal worm gear shaft 27, effects rotation of the horizontal transfer shaft 28, through meshing of the first transfer gear 24 and the feed stop rack pinion gear 31. This action also drives the horizontal feed pinion gear shaft 34 by interaction between the third transfer gear 32 and the fourth transfer gear 33, to rotate the feed pinion gear 35, which, in turn, interacts with the rack 58 to move the quill assembly 3. Accordingly, the quill assembly 3 will move into or from the horizontal quill housing 4, depending upon the relative position of the forward-reverse shift dog 20 with respect to the top and bottom forward and reverse bevel gears 19. Manual movement of the quill assembly 3 to and from the horizontal quill housing 4 may be effected by initially disengaging the toothed clutch engaging members 23 and positioning the hand feed wheel 42 on the transfer shaft 28 for rapid adjustment of the quill assembly 3, or on the fine hand feed shaft 48 to effect fine extension or retraction of the quill assembly 3, as heretofore described. Accordingly, under circumstances where it is desired to manually move the quill assembly 3, the power feed handle 47 is pulled downwardly to pivot the feed-engaging lever 50 on the pivot pin 72, release the feed trip plunger 69 from the depression in the feed engage lever 50 to separate the toothed clutch engaging members 23 against the bias of the toothed clutch spring 25, which seats against the spring tension nut 26 on the worm gear shaft 27 and thus terminate power to the worm gear shaft 27 and transfer shaft 28. This disengagement of the toothed clutch engaging members 23 thus facilitates manual rotation of the transfer shaft 28 using the removable hand feed wheel 42, as heretofore described. To facilitate use of the fine hand feed shaft 48, the swing worm gear 6 should be disengaged from the power coupling worm 5a and the hand feed wheel 42 should be mounted on the fine hand feed shaft 48.
Under circumstances where it is desired to automatically adjust the speed of extension or retraction of the quill assembly 3 from the horizontal quill housing 4, the feed rate change handle 44 can be manipulated to rotate the corresponding shift crank 65 and shift shoe 67, shift the sliding cluster gears 13 on the sliding cluster gear shaft 14 to reposition the sliding cluster gears 13, which are of varying size, on the sliding cluster gear shaft 14 into engagement with the corresponding cluster gears 12, also of varying size, mounted on the fixed cluster gear shaft 11, as illustrated in FIG. 13 Accordingly, power transferred from the rotating wormed power coupling 5 to the swinging worm gear shaft 7 and corresponding first bevel gear 8 is transferred to the cluster gear shaft 11 means of the second bevel gear 10 and the speed of the corresponding forward-reverse shift shaft 16 can be adjusted with respect to the speed of rotation of the cluster gear shaft ill by shifting the sliding cluster gears 13 on the sliding cluster gear shaft 14 by operation of the feed rate change handle 44, as described above.
Referring again to FIGS. 2, 3a and 4 of the drawings, under circumstances where it is desired to extend the quill assembly 3 a preselected distance from the horizontal quill housing 4 in order to place a tool located in the spindle 79 into a precise position with respect to a workstock, the micrometer nut 54 and lock nut 53 are threadably manipulated on the corresponding threaded feed stop adjusting screw 51, as follows. The lock nut 53 is threadably released from engagement with the micrometer nut 54 and the micrometer nut 54 is threadably adjusted on the feed stop adjusting screw 51 until it is aligned precisely with a selected mark on the fixed adjacent scale 59. The lock nut 53 is then threadably advanced on the feed stop adjusting screw 51 until it again contacts and locks the micrometer nut 54 in position at that desired marking. The power feed handle 47 is then raised into the engaged position to effect operation of the power train, which receives power from the rotating wormed power coupling 5 in the quill-extending direction, as dictated by the relative position of the forward-reverse shift dog 20 with respect to the top and bottom forward and reverse bevel gears 19, as heretofore described. This engaged position of the forward-reverse shift dog 20 is dictated by adjustment of the forward-reverse feed handle 45, as heretofore described. Operation of the side mount quill assembly 80 illustrated in FIGS. 14 and 15 is effected in the same manner as described above with respect to the quill assembly 3.
It will be appreciated by those skilled in the art that the horizontal insert 1 of this invention can be quickly and easily mounted on substantially any Bridgeport-type milling machine, either as illustrated in FIG. 2 or in FIGS. 14 and 15 to facilitate horizontal milling, boring and related operations. The various feed modes, feed rate changes, forward and reverse and feed engaging and disengaging controls are positioned at convenient locations in the horizontal insert 1 and power is derived from a conventional top housing 2 which may be identical to the top housing 2 vertically mounted on the vertical quill housing assembly 101 of the universal turret milling machine 106. The horizontal insert of this invention facilitates a broad-based extension of possible machine functions and may be altered to utilize any combination of the various feed features described above and to fit substantially any universal turret milling machine.
While the preferred embodiments of the invention have been described above, it will be recognized and understood that various modifications may be made in the invention and the appended claims are intended to cover all such modifications which may fall within the spirit and scope of the invention.
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A horizontal insert designed for horizontal insertion in a universal turret milling machine, particularly Bridgeport-type milling machine, to facilitate performance of horizontal milling, drilling, boring and tapping operations, as well as standard vertical machining operations, in one setup. The horizontal insert is characterized by a generally cylindrical quill housing designed for insertion between the bottom column element and top ram element of a Bridgeport-type milling machine or secured to a plate so mounted. In the first embodiment the bottom surface of the quill housing is bolted to the top surface of the column and the upper surface of the quill housing is bolted to the bottom surface of the turret. A quill assembly which terminates in a spindle for mounting milling tools, drill chucks, end mills and the like, is manually or automatically horizontally-extendible from the quill housing and a splined end of the spindle is driven by a motor mounted on a top housing which is mounted to the rear surface of the insert. The reversible spindle is selectively coupled by means of a lever to a gear train located in the quill housing, to transmit torsion from the spindle to a feed pinion gear which advances the quill a selected distance from the quill housing to the workpiece, or retracts the quills from the workpiece into the housing. Alternatively, the spindle can be disengaged from the gear train and the quill advanced from or retracted into the quill housing a selected distance by manually rotating a hand feed wheel on the housing. Forward-reverse and speed control mechanisms are also provided for controlling the direction and speed of rotation of the spindle.
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BACKGROUND OF THE INVENTION
This invention relates to safety devices for motor vehicles which protect passengers during an impact affecting the vehicle.
As a result of space limitations, the sides of a vehicle have relatively short lateral deformable distances. Thus, serious injuries to passengers may result if the vehicle is struck from a side. The passengers in a vehicle are especially exposed to considerable injury hazard when an impacting object penetrates into a passenger compartment. In order to protect the passengers, a greater resistance to lateral penetration of an impacting object should be provided. It is well known that bend-resistant supports or beam barriers can be built into the sides of a vehicle.
European Published Application No. A1 02 35 635 discloses a safety device which transfers most of the impact energy of a lateral impacting object to a door sill. Since vehicle door sills usually have a relatively high degree of rigidity, a door sill is effective to reduce significantly the penetration depth of the impacting object during a lateral impact.
Another arrangement is shown in German Offenlegungsschrift No. 31 51 861, which discloses vehicle doors designed so that the door sill is greatly relied upon for absorption of the impact energy during a lateral impact. The door sill is highly torsion-resistant because of its load-bearing function.
German Patent Specification 31 11 045 discloses a safety device using a beam tie arrangement to transfer the impact energy to damping elements of the vehicle. The beam tie arrangement is intended to function as an impact protection device without low-deformation supports and energy-absorbing crusher zones.
SUMMARY OF THE INVENTION
Accordingly, an object of the invention is to provide a new and improved safety device for passenger vehicles.
Another object of the invention is to further enhance the protection of passengers during an impact affecting a side of the vehicle.
These and other objects of the invention are attained by providing a safety device for a motor vehicle including an impact-resistant, low-deformation body part in the vicinity of a support structure which has a high resistance to deformation in a direction transverse to the direction of motion of the vehicle.
BRIEF DESCRIPTION OF THE DRAWINGS
Further objects and advantages of the invention will be apparent from a reading of the following description of preferred embodiments in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic diagram illustrating a lateral impact of one vehicle by another vehicle;
FIG. 2 is a sectional view of the diagram shown in FIG. 1 illustrating an impacted vehicle provided with representative embodiments of the safety device of the invention; and
FIG. 2a is a fragmentary sectional view similar to that of FIG. 2 showing another embodiment of the invention.
For convenience of reference, like components, elements, and features in the figures are designated by the same reference numerals.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the diagram shown in FIG. 1, an impacting vehicle 1 frontally collides with a side of a safety vehicle 2. The safety vehicle 2 includes two longitudinal side supports 3.1 and 3.2 having a high bending resistance which are integrated into the body of safety vehicle 2. Two seats 5.1 and 5.2, provided with integrated braces 6.1 and 6.2, which are buckle-resistant in the lateral direction, are located between opposite vehicle doors 4.1 and 4.2 provided with low-deformation sections. A low-deformation element 7, which may be a central tunnel provided with reinforcements, is located between the buckle-resistant braces 6.1 and 6.2.
When the impacting vehicle 1 collides with the left side of the safety vehicle 2, as shown in FIG. 1, the vehicle door 4.1, which has a low-deformation section, is impacted by the force of the collision. In this regard, the vehicle door 4.1 of the safety vehicle can be arranged so that part of the impact energy of impacting vehicle 1 is first reduced by deformation of the longitudinal support 3.1. According to the invention, the safety vehicle is arranged so that a much greater portion of the remaining impact energy is absorbed by the front or by the rear area of the impacting vehicle 1. In addition, a smaller portion of the remaining impact energy is transferred via the vehicle door 4.1, which has a low-deformation section, the two buckle-resistant braces 6.1 and 6.2, and the low-deformation element 7, to the other side of the safety vehicle 2 where the remaining impact energy can be converted into deformation energy. However, it is also conceivable that other vehicle body areas near the low-deformation element 7 have already reduced part of the impact energy.
With the safety device of the invention, the low-deformation section of the door 4.1 reduces the penetration depth of the impacting vehicle 1 into the passenger compartment of the safety vehicle 2. Referring to FIG. 1, the impact of the vehicle door 4.1 against the buckle-resistant brace 6.1 allows a passenger seated on the seat 5.1 to avoid the point of impact, thereby reducing considerably the injury hazard. Moreover, the low-deformation element 7 advantageously pushes the seat 5.2, along with the passenger in that seat, away from the point of impact. Thus, the distance between the seats 5.1 and 5.2 remains almost unchanged, and the passengers cannot injure each other. In this way, passenger protection is greatly improved with the safety device of the safety vehicle 2 since the force of impact of impacting vehicle 1 can be absorbed by body areas far removed from the point of impact and since relative motions of the passengers seated side by side cannot endanger them.
Providing a more detailed illustration of the embodiments of the safety device of the invention, FIG. 2 shows a sectional view of the safety vehicle 2 taken along a line perpendicular to a direction of travel. The buckle-resistant braces 6.1 and 6.2, shown as seat frames, are arranged on two schematically illustrated seat slide guides 8.1 and 8.2. These slide guides 8.1 and 8.2 are attached to a body floor 10 which is also provided with two door sills 9.1 and 9.2. The vehicle door 4.1 has a low-deformation section 11.1 totally surrounded by an outer door shell and by an inner door shell. Such a low-deformation door section may also have the form of the door section 11.2 arranged on the vehicle door 4.2. The low-deformation section 11.2 is not an integral part of the vehicle door 4.2; rather, the section 11.2 is an independent component mounted on the vehicle door 4.2. Another design characteristic of the vehicle door 4.2 is a claw-like projection 17, by which the vehicle door 4.2 engages the door sill 9.2 during a lateral impact. Wedgeshaped widenings 12.1 and 12.2 at the outer ends of the buckle-resistant braces 6.1 and 6.2 may be impacted by the door sections 11.1 and 11.2. The ends of the braces 6.1 and 6.2 adjacent to the low-deformation element 7 also have wedgeshaped widenings 13.1 and 13.2 to provide better force absorption. In addition, the buckle-resistant brace 6.2 and the low-deformation element 7 have catch plates 14 and 15, respectively. Finally, the vehicle doors 4.1 and 4.2 have paddings 16.1 and 16.2, respectively.
During an impact of the vehicle 1 against the safety vehicle 2, the low-deformation door section 11.1 is affected first. The impact energy is transferred from this component through the buckle-resistant brace 6.1, the low-deformation element 7, the buckle-resistant brace 6.2, and the low-deformation door section 11.2 to the other side of the vehicle body. The slide guides 8.1 and 8.2 are arranged to provide minimum resistance to lateral movements of the seats 5.1 and 5.2 in case of a lateral impact. The geometry and strength of the catch plates 14 and 15 are arranged so that the components located along the path of impact force flow cannot slide over one another.
The design of the vehicle doors 4.1 and 4.2 is especially important in the safety device of the invention. To passengers on the side of impact, the doors represent a life-saving barrier against an object impacting from outside. Consequently, the design of inner and outer sides of the safety doors requires special consideration. FIG. 2 illustrates two embodiments of the safety door design.
As FIG. 2 shows, the vehicle door 4.1 has a partial padding 16.1 in areas of the door that must be flexible for passenger safety. The low-deformation lower door section 11.1 is totally surrounded by the outer and inner shells of the vehicle door 4.1. However, arrangements in which the low-deformation lower door section 11.1 is fully covered only by the outer shell are also possible. The low-deformation lower door sections 11.1 and 11.2 may, for example, be made of fiber-reinforced synthetic material, of light metal, or of a synthetic material-steel composite. In a lateral impact, the lower edge of the vehicle door 4.1 will be displaced relative to the door sill 9.1. Good collision protection and force transfer, together with light weight, are desirable features for any new design of a vehicle door.
In another embodiment of the safety door, the door 4.2 in FIG. 2 has full padding 16.2. One original feature of the vehicle door 4.2 is its two-part design with an upper part 18 and a low-deformation lower section 11.2. These door sections may be manufactured separately and assembled as independent components into a safety door. Such a safety door is well suited for a safety vehicle equipped with a safety device according to the invention. A door arrangement such as the vehicle door 4.2 can also be used in vehicles using the lower door section 11.2 as impact protection and not as a force transfer element in case of lateral impact. Another feature of the vehicle door 4.2 is the projection 17 on the lower door section 11.2 which provides a claw-like engagement between the door 4.2 and the door sill 9.2. This arrangement allows partial deflection of the impact energy to the longitudinal support 3.2 of the safety vehicle 2. Of course, the individual features of the vehicle doors 4.1 and 4.2 may be combined in any manner.
The design of a safety door must take into account that a front area, a rear area, or a side area of the impacting vehicle may impact against the safety door. In addition to safety considerations, other aspects, such as convenient entry, automated assembly, and possible use of available standard parts, should be taken into account.
The safety device of the invention can also be arranged so that the door sills 9.1 and 9.2 have the main function of transferring impact energy to the buckle-resistant braces 6.1 and 6.2. FIG. 2a shows a similar arrangement in which the door sill 9.2 includes an impact-resistant, low-deformation body part 3.2. This requires the impacting vehicle 1 to have a bend-resistant support perpendicular to the longitudinal direction of the vehicle and approximately at the height of the door sills 9.1 and 9.2, as described in German Offenlegungsschrift No. 36 07 171. The vehicle doors 4.1 and 4.2 can also be designed so that the low-deformation lower door sections 11.1 and 11.2 and the door sills 9.1 and 9.2 impact against the buckle-resistant braces 6.1 and 6.2 jointly.
Although the invention has been described herein with reference to specific embodiments, many modifications and variations of the invention will readily occur to those skilled in the art. Accordingly, all such variations and modifications are included within the intended scope of the invention.
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In order to protect passengers during an impact affecting a side of a vehicle, a safety device is provided in a motor vehicle. The safety device comprises an impact-resistant, low-deformation body part and a support structure adjacent to the low-deformation body part attached to the vehicle body. The support structure exhibits extremely low deformation in a direction perpendicular to a direction of travel so that impact energy resulting from a side impact may be transferred through the vehicle by engagement of the low-deformation body part with the low-deformation support structure. As a result of these features, the safety device opposes penetration of an impacting object into a passenger compartment and provides good collision protection and force transfer.
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BACKGROUND OF THE INVENTION
The present invention relates to the fixation of water-soluble, carboxyl-containing vinyl monomers on fibrous substrates in the form of polymeric compositions and to the method of accomplishing the same.
Methods have been provided for the deposition of preformed polymeric materials on fibers or fabric substrates and for the development of graft polymers on fibrous or fabric substrates. The deposition of preformed polymers provides a means for modifying the surface properties of fibers and fabrics, but this method is characterized by several limitations and deficiencies. The preformed polymer is viscous if dissolved in the medium in which it is applied; or it is present in a particulate form as an emulsion or dispersion in a continuous phase which is often water. In either case the penetration of the polymer into the fabric or the yarns or the fibers occurs slowly, being limited by the size of the dispersed particles or the size of the molecular species. As a consequence, penetration is limited and is relatively poor, polymer concentrates at fiber crossover points, and stiffness becomes pronounced even at low levels of polymer deposition.
In the case of graft polymerization on fibers and fabric substrates, numerous methods are now known for accomplishing such reactions. The most common reactions involve free-radical initiation by one of a variety of means such as peroxide catalyst, high or low energy irradiations, heat, oxidation-reduction reactions, and electrical discharge. Each of these means of generating free radicals is subject to practical limitations as described by K. Hoshino in Chemical Aftertreatment of Textiles, ed. H. F. Mark, M. S. Wooding, and S. M. Atlas, Chapter VB, p. 235, Wiley-Interscience, New York, 1971, by E. H. Immergut in Encyclopedia of Polymer Science and Technology, Vol. 3, p. 242, Interscience Publishers, New York, 1965, and by J. C. Arthur, Jr. in Macromolecular Chemistry, Vol. 2, p. 1, Academic Press, London, 1970.
Two interrelated problems appear to be responsible for the difficulties experienced in thorough cleaning (and preventing soil staining) of fabrics composed of polyester, nylon, or durable-press synthetic fiber/cotton blends in aqueous wash baths such as employed in home and commercial laundry washing machines. Compared to unmodified cotton, synthetic fibers and durable-press cotton fibers display somewhat more hydrophobic surface properties that prevent good water penetration in the fibers for removal of soil therefrom; moreover, synthetic fibers are of an oleophilic nature. Thus the first problem involves the attraction of dirt and oily grime to the synthetic fibers; these become embedded therein and are not removed during subsequent washing cycles because of the inability of water to thoroughly penetrate the synthetic fibers in a manner similar to the swelling of unmodified cellulosic fibers in water. Second, and also due to the above described surface properties, oily soil materials that are washed out of the fabric during the laundering operation are continuously attracted to the surface of the fabric and become redeposited thereon. As a result, the fabric never returns to a truly clean condition and, instead, assumes a discolored, stained appearance which eventually renders it unfit for further use. The present invention obviates the problem of soiling and staining by modifying the surface characteristics of natural and synthetic fiber-containing fabrics, as fully disclosed hereinafter.
A substantial increase in the hydrophilic characteristics of chemically modified or finished cotton, cotton/synthetic fiber blends, and synthetic fibers is desirable and consistent with improvements in antistatic characteristics and comfort in apparel as well as improvements in soil release and the reduction in soil redeposition.
It is accordingly a primary object of the present invention to provide for a deposition and polymerization of water-soluble carboxyl-containing vinyl monomers, alone and in combination with other vinyl monomers, in and on fibrous and fabric substrates in a single stage operation utilizing a single aqueous reaction medium for conveying the reactions systems to the fibers or fabrics.
It is further object of the present invention to provide a simplified method of simultaneous polymerization and crosslinking to form a network polymeric material deposited in and on the fibrous or fabric substrate in a highly durable manner.
It is another object of the present invention to provide a process of fixing polymers on fibrous and fabric substrates with high efficiency of conversion of monomers so that the monomers are neither wasted by polymerization in a solution phase away from the substrate nor are lost by volatilization in the curing step.
It is a still further object of the present invention to produce chemically modified fibers and fabrics that are improved in hydrophilic characteristics, comfort, soil release, resistance to soil redeposition, antistatic properties, dyeing behavior, and pleasing hand.
It is an additional object of the present invention to achieve the modification of surface and bulk properties of fibers, yarns, and fabrics by an efficient polymerization and fixation of monomers, which reactions do not depend upon grafting or polymer chain initiation from the molecular chains of the substrates for development of durable fixation of the polymer to the substrate.
It is another object of this invention to provide a process for the fixation of polymers in and on fibrous substrates, which process is free of one or more of the limitations or disadvantages of prior art coating processes involving preformed polymers or prior art graft polymerization processes.
THE INVENTION
It has now been found that certain carboxyl-containing vinyl monomers can be deposited, polymerized, and fixed rapidly and efficiently in and on various types of fibers by a process wherein the aqueous solution of carboxyl-containing vinyl monomers is brought to a pH above 3.6, combined with a free-radical initiator with or without additional comonomers, applied to a fibrous substrate, and subjected to curing conditions during which the vinyl monomer(s) is polymerized and fixed in and on the fibrous substrate.
The polymer fixation that are a subject of this invention are novel in several respects. In copending application, PC 6045, it is shown that water-soluble vinyl monomers can be polymerized and durably fixed to fibrous substrate in a simple, rapid, and effective manner. Various carboxyl-containing vinyl monomers undergo polymerization and fixation to the various fibrous substrates when treated according to the conditions described in the aforementioned application. Among the monomers cited in the aforementioned application, carboxyl-containing vinyl monomers exhibited lower levels of efficiency of conversion to polymer than other water-soluble monomers. This is not unexpected, because monomers of this type have been observed by previous investigators to be more sluggish in graft polymerization to the point that substantially less polymer was fixed or to the point that little or no polymer was formed at all.
It has now been unexpectedly discovered that the conversion of carboxyl-containing vinyl monomers to polymer under the conditions described in the aforementioned application can be increased substantially, in some cases to the theoretical maximum conversion that is possible, by raising the pH of the reaction medium above a level of 3.6 by the introduction of basic materials. Carboxyl-containing vinyl monomers are moderately strong acids, readily generating pH values below 2.0 in aqueous media. For reasons that are not completely understood, it is now evident that by raising the pH of reagent solutions involving carboxyl-containing vinyl monomers to values above 3.6, the conversion of monomers to polymers is improved very substantially. While all bases are beneficial in this regard, certain bases are more effective than others in raising the efficiency of conversion of monomers to polymers. This is evidently not the simple consequence of converting the carboxyl-containing vinyl monomer to a water-soluble form, because the carboxyl-containing vinyl monomers of this invention are water soluble in the acid form. It is, therefore, surprising that raising the pH values of reagent solutions involving carboxyl-containing vinyl monomers exerts such a beneficial effect on the efficiency of conversion of monomers to polymers.
In order to achieve the desired conversions of monomers to polymers and desired fixation of these polymers to substrates, it is necessary to conduct the polymerization or curing step under controlled conditions such that contact with air during this stage is not excessive. In general, the curing step may be conducted in the complete presence of air when the transfer of heat to the substrate is achieved through conduction from hot solid surfaces such as rolls, "cans," calender, press, or conventional household iron. Similarly, special precautions to exclude oxygen or air are not essential when steam or solvent vapors are the heat transfer media. However, when the transfer of heat to the substrate impregnated with aqueous reagent solution is through the gaseous stage, it is desirable that air be diluted with an inert gas such as nitrogen, carbon dioxide, or steam; a direct blast of hot air on the fibrous substrate impregnated with the aqueous solution of reagent is undesirable and detrimental to polymerization and fixation. It is not essential that air or oxygen be completely absent; the extent of dilution that is required is relatively low since the vaporization of water from the reagent solution provides a degree of dilution that is sufficient in some cases.
Although it is not essential in order to achieve the objective of this invention, it is beneficial to include small amounts of water-soluble, di- or polyfunctional vinyl monomers. The presence of such comonomers has the general effects of raising the efficiency of conversion of monomer to polymer by a few percentage points and of improving the durability of the fixed polymer to more strenuous conditions of extraction.
The essence of the invention, then, is the realization of high levels of efficiency of conversion of certain carboxyl-containing vinyl monomers, with and without comonomers, to polymers under controlled conditions of cure that are well suited to use in textile mills to obtain modified substrates wherein the hydrophilic characteristics conferred by the fixed polymers are the basis for valuable performance qualities in the fibers, yarns, and textile products.
The primary monomers of this invention are water-soluble, carboxyl-containing vinyl compounds illustrated by the following: acrylic acid, methacrylic acid, itatonic acid, maleic acid, and fumaric acid. The comonomers of this invention are water-soluble vinyl monomers, generally selected from the acrylic monomer series, as illustrated by: acrylamides, methacrylamides, diacetoneacrylamide, and the N-alkyl and N-methylol derivatives thereof; hydroxyethylacrylamide, hydroxyethylmethacrylamide; dimethyl-2-hydroxypropylaminemethacrylimide; aminoethyl acrylate and methacrylate; hydroxyethyl acrylate and methacrylate, and hydroxypropyl acrylate and methacrylate; and dialkylaminoethyl acrylates and methacrylates.
The catalysts or initiators that are preferred for this invention are: ammonium and alkali metal persulfates, hydrogen peroxide, t-butyl-hydroperoxide, peracetic acid, and combinations of these.
Water-soluble di- or polyfunctional vinyl reagents such as methylenebisacrylamide and 1,3,5-triacrylolhexahydro-s-triazine are employed with beneficial effects in this invention.
The bases that have been found to be desirable and suitable for this invention are those involving the alkali and the alkaline earth metals, which may be employed as hydroxides, oxides, carbonates, or other less basic forms such as bicarbonates, silicates, and phosphates. Ammonia or ammonium hydroxide may be beneficially employed to neutralize the carboxyl-containing vinyl monomers of this invention. Organic bases are also effective; methyl and ethyl amines and pyridine may be employed. Quaternary ammonium hydroxides such as tetramethylammonium hydroxide tetraethylammonium hydroxide tetra(hydroxyethyl)ammonium hydroxide, and tribenzylammonium hydroxide are suitable for neutralization of the carboxy-containing monomers in the process and products of this invention.
A wetting agent is commonly employed, although not essential, to facilitate the contact of the vinyl monomers with the substrates and to aid penetration into the substrates. The agents that are preferred are alkali metal alkylsulfosuccinates and ethylene oxide derivatives of phenols and alcohols.
The following are among the substrates which may be treated by the process of this invention: cotton fibers and fabrics; rayon fibers and fabrics; paper and nonwoven fabrics; nylon fibers and fabrics; polyester fibers and fabrics; cellulose acetate and triacetate fibers and fabrics; polyethylene and polypropylene fibers and fabrics; spandex fibers and fabrics; acrylonitrile polymer and copolymer fibers and fabrics; wool, silk, jute, ramie, and flax fibers and fabrics; and blends of cotton with any and all of the fibrous materials noted above.
The vinyl monomers, initiators, and wetting agents are dissolved in water and the pH of the system is raised to value above 3.6. A portion of the carboxyl-containing vinyl monomers is thus converted to the salt form, this apparently being an essential feature of the invention because it appears to be directly responsible for a substantial increase in the rate of polymerization and the extent of conversion of monomers to polymers. The actual process of polymerization of monomers and fixation of polymers onto the various fibrous substrates involves application of the aqueous solution of monomers and initiator to the substrate, and subjection of the wet substrate to curing conditions at elevated temperatures.
DESCRIPTION OF PREFERRED EMBODIMENTS
The following examples are given to further illustrate the present invention. The scope of the invention is not, however, meant to be limited to the specific details of the examples.
EXAMPLE 1
The effects of pH and of curing conditions upon the efficiencies of conversion of monomer on fabric to polymer on fabric are illustrated in results summarized in the following table. In all of these cases the reagent solution contained 15 parts of acrylic acid, 0.5 parts of ammonium persulfate, a trace of wetting agent, ammonium hydroxide to adjust the pH to the level indicated, and water to bring the total to 100 parts by weight. Fabric was impregnated with the reagent solution and passed through squeeze rolls to obtain wet pickups in the range of 95-105%. Samples of fabric were cured under various conditions: (A) 10 minutes at 120° C in a forced draft oven followed by 8 minutes at 160° C in a forced draft oven, (B) 10 minutes at 130° C in a plastic bag followed by 8 minutes at 160° C in a forced draft oven, (C) 5 minutes at 130° C in a nitrogen-steam atmosphere followed by 8 minutes at 160° C in a forced draft oven, and (D) 10 minutes at 120° C in a nitrogen-steam atmosphere. Pin frames to maintain the fabric at the original dimensions throughout the cure were generally useful. Cured fabric samples were washed vigorously in hot running tap water for 20-30 minutes and air dried at room temperature. The conversions of monomer to polymer are calculated from the wet pickups of reagent solution and the weight gains of the air-equilibrated fabrics after vigorous washing. The reagent solution containing no base had a pH of 2. The pH values were adjusted upward with ammonium hydroxide. Results are summarized in the table below.
______________________________________pH Cure Add-on (%) Conversion (%)______________________________________2.0 A 2.1 142.0 B 4.2 282.0 C 4.6 312.0 D 4.7 314.0 A 4.6 374.0 B 7.5 504.0 D 7.8 526.0 A 8.0 536.0 B 11.3 766.0 D 10.7 718.0 A 8.4 568.0 B 10.3 688.0 D 11.1 74______________________________________ Samples of fabric subjected to cures between aluminum plates at 140° C or by ironing with a conventional household iron at the "cotton setting" were characterized by conversions of monomer to polymer very similar to those tabulated above for curing condition D.
EXAMPLE 2
The beneficial effect of small amount of di- and polyfunctional vinyl compounds is illustrated in this example. Reagent solutions were prepared from 14.5 parts of acrylic acid, 0.2 parts of di- or polyfunctional vinyl monomer, a trace of wetting agent, ammonium hydroxide to adjust the pH to 7.0, 0.5 parts of ammonium persulfate, and water to bring the total to 100 parts by weight. The di- and polyfunctional agents were methylenebisacrylamide (I) and trisacrylolhexahydro-s-triazine (II). Samples of fabric were impregnated with reagent solutions, passed through squeeze rolls to obtain wet pickups of approximately 100%, placed on pin frames, cured (A) for 10 minutes at 120° C in a forced draft oven in air or (B) for 5 minutes at 120° C in a steam-nitrogen atmosphere, rinsed extensively in hot running tap water, and air dried. The results are tabulated below.
______________________________________PolyfunctionalVinyl Reagent Cure Add-on (%) Conversion (%)______________________________________None A 4.1 27I A 11.8 79II A 12.9 86None B 4.6 31I B 16.1 107.sup.aII B 17.5 117.sup.a______________________________________ .sup.a Apparent conversions above 100% are due to experimental error and to the fact that products of this type have higher moisture regain values than the original cotton; thus, a fraction of the apparent add-on is due to increased moisture content in the polymer-containing fabric.
EXAMPLE 3
Reagent solutions made up to contain 14.5 parts of acrylic acid, 0.5 parts of methylenebisacrylamide, a trace of wetting agent, 0.5 parts of ammonium persulfate, ammonium hydroxide to adjust the pH to 7.0, and water to bring the total to 100 parts by weight were applied to cotton fabric by immersion and squeezing. Impregnated samples of fabric were subjected to cures as follows: (a) 40 minutes at 60° under nitrogen, (b) 20 minutes at 80° C in nitrogen, (c) 10 minutes at 100° C in nitrogen-steam, (d) 5 minutes at 120° C in nitrogen-steam, and (e) 1 minute at 160° C in nitrogen-steam. The respective conversions of monomer on fabric to polymer durably fixed to the fabric (following washing treatments as described in the preceding examples) were as follows: (a) 2.9%, (b) 77%, (c) 116%, (d) 110%, and (e) 114%.
EXAMPLE 4
The effectiveness of ammonium and sodium hydroxides for increasing the extent of conversion in polymerization of acrylic acid is illustrated in the results summarized here. Reagent solutions were prepared from 14.5 parts of acrylic acid, 0.5 parts of methylenebisacrylamide, 0.483 of ammonium persulfate, a trace of wetting agent, base to adjust the pH to the desired level, and water to bring the total to 100 parts by weight. Samples of fabrics were impregnated, cured, washed thoroughly, and air dried. The cure was for 5 minutes at 120° in an atmosphere of steam-nitrogen; the wash was a one-hour boil in distilled water following a vigorous wash in hot running tap water. The results are summarized in the table below.
______________________________________ Conversion (%)______________________________________pH NH.sub.4 OH NaOH______________________________________1.8 (29).sup.a (29).sup.a3.5 25 284.0 52 555.0 61.3 1047.0 65 1258.8 69.5 --9.6 -- 127______________________________________ .sup.a The pH value of 1.8 was the result of no neutralization with base.
Polymerizations that were conducted with reagent systems neutralized with LiOH and KOH resulted in polymerization efficiencies very similar to those listed above for systems neutralized with NaOH.
EXAMPLE 5
Reagent solutions were prepared to contain 14.5 parts of methacrylic acid, 0.5 parts of methylenebisacrylamide, 0.5 parts of ammonium persulfate, a trace of wetting agent, sodium hydroxide to adjust the pH to the desired level, and water to bring the total to 100 parts. Samples of cotton/polyester (50/50) blend fabric were impregnated with the reagent solutions, cured for 5 minutes at 120° in steam-nitrogen, washed vigorously in hot running tap water and boiled for one hour in distilled water, and air dried at room temperature. The percentages of conversion of monomer on fabric to durably-attached polymer on fabric were as follows: at pH 2.2 (no neutralization), 10%; at pH 3.5, 11%; at pH 4.0, 35%; at pH 5.0, 51%; at pH 7.0, 82%; and at pH 11.0, 75%.
EXAMPLE 6
Reagent solutions were prepared to contain 14.5 parts of acrylic acid, 0.5 parts of methylenebisacrylamide, 0.5 parts of sodium persulfate, a trace of wetting agent, organic amino compounds as indicated in the tables below, and water to make the total up to 100 parts by weight. Cotton fabric was employed. Impregnation, cures, washing procedures and drying procedures were similar to those described in example 5. The results are summarized in the following table.
______________________________________ Extent of Neutralization ConversionOrganic Amine with Amine (%)______________________________________Diethylamine to pH = 7.0 51%.sup.aEthylenediamine to pH = 7.0 75%.sup.bDiethylaminoethyl acrylate to pH = 5.0 59%.sup.c______________________________________ .sup.a Only 24% of the original amine remained in the final fixed on the fabric. .sup.b As measured by nitrogen-content of the dry fabric containing the fixed polymer, 63% of the amine remained with the polymeric acid. .sup.c In this case, 48% of the amino compounds remained associated with the polymeric acid that was fixed on the fabric.
Triethanolamine, tetramethylammonium hydroxide, and tetra(hydroxyethyl) ammonium hydroxide, when employed as above to bring the pH of acrylic acid into the range of 5-7, yielded results very similar to those obtained and described for ethylenediamine. In the case of pyridine and piperazine, the results were generally similar to those obtained with diethylamine.
EXAMPLE 7
Reagent solutions were made up to contain 7.25 parts of polymerizable carboxyl-containing monomer, 7.25 parts of comonomer, 0.5 parts of methylenebisacrylamide, (MBA) or 0.2 parts of tris(acryloyl)hexahydro-s-triazine(THT), 2.0 parts of sodium persulfate, 0.1 part of wetting agent (Tergitol TMN), base to adjust the pH to a value of 7.0, and water to bring the total to 100 parts by weight. Samples of durable-press cotton/polyester (50/50) fabric were impregnated with the reagent solutions, cured for 5 minutes at 120° in an atmosphere of steam-nitrogen, washed vigorously for 20-30 minutes in hot running tap water and boiled for one-hour in distilled water, and air dried. The results that were obtained from these polymerizations with and without the adjustment of the pH with base are summarized in the following table.
__________________________________________________________________________Carboxyl-containing Di- or polyfunctional Add-on ConversionMonomer Monomer Comonomer Base (%) (%)__________________________________________________________________________Acrylic acid MBA Hydroxyethyl meth- None 6.5 43 acrylateAcrylic acid " NaOH 13.5 75Methacrylic acid THT Diacetoneacrylamide None 7.2 50Methacrylic acid " 12.8 75__________________________________________________________________________
The above results illustrate the beneficial effects that follow from the neutralization of the carboxyl-containing monomer in copolymerizations. These beneficial effects carry over into various combinations and various ratios of combinations of carboxyl-containing monomers with comonomers.
EXAMPLE 8
Swatches of cotton fabric were treated with reagent solutions containing 14.5 parts of acrylic acid, 0.5 parts of methylenebisacrylamide, 0.5 parts of ammonium persulfate, a trace of wetting agent, base to adjust the pH to a value of 7, and water to bring the total to 100 parts. Cures were conducted at 120° for five minutes in a steam-nitrogen atmosphere. Samples of fabrics were washed vigorously in hot running tap water and given a one-hour boil in distilled water. Samples were air dried at room temperature and efficiencies of conversion of monomer to polymer were calculated from the wet pickups of reagent solution and the add-ons of durable polymer. These results are listed in the following table under the heading of "efficiency of polymerization." These same samples were subjected to a one-hour boil in 2% caustic containing 0.1% of surfactant (Triton 770). The percentage of the original polymer that was lost during this process is listed under the heading of loss during caustic scouring. Finally, the samples of fabric were soaked in 2% acetic acid and rinsed thoroughly. The weight loss that occurred as a result of this step is listed under loss due to acid scouring. Also summarized in the following table are data obtained from a sample of acrylic acid/cotton fabric graft copolymer prepared by the conventional high-energy irradiation initiation process.
__________________________________________________________________________ Loss of Polymer Loss of Efficiency of Due to Caustic Polymer Due to Polymerization Scouring Acid ScouringProcess (%) (%) (%)__________________________________________________________________________Acrylic acidneutralized withNH.sub.4 OH 70 3 18Acrylic acidneutralized withNaOH 100 + 13 13Acrylic Acidunneutralized 29 38 33Acrylic acidneutralized withCa(OH).sub.2 ; no difunctionalmonomer 95 64 100Acrylic acid graftpolymerized by highenergy irradiation -- 61 --__________________________________________________________________________
EXAMPLE 9
A reagent solution was prepared to contain 14.5 parts of acrylic acid, neutralized to pH 7 with sodium hydroxide, 0.5 parts of methylenebisacrylamide, 0.5 parts of ammonium persulfate, a trace of wetting agent, and water to bring the total to 100 parts by weight. Samples of fibrous materials were immersed in this solution, squeezed with rollers to express the excess reagent solution, subjected to cures for 5 minutes at 120° C in atmospheres of steam-nitrogen, washed vigorously in hot running tap water, boiled for one hour in distilled water, and air-dried at room temperature. The efficiencies of conversion of monomer on fabric to polymer durably fixed on fabric were calculated on the basis of the wet pickup of reagent solution and the durable polymer add-on to the fabric after the cure, etc. Results are summarized in the following table.
______________________________________Fibrous Composition Efficiency of Fixation (%)______________________________________Cotton Batting 100Cotton Pickerlap 100Cotton Yarn 100Paper 100Nylon Tricot 70Polyester (polyethylene terephthalate) 98Cellulose Acetate 82Polypropylene Fabric 79Spandex-nylon 95Acrylic Fabric (Orlon) 100Wool 100Flax 98Cotton/Polyester (50/50) 100Cotton/Polyester (35/65) 95Durable Press Cotton/Polyester(35/65) 95______________________________________
The efficiencies in these fixations of network polymer on the various substrates are almost independent of the nature of the substrate. Variation appears to be a function of the proper preparation of the substrate (removal of oils, lubricants, etc.) and the degree of wetting of the surface of the substrate that is achieved by the reagent solution, which is dependent upon the effectiveness of the wetting agent and, to some degree, upon the nature of the base used to neutralize the carboxyl-containing monomer.
EXAMPLE 10
In this example, the contribution of fixed polymer to fabric performance properties is illustrated. The illustration is based on treatment of an 80 ×80 cotton print cloth that was desized, scoured, and bleached prior to fixation of various levels of poly(sodium acrylate) network polymer on the fabric. The polymer was fixed on the cotton fabric by use of reagent solutions containing acrylic acid, methylenebisacrylamide, wetting agent, sodium hydroxide to adjust the pH to 7.0, and water. The concentrations of agents ranged downward from the 15% concentration of total monomers that is generally illustrated in the preceding examples.
Cures were conducted in the normal manner; all samples were given extensive washes in hot running tap water, boiling water, and boiling 2% caustic prior to air-drying and evaluation. Results are summarized in the following table.
__________________________________________________________________________ Cotton Containing Fixed Polymer__________________________________________________________________________ UnmodifiedPerformance Property Cotton 2% Add-on 5% Add-on 10% Add-on__________________________________________________________________________Moisture Regain 6.3% 7.8% 9.3% 11.6%Wicking Time (3 cm.) 48 sec. 17 sec. 22 sec. 26 sec.Water Vapor Perme-ability(g/24 hr.) 3.96 4.17 4.10 4.04Bending Moment(× 10.sup..sup.-4 in. lb.) 4.3 4.0 3.4 6.2Wet Wrinkle RecoveryAngle (°, W+F) 151 165 188 210Water of Imbibition 31 40 52 62__________________________________________________________________________
The increase in hydrophilic characteristics which are illustrated in this table and which are contributed to cotton fabric by the fixation of poly)sodium acrylate) in the cotton fabric carry over into other fibrous substrates. In general, the same performance characteristics that are listed above are increased when the same treatment is applied to cotton/polyester blend, 100% polyester, nylon, and acrylic fabric. The deposition and fixation of other polymers, that are exemplified in the disclosure of this invention, in various fibrous substrates generate increases in these same performance properties, although to degrees which depend upon the specific carboxyl-containing monomer, the comonomer, and the base involved in the neutralization of the carboxyl-containing monomers. On essentially all fibrous substrates, the carboxyl-containing polymers and copolymers contribute soft hand or full-bodied mellow hand. In all cases, soil release is improved, the improvement being the smallest for the fibrous substrate that starts out most hydrophilic in nature, such as cotton fabric, and the improvement being the largest in the case of the fabric which starts out most hydrophobic, such as polyester fabric. The polymer illustrated in this example contributes antistatic properties to hydrophobic fibrous substances such as nylon, polyester, and polypropylene.
EXAMPLE 11
A network polymer of acrylic acid and methylenebisacrylamide was applied to polyester fabrics by the general procedure described in Example 8; sodium hydroxide was employed to neutralize the acrylic acid and to bring the pH to 7.0. The samples of fabric were evaluated for change in wettability characteristics: the wicking test is a measure of the rate at which an aqueous solution of dye rises a vertical distance of 2 cm. and the results are expressed in seconds. The drop absorbency test is a measure of the time required for the complete absorption of a drop of water into the fabric; the time is recorded in seconds. In both of these cases the shorter the time, the better the hydrophilic characteristics are for the fabric. Results are summarized in the following table.
______________________________________ Add-on Wicking Time Drop AbsorbencyFabric (%) (2 cm.) sec. sec.______________________________________Pocketing fabricoriginal fabric -- 1200+.sup.a 1200+.sup.btreated fabric 6.8 345 66.3Twill fabricoriginal fabric -- 128.3 47.4treated fabric 13.8 22.3 1.7Knit fabricoriginal fabric -- 1200+.sup.a 1200+.sup.btreated fabric 12.9 47.7 2.0______________________________________ .sup.a In these cases the aqueous solution did not reach the 2 cm. level in the course of 1200 seconds. .sup.b In this case a drop of water was not absorbed in the course of 120 seconds.
EXAMPLE 12
A series of reagent solutions was prepared to contain itaconic acid (9.7 to 14.5%), methylenebisacrylamide (0.3 to 0.5%), sodium persulfate (0.3 to 0.5%), and water; in some cases, sodium hydroxide was added in molar equivalence to the itaconic acid. Cotton fabric was treated, cured, and washed as described in Example 4. The efficiency of conversion of monomer to polymer on fabric when the acid waS unneutralized was approximately 50%; when sodium hydroxide was introduced as indicated above, the efficiency of the conversion of monomer to polymer was 74-83%.
EXAMPLE 13
A series of cotton fabrics, cotton/polyester blend fabrics, and polyester fabrics was treated by the procedure described in Example 4 to introduce various levels of poly(sodium acrylate). After extensive rinsing in hot tap water and then boiling these samples for one hour in distilled water, it was found that approximately 60% of the stoichiometric amount of Na remained relative to the poly(acrylic acid). Comparison of textile properties of these modified fabrics with a corresponding set of fabrics containing unneutralized poly(acrylic acid) showed the following:
______________________________________Stoll flex abrasion resistance: equivalent at comparable add-onBreaking strength: equivalent at comparable add-onElongation: generally similarStiffness: lower for cotton- containing compositions bearing poly(acrylic acid) in Na formComfort-related hydrophilic characteristics (theseinclude moisture regain, water of imbibition, wickingtime, drop absorbency, and water vapor transmission)Soil resistance and release: very substantial superiority of poly(sodium acrylate)- fabrics in resistance to and release of aqueous soil and release of oily soil.______________________________________
It is notable that stiffness is lower for the poly(sodium acrylate)-fabrics compared to the poly(acrylic acid)-fabrics; the former, in the case of the cotton-containing compositions, were even lower in stiffness than the original unmodified fabrics until add-ons of approximately 8% were reached. The substantial superiority of the poly(sodium acrylate)-fabrics in soil resistance and release was maintained even though the laundry detergent contained basic materials (phosphates or carbonates) normally considered capable of introducing alkali metal ions into a polycarboxylic acid such as poly(acrylic acid).
Fabrics modified to contain poly (acrylic acid) in the form of Li, K, NH 4 or amine salts showed similar superiorities over the unneutralized poly(acrylic acid)-fabrics.
Fabrics modified to contain poly(sodium methacrylate) according to Example 5 or poly(sodium itaconate) according to Example 12 exhibited superiorities over the unneutralized polymer-modified fabrics similar to those summarized above for the poly(sodium acrylate)-fabrics.
Fabrics modified to contain copolymers of acrylic acid, methacrylic acid, or itaconic acid with substantial portions of the carboxyl groups neutralized to introduce Na, K, Li, NH 4 or amine cations exhibited trends of performance property differences in the direction indicated above. In cases involving non-ionic comonomers the efficiency of conversion of monomers and performance of the modified fabric were superior when the carboxyl-containing monomers were neutralized to or above pH 3.6; the desirable differences summarized above for the poly(cation acrylate)-fabrics became disappearingly small as the mole ratio of carboxyl-containing monomer to comonomer decreased below 0.3:1.0. The preferred comonomers in this regard include amides of acrylic and methacrylic acids and hydroxyalkyl esters of acrylic acid and methacrylic acid: specifically, they are acrylamide, methacrylamide; N-methylol acrylamide and methacrylamide; hydroxyethyl acrylamide and methacrylamide; diacetoneacrylamide, hydroxymethyldiacetoneacrylamide; and hydroxyethyl and hydroxypropyl acrylates and methacrylates.
Although illustrations of the process and products have been given in terms of fabric, the treatments can be applied equally as well to fibers in the form of batting, pickerlap, sliver, roving, or yarn. The following are among the substrates that may be treated beneficially by the process of this invention: cotton fibers and fabrics; rayon fibers and fabrics; paper, non-woven fabrics; nylon fibers and fabrics; polyester fibers and fabrics; blends of cotton fibers with nylon, polyester and other fibers; cellulose acetate and triacetate fibers and fabrics; polyethylene and polyproplene fibers and fabrics; spandex fibers and fabrics; acrylonitrile polymer and copolymer fiber and fabrics; wool, silk, jute, ramie, and flax fibers and fabrics.
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A fibrous material consisting of cellulosic or other natural fiber, synthetic fibers, or blends of various fibers is treated with an aqueous reagent system having a pH above 3.6 that is comprised of one or more carboxyl-containing vinyl monomers, a free-radical initiator, and a suitable base to adjust the pH. Comonomers and water-soluble di- or polyfunctional vinyl monomers may be included. Polymerization is conducted at elevated temperature in an atmosphere in which air may be diluted by steam and/or steam-nitrogen. The polymer is durably fixed to the fibrous substrate and contributes various special performance properties thereto.
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PRIORITY
[0001] This patent application claims priority to Indian application number 3893/CHE/2011, filed on Nov. 14, 2011, the contents of which are incorporated by reference herein in their entirety.
FIELD OF THE INVENTION
[0002] Technical field of the present invention relates to fast release solid oral compositions of entecavir or its pharmaceutically acceptable salts and process for preparing the same.
BACKGROUND
[0003] Chemically entecavir is 2-amino-1,9-dihydro-9-[(1S,3R,4S)-4-hydroxy-3-(hydroxymethyl)-2-methylenecyclopentyl]-6H-purin-6-one, monohydrate. Its molecular formula is C 12 H 15 N 5 O 3 .H 2 O, corresponding to a molecular weight of 295.3 and having the following structural formula:
[0000]
[0004] Entecavir is a guanosine nucleoside analogue indicated for the treatment of chronic Hepatitis B virus infection.
[0005] Entecavir is marketed under the trade name Baraclude® in United States by Bristol Myers Squibb in the form of oral tablets and solution.
[0006] U.S. Pat. No. 5,206,244 assigned to Squibb & Sons describes entecavir and its use as an antiviral agent.
[0007] U.S. Pat. No. 6,627,224 assigned to Bristol-Myers Squibb describes method of preparing pharmaceutical composition of entecavir by dissolving the entecavir and an adhesive substance in a solvent, followed by spraying said solution onto a carrier substrate while is in motion, then drying the coated carrier substrate to remove the solvent, and finally combining dried coated carrier substrate with other desired ingredients to form said pharmaceutical composition. The process described is time consuming, requires specialized expensive equipment like fluidized bed processor with controlled parameters such as temperature, airflow, spray rate and the like and is tedious.
[0008] Thus, there is a need to develop compositions of entecavir using simplified process that minimizes the need for specialized equipments and brings down the manufacturing cost and time.
[0009] Inventors of the present invention have developed the compositions of entecavir with specific excipients using simplified process that exhibited fast disintegration and short dissolving time with better blend/content uniformity, which were also found to be comparable with marketed Baraclude® tablets.
SUMMARY
[0010] The present invention relates to pharmaceutical composition comprising entecavir and one or more pharmaceutically acceptable excipients and process for their preparation.
[0011] In one embodiment, the present invention relates to fast release pharmaceutical composition comprising entecavir, a diluent selected from carbonates/bicarbonates of alkali metals or alkaline earth metals and an acid component.
[0012] In another embodiment, the present invention relates to fast release pharmaceutical composition comprising entecavir, acid component, carbonates/bicarbonates of alkali metals or alkaline earth metals, superdisintegrant and one or more pharmaceutically acceptable excipients.
[0013] In another aspect, the present invention provides pharmaceutical composition comprising entecavir, acid component, carbonates/bicarbonates of sodium, magnesium, potassium and calcium, superdisintegrant and one or more pharmaceutically acceptable excipients selected from diluent(s), binder(s), lubricant(s), and glidant(s).
[0014] In another embodiment, the present invention provides wet granulation process for preparing a pharmaceutical composition comprising entecavir and at least one pharmaceutically acceptable excipient.
[0015] Accordingly, the present invention provides a process for preparing compositions of entecavir by wet granulation method involving: (i) sifting and blending one or more excipients including carbonates/bicarbonates of alkali metals or alkaline earth metals optionally with entecavir to form a dry mix, (ii) granulating the dry mix of step no. (i) using drug solution to form granules followed by drying, (iii) blending the granules of step no. (ii) with remaining portion of excipients including acid component, optionally carbonates/bicarbonates of alkali metals or alkaline earth metals and finally compressing into tablets or filled in to capsules.
[0016] Further embodiment of the present invention relates to pharmaceutical composition comprising entecavir, where in the composition is free of sweetening agents and flavouring agents.
[0017] In a preferred embodiment, the present invention relates to pharmaceutical composition comprising 0.05-1% by weight of entecavir, 1-6% by weight of acid component, 1-90% by weight of carbonates/bicarbonates of sodium, magnesium, potassium and calcium and 1-20% by weight of superdisintegrant based on total weight of the composition.
[0018] In a specific embodiment, fast release pharmaceutical tablet composition comprises entecavir, citric acid, calcium carbonate and soy polysaccharide; wherein said composition is prepared by wet granulation method.
[0019] In yet another embodiment, the pharmaceutical compositions of the present invention comprising entecavir are useful for treating chronic Hepatitis B virus infection.
DETAILED DESCRIPTION
[0020] In accordance with the present invention the term “entecavir” includes entecavir in the form of free base, in the form of a pharmaceutically acceptable salt, amorphous entecavir, crystalline entecavir or any isomer, derivative, hydrate, solvate, or prodrug or combinations thereof.
[0021] The term “pharmaceutical composition” or “solid dosage form” or “solid oral compositions” as used herein synonymously include tablets, capsules, granules, mini-tablets and fast disintegrating tablets meant for oral administration.
[0022] The term “fast release compositions” according to the present invention refers to compositions meant for disintegration in the stomach in not more than 5 minutes, preferably less than 3 minutes, more preferably less than 1 minute.
[0023] The term “sweetening agents” refers to agents that mask the unpleasant taste of the drug.
[0024] The term “flavouring agents” refers to agents that impart flavour to the formulations.
[0025] The present invention relates to fast release pharmaceutical composition comprising entecavir, a diluent selected from carbonates/bicarbonates of alkali metals or alkaline earth metals and an acid component.
[0026] The present invention also relates to fast release pharmaceutical composition comprising entecavir, acid component, carbonates/bicarbonates of alkali metals or alkaline earth metals, superdisintegrant and one or more pharmaceutically acceptable excipients.
[0027] Suitable acid component according to the present invention include, but not limited to citric acid, tartaric acid, fumaric acid and ascorbic acid or mixtures thereof.
[0028] Suitable alkali metals according to the present invention include sodium, potassium or mixtures thereof.
[0029] Suitable alkaline earth metals according to the present invention include magnesium, calcium or mixtures thereof.
[0030] Suitable carbonates/bicarbonates of sodium, magnesium, potassium and calcium include, but not limited to sodium carbonate, magnesium carbonate, potassium carbonate, calcium carbonate, sodium bicarbonate, magnesium bicarbonate, potassium bicarbonate and calcium bicarbonate or mixtures thereof.
[0031] Suitable superdisintegrants according to the present invention include, but not limited to natural or synthetic superdisintegrants selected from soy polysaccharide, sodium starch glycolate, croscarmellose sodium, cross linked alginic acid, gellan gum and xanthan gum or mixtures thereof.
[0032] Preferably, natural superdisintegrant according to the present invention is selected from soy polysaccharide, cross linked alginic acid, gellan gum and xanthan gum or mixtures thereof. More preferably the natural superdisintegrant is soy polysaccharide.
[0033] In a preferred aspect, the present invention relates to pharmaceutical composition comprising 0.05-1% by weight of entecavir, 1-6% by weight of acid component, 1-90% by weight of carbonates/bicarbonates of sodium, magnesium, potassium and calcium and 1-20% by weight of superdisintegrant based on total weight of the composition.
[0034] More preferably, the present invention relates to pharmaceutical composition comprising 0.05-1% by weight of entecavir; 1-6% by weight of acid component; 1-90% by weight of carbonates/bicarbonates of magnesium and calcium; and 1-20% by weight of soy polysaccharide as superdisintegrant based on total weight of the composition.
[0035] More specifically, fast release pharmaceutical tablet composition comprises entecavir, citric acid, calcium carbonate and soy polysaccharide; wherein said composition is prepared by wet granulation method.
[0036] In an embodiment the present invention relates to fast release pharmaceutical composition comprising entecavir, acid component, carbonates/bicarbonates of sodium, magnesium, potassium and calcium, superdisintegrant, and one or more pharmaceutically acceptable excipients selected from diluent(s), binder(s), lubricant(s), and glidant(s).
[0037] Suitable diluents include, but are not limited to pregelatinized starch, talc, lactose, sugar, starches, modified starches, mannitol, sorbitol, inorganic salts, cellulose derivatives (e.g. microcrystalline cellulose), xylitol, lactitol, starch, kaolin, sucrose, mannitol, sorbitol, dextrates, dextrin, maltodextrin, dextrose, calcium sulfate, dibasic calcium phosphate, tribasic calcium phosphate, magnesium oxide and the like and mixtures thereof.
[0038] Suitable binders include, but are not limited to, carboxymethylcellulose sodium, pregelatinized starch, lactose, starches such as corn starch, potato starch, modified starches, sugars, guar gum, pectin, wax binders, microcrystalline cellulose, methylcellulose, carboxymethylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, copolyvidone, sodium alginate, acacia, alginic acid, tragacanth, gelatin, liquid glucose, povidone and the like and mixtures thereof.
[0039] Suitable lubricants include, but are not limited to, sodium stearyl fumarate, calcium stearate, magnesium stearate, zinc stearate, stearic acid, fumaric acid, palmitic acid, talc, carnauba wax, hydrogenated vegetable oils, mineral oil, polyethylene glycols and the like and mixtures thereof.
[0040] Suitable glidants include, but are not limited to, colloidal silica, calcium silicate, magnesium silicate, silicon hydrogel, cornstarch, talc and the like and mixtures thereof.
[0041] Sweetening and flavouring agents are essential when the compositions are meant for disintegration in the mouth to mask the taste of drug and to have better feel by the patient.
[0042] Fast release compositions of the present invention are not meant for disintegration in the mouth, accordingly compositions of the present invention are free of sweetening agents and flavouring agents.
[0043] In yet another embodiment, the present invention provides wet granulation process for preparing pharmaceutical composition comprising entecavir and at least one pharmaceutically acceptable excipient.
[0044] Wet granulation process comprise the steps of: (i) sifting and blending one or more excipients including carbonates/bicarbonates of alkali metals or alkaline earth metals optionally with entecavir to form a dry mix, (ii) granulating the dry mix of step no. (i) using drug solution to form granules followed by drying, (iii) blending the granules of step no. (ii) with remaining portion of excipients including acid component, optionally carbonates/bicarbonates of alkali metals or alkaline earth metals and finally compressing in to tablets or filled in to capsules.
[0045] When the dosage form is a tablet then it may additionally be coated with an aqueous or non aqueous solution or dispersion of film forming agents.
[0046] In another embodiment fast release composition of the present invention comprising entecavir is useful for treating chronic Hepatitis B virus infection.
[0047] The invention described herein can further be illustrated by the following examples but these do not limit the scope of the invention.
EXAMPLE 1-3
Entecavir Compositions Prepared by Wet Granulation
[0048]
[0000]
Example 1
Example 2
Example 3
Ingredients
Mg/tablet
Mg/tablet
Mg/tablet
Intra-granular ingredients
Calcium carbonate
304.2
304.2
320.2
Pregelatinized starch
40
40
40
Sodium starch glycolate
24
—
—
Croscarmellose sodium
—
24
—
Alginic acid
—
—
12
Sodium carboxy methylcellulose
0.8
0.8
0.8
Drug solution
Entecavir
1
1
1
Purified water
q.s.
q.s.
q.s.
Extra-granular ingredients
Citric acid monohydrate
8
8
4
Alginic acid
—
—
16
Croscaramellose sodium
—
16
—
Sodium starch glycolate
16
—
—
Lubrication
Sodium stearyl fumarate
6
6
6
Total tablet Weight
400
400
400
Brief Manufacturing Process:
[0049] i) Intra-granular ingredients were sifted and blended together,
[0050] ii) entecavir was added to hot water at 60° C. to 70° C. under stirring to get clear drug solution followed by cooling,
[0051] iii) the blended material of step no. (i) was granulated using drug solution of step no. (ii) and the resulted granules were dried and milled using a multimill or cone mill,
[0052] iv) milled granules of step no. (iii) were sifted through # 30 mesh completely,
[0053] v) extra granular ingredients were sifted together through # 40 mesh,
[0054] vi) sodium stearyl fumarate was sifted through # 60 mesh,
[0055] vii) materials of step no. (iv), (v) and (vi) were blended together and compressed into tablets or filled into capsules,
[0056] viii) compressed tablets were optionally coated with Opadry II Pink.
Study on Dissolution:
[0057] Dissolution test was performed for tablets of Example 1 to 3, in 1000 ml of 50 mM phosphate buffer pH 6.8 using paddle method at 50 rpm.
[0000]
TABLE 1
Cumulative % drug release
Time in minutes
Example 1
Example 2
Example 3
5
96
90
84
10
97
94
91
15
98
96
92
30
99
97
96
45
99
98
98
60
100
98
99
EXAMPLE 4-5
Entecavir Compositions Prepared by Wet Granulation
[0058]
[0000] Example 4 Example 5 Ingredients Mg/tablet Mg/tablet Intra-granular ingredients Calcium carbonate — 292.2 Magnesium carbonate 200.2 — Pregelatinized starch 132 40 Soy polysaccharide 32 32 Sodium carboxy methylcellulose 0.8 0.8 Drug solution Entecavir 1 1 Purified water q.s. q.s. Extra-granular ingredients Citric acid monohydrate 8 — Ascorbic acid — 8 Soy polysaccharide 20 20 Lubrication Sodium stearyl fumarate 6 6 Total tablet weight 400 400
Manufacturing Process: Same as given for Example 1.
Study on Dissolution:
[0059] Dissolution test was performed for tablets of Example 4 to 5, in 1000 ml of 50 mM phosphate buffer pH 6.8 using paddle method at 50 rpm.
[0000]
TABLE 2
Cumulative % drug release
Time in minutes
Example 4
Example 5
5
89
92
10
94
93
15
95
94
30
96
95
45
97
95
60
97
96
EXAMPLE-6
Entecavir Compositions Prepared by Wet Granulation
[0060]
[0000] Ingredients Mg/tablet Intra-granular ingredients Calcium carbonate 292.2 Pregelatinized starch 40 Soy•polysaccharide 32 Sodium carboxy methylcellulose 0.8 Drug solution Entecavir monohydrate 1 Purified water q.s. Extra-granular ingredients Citric acid monohydrate 8 Soy•polysaccharide 20 Lubrication Sodium stearyl fumarate 6 Total tablet weight 400
Manufacturing Process: Same as given for Example 1.
EXAMPLE-7
Comparative Composition
Entecavir Compositions Prepared by Dry Granulation Process
[0061]
[0000]
Ingredients
Mg/tablet
Intra-granular ingredients
Entecavir
1
Calcium carbonate
296.2
Soy•polysaccharide
30
Sodium carboxy methylcellulose
0.8
Pregelatinized starch
40
Sodium stearyl fumarate
2
Extra-granular ingredients
Soy•polysaccharide
20
Citric acid
8
Sodium stearyl fumarate
2
Total tablet weight
400
Brief Manufacturing Process:
[0062] i) Intra-granular ingredients were sifted and blended together,
[0063] ii) the blended material of step no. (i) was slugged/compacted and the resulted slugs/compacts were milled using multimill or cone mill,
[0064] iii) milled granules of step no. (ii) were sifted through # 30 mesh completely,
[0065] iv) extra-granular ingredients were sifted together through # 40 mesh,
[0066] v) sodium stearyl fumarate was sifted through # 60 mesh,
[0067] vi) materials of step no. (iii), (iv) and (v) were blended together and compressed into tablets or filled in to capsules,
[0068] vii) compressed tablets were optionally coated with Opadry II Pink.
Comparative Study on Dissolution and Disintegration Time:
[0069] Dissolution Profile (in 1000 ml of 50 mM phosphate buffer pH 6.8 using paddle method at 50 rpm) and disintegration time of Baraclude®, Example-6 (composition of the present invention) and Example-7 (composition prepared by dry granulation).
[0000] TABLE 3 Time in Cumulative % drug release Disintegration time minutes Baraclude ® Example 6 Example 7 Example 6 Example 7 5 88 92 78 28 sec 1-2 min 10 93 95 82 15 95 97 85 30 97 98 90 45 98 99 93 60 98 99 96
Comparison of blend uniformity for Example 6 and 7:
[0000]
TABLE 4
% labeled amount
S. No.
Example 6
Example 7
1
104
95
2
102
103
3
103
102
4
104
106
5
103
107
6
105
106
7
104
102
8
104
102
9
102
102
10
105
101
RSD (%)
1.06
3.31
[0070] The pharmaceutical composition prepared in Example 6 (wet granulation) and 7 (dry granulation) were tested for dissolution, disintegration and blend uniformity.
[0071] Results from Table 3, reveals that entecavir compositions of the present invention prepared by wet granulation have better dissolution and disintegration time.
[0072] The final blend was sampled with ten samples taken from different places in the storage container, and every sample was tested for assay. The results are summarized in Table 4, where “RSD” refers to the relative standard deviation. Thus as illustrated in Table 4, entecavir compositions of the present invention prepared by wet granulation have acceptable RSD limits, while those prepared by dry granulation suffer from a lack of blend uniformity.
EXAMPLE-8
Compositions of Entecavir Tablets (Free of Acid Component)
[0073]
[0000] Ingredients Mg/tablet Intra-granular ingredients Calcium carbonate 302.2 Pregelatinized starch 40 Soy•Polysaccharide 32 Sodium carboxy methylcellulose 0.8 Drug solution Entecavir 1 Purified water q.s. Extra-granular ingredients Soy•Polysaccharide 20 Lubrication Sodium stearyl fumarate 4 Total tablet weight 400
Manufacturing Process: Same as given for Example 1.
Comparative Study on Dissolution:
[0074] Dissolution test was performed for tablets of Example 6 and 8, in 1000 ml of 50 mM phosphate buffer pH 6.8 using paddle method at 50 rpm.
[0000]
TABLE 5
Time in
Cumulative % drug release
minutes
Example 8
Example 6
5
78
92
10
83
95
15
86
97
30
90
98
45
94
99
60
96
99
[0075] Results from Table 5, reveal that % drug release is better and comparable with Baraclude® in example 6 of the present invention (containing acid component) when compared with example 8 (entecavir compositions free of acid component).
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The present invention is directed to fast release pharmaceutical compositions comprising entecavir or its pharmaceutically acceptable salts, process for preparing the same and use of such compositions for the treatment of Hepatitis B virus infection.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is based upon and claims the benefit of priority from the prior Japanese Patent Application No. 2001-138727, filed May 9, 2001, the entire contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a switch box for a vehicle door apparatus having a powered door lock function.
2. Description of the Related Art
FIGS. 1 and 2 show the arrangement of part of a vehicle door lock device having a powered door lock function (see Jpn. Pat. Appln. KOKAI Publication No. 8-326387). Referring to FIGS. 1 and 2, a recess 2 is formed in the lower portion of the front surface of a synthetic-resin body 1 of the door lock device. A latch 3 and ratchet 4 are pivotally supported in the recess 2 by shafts 5 and 6 , respectively.
The latch 3 is biased counterclockwise in FIG. 1 by a spring (not shown). Upon a door closing operation, when the latch 3 engages with a striker 7 fixed to the car body, it rotates counterclockwise. Hence, the latch 3 rotates to its full-latch state through a state (a so-called half-latch state) where it engages with its half-latch stepped portion 8 .
A switch 34 is provided to abut against the side surface of the latch 3 . The switch 34 detects the full-latch state of the latch 3 which engages with the striker 7 fixed to the car body side when the door is closed.
The switch 34 has an electrical switch mechanism which is ON when the latch is in the full-latch state. As shown in FIG. 1, most of the switch 34 , excluding one end of its pin abutting against the side surface of the latch 3 , is housed in an actuator housing chamber 20 which houses a powered actuator unit 17 (to be described later).
The actuator housing chamber 20 is surrounded by a base case 18 and a cover case (not shown). The base case 18 is integrally formed with the upper portion of the body 1 . The cover case is fixed to the base case 18 .
A lock lever (not shown) is axially supported by the latch shaft 5 and is switched between a lock position and unlock position. The actuator unit 17 in the actuator housing chamber 20 switches this lock lever between the lock position and unlock position.
FIG. 2 is a view schematically showing the actuator unit 17 housed in the actuator housing chamber 20 together with the switch 34 . A gear 22 is fixed to the rotating shaft of a motor 21 . A gear disk 23 meshes with the gear 22 .
The gear disk 23 has a small-diameter gear 24 coaxial with it. A sector gear 25 rotatably axially supported by a shaft 26 meshes with the small-diameter gear 24 .
The sector gear 25 is held at a neutral position at the center by a spring (not shown). When the motor 21 rotates in the forward or reverse direction, the sector gear 25 rotates clockwise or counterclockwise.
A projection 28 is formed on the distal end of a change lever 27 fixed to the shaft 26 . The projection 28 engages with a wide recess 29 of the sector gear 25 with a lost motion linkage.
One end of the shaft 26 projects outward through the shaft hole of the cover case, and an output gear is fixed to this projecting portion. The output gear meshes with a gear portion formed on the lock lever.
The gear 22 fixed to the rotating shaft of the motor 21 rotates in the forward or reverse direction to rotate the gear disk 23 . Then, the small-diameter gear 24 integrally formed with the gear disk 23 rotates the sector gear 25 within a predetermined range from the neutral position at the center.
Thus, the projection 28 of the change lever 27 engaging with the large-width recess 29 with the lost motion linkage engages with the sector gear 25 over the lost motion linkage and is rotated by it. Then, an output gear 31 fixed to the other end of the shaft 26 of the change lever 27 is rotated to pivot a lock gear 14 through its gear portion 32 .
Therefore, the forward/reverse rotation of the motor 21 is transmitted to the lock lever (not shown) through a mechanism in the actuator unit 17 . Thus, the lock lever is switched from the lock position to the unlock position or vice versa. After this, power supply to the motor 21 is ended and the rotational torque of the motor 21 disappears. Then, the sector gear 25 is automatically restored to the neutral position at the center by the elasticity of the spring.
As described above, the switch 34 is housed in the actuator housing chamber 20 together with the actuator unit 17 . The distal end of the projecting pin of the switch 34 abuts against the side surface of the latch 3 .
In the switch 34 , one end of the pin biased by the spring projects to abut against the side surface of the latch 3 , as described above. The other end of the pin is connected to an electrical contact piece which is ON when the latch 3 is in the full-latch state.
Since a vehicle door lock device is attached and fixed to the inner side of the steel plate of a vehicle door, it is adversely affected by the atmospheric temperature more easily than various types of components provided in the vehicle compartment.
The switch 34 is housed in the actuator housing chamber 20 together with other actuator unit 17 and the like. However, since the switch 34 particularly has an electric contact or the like, it may result in an operation failure due to dew condensation or the like.
BRIEF SUMMARY OF THE INVENTION
It is an object of the present invention to provide a switch box for a vehicle door lock device, in which the adverse influence of dew condensation and the like caused by a temperature change is eliminated as much as possible so the operating state of a latch can be reliably detected under any condition.
A switch box for a vehicle door lock device for a vehicle door lock device, which is integrally housed in a lock body case and engages with and is fixed to a striker of a vehicle door, according to one aspect of the present invention is characterized by comprising: a slide pin which has one end abutting against a side surface of a latch that engages with and is fixed to the striker of a vehicle, and which slides in response to a pivot motion of the latch when biased by a spring; a slider which is connected and fixed to the other end of the slide pin and on which an elastic slide contact is disposed; a pair of terminals which are short-circuited to be connected to each other by the slide contact depending on a slide position of the slider; and a switch box cover which substantially hermetically covers most of the slide pin, excluding one end thereof abutting against the side surface of the latch, the spring, the slider, and the terminals in the lock body case, and the switch box cover has a through hole for ventilation at that position thereof which corresponds to a lower side of one side surface thereof when the switch box cover is attached to the vehicle door. The adverse influence of dew condensation and the like caused by a temperature change is eliminated as much as possible, so the operating state of the latch can be reliably detected under any condition.
Preferred manners of the switch box for a vehicle door lock device described above are as follows. The following manners may be used alone each, or may be appropriately combined.
(1) A path extending from the through hole for ventilation to an interior of the switch box is bent. The possibility that water may enter the switch box directly by any chance can be minimized.
(2) The switch box cover further has a through hole for drainage at that position thereof which corresponds to a lowermost end of one side surface of the switch box cover when the switch box cover is attached to the vehicle door. Water in the switch box can be drained immediately.
Additional objects and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objects and advantages of the invention may be realized and obtained by means of the instrumentalities and combinations particularly pointed out hereinafter.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the invention, and together with the general description given above and the detailed description of the embodiments given below, serve to explain the principles of the invention.
FIG. 1 is a cross-sectional plan view showing the arrangement of mainly a latch, ratchet, and car body striker in a conventional door lock device;
FIG. 2 is a cross-sectional plan view showing the arrangement of mainly an actuator unit in the conventional door lock device;
FIG. 3 is a perspective view showing the arrangement of a synthetic-resin body in a vehicle door lock device according to an embodiment of the present invention;
FIG. 4 is a perspective view showing the arrangement of a switch cover, slide pin, and slider;
FIG. 5 is a view for explaining a path extending from a vent hole to the interior of a switch box (a portion covered by the switch cover);
FIG. 6 is a perspective view showing the respective members that form the switch box;
FIG. 7 is a perspective view showing how the slider and slide pin are attached to the lower portion of the switch box; and
FIG. 8 is a perspective view showing how the switch cover is attached to the lower portion of the switch box.
DETAILED DESCRIPTION OF THE INVENTION
A vehicle door lock device according to an embodiment of the present invention will be described with reference to the accompanying drawings.
FIG. 3 is a view showing the arrangement of a synthetic-resin body 51 in the vehicle door lock device. As shown in FIG. 3, a switch box lower portion 52 is formed on the inner surface of the synthetic resin body 51 to be integral with it. A notch 53 is formed in part of the side wall of the switch box lower portion 52 . The notch 53 forms a vent maze (to be described later).
FIG. 4 is a view showing the arrangement of a switch cover 54 , slide pin 55 , slider 56 , and the like. The switch cover 54 is fitted in the switch box lower portion 52 to form a switch box. The slide pin 55 and slider 56 are sealed in the switch box.
Referring to FIG. 4, one distal end of the slide pin 55 provided in the body 51 forms a hemispherical shape and abuts against the side surface of a latch (not shown). A coiled spring 57 is mounted on the slide pin 55 . The other distal end of the slide pin 55 forms a stepped portion. This stepped portion is fitted in a stepped groove 56 a of the slider 56 . Hence, the slide pin 55 and slider 56 integrally slide in the switch box.
The slider 56 is formed of an insulating member. A slide contact 58 is attached and fixed to one side surface of the slider 56 . The slide contact 58 has a pair of open legs formed by bending an elastic metal plate.
The switch cover 54 has a thin structure. Thus, part of the side wall of the switch cover 54 which abuts against the notch 53 forms a recess 59 with respect to the surrounding wall surface. The recess 59 has a vent hole 60 at its one end. The vent hole 60 extends to that upper surface of the cover which corresponds to the lower side in FIG. 4 .
Assume that the switch box is formed by covering the switch box lower portion 52 with the switch cover 54 such that the inner surface of the side wall of the switch cover 54 abuts against the outer surface of the side wall of the switch box lower portion 52 . In this case, the bent vent maze formed of the vent hole 60 , recess 59 , and notch 53 realizes ventilation between the interior and the outer side of the switch box.
In addition, similarly to the vent hole 60 , a drain hole 64 is formed at that position in the switch cover 54 which is in the vicinity of the lowermost end of the switch box when the door lock device is attached to the vehicle door. The drain 64 extends to the upper surface of the cover.
A path extending from the vent hole 60 to the interior of the switch box (portion covered by the switch cover) will be described with reference to FIG. 5 . The vent hole 60 extending to the upper surface of the switch cover 54 is formed at the end of the recess 59 . Thus, the recess 59 is ventilated by the vent hole 60 extending to the upper surface of the switch cover 54 . The interior of the switch box communicates with the recess 59 through the notch 53 . In this manner, ventilation is ensured in the switch box. The path extending from the vent hole 60 to the interior of the switch box is bent twice, as is apparent from FIG. 5 . Therefore, direct entering of water from the vent hole 60 into the switch box can be avoided as much as possible. That portion of the switch cover 54 which is provided with the slide pin 55 communicates with the recess 59 through the notch 53 . That portion of the switch cover 54 which is provided with the slide pin 55 has the drain hole 64 . Thus, water in the switch box can be discharged immediately.
A protrusion 61 is formed on the inner side of the upper surface of the switch cover 54 . The protrusion 61 fits in a groove formed in the lower surface of the slider 56 to define the slide direction of the slider 56 . A stopper 62 formed of a protrusion and a pair of terminal retaining protrusions 63 are also formed on the inner side of the upper surface of the switch cover 54 . The stopper 62 regulates the slide range of the slider 56 . The pair of terminal retaining protrusions 63 are parallel to each other to sandwich the protrusion 61 , and press terminals (to be described later) against the inner bottom surface of the switch box lower portion 52 .
FIG. 6 is an exploded perspective view showing the respective members that are attached to the switch box lower portion 52 to form the switch box.
Terminal grooves are formed in the inner surface of the switch box lower portion 52 shown in FIG. 3. A pair of terminals 65 A and 65 B formed by bending are fitted in the terminal grooves from below in FIG. 6 . The slider 56 and the slide pin 55 are integrally placed above the pair of terminals 65 A and 65 B, as shown in FIG. 7 . The slider 56 has the slide contact 58 . The spring 57 is mounted on the slide pin 55 .
The switch cover 54 is attached and fixed to the switch box lower portion 52 through a waterproof packing 66 by threadable engagement of, e.g., three set screws 67 . Hence, the switch box as shown in FIG. 8 is completed.
One projecting end of the slide pin 55 in the switch box abuts against the side surface of the latch 3 (not shown) upon a biasing operation of the spring 57 , as shown in FIG. 7 . Thus, the slide pin 55 slides the slider 56 to a position corresponding to the pivoting state of the latch 3 . At a slide position where the latch 3 becomes full-latched, the slide contact 58 attached to the slider 56 short-circuits the pair of terminals 65 A and 65 B.
Therefore, whether or not the latch 3 is in the full-latch state can be known by, e.g., detecting electrical connection between the terminals 65 A and 65 B from the outside.
In the above arrangement, the switch cover 54 is attached to the switch box lower portion 52 by using the waterproof packing 66 as well. Thus, hermeticity in the switch box is maintained. Also, water and the like can be prevented from entering the switch box from the attaching surface of the switch cover 54 .
With an ordinary hermetic structure, when a sharp temperature change or the like occurs, dew condensation may occur in it. According to the present invention, even in such a case, ventilation between the interior and the outer side of the switch box is maintained through the vent hole 60 , as shown in FIG. 8 . Thus, no large temperature difference occurs. This minimizes the possibility of dew condensation in the switch box. Consequently, the operating state of the latch can be detected reliably.
Particularly, the vent path is formed in a bent manner of the vent hole 60 and recess 59 of the switch cover 54 , and the notch 53 of the switch box lower portion 52 . This minimizes the possibility of direct water entering into the switch box.
The drain hole 64 is formed at that position of the switch cover 54 which corresponds to the lowermost end when the door lock device according to this embodiment is attached to the vehicle door, as shown in FIG. 8 . Hence, even if water should enter the switch box, it can be discharged quickly.
The shapes and the like of the respective components of the present invention are not limited to this embodiment, but can obviously be appropriately modified in accordance with their mutual connection, engaging relationship, and the like.
The present invention is not limited to the embodiment described above, but can be modified and practiced in various manners within a range not departing from the spirit and scope of the invention.
The above embodiments include inventions of various stages, and various types of inventions can be extracted through appropriate combinations of a plurality of disclosed constituent elements. For example, assume that even when several constituent elements are eliminated from all constituent elements shown in the embodiment, at least one of problems described referring to the problems to be solved by the invention can be solved, and at least one of the effects described referring to the effect of the invention can be obtained. In this case, an arrangement from which these several constituent elements are eliminated can be extracted as an invention.
Additional advantages and modifications will readily occur to those skilled in the art. Therefore, the invention in its broader aspects is not limited to the specific details and representative embodiments shown and described herein. Accordingly, various modifications may be made without departing from the spirit or scope of the general inventive concept as defined by the appended claims and their equivalents.
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A switch box for a vehicle door lock device comprises a slide pin which has one end abutting against a side surface of a latch that engages with and is fixed to the striker and slides in response to a pivot motion of the latch, a slider which is connected and fixed to the other end of the slide pin and on which an elastic slide contact is disposed, a pair of terminals which are short-circuited to be connected to each other by the slide contact depending on a slide position of the slider, and a switch box cover substantially covering them in the lock body case, and the switch box cover has a through hole for ventilation at that position thereof which corresponds to a lower side of one side surface thereof when the switch box cover is attached to the vehicle door.
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TECHNICAL FIELD
This invention relates to one-part, solvent-free thermosettable prepolymer compositions, adhesives and coatings containing such compositions, and a method for "staging" said adhesives and coatings.
BACKGROUND ART
Prepolymer compositions which thermally cure into solidified adhesives and coatings should desirably be one part compositions. Multiple part adhesive and coating compositions must be carefully measured, thoroughly mixed, and promptly used, requirements which are inconvenient and may cause waste of materials.
Many adhesive and coating compositions must be dissolved or dispersed in an organic solvent before they can be applied to a workpiece. These solvents are environmentally hazardous and their use should be avoided whenever possible, see "Adhesion and Bonding", Enc. of Polymer Science and Technology, 1, 486, Interscience, 1964.
Processing applications such as printed circuit manufacture often employ "stageable" adhesives, that is, adhesive compositions which can be partially cured to a tack-free coating, fastened to an adherend, and cured using heat, pressure, or both (see. U.S. Pat. No. 4,118,377). The tack-free state is sometimes referred to as the "B-Stage".
Several compositions have been described which embody some but not all of the features of one part formulation, freedom from solvents, and stageability. For example, blocked polyisocyanates which can be used as one-part thermosetting adhesive or coating compositions have been described in Levine and Fech Jr., J. Org. Chem., 37, 1500 (1972), Levine and Fech Jr., J. Paint Tech., 45 (578) 56 (1973), U.S. Pat. No. 3,808,160, and British Patent Specification Nos. 970,459 and 1,085,454. However, these compositions begin to cross-link upon being heated to their deblocking temperature, and therefore cannot be readily B-staged.
U.S. Pat. No. 3,435,003 discloses a method for cross-linking a saturated condensation polymer backbone bearing furan groups by reacting it with a bis-maleimide. The starting polymer backbone is a solid at room temperature, and is mixed with the bis-maleimide by dissolving the polymer in a solvent with heating or by heating the polymer to its melting point. Upon cooling, the composition forms a solid and is said to cross-link to its cured state within a few days at room temperature. The composition of that patent would therefore be difficult to formulate as a one part, stageable composition.
Disclosure of Invention
It is an object of the present invention to provide a one-part, solvent-free thermosettable composition useful as an adhesive and coating. It is also an object of the present invention to provide a stageable adhesive composition with a long storage life in its B-staged state. It is an additional object of the present invention to provide an adhesive and coating composition with low viscosity, low sensitivity to moisture, and good adhesive properties.
The present invention provides, in one aspect, a one-part, solvent-free thermosettable adhesive and coating composition, comprising in admixture:
(A) a prepolymer having terminal isocyanate substituents of the formula: ##STR1## wherein R 1 is C 6 H 5 -- or a radical of the formula (R 2 ) 2 C═N-- with each R 2 being the same as or different from any other R 2 and selected from the group consisting of hydrogen atoms, aliphatic radicals of 1 to 6 carbon atoms and phenyl radicals, and wherein the prepolymer has a number average molecular weight greater than 400 and a melting point less than 95° C.;
(B) about 50 to about 100 mole percent, based on the number of moles of said prepolymer, of at least one difunctional primary or secondary amine or difunctional primary or secondary alcohol chain extender, said chain extender being soluble in said prepolymer at 95° C.;
(C) up to 100 mole percent, based on the number of moles of said prepolymer, of at least one monofunctional primary or secondary amine or monofunctional primary or secondary alcohol chain terminator, said chain terminator being soluble in said prepolymer at 95° C.; and
(D) a dienophile selected from the group consisting of:
(i) bis-maleimides of the formula: ##STR2## wherein R 3 is phenylene, alkylene, or a radical of the formula: ##STR3## wherein R 4 is --O--, --S--, methylene, or isopropylene; (ii) tris-maleimides of the formula: ##STR4## (iii) α,β unsaturated diketones having 6 to 22 carbon atoms; (iv) diacrylates having 8 to 22 carbon atoms;
(v) α,β unsaturated dialdehydes having 8 to 22 carbon atoms; and
(vi) α,β unsaturated dinitriles having 8 to 22 carbon atoms;
with said dienophile being soluble in said prepolymer at 95° C., and wherein at least one of said prepolymer, said chain extender, or said chain terminator has furyl or furfuryl substituents of the formula: ##STR5## wherein R 5 is a carbon, oxygen, sulfur, or nitrogen atom and n is 0 to 10, and wherein the number of moles of dienophilic sites in said dienophile is between about 30 and about 100 percent of the total number of moles of said furyl or furfuryl substituents in said prepolymer, said chain extender, and said chain terminator.
DETAILED DESCRIPTION
In the practice of the present invention, the prepolymer (A) is a straight chain or branched chain, substituted or unsubstituted, saturated or unsaturated, aliphatic or aromatic organic composition having terminal isocyanate groups which are blocked with a leaving group which deblocks at a temperature below about 150° to 175° C. The prepolymer may contain, for example, urethane, urea, ether, ester, amide, or acrylate linkages. Terminal isocyanate groups can be attached to the prepolymer by reacting a diol derivative of the prepolymer with an organic polyisocyanate such as toluene diisocyanate to form an isocyanate terminated polyurethane prepolymer, or by other methods well known in the art. The isocyanate groups can then be blocked with an oxime or a phenol following the procedures described in "Blocked Isocyanates", Z. W. Wicks, Jr., Progress in Organic Coatings, 3 (1975) 73-99. If the furyl or furfuryl groups (formula IV) are to be substituents on the prepolymer, then they can be attached to the prepolymer using methods well known in the art such as esterification of a hydroxyl group on the prepolymer with a furoyl halide, dehydration of a 1,4 diketone, or Michael addition of furyl or furfuryl amine to a suitable electron acceptor such as an α,β unsaturated ketone, a nitrile, or an acrylate. Mixtures of more than one prepolymer can be used in this invention. Commercially prepared prepolymers having terminal isocyanate groups and number average molecular weights up to about 3,000, but not containing furyl or furfuryl groups, are commercially available from E. I. du Pont de Nemours & Co. under the trademark "Adiprene" and from Mobay Chemical Corp. under the trademark "Mondour HCB". The ketoxime blocked prepolymer "Adiprene BL16" is a preferred prepolymer.
The chain extender (B) is a difunctional primary or secondary amine or alcohol. Diamines react more rapidly than diols with unblocked isocyanate groups and are preferred. If the furyl or furfuryl groups IV are to be substituents on the chain extender, then extenders which contain furyl or furfuryl groups IV are used, such as N,N-bis(2-hydroxyethyl)furfurylamine, N,N'-bis(furfuryl)-1,6-hexanediamine, N,N'-bis(furfuryl)-ethylenediamine, N,N'-bis(furfuryl)-1,10-decanediamine, bis(3-furfurylaminopropyl)methylamine, 1,4-bis(3-furfurylaminopropyl)piperazine, N,N'-bis-(furfuryl)-1,2-propylenediamine, N-methyl-N'-furfuryl-1,6-hexanediamine, 2-(furfurylamino)ethanol, N,N-bis(3-aminopropyl)furfurylamine, bis(3-furfurylaminopropyl)furfurylamine, N-furfuryl-1,3-propanediamine, furfurylsuccinic acid, 2-furfuryl-1,4-butanediol, N,N-bis(2-hydroxyethyl)-2-furanpropylamine, and 2,5 dihydroxymethyl furan. Diamine and diol chain extenders having about 2 to 18 carbon atoms but no furyl or furfuryl groups IV can also be used in the present invention. Suitable chain extenders which do not contain furyl or furfuryl groups IV include 4,4-methylenedianiline, 1,6-hexanediamine, 1,12-dodecanediamine, and 1,6-hexanediol. Mixtures of more than one chain extender can be used. Preferred chain extenders are N,N'-bis(furfuryl)-1,6-hexanediamine and 2,5-dihydroxymethyl furan. The chain extender is combined with prepolymer is a mole ratio between about 50 and about 100 percent, preferably between about 65 and about 85 percent, and most preferably at about 80 percent.
The chain terminator (C) is a monofunctional amine or alcohol. Amines react more readily than alcohols with unblocked isocyanate groups and are preferred. If the furyl or furfuryl groups IV are to be substituents on the chain terminator, then suiable chain terminators which contain furyl or furyl groups IV are used, such as furfurylamine or furfuryl alcohol. Monofunctional amine or alcohol chain terminators having about 1 to 18 carbon atoms but no furyl or furfuryl groups IV can also be used in the present invention, such as diethyl amine, methanol, and ethanol. Mixtures of more than one chain terminator can be used. A preferred chain terminator is furfurylamine. The chain terminator is combined with prepolymer in a mole ratio between about 0 and about 100 percent, preferably between about 15 and about 35 percent, and most preferably at about 20 percent.
The total amount of diamine or diol chain extender and amine or alcohol chain terminator should be sufficient to react with all of the prepolymer terminal isocyanate groups. Ordinarily a slight excess of chain extender and chain terminator is used in order to compensate for loss due to the volatility of these components.
The dienophile (D) undergoes Diels-Alder ring formation with furyl or furfuryl groups IV, thereby serving as a cross-linking agent. Suitable dienophiles include benzoquinone, ethylene glycol diacrylate, and non-activated (e.g. non-conjugated), sterically non-hindered olefins such as cyclohexene, ethylene, and propylene. Mixtures of more than one dienophile can be used. A preferred dieneophile is N,N'-m-phenylenedimaleimide. The dieneophile is combined with prepolymer, chain extender, and chain terminator in a mole ratio of between about 10 and about 100 percent, preferably about 30 and about 50 mole percent, based upon a comparison of the number of moles of dienophilic sites (i.e., the number of sites in the dienophile which could undergo ring formation with a diene) in the crosslinking agent D with the total number of moles of furyl or furfuryl groups IV in the prepolymer, chain extender, and chain terminator.
Other adjuvants commonly used in adhesives and coatings such as catalysts, fillers, extenders, colorants, wetting agents, surfactants, and antioxidants, can also be added to the compositions of the present invention in order to improve the handling properties of uncured compositions or the performance characteristics of cured compositions. Useful catalysts include dibutyltin dilaurate, stannous octoate, lead octoate, 2,2,1-diazobicyclooctane, tetramethylbutane diamine, dibutyltin di-2-ethylhexoate, metallic napthenates, metallic acetylacetonates, and others well known in the art. Dibutyltin dilaurate is a preferred catalyst.
When a composition of the present invention is heated sufficiently to deblock the isocyanate groups on prepolymer (A), then the prepolymer, chain extender (B), and chain terminator (C) react together to form longer polymer chains containing alternating prepolymer and chain extender units and terminal chain terminator units. This chain lengthening reaction proceeds substantially to completion in about 3 to 10 minutes at a temperature of about 150° C. for ketoxime blocked prepolymer and at a temperature of about 175° C. for phenol blocked prepolymers. If heating is continued for another 3 to 10 minutes at about 150° C. or for a shorter period at higher temperatures, a cross-linking reaction will then take place between the furyl or furfuryl groups IV (which are carried on the prepolymer, chain extender, or chain terminator) and the dieneophile (D). As the compositions of the present invention are heated, two distinct reactions therefore take place substantially in succession --chain lengthening by the prepolymer, chain extender, and chain terminator, and cross-linking by the furyl or furfuryl groups IV and the dieneophile. This gives the compositions of the present invention their stageable character and enables the physical properties (e.g. viscosity) of the uncured, B-staged, and cured compositions to be readily altered through the use of different amounts of each component A, B and C or through the use of species of components A, B, and C having increased or decreased molecular weight.
For example, the physical properites of a B-staged composition of the present invention are controlled, in part, by the molecular weight of the lengthened linear chains. Lower molecular weights for such a B-staged composition can be obtained, for example, by using an excess of chain terminator, an amine chain terminator in combination with a diol chain extender, or by using a prepolymer, a chain extender, and a chain terminator having low molecular weight. Also, higher molecular weights for such a B-staged composition can be obtained, for example, by using lesser amounts of chain terminator, an alcohol chain terminator in combination with a diamine chain extender, or by using a prepolymer, a chain extender, and a chain terminator having high molecular weight.
The compositions of the present invention are prepared by combining prepolymer, chain extender, chain terminator, and dienophile using a mixer such as an air stirrer. The resulting mixture has a long shelf life at room temperature, viz. up to one year or more. Although small amounts of the blocking agent volatilize during the chain extension reaction, the product will chain-extend and cross-link without substantial liberation of organic solvents. The compositions of the present invention can be chain-extended and cross-linked by heating them for about 6 to about 20 minutes at about 150° to 175° C., or for about 4 hours at about 95° C., or for intermediate times and temperatures between the above values. The compositions of the present invention can be staged to a solid, tack-free B-stage by heating them for approximately one-half the above time periods, i.e. for about 3 to about 10 minutes at 150° to 175° C., or for about 2 hours at about 95° C., or for intermediate times and temperatures between these values. The B-staged solid can be formed into sheets or granulated into a powder and stored for long periods at room temperature, viz. up to one year or more. The B-staged solid can be cured by reheating for about 3 to about 10 minutes at 150° C. to 175° C., or for about 2 hours at about 95° C., or for intermediate times and temperatures between these values. Bonding of the B-staged composition can be carried out by placing an adherend in contact with the cooled B-staged solid, and by heating the composition and adherend until a bond is formed. Alternatively, the cooled B-staged composition can be heated until it is tacky and then placed in contact with the adherend and bonded using pressure.
The following examples are offered to aid understanding of the present invention and are not to be construed as limiting the scope thereof.
EXAMPLE 1
One hundred grams of toluenediisocyanate/polyether/methylethyl ketoxime prepolymer ("Adiprene BL16", having 5.3 to 5.8 percent available isocyanate, commercially available from E. I. du Pont de Nemours & Co.) were combined with 7.11 g of N,N'-bis(furfuryl)-1,6-hexanediamine chain extender, 5.1 g of 4,4'-methylenedianiline chain extender, and 2.5 g of furfurylamine chain terminator in a 500 ml vessel. After thorough mixing, 8.3 g of N,N'-m-phenylenedimaleimide and 200 mg of dibutyltin dilaurate were added. The mixture was stirred until it became homogeneous. The resulting yellow-colored paste was brushed onto 25 mm×100 mm strips of 4 kg cotton duck canvas. Several test substrate sample strips measuring 25 mm×100 mm were obtained. The sample strips were wiped with toluene (except for a sample strip of cold rolled steel which was left coated with the protective oil applied by the steel manufacturer) and brushed with the above yellow-colored paste. The cotton duck and sample strips were then heated in an oven at a temperature of 150° C. (this temperature being referred to hereafter as the "activation temperature") for 4 minutes (this time being referred to hereafter as the "activation time") to convert the paste to a B-staged composition. The canvas strips and test substrates were tacky upon removal from the oven and were immediately bonded together with hand pressure and aged overnight. The aged samples were tested for T-peel strength according to ASTM D-903. The results for each test substrate are set out below in Table I.
TABLE I______________________________________Substrate Peel strength, kg/cm______________________________________Aluminum 5.4-7.1Cold rolled steel 7.1-8.9Cold rolled steel coatedwith protective oil 5.9.sup.aChrome plated steel 6.3-7.1Rigid PVC 6.3-7.5Plasticized PVC .sup.b______________________________________ .sup.a only one sample tested .sup.b substrate failed
EXAMPLE 2
Adhesive compositions containing 250 g (100 mole percent) "Adiprene BL16" prepolymer, 20.8 g (65 mole percent) furfurylamine chain terminator, 15.8 g (35 mole percent) N,N'-bis-furfuryl-1,6-hexanediamine chain extender, 944 mg (0.5 mole percent) dibutyltin dilaurate, and varying amounts of N,N'-m-phenylenedimaleimide dienophile (at amounts of 22 g for a 50 mole percent addition, and 44.1 g for a 100 mole percent addition) were prepared as described in Example 1. The adhesive qualities of these compositions after various activation temperatures and times were evaluated using the following test. Two strips of 6 mm birch plywood 25 mm×100 mm in size were coated with adhesive. A 25 mm wide×175 mm long bonded assembly was formed by adhering one end of one strip to one end of the other strip with a 25 mm overlap between adjacent ends. The adhesive bond was pressed with a 1.81 kg roller. The bond was allowed to set for a measured period (this setting time being referred to hereafter as the "set time") and then tested by supporting the ends of the bonded assembly in a horizontal plane and fastening a 2.267 kg weight to the center of the bonded area.
The mole percent dienophile used (compared to the number of moles of furyl and furfuryl groups present), activation temperature, activation time, set time, and test results are set forth below in table II.
TABLE II______________________________________Mole SetRun percent Activation Activation time, Testno. dienophile temperature, °C. time, min. min. result.sup.a______________________________________1 50 121 6 3 F2 50 121 12 3 F3 50 135 12 3 F4 100 121 6 60 F5 100 121 8 3 F6 100 121 8 60 F7 100 135 8 3 F8 100 135 8 60 H9 100 121 10 3 F10 100 121 10 60 H11 100 135 10 3 H12 100 121 12 3 H______________________________________ .sup.a F = bond failed, H = bond held
EXAMPLE 3
An adhesive composition containing 100 mole percent dienophile (compared to the number of moles of furyl and furfuryl groups present) was prepared as described in Example 2. The stageability and "open time" of this composition was evaluated as follows.
The adhesive composition was coated onto 6 mm birch plywood strips as described in Example 2. The adhesive was brought to a "B-staged" condition by heating in an oven at 135° for 8 minutes. The samples were cooled to room temperature for 24 hours. The samples were reactivated by heating in an oven at 135° C. for various measured times, pressed together using hand pressure, and tested as in Example 2. Set out below in Table III are the activation temperature, activation time, set time and bond test results for this composition.
TABLE III______________________________________ Activation Activation Set TestRun no. temperature °C. time, min time, min result______________________________________13 121 10 3 F14 135 10 3 F15 121 12 3 H16 135 12 3 H______________________________________
Open time was evaluated for this composition by placing a sheet of Kraft paper against a reactivated sample. The Kraft paper could be applied to and removed from the bond with fibre tearing up to 150 seconds after removal of the reactivated sample from the oven.
EXAMPLE 4
An adhesive composition was prepared as described in Example 3. The composition was tested for overlap shear strength using 6 mm birch plywood strips bonded to one another as in Example 2. Overlap shear strengths were measured on a Scott tensile tester (Scott Testing Inc.). Set out below in Table IV are the overlap shear strength for several samples after various activation temperatures and activation times.
TABLE IV______________________________________ Activation Activation Overlap shearRun no. temperature, °C. time, min strength, kg/cm.sup.2______________________________________17 93 12 <718 93 14 20.419 121 10 17.620 121 12 22.521 121 14 25.722 135 6 17.623 135 8 28.824 135 12 33.025 135 14 33.7______________________________________
EXAMPLE 5
An adhesive composition was prepared and coated onto birch plywood strips as described in Example 4. The adhesive was activated to its B-Stage by heating in an oven at 135° C. for 8 minutes. The B-staged samples were cooled overnight and then reactivated at 135° C. for various periods of time. The reactivated samples were bonded together and tested for overlap shear strength as described in Example 4. Set out below in Table V are the reactivation temperature, reactivation time, and overlap shear strength for several samples. The data indicate a good "pot life" during reactivation.
TABLE V______________________________________ Reactivation Reactivation Overlap shearRun no. temperature, °C. time, min. strength, kg/cm.sup.2______________________________________26 135 10 26.427 135 12 29.528 135 18 >33.729 135 20 >33.730 135 22 >33.7______________________________________
EXAMPLE 6
An adhesive composition was prepared and coated onto birch plywood strips as described in Example 4. The adhesive was activated in an oven at 135° C. for various periods of time. The plywood strips were then bonded to one another with 625 mm 2 overlap area and hung vertically in an oven. The bonds were tested for heat resistance by hanging a 0.9 kg weight from the bonded assembly and raising the oven temperature at the rate of 5.5° C. every 3 minutes until the bond failed. Set out below in Table VI are the activation temperature, activation time, and bond failure temperature for several samples.
TABLE VI______________________________________ Activation Activation Bond failureRun no. temperature, °C. time, min temperature, °C.______________________________________31 135 10 6032 135 12 71.133 135 14 76.734 135 18 82.235 135 20 87.8______________________________________
EXAMPLE 7
An adhesive composition was prepared containing 250 g (100 mole percent) "Adiprene BL16" prepolymer, 12.8 g (40 mole percent) furfurylamine chain terminator, 18.1 g (40 mole percent) N,N-bis(furfuryl)-1,6-hexanediamine chain extender, 6.5 g (20 mole percent) 4,4-methylene dianiline chain extender, 31.8 g (72 mole percent) N,N'-m-phenylenedimaleimide dienophile, and 944 mg (0.5 mole percent) dibutyltin dilaurate. The composition was activated and tested as in Example 1. Set out below in Table VII are peel strength tests for solvent wiped cold rolled steel bonded to canvas at several activation times.
TABLE VII______________________________________ Activation Activation Peel strengthRun no. temperature, °C. time, min kg/cm______________________________________36 150 4 4.5-4.8.sup.a37 150 5 6.3.sup.a38 150 6 8.0.sup.a39 150 8 8.9-9.8.sup.a40 150 10 4.3.sup.b______________________________________ .sup.a tested at room temperature .sup.b tested at 65° C. Samples tested at room temperature did not fail at the bond line.
EXAMPLE 8
An adhesive composition was prepared containing 100 mole percent "Adiprene BL16" prepolymer, 30 mole percent furfurylamine chain terminator, 30 mole percent N,N'-bis-furfuryl-1,6-hexanediamine chain extender, 40 mole percent 4,4-methylene dianiline chain extender, 72 mole percent N,N'-m-phenylenedimaleimide dienophile, and 0.5 mole percent dibutyltin dilaurate. The composition was coated onto cold rolled steel and canvas as in Example 1. The composition was next activated in an oven at 149° C. for 10 minutes. Test samples were immediately bonded and then stored for 24 hours prior to testing. The samples were tested for peel strength at elevated temperatures by heating to various temperatures and testing for peel strength as in Example 1. Set out below in Table VIII are the test temperature and peel strength for several samples. This data illustrates the excellent peel strength of the composition of this example at elevated temperatures.
TABLE VIII______________________________________ Test Peel Strength,Run No. temperature, °C. kg/cm______________________________________41 20 7.142 51.7 5.043 65.6 4.144 79.4 3.845 93.3 2.746 101.7 1.3-1.4______________________________________
EXAMPLE 9
In a series of 9 runs, adhesive compositions containing 3 different levels of chain terminator and chain extender were prepared and activated for 3 different periods of time. Each of the compositions contained 100 mole percent "Adiprene BL16" prepolymer and a total of 100 mole percent furfurylamine chain terminator and N,N-bis(furfuryl)-1,6-hexanediamine chain extender. The compositions also contained sufficient N,N'-m-phenylenedimaleimide dienophile to react with 60 percent of available furan groups, and 0.5 mole percent dibutyltin dilaurate catalyst. The compositions were adhered to cold rolled steel (which had been previously wiped with toluene) and tested for peel strength as in Example 1. Set out below in Table IX are the mole ratio of chain terminator to chain extender, activation time, and peel strength for the resulting compositions. As the amount of chain terminator relative to chain extender is increased in these runs, peel strength decreases.
TABLE IX______________________________________ Ratio of chain Activation PeelRun terminator temperature, Activation strength,no. to chain extender °C. time, min kg/cm______________________________________47 40/60 149 5 6.148 " " 6 7.949 " " 8 9.850 50/50 " 6 4.151 " " 8 5.952 " " 9 7.753 55/45 " 5 1.154 " " 7 3.655 " " 9 5.4______________________________________
EXAMPLE 10
In a series of 9 runs, adhesive compositions containing 3 different levels of dienophile were prepared and adhered to 3 different substrates. Each of the compositions contained 100 mole percent "Adiprene BL16" prepolymer, 40 mole percent furfurylamine chain terminator, 40 mole percent N,N-bis(furfuryl)-1,6-hexanediamine chain extender, 20 mole percent 4,4'-methylene dianiline chain terminator, and 0.5 mole percent dibutyltin dilaurate catalyst. The compositions were coated on various substrates, activated in an oven at 149° C. for 10 minutes, and tested as in Example 1. Set out below in Table X are the amount of N,N'-m-phenylenedimaleimide dienophile (based on the mole percent of available furan groups), test substrate used, and peel strength for each of the resulting compositions.
TABLE X______________________________________ Mole percent Test Peel strengthRun no. dienophile substrate kg/cm______________________________________56 0 cold rolled steel/canvas 1.357 " aluminum/canvas 1.158 " PVC/canvas 1.459 10 cold rolled steel/canvas 2.5-2.960 " aluminum/canvas 2.5-2.961 " PVC/canvas 1.3-2.962 25 cold rolled steel/canvas 2.9-3.863 " aluminum/canvas 3.464 " PVC/canvas 3.6-4.3______________________________________
EXAMPLE 11
An adhesive composition was prepared according to Example 5 but containing 60 mole percent ethylene glycol diacrylate as the dienophile. The composition was applied to various substrates, activated in an oven for various periods of time, and tested as in Example 1. Set out below in Table XI are the activation temperature, activation time, test substrate used, and peel strength for this composition.
TABLE XI______________________________________ Acti-Activation vation PeelRun temperature, time, Test strength,no. °C. min substrate kg/cm______________________________________65 149 8 cold rolled steel/canvas 1.866 " " aluminum/canvas 1.467 " 16 cold rolled steel/canvas 2.968 " " aluminum/canvas 2.3______________________________________
Various modifications and alterations of this invention will be apparent to those skilled in the art without departing from the scope and spirit of this invention and the latter should not be restricted to that set forth herein for illustrative purposes.
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A one-part, solvent free, thermosettable adhesive and coating composition comprising a prepolymer terminated with blocked isocyanate groups and having a melting point below 95° C., a difunctional amine or alcohol which is soluble in the prepolymer at 95° C., a monofunctional amine or alcohol which is soluble in the prepolymer at 95° C., with at least one of the foregoing bearing furyl or furfuryl substituents, and a bis-dieneophile.
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[0001] This application claims the benefit of priority of U.S. provisional application No. 60/748,822, filed Dec. 9, 2005, U.S. provisional application No. 60/784,644, filed Mar. 20, 2006, and U.S. provisional application No. 60/802,829, filed May 22, 2006, the disclosures of which are hereby incorporated by reference as if written herein in their entirety.
FIELD OF THE INVENTION
[0002] The present invention is directed to carbonyl compounds as inhibitors of histone deacetylase (HDAC). More particularly, the invention relates to compounds containing a terminal amine to enhance aqueous solubility. These compounds are useful in treating disease states including cancers, autoimmune diseases, tissue damage, central nervous system disorders, neurodegenerative disorders, fibrosis, bone disorders, polyglutamine-repeat disorders, anemias, thalassemias, inflammatory conditions, cardiovascular conditions, and disorders in which angiogenesis plays a role in pathogenesis.
BACKGROUND OF THE INVENTION
[0003] Histone proteins organize DNA into nucleosomes, which are regular repeating structures of chromatin. The acetylation status of histones alters chromatin structure, which, in turn, is involved in gene expression. Two classes of enzymes can affect the acetylation of histones—histone acetyltransferases (HATs) and histone deacetylases (HDACs). A number of HDAC inhibitors have been characterized. One of the potent inhibitors of HDAC is (SAHA), a hydroxamic acid-based compound. It is also known as vorinostat or ZOLINZA™, which is currently in clinical trials. (“Merck Announces Pivotal Phase IIb Study Results of the Company's Investigational HDAC Inhibitor ZOLINZA™ and Glaxo's Cancer Vaccine Shows Response,” M2 Presswire, 5 Jun. 2006.) The Food and Drug Administration (FDA) has also accepted the New Drug Application (NDA) for ZOLINZA™ for the treatment of advanced cutaneous T-cell-lymphoma (CTCL) in June 2006. (WHITEHOUSE STATION, N.J., “ZOLINZA™, Merck's Investigational Medicine for Advanced Cutaneous T-Cell Lymphoma (CTCL), to Receive Priority Review from U.S. Food and Drug Administration,” Business Wire, 7 Jun. 2006.) Hydroxamic acid derivatives, which are related to SARA, and their use for inhibiting HDAC have been disclosed by Columbia University and Memorial Sloan-Kettering Cancer Center in WO Patent Application No. W02004089293, published Oct. 21, 2004. Other hydroxamic acid based compounds are pyroxamide, CBRA, oxamfiatin and scriptaid. Nevertheless, although hydroxamic acids can be potent inhibitors of HDAC activity, hydroxamate-based compounds are known to have suboptimal pharmacological properties including low oral bioavailability, poor in vivo stability and poor pharmacokinetic profiles. Therefore, a need still exists in the art to identify non-hydroxamate HDAC inhibitors which have improved aqueous solubility, oral bioavailability, and other properties.
[0004] Certain non-hydroxamate carbonyl compounds as HDAC inhibitors have previously been published. In PCT Patent Application Publication No. WO 04/110418, published Dec. 23, 2004, Wash et al. first discloses a novel, non-hydroxamate carbonyl class of HDAC inhibitor. In PCT Patent Application Publication No. WO 05/123089, published Dec. 29, 2005, Malecha et al. describes multicyclic sulfonamide carbonyl compounds as HDAC inhibitors. In PCT Patent Application Publication No. WO 05/120515, published Dec. 29, 2005, Malecha et al. discloses somewhat different sulfonamide carbonyl compounds as HDAC inhibitors.
[0005] The present invention features carbonyl compounds having a terminal amine. This terminal amine has been found to add to an already potent class of HDAC inhibitors the long-sought property of enhanced aqueous solubility and the concomitant oral bioavailability.
SUMMARY OF THE INVENTION
[0006] Disclosed herein are carbonyl compounds, including their pharmaceutically acceptable salts, esters, and prodrugs thereof, having structural Formula (I) or related formulae as described herein:
[0007] A compound having structural Formula (I)
[0008] or a pharmaceutically acceptable salt, ester, or prodrug thereof, wherein:
[0009] G 1 is optionally substituted 5 or 6 membered heteroaryl;
[0010] G 2 is an N-sulfonamide moiety having structure (II), an S-sulfonamide moiety having structure (III), or an amide of the form —NR 3 C(O)— or —C(O)NR 3 —:
[0011] G 3 is optionally substituted phenyl, optionally substituted 5 or 6 membered aryl, or optionally substituted 5 or 6 membered heteroaryl;
[0012] R 1 and R 2 are each independently selected from the group consisting of hydrogen, lower alkyl, halogen and perhaloalkyl, or R 1 and R 2 taken together may form an optionally substituted cycloalkyl or optionally substituted heterocycloalkyl;
[0013] R 3 and R 4 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, and optionally substituted aryl;
[0014] G 4 is selected from the group consisting of —(X 1 ) n1 O(X 2 ) n2 —, —(X 1 ) n1 S(X 2 ) n2 — and —(X 1 ) n1 NR 7 (X 2 ) n2 —, wherein each member of the group may be optionally substituted with one or more R 9 moieties attached to any carbon atom, and each member of the group is drawn with its left end attached to G 3 and its right end attached to —NR 5 R 6 ;
[0015] R 5 and R 6 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted lower alkenyl, optionally substituted alkynyl, optionally substituted aryl, optionally substituted heteroaryl, optionally substituted cycloalkyl, optionally substituted cycloheteroalkyl, optionally substituted cycloaklenyl, optionally substituted fused aryl, optionally substituted fused heteroaryl, optionally substituted fused heterocycloalkyl, and optionally substituted fused cycloalkyl;
[0016] R 7 is selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted heteroalkyl, and optionally substituted lower alkoxy;
[0017] R 9 is selected from the group consisting of lower alkyl, lower alkylene, lower alkynylene, lower alkoxy, lower amine, halogen, lower perhaloalkyl, and hydroxyl;
[0018] X 1 and X 2 are each independently selected from the group consisting of optionally substituted lower alkylene, optionally substituted alkenylene, and optionally substituted alkynylene;
[0019] n1 is 0-5;
[0020] n2 is 1-5;
[0021] G 5 is selected from the group consisting of hydrogen, optionally substituted acyl, optionally substituted aryl, optionally substituted alkyl, optionally substituted heteroaryl, optionally substituted alkylthio, optionally substituted arylthio and optionally substituted heteroarylthio or G 5 may have the structural Formula (IV):
[0022] thereby forming a homodisulfide or heterodisulfide dimer of a compound of the present invention, wherein:
[0023] R 11 and R 12 are each independently selected from the group consisting of hydrogen, lower alkyl, halogen and perhaloalkyl, or R 11 and R 12 taken together may form an optionally substituted cycloalkyl or optionally substituted heterocycloalkyl;
[0024] R 13 and R 14 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted lower alkenyl, optionally substituted alkynyl, optionally substituted aryl, optionally substituted heteroaryl, optionally substituted cycloalkyl, optionally substituted cycloheteroalkyl, optionally substituted cycloaklenyl, optionally substituted fused aryl, optionally substituted fused heteroaryl, optionally substituted fused heterocycloalkyl, and optionally substituted fused cycloalkyl;
[0025] G 6 is optionally substituted 5 or 6 membered heteroaryl;
[0026] G 7 is an N-sulfonamide moiety having structure (V), an S-sulfonamide moiety having structure (VI), or an amide of the form —NR 15 C(O)— or —C(O)NR 15 —:
[0027] R 15 and R 16 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, and optionally substituted aryl;
[0028] G 8 is optionally substituted phenyl, optionally substituted 5 or 6 membered aryl, or optionally substituted 5 or 6 membered heteroaryl;
[0029] G 9 is selected from the group consisting of —(X 3 ) n3 O(X 4 ) n4 —, —(X 3 ) n3 S(X 4 ) n4 — and —(X 3 ) n3 NR 20 (X 4 ) n4 —, wherein each may be optionally substituted with one or more R 21 s attached to any carbon atom, and each group is drawn with its left end attached to G 8 and its right end attached to —NR 13 R 14 ;
[0030] X 3 and X 4 are each independently selected from the group consisting of optionally substituted lower alkylene, optionally substituted alkenylene, and optionally substituted alkynylene;
[0031] n3 is 0-5;
[0032] n4 is 1-5;
[0033] R 20 is selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted heteroalkyl, and optionally substituted lower alkoxy; and
[0034] R 21 is selected from the group consisting of lower alkyl, lower alkylene, lower alkynylene, lower alkoxy, lower amine, halogen, lower perhaloalkyl, and hydroxyl.
[0035] In a broad aspect, compounds according to the present invention are capable of inhibiting the catalytic activity of histone deacetylase (HDAC), and may be used in the treatment or prophylaxis of a disease or condition in which HDAC plays an active role. Thus, in broad aspect, the present invention provides methods and pharmaceutical compositions comprising one or more compounds of the present invention together with a pharmaceutically acceptable carrier, for treating diseases in mammals using compounds of the invention, including but not limited to, treating cancers, autoimmune diseases, tissue damage, central nervous system disorders, neurodegenerative disorders, fibrosis, bone disorders, polyglutamine-repeat disorders, anemias, thalassemias, inflammatory conditions, cardiovascular conditions, and disorders in which angiogenesis plays a role in pathogenesis.
[0036] In certain embodiments, the present invention provides methods for inhibiting the catalytic activity and cellular function of HDAC. In other embodiments, the present invention provides methods for treating a HDAC mediated disorder in a patient in need of such treatment comprising administering to said patient a therapeutically effective amount of a compound or composition according to the present invention. The present invention also contemplates the use of compounds disclosed herein for use in the manufacture of a medicament for the treatment of a disease or condition ameliorated by the inhibition/modulation of HDAC.
DETAILED DESCRIPTION OF THE INVENTION
[0037] In certain embodiments, the invention provides compounds wherein G 4 is —(X 1 ) n1 O(X 2 ) n2 — and n1 is 0.
[0038] In certain embodiments, G 2 is N-sulfonamide.
[0039] In certain embodiments, G 5 is selected from the group consisting of optionally substituted acyl and hydrogen.
[0040] In certain embodiments, G 1 is pyridinyl.
[0041] In certain embodiments, G 3 is phenyl.
[0042] In further embodiments, R 5 and R 6 is lower alkyl.
[0043] In yet further embodiments, R 5 and R 6 is methyl.
[0044] In other embodiments, G 4 is —(X 1 ) n1 S(X 2 ) n2 — and n1 is 0.
[0045] In further embodiments, G 1 is pyridinyl; G 3 is phenyl; and R 5 and R 6 are each independently selected from the group consisting of hydrogen, and optionally substituted lower alkyl.
[0046] In yet other embodiments, G 4 is —(X 1 ) n1 NR 7 (X 2 ) n2 — and n1 is 0.
[0047] In further embodiments, G 1 is pyridinyl; G 3 is phenyl; and R 5 and R 6 are each independently selected from the group consisting of hydrogen, and optionally substituted lower alkyl.
[0048] In certain embodiments, the compounds of the present invention have structural Formula (VII):
[0049] or a pharmaceutically acceptable salt, ester, or prodrug thereof, wherein:
[0050] W, Y and Z are each independently selected from the group consisting of N and CR 8 , provided at least one of W, Y, or Z is N;
[0051] R 8 and R 25 are each independently selected from the group consisting of hydrogen, halogen, hydroxy, optionally substituted lower alkyl, optionally substituted lower alkenyl, optionally substituted lower alkynyl, optionally substituted cycloalkyl, optionally substituted lower heteroalkyl, optionally substituted lower heterocycloalkyl, optionally substituted lower haloalkyl, optionally substituted lower haloalkenyl, optionally substituted lower haloalkynyl, lower perhaloalkyl, lower perhaloalkoxy, optionally substituted lower alkoxy, nitro, cyano, and NH 2 ;
[0052] X 2 is selected from the group consisting of optionally substituted lower alkylene, optionally substituted alkenylene, and optionally substituted alkynylene;
[0053] n2 is 1-5;
[0054] R 5 and R 6 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted lower alkenyl, optionally substituted alkynyl, optionally substituted aryl, optionally substituted heteroaryl, optionally substituted cycloalkyl, optionally substituted cycloheteroalkyl, optionally substituted cycloaklenyl, optionally substituted fused aryl, optionally substituted fused heteroaryl, optionally substituted fused heterocycloalkyl, and optionally substituted fused cycloalkyl;
[0055] G 5 is selected from the group consisting of hydrogen, optionally substituted acyl, optionally substituted aryl, optionally substituted alkyl, optionally substituted heteroaryl, optionally substituted alkylthio, optionally substituted arylthio and optionally substituted heteroarylthio or G 5 may have the structural Formula (IV):
[0056] thereby forming a homodisulfide or heterodisulfide dimer of a compound of the present invention, wherein:
[0057] R 11 and R 12 are each independently selected from the group consisting of hydrogen, lower alkyl, halogen and perhaloalkyl, or R 11 and R 12 taken together may form an optionally substituted cycloalkyl or optionally substituted heterocycloalkyl;
[0058] R 13 and R 14 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted lower alkenyl, optionally substituted alkynyl, optionally substituted aryl, optionally substituted heteroaryl, optionally substituted cycloalkyl, optionally substituted cycloheteroalkyl, optionally substituted cycloaklenyl, optionally substituted fused aryl, optionally substituted fused heteroaryl, optionally substituted fused heterocycloalkyl, and optionally substituted fused cycloalkyl;
[0059] G 6 is optionally substituted 5 or 6 membered heteroaryl;
[0060] G 7 is an N-sulfonamide moiety having structure (V), an S-sulfonamide moiety having structure (VI), or an amide of the form —NR 15 C(O)— or —C(O)NR 15 —:
[0061] R 15 and R 16 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl, and optionally substituted aryl;
[0062] G 8 is optionally substituted phenyl, optionally substituted 5 or 6 membered aryl, or optionally substituted 5 or 6 membered heteroaryl;
[0063] G 9 is selected from the group consisting of —(X 3 ) n3 O(X 4 ) n4 , —(X 3 ) n3 S(X 4 ) n4 — and —(X 3 ) n3 NR 20 (X 4 ) n4 —, wherein each may be optionally substituted with one or more R 21 s attached to any carbon atom, and each group is drawn with its left end attached to G 8 and its right end attached to —NR 13 R 14 ;
[0064] X 3 and X 4 are each independently selected from the group consisting of optionally substituted lower alkylene, optionally substituted alkenylene, and optionally substituted alkynylene;
[0065] n3 is 0-5;
[0066] n4 is 1-5;
[0067] R 20 is selected from the group consisting of hydrogen, optionally substituted lower alkyl, optionally substituted heteroalkyl, and optionally substituted lower alkoxy; and
[0068] R 21 is selected from the group consisting of lower alkyl, lower alkylene, lower alkynylene, lower alkoxy, lower amine, halogen, lower perhaloalkyl, and hydroxyl.
[0069] In further embodiments, Y is N; W is CR 8 ; Z is CR 8 ; and G 5 is selected from the group consisting of hydrogen and optionally substituted acyl.
[0070] In yet further embodiments, R 5 and R 6 are each independently selected from the group consisting of hydrogen, optionally substituted lower alkyl; and X 2 is optionally substituted lower alkylene.
[0071] In yet further embodiments, R 8 and R 25 are each independently selected from the group consisting of hydrogen, and lower alkyl.
[0072] In certain embodiments, G 4 is —(X 1 ) n1 O(X 2 ) n2 — and n1 is O. The selection of this alkoxyalkylene-type linker, in combination with the aforementioned terminal amine, yields even further improvements in aqueous solubility.
[0073] In certain embodiments, the compound of the invention has a solubility of at least 1 mg/mL.
[0074] In further embodiments, the compound of the invention has a solubility of at least 5 mg/mL.
[0075] In yet further embodiments, the compound of the invention has a solubility of at least 20 mg/mL.
[0076] In accordance with yet another aspect of the invention, the present invention provides methods and compositions for treating certain diseases.
[0077] In some aspects of the invention, the disease is a hyperproliferative condition of the human or animal body.
[0078] In further embodiments, said hyperproliferative condition is selected from the group consisting of hematologic and nonhematologic cancers. In yet further embodiments, said hematologic cancer is selected from the group consisting of multiple myeloma, leukemias, and lymphomas. In yet further embodiments, said leukemia is selected from the group consisting of acute and chronic leukemias. In yet further embodiments, said acute leukemia is selected from the group consisting of acute lymphocytic leukemia (ALL) and acute nonlymphocytic leukemia (ANLL). In yet further embodiments, said chronic leukemia is selected from the group consisting of chronic lymphocytic leukemia (CLL) and chronic myelogenous leukemia (CML). In further embodiments, said lymphoma is selected from the group consisting of Hodgkin's lymphoma and non-Hodgkin's lymphoma. In further embodiments, said lymophoma is selected from the group consisting of cutaneous t-cell lymphoma (CTCL) and mantle cell lymphoma (MCL). In further embodiments, said hematologic cancer is multiple myeloma. In other embodiments, said hematologic cancer is of low, intermediate, or high grade. In other embodiments, said nonhematologic cancer is selected from the group consisting of: brain cancer, cancers of the head and neck, lung cancer, breast cancer, cancers of the reproductive system, cancers of the digestive system, pancreatic cancer, and cancers of the urinary system. In further embodiments, said cancer of the digestive system is a cancer of the upper digestive tract or colorectal cancer. In further embodiments, said cancer of the urinary system is bladder cancer or renal cell carcinoma. In further embodiments, said cancer of the reproductive system is prostate cancer.
[0079] Additional types of cancers which may be treated using the compounds and methods described herein include: cancers of oral cavity and pharynx, cancers of the respiratory system, cancers of bones and joints, cancers of soft tissue, skin cancers, cancers of the genital system, cancers of the eye and orbit, cancers of the nervous system, cancers of the lymphatic system, and cancers of the endocrine system. In certain embodiments, these cancers may be selected from the group consisting of: cancer of the tongue, mouth, pharynx, or other oral cavity; esophageal cancer, stomach cancer, or cancer of the small intestine; colon cancer or rectal, anal, or anorectal cancer; cancer of the liver, intrahepatic bile duct, gallbladder, pancreas, or other biliary or digestive organs; laryngeal, bronchial, and other cancers of the respiratory organs; heart cancer, melanoma, basal cell carcinoma, squamous cell carcinoma, other non-epithelial skin cancer; uterine or cervical cancer; uterine corpus cancer; ovarian, vulvar, vaginal, or other female genital cancer; prostate, testicular, penile or other male genital cancer; urinary bladder cancer; cancer of the kidney; renal, pelvic, or urethral cancer or other cancer of the genito-urinary organs; thyroid cancer or other endocrine cancer; chronic lymphocytic leukemia; and cutaneous T-cell lymphoma, both granulocytic and monocytic.
[0080] Yet other types of cancers which may be treated using the compounds and methods described herein include: adenocarcinoma, angiosarcoma, astrocytoma, acoustic neuroma, anaplastic astrocytoma, basal cell carcinoma, blastoglioma, chondrosarcoma, choriocarcinoma, chordoma, craniopharyngioma, cutaneous melanoma, cystadenocarcinoma, endotheliosarcoma, embryonal carcinoma, ependymoma, Ewing's tumor, epithelial carcinoma, fibrosarcoma, gastric cancer, genitourinary tract cancers, glioblastoma multiforme, hemangioblastoma, hepatocellular carcinoma, hepatoma, Kaposi's sarcoma, large cell carcinoma, leiomyosarcoma, liposarcoma, lymphangiosarcoma, lymphangioendotheliosarcoma, medullary thyroid carcinoma, medulloblastoma, meningioma mesothelioma, myelomas, myxosarcoma neuroblastoma, neurofibrosarcoma, oligodendroglioma, osteogenic sarcoma, epithelial ovarian cancer, papillary carcinoma, papillary adenocarcinomas, parathyroid tumors, pheochromocytoma, pinealoma, plasmacytomas, retinoblastoma, rhabdomyosarcoma, sebaceous gland carcinoma, seminoma, skin cancers, melanoma, small cell lung carcinoma, squamous cell carcinoma, sweat gland carcinoma, synovioma, thyroid cancer, uveal melanoma, and Wilm's tumor.
[0081] In some aspects of the invention, the disease to be treated by the methods of the present invention may be a hematologic disorder. In certain embodiments, said hematologic disorder is selected from the group consisting of sickle cell anemia, myelodysplastic disorders (MDS), and myeloproliferative disorders. In further embodiments, said myeloproliferative disorder is selected from the group consisting of polycythemia vera, myelofibrosis and essential thrombocythemia.
[0082] In some aspects of the invention, the disease to be treated by the methods of the present invention may be a neurological disorder. In further embodiments, said neurological disorder is selected from the group consisting of epilepsy, neuropathic pain, depression and bipolar disorders.
[0083] In some aspects of the invention, the disease to be treated by the methods of the present invention may be a cardiovascular condition. In certain embodiments, said cardiovascular condition is selected from the group consisting of cardiac hypertrophy, idiopathic cardiomyopathies, and heart failure.
[0084] In some aspects of the invention, the disease to be treated by the methods of the present invention may be an autoimmune disease. In certain embodiments, said autoimmune disease is selected from the group consisting of systemic lupus erythromatosus (SLE), multiple sclerosis (MS), and systemic lupus nephritis.
[0085] In some aspects of the invention, the disease to be treated by the methods of the present invention may be a dermatologic disorder. In certain embodiments, said dermatologic disorder is selected from the group consisting of psoriasis, melanoma, basal cell carcinoma, squamous cell carcinoma, and other non-epithelial skin cancers.
[0086] In some aspects of the invention, the disease to be treated by the methods of the present invention may be an ophthalmologic disorder. In certain embodiments, said ophthalmologic disorder is selected from the group consisting of dry eye, closed angle glaucoma and wide angle glaucoma.
[0087] In some aspects of the invention, the disease to be treated by the methods of the present invention may be a polyglutamine-repeat disorders. In some embodiments, the polyglutamine-repeat disorder is selected from the group consisting of Huntington's disease, Spinocerebellar ataxia 1 (SCA 1), Machado-Joseph disease (MJD)/Spinocerebella ataxia 3 (SCA 3), Kennedy disease/Spinal and bulbar muscular atrophy (SBMA) and Dentatorubral pallidolusyian atrophy (DRPLA).
[0088] In some aspects of the invention, the disease to be treated by the methods of the present invention may be an inflammatory condition. In some embodiments, the inflammatory condition is selected from the group consisting of Rheumatoid Arthritis (RA), Inflammatory Bowel Disease (IBD), ulcerative colitis and psoriasis.
[0089] In another aspect are compounds or compositions comprising compounds that inhibit the catalytic or cellular activity of histone deacetylase (HDAC).
[0090] As used in the present specification, the following terms have the meanings indicated.
[0091] The term “acyl,” as used herein, alone or in combination, refers to a carbonyl attached to an alkenyl, alkyl, aryl, cycloalkyl, heteroaryl, heterocycle, or any other moiety were the atom attached to the carbonyl is carbon. An “acetyl” group refers to a —C(O)CH 3 group. An “alkylcarbonyl” or “alkanoyl” group refers to an alkyl group attached to the parent molecular moiety through a carbonyl group. Examples of such groups include methylcarbonyl and ethylcarbonyl. Examples of acyl groups include formyl, alkanoyl and aroyl.
[0092] The term “alkenyl,” as used herein, alone or in combination, refers to a straight-chain or branched-chain hydrocarbon radical having one or more double bonds and containing from 2 to 20, preferably 2 to 6, carbon atoms. Alkenylene refers to a carbon-carbon double bond system attached at two or more positions such as ethenylene [(—CH═CH—),(—C::C—)]. Examples of suitable alkenyl radicals include ethenyl, propenyl, 2-methylpropenyl, 1,4-butadienyl and the like.
[0093] The term “alkoxy,” as used herein, alone or in combination, refers to an alkyl ether radical, wherein the term alkyl is as defined below. Examples of suitable alkyl ether radicals include methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, iso-butoxy, sec-butoxy, tert-butoxy, and the like.
[0094] The term “alkyl,” as used herein, alone or in combination, refers to a straight-chain or branched-chain alkyl radical containing from 1 to and including 20, preferably 1 to 10, and more preferably 1 to 6, carbon atoms. Alkyl groups may be optionally substituted as defined herein. Examples of alkyl radicals include methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, pentyl, iso-amyl, hexyl, octyl, noyl and the like. The term “alkylene,” as used herein, alone or in combination, refers to a saturated aliphatic group derived from a straight or branched chain saturated hydrocarbon attached at two or more positions, such as methylene (—CH 2 —).
[0095] The term “alkylamino,” as used herein, alone or in combination, refers to an alkyl group attached to the parent molecular moiety through an amino group. Suitable alkylamino groups may be mono- or dialkylated, forming groups such as, for example, N-methylamino, N-ethylamino, N,N-dimethylamino, N,N-ethylmethylamino and the like.
[0096] The term “alkylidene,” as used herein, alone or in combination, refers to an alkenyl group in which one carbon atom of the carbon-carbon double bond belongs to the moiety to which the alkenyl group is attached.
[0097] The term “alkylthio,” as used herein, alone or in combination, refers to an alkyl thioether (R—S—) radical wherein the term alkyl is as defined above and wherein the sulfur may be singly or doubly oxidized. Examples of suitable alkyl thioether radicals include methylthio, ethylthio, n-propylthio, isopropylthio, n-butylthio, iso-butylthio, sec-butylthio, tert-butylthio, methanesulfonyl, ethanesulfinyl, and the like.
[0098] The term “alkynyl,” as used herein, alone or in combination, refers to a straight-chain or branched chain hydrocarbon radical having one or more triple bonds and containing from 2 to 20, preferably from 2 to 6, more preferably from 2 to 4, carbon atoms. “Alkynylene” refers to a carbon-carbon triple bond attached at two positions such as ethynylene (—C:::C—, —C≡C—). Examples of alkynyl radicals include ethynyl, propynyl, hydroxypropynyl, butyn-1-yl, butyn-2-yl, pentyn-1-yl, 3-methylbutyn-1-yl, hexyn-2-yl, and the like.
[0099] The terms “amido” and “carbamoyl,” as used herein, alone or in combination, refer to an amino group as described below attached to the parent molecular moiety through a carbonyl group, or vice versa. The term “C-amido” as used herein, alone or in combination, refers to a —C(═O)—NR 2 group with R as defined herein. The term “N-amido” as used herein, alone or in combination, refers to a RC(═O)NH— group, with R as defined herein. The term “acylamino” as used herein, alone or in combination, embraces an acyl group attached to the parent moiety through an amino group. An example of an “acylamino” group is acetylamino (CH 3 C(O)NH—).
[0100] The term “amino,” as used herein, alone or in combination, refers to —NRR′, wherein R and R′ are independently selected from the group consisting of hydrogen, alkyl, acyl, heteroalkyl, aryl, cycloalkyl, heteroaryl, and heterocycloalkyl, any of which may themselves be optionally substituted.
[0101] The term “aryl,” as used herein, alone or in combination, means a carbocyclic aromatic system containing one, two or three rings wherein such rings may be attached together in a pendent manner or may be fused. The term “aryl” embraces aromatic radicals such as benzyl, phenyl, naphthyl, anthracenyl, phenanthryl, indanyl, indenyl, annulenyl, azulenyl, tetrahydronaphthyl, and biphenyl.
[0102] The term “arylalkenyl” or “aralkenyl,” as used herein, alone or in combination, refers to an aryl group attached to the parent molecular moiety through an alkenyl group.
[0103] The term “arylalkoxy” or “aralkoxy,” as used herein, alone or in combination, refers to an aryl group attached to the parent molecular moiety through an alkoxy group.
[0104] The term “arylalkyl” or “aralkyl,” as used herein, alone or in combination, refers to an aryl group attached to the parent molecular moiety through an alkyl group.
[0105] The term “arylalkynyl” or “aralkynyl,” as used herein, alone or in combination, refers to an aryl group attached to the parent molecular moiety through an alkynyl group.
[0106] The term “arylalkanoyl” or “aralkanoyl” or “aroyl,” as used herein, alone or in combination, refers to an acyl radical derived from an aryl-substituted alkanecarboxylic acid such as benzoyl, napthoyl, phenylacetyl, 3-phenylpropionyl(hydrocinnamoyl), 4-phenylbutyryl, (2-naphthyl)acetyl, 4-chlorohydrocinnamoyl, and the like.
[0107] The term aryloxy as used herein, alone or in combination, refers to an aryl group attached to the parent molecular moiety through an oxy.
[0108] The terms “benzo” and “benz,” as used herein, alone or in combination, refer to the divalent radical C 6 H 4 =derived from benzene. Examples include benzothiophene and benzimidazole.
[0109] The term “carbamate,” as used herein, alone or in combination, refers to an ester of carbamic acid (—NHCOO—) which may be attached to the parent molecular moiety from either the nitrogen or acid end, and which may be optionally substituted as defined herein.
[0110] The term “O-carbamyl” as used herein, alone or in combination, refers to a —OC(O)NRR′, group-with R and R′ as defined herein.
[0111] The term “N-carbamyl” as used herein, alone or in combination, refers to a ROC(O)NR′— group, with R and R′ as defined herein.
[0112] The term “carbonyl,” as used herein, when alone includes formyl [—C(O)H] and in combination is a —C(O)— group.
[0113] The term “carboxy,” as used herein, refers to —C(O)OH or the corresponding “carboxylate” anion, such as is in a carboxylic acid salt. An “O-carboxy” group refers to a RC(O)O— group, where R is as defined herein. A “C-carboxy” group refers to a —C(O)OR groups where R is as defined herein.
[0114] The term “cyano,” as used herein, alone or in combination, refers to —CN.
[0115] The term “cycloalkyl,” as used herein, alone or in combination, refers to a saturated or partially saturated monocyclic, bicyclic or tricyclic alkyl radical wherein each cyclic moiety contains from 3 to 12, preferably five to seven, carbon atom ring members and which may optionally be a benzo fused ring system which is optionally substituted as defined herein. Examples of such cycloalkyl radicals include cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cycloheptyl, octahydronaphthyl, 2,3-dihydro-1H-indenyl, adamantyl and the like. “Bicyclic” and “tricyclic” as used herein are intended to include both fused ring systems, such as decahydonapthalene, octahydronapthalene as well as the multicyclic (multicentered) saturated or partially unsaturated type. The latter type of isomer is exemplified in general by, bicyclo[1,1,1]pentane, camphor, adamantane, and bicyclo[3,2,1]octane.
[0116] The term “ester,” as used herein, alone or in combination, refers to a carboxy group bridging two moieties linked at carbon atoms.
[0117] The term “ether,” as used herein, alone or in combination, refers to an oxy group bridging two moieties linked at carbon atoms.
[0118] The term “halo,” or “halogen,” as used herein, alone or in combination, refers to fluorine, chlorine, bromine, or iodine.
[0119] The term “haloalkoxy,” as used herein, alone or in combination, refers to a haloalkyl group attached to the parent molecular moiety through an oxygen atom.
[0120] The term “haloalkyl,” as used herein, alone or in combination, refers to an alkyl radical having the meaning as defined above wherein one or more hydrogens are replaced with a halogen. Specifically embraced are monohaloalkyl, dihaloalkyl and polyhaloalkyl radicals. A monohaloalkyl radical, for one example, may have an iodo, bromo, chloro or fluoro atom within the radical. Dihalo and polyhaloalkyl radicals may have two or more of the same halo atoms or a combination of different halo radicals. Examples of haloalkyl radicals include fluoromethyl, difluoromethyl, trifluoromethyl, chloromethyl, dichloromethyl, trichloromethyl, pentafluoroethyl, heptafluoropropyl, difluorochloromethyl, dichlorofluoromethyl, difluoroethyl, difluoropropyl, dichloroethyl and dichloropropyl. “Haloalkylene” refers to a haloalkyl group attached at two or more positions. Examples include fluoromethylene (—CFH—), difluoromethylene (—CF 2 —), chloromethylene (—CHCl—) and the like.
[0121] The term “heteroalkyl,” as used herein, alone or in combination, refers to a stable straight or branched chain, or cyclic hydrocarbon radical, or combinations thereof, fully saturated or containing from 1 to 3 degrees of unsaturation, consisting of the stated number of carbon atoms and from one to three heteroatoms selected from the group consisting of O, N, and S, and wherein the nitrogen and sulfur atoms may optionally be oxidized and the nitrogen heteroatom may optionally be quaternized. The heteroatom(s) O, N and S may be placed at any interior position of the heteroalkyl group. Up to two heteroatoms may be consecutive, such as, for example, —CH 2 —NH—OCH 3 .
[0122] The term “heteroaryl,” as used herein, alone or in combination, refers to 3 to 7 membered, preferably 5 to 7 membered, unsaturated heteromonocyclic rings, or fused polycyclic rings in which at least one of the fused rings is unsaturated, wherein at least one atom is selected from the group consisting of O, S, and N. The term also embraces fused polycyclic groups wherein heterocyclic radicals are fused with aryl radicals, wherein heteroaryl radicals are fused with other heteroaryl radicals, or wherein heteroaryl radicals are fused with cycloalkyl radicals. Examples of heteroaryl groups include pyrrolyl, pyrrolinyl, imidazolyl, pyrazolyl, pyridyl, pyrimidinyl, pyrazinyl, pyridazinyl, triazolyl, pyranyl, furyl, thienyl, oxazolyl, isoxazolyl, oxadiazolyl, thiazolyl, thiadiazolyl, isothiazolyl, indolyl, isoindolyl, indolizinyl, benzimidazolyl, quinolyl, isoquinolyl, quinoxalinyl, quinazolinyl, indazolyl, benzotriazolyl, benzodioxolyl, benzopyranyl, benzoxazolyl, benzoxadiazolyl, benzothiazolyl, benzothiadiazolyl, benzofuryl, benzothienyl, chromonyl, coumarinyl, benzopyranyl, tetrahydroquinolinyl, tetrazolopyridazinyl, tetrahydroisoquinolinyl, thienopyridinyl, furopyridinyl, pyrrolopyridinyl and the like. Exemplary tricyclic heterocyclic groupsinclude carbazolyl, benzidolyl, phenanthrolinyl, dibenzofuranyl, acridinyl, phenanthridinyl, xanthenyl and the like.
[0123] The terms “heterocycloalkyl” and, interchangeably, “heterocycle,” as used herein, alone or in combination, each refer to a saturated, partially unsaturated, or fully unsaturated monocyclic, bicyclic, or tricyclic heterocyclic radical containing at least one, preferably 1 to 4, and more preferably 1 to 2 heteroatoms as ring members, wherein each said heteroatom may be independently selected from the group consisting of nitrogen, oxygen, and sulfur, and wherein there are preferably 3 to 8 ring members in each ring, more preferably 3 to 7 ring members in each ring, and most preferably 5 to 6 ring members in each ring. “Heterocycloalkyl” and “heterocycle” are intended to include sulfones, sulfoxides, N-oxides of tertiary nitrogen ring members, and carbocyclic fused and benzo fused ring systems; additionally, both terms also include systems where a heterocycle ring is fused to an aryl group, as defined herein, or an additional heterocycle group. Heterocycle groups of the invention are exemplified by aziridinyl, azetidinyl, 1,3-benzodioxolyl, dihydroisoindolyl, dihydroisoquinolinyl, dihydrocinnolinyl, dihydrobenzodioxinyl, dihydro[1,3]oxazolo[4,5-b]pyridinyl, benzothiazolyl, dihydroindolyl, dihy-dropyridinyl, 1,3-dioxanyl, 1,4-dioxanyl, 1,3-dioxolanyl, isoindolinyl, morpholinyl, piperazinyl, pyrrolidinyl, tetrahydropyridinyl, piperidinyl, thiomorpholinyl, and the like. The heterocycle groups may be optionally substituted unless specifically prohibited.
[0124] The term “hydrazinyl” as used herein, alone or in combination, refers to two amino groups joined by a single bond, i.e., —N—N—.
[0125] The term “hydroxy,” as used herein, alone or in combination, refers to —OH.
[0126] The term “hydroxyalkyl,” as used herein, alone or in combination, refers to a hydroxy group attached to the parent molecular moiety through an alkyl group.
[0127] The term “imino,” as used herein, alone or in combination, refers to ═N—.
[0128] The term “iminohydroxy,” as used herein, alone or in combination, refers to ═N(OH) and ═N—O—.
[0129] The phrase “in the main chain” refers to the longest contiguous or adjacent chain of carbon atoms starting at the point of attachment of a group to the compounds of this invention.
[0130] The term “isocyanato” refers to a —NCO group.
[0131] The term “isothiocyanato” refers to a —NCS group.
[0132] The phrase “linear chain of atoms” refers to the longest straight chain of atoms independently selected from carbon, nitrogen, oxygen and sulfur.
[0133] The term “lower,” as used herein, alone or in combination, means containing from 1 to and including 6 carbon atoms.
[0134] The term “mercaptyl” as used herein, alone or in combination, refers to an RS— group, where R is as defined herein.
[0135] The term “nitro,” as used herein, alone or in combination, refers to —NO 2 .
[0136] The terms “oxy” or “oxa,” as used herein, alone or in combination, refer to —O—.
[0137] The term “oxo,” as used herein, alone or in combination, refers to ═O.
[0138] The term “perhaloalkoxy” refers to an alkoxy group where all of the hydrogen atoms are replaced by halogen atoms.
[0139] The term “perhaloalkyl” as used herein, alone or in combination, refers to an alkyl group where all of the hydrogen atoms are replaced by halogen atoms.
[0140] The terms “sulfonate,” “sulfonic acid,” and “sulfonic,” as used herein, alone or in combination, refer the —SO 3 H group and its anion as the sulfonic acid is used in salt formation.
[0141] The term “sulfanyl,” as used herein, alone or in combination, refers to —S—.
[0142] The term “sulfinyl,” as used herein, alone or in combination, refers to —S(O)—.
[0143] The term “sulfonyl,” as used herein, alone or in combination, refers to —SO 2 —.
[0144] The term “N-sulfonamide” refers to a —S(═O) 2 NR— group with R as defined herein.
[0145] The term “S-sulfonamide” refers to a —NRS(═O) 2 —, group, with R as defined herein.
[0146] The terms “thia” and “thio,” as used herein, alone or in combination, refer to a S group or an ether wherein the oxygen is replaced with sulfur. The oxidized derivatives of the thio group, namely sulfinyl and sulfonyl, are included in the definition of thia and thio.
[0147] The term “thiol,” as used herein, alone or in combination, refers to an —SH group.
[0148] The term “thiocarbonyl,” as used herein, when alone includes thioformyl C(S)H and in combination is a —C(S)— group.
[0149] The term “N-thiocarbamyl” refers to an ROC(S)NR′ group, with R and R′ as defined herein.
[0150] The term “O-thiocarbamyl” refers to a —OC(S)NRR′, group with R and R′ as defined herein.
[0151] The term “thiocyanato” refers to a —CNS group.
[0152] The term “trihalomethanesulfonamido” refers to a X 3 CS(O) 2 NR— group with X is a halogen and R as defined herein.
[0153] The term “trihalomethanesulfonyl” refers to a X 3 CS(O) 2 — group where X is a halogen.
[0154] The term “trihalomethoxy” refers to a X 3 CO— group where X is a halogen.
[0155] The term “trisubstituted silyl,” as used herein, alone or in combination, refers to a silicone group substituted at its three free valences with groups as listed herein under the definition of substituted amino. Examples include trimethysilyl, tert-butyldimethylsilyl, triphenylsilyl and the like.
[0156] Any definition herein may be used in combination with any other definition to describe a composite structural group. By convention, the trailing element of any such definition is that which attaches to the parent moiety. For example, the composite group alkylamido would represent an alkyl group attached to the parent molecule through an amido group, and the term alkoxyalkyl would represent an alkoxy group attached to the parent molecule through an alkyl group.
[0157] When a group is defined to be “null,” what is meant is that said group is absent.
[0158] The term “optionally substituted” means the anteceding group may be substituted or unsubstituted. When substituted, the substituents of an “optionally substituted” group may include, without limitation, one or more substituents independently selected from the following groups or a particular designated set of groups, alone or in combination: lower alkyl, lower alkenyl, lower alkynyl, lower alkanoyl, lower heteroalkyl, lower heterocycloalkyl, lower haloalkyl, lower haloalkenyl, lower haloalkynyl, lower perhaloalkyl, lower perhaloalkoxy, lower cycloalkyl, phenyl, aryl, aryloxy, lower alkoxy, lower haloalkoxy, oxo, lower acyloxy, carbonyl, carboxyl, lower alkylcarbonyl, lower carboxyester, lower carboxamido, cyano, hydrogen, halogen, hydroxy, amino, lower alkylamino, arylamino, amido, nitro, thiol, lower alkylthio, arylthio, lower alkylsulfinyl, lower alkylsulfonyl, arylsulfinyl, arylsulfonyl, arylthio, sulfonate, sulfonic acid, trisubstituted silyl, N 3 , SH, SCH 3 , C(O)CH 3 , CO 2 CH 3 , CO 2 H, pyridinyl, thiophene, furanyl, lower carbamate, and lower urea. Two substituents may be joined together to form a fused five-, six-, or seven-membered carbocyclic or heterocyclic ring consisting of zero to three heteroatoms, for example forming methylenedioxy or ethylenedioxy. An optionally substituted group may be unsubstituted (e.g., —CH 2 CH 3 ), fully substituted (e.g., —CF 2 CF 3 ), monosubstituted (e.g., —CH 2 CH 2 F) or substituted at a level anywhere in-between fully substituted and monosubstituted (e.g., —CH 2 CF 3 ). Where substituents are recited without qualification as to substitution, both substituted and unsubstituted forms are encompassed. Where a substituent is qualified as “substituted,” the substituted form is specifically intended. Additionally, different sets of optional substituents to a particular moiety may be defined as needed; in these cases, the optional substitution will be as defined, often immediately following the phrase, “optionally substituted with.”
[0159] The term R or the term R′, appearing by itself and without a number designation, unless otherwise defined, refers to a moiety selected from the group consisting of null, hydrogen, alkyl, cycloalkyl, heteroalkyl, aryl, heteroaryl and heterocycloalkyl, any of which may be optionally substituted. Such R and R′ groups should be understood to be optionally substituted as defined herein. Whether an R group has a number designation or not, every R group, including R, R′ and R n where n=(1, 2, 3, . . . n), every substituent, and every term should be understood to be independent of every other in terms of selection from a group. Should any variable, substituent, or term (e.g. aryl, heterocycle, R, etc.) occur more than one time in a formula or generic structure, its definition at each occurrence is independent of the definition at every other occurrence. Those of skill in the art will further recognize that certain groups may be attached to a parent molecule or may occupy a position in a chain of elements from either end as written. Thus, by way of example only, an unsymmetrical group such as C(O)N(R) may be attached to the parent moiety at either the carbon or the nitrogen.
[0160] Asymmetric centers exist in the compounds of the present invention. These centers are designated by the symbols “R” or “S,” depending on the configuration of substituents around the chiral carbon atom. It should be understood that the invention encompasses all stereochemical isomeric forms, including diastereomeric, enantiomeric, and epimeric forms, as well as d-isomers and 1-isomers, and mixtures thereof. Individual stereoisomers of compounds can be prepared synthetically from commercially available starting materials which contain chiral centers or by preparation of mixtures of enantiomeric products followed by separation such as conversion to a mixture of diastereomers followed by separation or recrystallization, chromatographic techniques, direct separation of enantiomers on chiral chromatographic columns, or any other appropriate method known in the art. Starting compounds of particular stereochemistry are either commercially available or can be made and resolved by techniques known in the art. Additionally, the compounds of the present invention may exist as geometric isomers. The present invention includes all cis, trans, syn, anti, entgegen (E), and zusammen (Z) isomers as well as the appropriate mixtures thereof. Additionally, compounds may exist as tautomers; all tautomeric isomers are provided by this invention. Additionally, the compounds of the present invention can exist in unsolvated as well as solvated forms with pharmaceutically acceptable solvents such as water, ethanol, and the like. In general, the solvated forms are considered equivalent to the unsolvated forms for the purposes of the present invention.
[0161] The term “bond” refers to a covalent linkage between two atoms, or two moieties when the atoms joined by the bond are considered to be part of larger substructure. A bond may be single, double, or triple unless otherwise specified. A dashed line between two atoms in a drawing of a molecule indicates that an additional bond may be present or absent at that position.
[0162] The term “combination therapy” means the administration of two or more therapeutic agents to treat a therapeutic condition or disorder described in the present disclosure. Such administration encompasses co-administration of these therapeutic agents in a substantially simultaneous manner, such as in a single capsule having a fixed ratio of active ingredients or in multiple, separate capsules for each active ingredient. In addition, such administration also encompasses use of each type of therapeutic agent in a sequential manner. In either case, the treatment regimen will provide beneficial effects of the drug combination in treating the conditions or disorders described herein.
[0163] The terms “therapy” or “treating” as used herein refer to (1) reducing the rate of progress of a disease, or, in case of cancer reducing the size of the tumor; (2) inhibiting to some extent further progress of the disease, which in case of cancer may mean slowing to some extent, or preferably stopping, tumor metastasis or tumor growth; and/or, (3) relieving to some extent (or, preferably, eliminating) one or more symptoms associated with the disease. Thus, the term “therapeutically effective amount” as used herein refers to that amount of the compound being administered which will provide therapy or affect treatment.
[0164] In some aspects of the invention, the compounds of the present invention are also anti-tumor compounds and/or inhibit the growth of a tumor, i.e., they are tumor-growth-inhibiting compounds. The terms “anti-tumor” and “tumor-growth-inhibiting,” when modifying the term “compound,” and the terms “inhibiting” and “reducing”, when modifying the terms “compound” and/or “tumor,” mean that the presence of the subject compound is correlated with at least the slowing of the rate of growth of the tumor. More preferably, the terms “anti-tumor,” “tumor-growth-inhibiting,” “inhibiting,” and “reducing” refer to a correlation between the presence of the subject compound and at least the temporary cessation of tumor growth. The terms “anti-tumor,” “tumor-growth-inhibiting,” “inhibiting,” and “reducing” also refer to, a correlation between the presence of the subject compound and at least the temporary reduction in the mass of the tumor.
[0165] The term “function” refers to the cellular role of HDAC. The term “catalytic activity”, in the context of the invention, defines the rate at which HDAC deacetylates a substrate. Catalytic activity can be measured, for example, by determining the amount of a substrate converted to a product as a function of time. Deacetylation of a substrate occurs at the active-site of HDAC. The active-site is normally a cavity in which the substrate binds to HDAC and is deacetylated.
[0166] The term “substrate” as used herein refers to a molecule deacetylated by HDAC. The substrate is preferably a peptide and more preferably a protein. In some embodiments, the protein is a histone, whereas in other embodiments, the protein is not a histone.
[0167] The term “inhibit” refers to decreasing the cellular function of HDAC. It is understood that compounds of the present invention may inhibit the cellular function of HDAC by various direct or indirect mechanisms, in particular by direct or indirect inhibition of the catalytic activity of HDAC.
[0168] The term “activates” refers to increasing the cellular function of HDAC.
[0169] The term “activate” refers to increasing the cellular function of HDAC.
[0170] HDAC function is preferably the interaction with a natural binding partner and most preferably catalytic activity.
[0171] The term “modulate” refers to altering the function of HDAC by increasing or decreasing the probability that a complex forms between HDAC and a natural binding partner. A modulator may increase the probability that such a complex forms between HDAC and the natural binding partner, or may increase or decrease the probability that a complex forms between HDAC and the natural binding partner depending on the concentration of the compound exposed to HDAC, or may decrease the probability that a complex forms between HDAC and the natural binding partner. A modulator may activate the catalytic activity of HDAC, or may activate or inhibit the catalytic activity of HDAC depending on the concentration of the compound exposed to HDAC, or may inhibit the catalytic activity of HDAC.
[0172] The term “complex” refers to an assembly of at least two molecules bound to one another. The term “natural binding partner” refers to polypeptides that bind to HDAC in cells. A change in the interaction between HDAC and a natural binding partner can manifest itself as an increased or decreased probability that the interaction forms, or an increased or decreased concentration of HDAC/natural binding partner complex.
[0173] The term “contacting” as used herein refers to mixing a solution comprising a compound of the invention with a liquid medium bathing the cells of the methods. The solution comprising the compound may also comprise another component, such as dimethylsulfoxide (DMSO), which facilitates the uptake of the compound or compounds into the cells of the methods. The solution comprising the compound of the invention may be added to the medium bathing the cells by utilizing a delivery apparatus, such as a pipet-based device or syringe-based device.
[0174] The term “monitoring” refers to observing the effect of adding the compound to the cells of the method. The effect can be manifested in a change in cell phenotype, cell proliferation, HDAC catalytic activity, substrate protein acetylation levels, gene expression changes, or in the interaction between HDAC and a natural binding partner.
[0175] The term “effect” describes a change or an absence of a change in cell phenotype or cell proliferation. “Effect” can also describe a change or an absence of a change in the catalytic activity of HDAC. “Effect” can also describe a change or an absence of a change in an interaction between HDAC and a natural binding partner.
[0176] The term “cell phenotype” refers to the outward appearance of a cell or tissue or the function of the cell or tissue. Examples of cell phenotype are cell size (reduction or enlargement), cell proliferation (increased or decreased numbers of cells), cell differentiation (a change or absence of a change in cell shape), cell survival, apoptosis (cell death), or the utilization of a metabolic nutrient (e.g., glucose uptake). Changes or the absence of changes in cell phenotype are readily measured by techniques known in the art.
[0177] “HDAC inhibitor” is used herein to refer to a compound that exhibits an IC 50 with respect to HDAC activity of no more than about 100 μM and more typically not more than about 50 μM, as measured in the biochemical in vitro HDAC-inhibition assay, cellular histone hyperacetylation assay, and differential cytotoxicity assay described generally herein below. “IC 50 ” is that concentration of inhibitor which reduces the activity of an enzyme (e.g., HDAC) to half-maximal level. Representative compounds of the present invention have been discovered to exhibit inhibitory activity against HDAC. Compounds of the present invention preferably exhibit an IC 50 with respect to HDAC of no more than about 10 μM, more preferably, no more than about 5 μM, even more preferably not more than about 1 μM, and most preferably, not more than about 200 nM, as measured in the HDAC assays described herein.
[0178] The term “prodrug” refers to a compound that is made more active in vivo. Certain compounds of the present invention may also exist as prodrugs, as described in Hydrolysis in Drug and Prodrug Metabolism: Chemistry, Biochemistry, and Enzymology (Testa, Bernard and Mayer, Joachim M. Wiley-VHCA, Zurich, Switzerland 2003). Prodrugs of the compounds described herein are structurally modified forms of the compound that readily undergo chemical changes under physiological conditions to provide the compound. Additionally, prodrugs can be converted to the compound by chemical or biochemical methods in an ex vivo environment. For example, prodrugs can be slowly converted to a compound when placed in a transdermal patch reservoir with a suitable enzyme or chemical reagent. Prodrugs are often useful because, in some situations, they may be easier to administer than the compound, or parent drug. They may, for instance, be bioavailable by oral administration whereas the parent drug is not. The prodrug may also have improved solubility in pharmaceutical compositions over the parent drug. A wide variety of prodrug derivatives are known in the art, such as those that rely on hydrolytic cleavage or oxidative activation of the prodrug. An example, without limitation, of a prodrug would be a compound which is administered as an ester (the “prodrug”), but then is metabolically hydrolyzed to the carboxylic acid, the active entity. Additional examples include peptidyl derivatives of a compound. Yet another example of a prodrug is protected thiol compounds. Thiols bearing hydrolyzable protecting groups can unmask protected SH groups prior to or simultaneous to use. As shown below, the moiety —C(O)—R E of a thioester may be hydrolyzed to yield a thiol and a pharmaceutically acceptable acid HO—C(O)—R E .
[0179] The term “therapeutically acceptable prodrug,” refers to those prodrugs or zwitterions which are suitable for use in contact with the tissues of patients without undue toxicity, irritation, and allergic response, are commensurate with a reasonable benefit/risk ratio, and are effective for their intended use.
[0180] A “pharmaceutically active metabolite” is intended to mean a pharmacologically active product produced through metabolism in the body of a specified compound or salt thereof. Metabolites of a compound may be identified using routine techniques known in the art and their activities determined using tests such as those decribed herein.
[0181] The term “thiol protecting group” refers to thiols bearing hydrolyzable protecting groups that can unmask protected SH groups prior to or simultaneous to use. Preferred thiol protecting groups include but are not limited to thiol esters which release pharmaceutically acceptable acids along with an active thiol moiety. Such pharmaceutically acceptable acids are generally nontoxic and do not abrogate the biological activity of the active thiol moiety. Examples of pharmaceutically acceptable acids include, but are not limited to: N,N-diethylglycine; 4-ethylpiperazinoacetic acid; ethyl 2-methoxy-2-phenylacetic acid; N,N-dimethylglycine; (nitrophenoxysulfonyl)benzoic acid; acetic acid; maleic acid; fumaric acid; benzoic acid; tartraric acid; natural amino acids (like glutamate, aspartate, cyclic amino acids such proline); D-amino acids; butyric acid; fatty acids like palmitic acid, stearic acid, oleate; pipecolic acid; phosphonic acid; phosphoric acid; pivalate (trimethylacetic acid); succinic acid; cinnamic acid; anthranilic acid; salicylic acid; lactic acid; and pyruvic acids.
[0182] Another aspect of the present invention are compounds containing at least one thiol in a protected form, which can be released to provide a SH group prior to or simultaneous to use. Thiol moieties are known to be unstable in the presence of air and are oxidized to the corresponding disulfide. Protected thiol groups are those that can be converted under mild conditions into free thiol groups without other undesired side reactions taking place. Suitable thiol protecting groups include but are not limited to trityl (Trt), allyloxycarbonyl (Alloc), 1-(4,4-dimethyl-2,6-dioxocyclohex-1-ylidene)ethyl (Dde), acetamidomethyl (Acm), t-butyl (tBu), or the like. Preferred thiol protecting groups include lower alkanoyl, e.g. acetyl. Free thiol, disulfides, and protected thiols are understood to be within the scope of this invention.
[0183] As used herein, reference to “treatment” of a patient is intended to include prophylaxis. The term “patient” means all mammals including humans. Examples of patients include humans, cows, dogs, cats, goats, sheep, pigs, and rabbits. Preferably, the patient is a human.
[0184] The term “therapeutically acceptable salt,” as used herein, represents salts or zwitterionic forms of the compounds of the present invention which are water or oil-soluble or dispersible; which are suitable for treatment of diseases without undue toxicity, irritation, and allergic-response; which are commensurate with a reasonable benefit/risk ratio; and which are effective for their intended use. The salts can be prepared during the final isolation and purification of the compounds or separately by reacting the appropriate compound in the form of the free base with a suitable acid. Representative acid addition salts include acetate, adipate, alginate, L-ascorbate, aspartate, benzoate, benzenesulfonate (besylate), bisulfate, butyrate, camphorate, camphorsulfonate, citrate, digluconate, formate, fumarate, gentisate, glutarate, glycerophosphate, glycolate, hemisulfate, heptanoate, hexanoate, hippurate, hydrochloride, hydrobromide, hydroiodide, 2-hydroxyethansulfonate (isethionate), lactate, maleate, malate, malonate, DL-mandelate, mesitylenesulfonate, methanesulfonate, naphthylenesulfonate, nicotinate, 2-naphthalenesulfonate, oxalate, pamoate, pectinate, persulfate, 3-phenylproprionate, phosphonate, picrate, pivalate, propionate, pyroglutamate, succinate, sulfonate, tartrate, L-tartrate, trichloroacetate, trifluoroacetate, phosphate, glutamate, bicarbonate, para-toluenesulfonate (p-tosylate), and undecanoate. Also, basic groups in the compounds of the present invention can be quaternized with methyl, ethyl, propyl, and butyl chlorides, bromides, and iodides; dimethyl, diethyl, dibutyl, and diamyl sulfates; decyl, lauryl, myristyl, and steryl chlorides, bromides, and iodides; and benzyl and phenethyl bromides. Examples of acids which can be employed to form therapeutically acceptable addition salts include inorganic acids such as hydrochloric, hydrobromic, sulfuric, and phosphoric, and organic acids such as oxalic, maleic, succinic, and citric. Salts can also be formed by coordination of the compounds with an alkali metal or alkaline earth ion. Hence, the present invention contemplates sodium, potassium, magnesium, and calcium salts of the compounds of the compounds of the present invention and the like.
[0185] Basic addition salts can be prepared during the final isolation and purification of the compounds by reacting a carboxy group with a suitable base such as the hydroxide, carbonate, or bicarbonate of a metal cation or with ammonia or an organic primary, secondary, or tertiary amine. The cations of therapeutically acceptable salts include lithium, sodium, potassium, calcium, magnesium, and aluminum, as well as nontoxic quaternary amine cations such as ammonium, tetramethylammonium, tetraethylammonium, methylamine, dimethylamine, trimethylamine, triethylamine, diethylamine, ethylamine, tributylamine, pyridine, N,N-dimethylaniline, N-methylpiperidine, N-methylmorpholine, dicyclohexylamine, procaine, dibenzylamine, N,N-dibenzylphenethylamine, 1-ephenamine, and N,N′-dibenzylethylenediamine. Other representative organic amines useful for the formation of base addition salts include ethylenediamine, ethanolamine, diethanolamine, piperidine, and piperazine.
[0186] The compounds of the present invention can exist as therapeutically acceptable salts. The present invention includes compounds listed above in the form of salts, in particular acid addition salts. Suitable salts include those formed with both organic and inorganic acids. Such acid addition salts will normally be pharmaceutically acceptable. However, salts of non-pharmaceutically acceptable salts may be of utility in the preparation and purification of the compound in question. For a more complete discussion of the preparation and selection of salts, refer to Pharmaceutical Salts: Properties, Selection, and Use (Stahl, P. Heinrich. Wiley-VCfHA, Zurich, Switzerland, 2002).
[0187] The terms “polymorphs” and “polymorphic forms” and related terms herein refer to crystal forms of the same compound, and the present invention provides for polymorphs of compounds disclosed herein, as well as polymorphs of their salts, esters, and prodrugs. Structurally, a polymorph will often be a stable crystal of the compound and counterion, along with a fixed ratio of one or more coordinated solvent molecules. Functionally, different polymorphs may have different physical properties such as, for example, melting temperatures, heats of fusion, solubilities, dissolution rates and/or vibrational spectra as a result of the arrangement or conformation of the molecules in the crystal lattice. The differences in physical properties exhibited by polymorphs affect pharmaceutical parameters such as storage stability, compressibility and density (important in formulation and product manufacturing), and dissolution rates (an important factor in bioavailability). Differences in stability can result from changes in chemical reactivity (e.g. differential oxidation, such that a dosage form discolors more rapidly when comprised of one polymorph than when comprised of another polymorph) or mechanical changes (e.g. tablets crumble on storage as a kinetically favored polymorph converts to thermodynamically more stable polymorph) or both (e.g., tablets of one polymorph are more susceptible to breakdown at high humidity). Polymorphs of a molecule can be obtained by a number of methods, as known in the art. Such methods include, but are not limited to, melt recrystallization, melt cooling, solvent recrystallization, desolvation, rapid evaporation, rapid cooling, slow cooling, vapor diffusion and sublimation. Techniques for characterizing polymorphs include, but are not limited to, differential scanning calorimetry (DSC), X-ray powder diffractometry (XRPD), single crystal X-ray diffractometry, vibrational spectroscopy, e.g. IR and Raman spectroscopy, solid state NMR, hot stage optical microscopy, scanning electron microscopy (SEM), electron crystallography and quantitative analysis, particle size analysis (PSA), surface area analysis, solubility studies and dissolution studies.
[0188] The term “solubility” is generally intended to be synonymous with the term “aqueous solubility,” and refers to the ability, and the degree of the ability, of a compound to dissolve in water or an aqueous solvent or buffer, as might be found under physiological conditions. Aqueous solubility is, in and of itself, a useful quantitative measure, but it has additional utility as a correlate and predictor, with some limitations which will be clear to those of skill in the art, of oral bioavailability. In practice, a soluble compound is generally desirable, and the more soluble, the better. There are notable exceptions; for example, certain compounds intended to be administered as depot injections, if stable over time, may actually benefit from low solubility, as this may assist in slow release from the injection site into the plasma. Solubility is typically reported in mg/mL, but other measures, such as gig, may be used. Solubilities typically deemed acceptable may range from 1 mg/mL into the hundreds or thousands of mg/mL.
[0189] While it may be possible for the compounds of the subject invention to be administered as the raw chemical, it is also possible to present them as a pharmaceutical formulation. Accordingly, the subject invention provides a pharmaceutical formulation comprising a compound or a pharmaceutically acceptable salt, ester, prodrug or solvate thereof, together with one or more pharmaceutically acceptable carriers thereof and optionally one or more other therapeutic ingredients. The carrier(s) must be “acceptable” in the sense of being compatible with the other ingredients of the formulation and not deleterious to the recipient thereof. Proper formulation is dependent upon the route of administration chosen. Any of the well-known techniques, carriers, and excipients may be used as suitable and as understood in the art; e.g., in Remington's Pharmaceutical Sciences. The pharmaceutical compositions of the present invention may be manufactured in a manner that is itself known, e.g., by means of conventional mixing, dissolving, granulating, dragee-making, levigating, emulsifying, encapsulating, entrapping or compression processes.
[0190] The formulations include those suitable for oral, parenteral (including subcutaneous, intradermal, intramuscular, intravenous, intraarticular, and intramedullary), intraperitoneal, transmucosal, transdermal, rectal and topical (including dermal, buccal, sublingual and intraocular) administration although the most suitable route may depend upon for example the condition and disorder of the recipient. The formulations may conveniently be presented in unit dosage form and may be prepared by any of the methods well known in the art of pharmacy. All methods include the step of bringing into association a compound of the subject invention or a pharmaceutically acceptable salt, ester, prodrug or solvate thereof (“active ingredient”) with the carrier which constitutes one or more accessory ingredients. In general, the formulations are prepared by uniformly and intimately bringing into association the active ingredient with liquid carriers or finely divided solid carriers or both and then, if necessary, shaping the product into the desired formulation.
[0191] Formulations of the present invention suitable for oral administration may be presented as discrete units such as capsules, cachets or tablets each containing a predetermined amount of the active ingredient; as a powder or granules; as a solution or a suspension in an aqueous liquid or a non-aqueous liquid; or as an oil-in-water liquid emulsion or a water-in-oil liquid emulsion. The active ingredient may also be presented as a bolus, electuary or paste.
[0192] Pharmaceutical preparations which can be used orally include tablets, push-fit capsules made of gelatin, as well as soft, sealed capsules made of gelatin and a plasticizer, such as glycerol or sorbitol. Tablets may be made by compression or molding, optionally with one or more accessory ingredients. Compressed tablets may be prepared by compressing in a suitable machine the active ingredient in a free-flowing form such as a powder or granules, optionally mixed with binders, inert diluents, or lubricating, surface active or dispersing agents. Molded tablets may be made by molding in a suitable machine a mixture of the powdered compound moistened with an inert liquid diluent. The tablets may optionally be coated or scored and may be formulated so as to provide slow or controlled release of the active ingredient therein. All formulations for oral administration should be in dosages suitable for such administration. The push-fit capsules can contain the active ingredients in admixture with filler such as lactose, binders such as starches, and/or lubricants such as talc or magnesium stearate and, optionally, stabilizers. In soft capsules, the active compounds may be dissolved or suspended in suitable liquids, such as fatty oils, liquid paraffin, or liquid polyethylene glycols. In addition, stabilizers may be added. Dragee cores are provided with suitable coatings. For this purpose, concentrated sugar solutions may be used, which may optionally contain gum arabic, talc, polyvinyl pyrrolidone, carbopol gel, polyethylene glycol, and/or titanium dioxide, lacquer solutions, and suitable organic solvents or solvent mixtures. Dyestuffs or pigments may be added to the tablets or dragee coatings for identification or to characterize different combinations of active compound doses.
[0193] The compounds may be formulated for parenteral administration by injection, e.g., by bolus injection or continuous infusion. Formulations for injection may be presented in unit dosage form, e.g., in ampoules or in multi-dose containers, with an added preservative. The compositions may take such forms as suspensions, solutions or emulsions in oily or aqueous vehicles, and may contain formulatory agents such as suspending, stabilizing and/or dispersing agents. The formulations may be presented in unit-dose or multi-dose containers, for example sealed ampoules and vials, and may be stored in powder form or in a freeze-dried (lyophilized) condition requiring only the addition of the sterile liquid carrier, for example, saline or sterile pyrogen-free water, immediately prior to use. Extemporaneous injection solutions and suspensions may be prepared from sterile powders, granules and tablets of the kind previously described.
[0194] Formulations for parenteral administration include aqueous and non-aqueous (oily) sterile injection solutions of the active compounds which may contain antioxidants, buffers, bacteriostats and solutes which render the formulation isotonic with the blood of the intended recipient; and aqueous and non-aqueous sterile suspensions which may include suspending agents and thickening agents. Suitable lipophilic solvents or vehicles include fatty oils such as sesame oil, or synthetic fatty acid esters, such as ethyl oleate or triglycerides, or liposomes. Aqueous injection suspensions may contain substances which increase the viscosity of the suspension, such as sodium carboxymethyl cellulose, sorbitol, or dextran. Optionally, the suspension may also contain suitable stabilizers or agents which increase the solubility of the compounds to allow for the preparation of highly concentrated solutions.
[0195] In addition to the formulations described previously, the compounds may also be formulated as a depot preparation. Such long acting formulations may be administered by implantation (for example subcutaneously or intramuscularly) or by intramuscular injection. Thus, for example, the compounds may be formulated with suitable polymeric or hydrophobic materials (for example as an emulsion in an acceptable oil) or ion exchange resins, or as sparingly soluble derivatives, for example, as a sparingly soluble salt.
[0196] For buccal or sublingual administration, the compositions may take the form of tablets, lozenges, pastilles, or gels formulated in conventional manner. Such compositions may comprise the active ingredient in a flavored basis such as sucrose and acacia or tragacanth.
[0197] The compounds may also be formulated in rectal compositions such as suppositories or retention enemas, e.g., containing conventional suppository bases such as cocoa butter, polyethylene glycol, or other glycerides.
[0198] Compounds of the present invention may be administered topically, that is by non-systemic administration. This includes the application of a compound of the present invention externally to the epidermis or the buccal cavity and the instillation of such a compound into the ear, eye and nose, such that the compound does not significantly enter the blood stream. In contrast, systemic administration refers to oral, intravenous, intraperitoneal and intramuscular administration.
[0199] Formulations suitable for topical administration include liquid or semi-liquid preparations suitable for penetration through the skin to the site of inflammation such as gels, liniments, lotions, creams, ointments or pastes, and drops suitable for administration to the eye, ear or nose. The active ingredient may comprise, for topical administration, from 0.001% to 10% w/w, for instance from 1% to 2% by weight of the formulation. It may however comprise as much as 10% w/w but preferably will comprise less than 5% w/w, more preferably from 0.1% to 1% w/w of the formulation.
[0200] For administration by inhalation the compounds according to the invention are conveniently delivered from an insufflator, nebulizer pressurized packs or other convenient means of delivering an aerosol spray. Pressurized packs may comprise a suitable propellant such as dichlorodifluoromethane, trichlorofluoromethane, dichlorotetrafluoroethane, carbon dioxide or other suitable gas. In the case of a pressurized aerosol, the dosage unit may be determined by providing a valve to deliver a metered amount. Alternatively, for administration by inhalation or insufflation, the compounds according to the invention may take the form of a dry powder composition, for example a powder mix of the compound and a suitable powder base such as lactose or starch. The powder composition may be presented in unit dosage form, in for example, capsules, cartridges, gelatin or blister packs from which the powder may be administered with the aid of an inhalator or insufflator.
[0201] In a certain embodiments, pharmaceutical preparations of compound(s) or active ingredient(s) of the present invention may be formulated by Latitude Pharmaceuticals Inc. located in 9865 Mesa Rim Road, STE 201, San Diego, Calif. 92121 using their trade secret and proprietary formulation named “F101”. The composition of said formulation F101 is known to contain triglyceride, soy lecithin, vitamin E and PEG400.
[0202] Preferred unit dosage formulations are those containing an effective dose, as herein below recited, or an appropriate fraction thereof, of the active ingredient.
[0203] It should be understood that in addition to the ingredients particularly mentioned above, the formulations of this invention may include other agents conventional in the art having regard to the type of formulation in question, for example those suitable for oral administration may include flavoring agents.
[0204] The compounds of the invention may be administered orally or via injection at a dose of from 0.1 to 500 mg/kg per day. The dose range for adult humans is generally from 5 mg to 2 g/day. Tablets or other forms of presentation provided in discrete units may conveniently contain an amount of compound of the invention which is effective at such dosage or as a multiple of the same, for instance, units containing 5 mg to 500 mg, usually around 10 mg to 200 mg.
[0205] Further, the compounds of the invention may be administered on a daily basis or on a schedule containing days where dosing does not take place. In certain embodiments, dosing may take place every other day. In other embodiments, dosing may take place for five consecutive days of a week, then be followed by two non-dosing days. The choice of dosing schedule will depend on many factors, including, for example, the formulation chosen, route of administration, and concurrent pharmacotherapies, and may vary on a patient-to-patient basis. It is considered within the capacity of one skilled in the art to select a schedule that will maximize the therapeutic benefit and minimize any potential side effects in a patient.
[0206] The amount of active ingredient that may be combined with the carrier materials to produce a single dosage form will vary depending upon the host treated and the particular mode of administration.
[0207] The compounds of the subject invention can be administered in various modes, e.g. orally, topically, or by injection. The precise amount of compound administered to a patient will be the responsibility of the attendant physician. The specific dose level for any particular patient will depend upon a variety of factors including the activity of the specific compound employed, the age, body weight, general health, sex, diets, time of administration, route of administration, rate of excretion, drug combination, the precise disorder being treated, and the severity of the indication or condition being treated. Also, the route of administration may vary depending on the condition and its severity.
[0208] In certain instances, it may be appropriate to administer at least one of the compounds described herein (or a pharmaceutically acceptable salt, ester, or prodrug thereof) in combination with another therapeutic agent. By way of example only, if one of the side effects experienced by a patient upon receiving one of the compounds herein is hypertension, then it may be appropriate to administer an anti-hypertensive agent in combination with the initial therapeutic agent. Or, by way of example only, the therapeutic effectiveness of one of the compounds described herein may be enhanced by administration of an adjuvant (i.e., by itself the adjuvant may only have minimal therapeutic benefit, but in combination with another therapeutic agent, the overall therapeutic benefit to the patient is enhanced). Or, by way of example only, the benefit of experienced by a patient may be increased by administering one of the compounds described herein with another therapeutic agent (which also includes a therapeutic regimen) that also has therapeutic benefit. By way of example only, in a treatment for cancer involving administration of one of the compounds described herein, increased therapeutic benefit may result by also providing the patient with another therapeutic agent for cancer. In any case, regardless of the disease, disorder, or condition being treated, the overall benefit experienced by the patient may simply be additive of the two therapeutic agents or the patient may experience a synergistic benefit.
[0209] Specific, non-limiting examples of possible combination therapies include use of the compounds of the invention with another chemotherapeutic agent such as aromatase inhibitors, antiestrogen, anti-androgen, or a gonadorelin agonists, topoisomerase 1 and 2 inhibitors, microtubule active agents, alkylating agents, antimeoplastic antimetabolite, or platin containing compound, lipid or protein kinase targeting agents, protein or lipid phosphatase targeting agents, anti-angiogentic agents, agents that induce cell differentiation, bradykinin 1 receptor and angiotensin II antagonists, cyclooxygenase inhibitors, heparanase inhibitors, lymphokines or cytokine inhibitors, bisphosphanates, rapamycin derivatives, anti-apoptotic pathway inhibitors, apoptotic pathway agonists, PPAR agonists, inhibitors of Ras isoforms, telomerase inhibitors, protease inhibitors, metalloproteinase inhibitors, aminopeptidase inhibitors, and biologic drugs including but not limited to antibodies, cytokines and growth factors.
[0210] In some aspects of the invention, the chemotherapeutic agents that are useful for the treatment of multiple myeloma include, but are not limited to, alkylating agents (eg, melphalan), anthracyclines (eg. doxorubicin), corticosteroids (eg. dexamethasome), IMiDs (eg. thalidomide, lenalidomide), protease inhibitors (eg. bortezomib, NPI0052), IGF-1 inhibitors, CD40 antibodies, Smac mimetics (eg. telomestatin), FGF3 modulator (eg. CHIR158), mTOR inhibitor (Rad 001), HDAC inhibitors (eg. SARA, Tubacin), IKK inhibitors, P38MAPK inhibitors, HSP90 inhibitors (eg 17-AAG), and akt inhibitors (eg. Perifosine).
[0211] Further, the preferred chemotherapeutic agents used in combination with the compounds of the present invention include without limitation melphalan, doxorubicin (including lyophilized), dexamethasone, prednisone, thalidomide, lenalidomide, bortezomib, and NPI0052.
[0212] In any case, the multiple chemotherapeutic agents (at least one of which is a compound of the present invention) may be administered in any order or even simultaneously. If simultaneously, the multiple chemotherapeutic agents may be provided in a single, unified form, or in multiple forms (by way of example only, either as a single pill or as two separate pills). One of the chemotherapeutic agents may be given in multiple doses, or both may be given as multiple doses. If not simultaneous, the timing between the multiple doses may be any duration of time ranging from a few minutes to four weeks.
[0213] Thus, in another aspect, the present invention provides methods for treating HDAC-mediated disorders in a human or animal subject in need of such treatment comprising administering to said subject an amount of a compound of the present invention effective to reduce or prevent said disorder in the subject in combination with at least one additional agent for the treatment of said disorder that is known in the art. In a related aspect, the present invention provides therapeutic compositions comprising at least one compound of the present invention in combination with one or more additional agents for the treatment of HDAC-mediated disorders.
[0214] Many of the compounds of the invention may be provided as salts with pharmaceutically compatible counterions. Acid addition salts can be obtained by contacting the neutral form of such compounds with a sufficient amount of the desired acid, either neat or in a suitable inert solvent. Examples of pharmaceutically acceptable acid addition salts include, but are not limited to: those derived from inorganic acids like hydrochloric, hydrobromic, nitric, carbonic, monohydrogencarbonic, phosphoric, monohydrogenphosphoric, dihydrogenphosphoric, sulfuric, monohydrogensulfuric, hydriodic, or phosphorous acids and the like; as well as the salts derived from relatively nontoxic organic acids like acetic; adipic; aspartate; propionic; isobutyric; lactic; maleic; malonic; benzoic; glucolic; succinic; suberic; fumaric; mandelic; phthalic; benzenesulfonic; toluenesulfonic, including p-toluenesulfonic, m-toluenesulfonic, and o-toluenesulfonic; citric; tartaric; methanesulfonic; ethanesulfonic; and the like. Also included are salts of amino acids such as arginate and the like, and salts of organic acids like glucuronic or galactunoric acids and the like (see, for example, Berge et al. J. Pharm. Sci. 66:1-19 (1977)). Salts tend to be more soluble in aqueous or other protonic solvents than are the corresponding free acid or base forms. Salts useful with the compounds of the present invention may include, without limitation, the adipate, aspartate, besylate (benzenesulfonate), citrate, ethanesulfonate, fumarate, glycolate, hydrobromide, hydrochloride, maleate, L-malate, malonate, methanesulfonate, succinate, sulfate, L-tartrate, and tosylate (p-toluenesulfonate) salts of compounds of Formula I. The compounds of Formula I can be contacted with an appropriate acid, either neat or in a suitable inert solvent, to yield the salt forms of the invention. In further embodiments, the salt is a besylate, citrate, hydrobromide, hydrochloride, maleate, L-malate, malonate, mesylate, sulfate or L-tartrate salt of a compound of Formula I. In yet further embodiments, the salt is a hydrobromide, hydrochloride, L-malate, or mesylate salt of compounds of Formula I.
[0215] By way of example, thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester prepared by any method can be contacted with a reagent selected from the group consisting of hydrochloric acid, L-malic acid, or methanesulfonic acid, often in a 1:1 ratio, in a suitable solvent. Such solvents include but are not limited to methanol, ethanol, water, ether, acetone, and acetonitrile, or an appropriate mixture of any of these. Any technique known in the art can be used to vary conditions to induce precipitation or crystallization, including, without limitation: stirring for varying lengths of time at varying ambient conditions, the addition of hexanes or diethyl ether, evaporation, and reduction of temperature.
[0216] In particular, thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester can be contacted with L-malic acid to yield the L-malate salt form of the invention, to form thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester L-malate salt. The present invention provides for thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester L-malate salt.
[0217] In certain embodiments, thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester can be contacted with methanesulfonic acid to yield the mesylate salt form of the invention, to form thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester mesylate salt. The present invention provides for thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester L-mesylate salt.
[0218] In certain embodiments, thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester can be contacted with hydrochloric acid to yield the hydrochloride salt form of the invention, to form thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester hydrochloride salt. The present invention provides for thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester hydrochloride salt.
[0219] Additionally, the present invention provides for pharmaceutical compositions comprising a salt of a compound of Formula I together with a pharmaceutically acceptable diluent or carrier.
[0220] All references, patents or applications, U.S. or foreign, cited in the application are hereby incorporated by reference as if written herein.
General Synthetic Methods for Preparing Compounds
[0221] Molecular embodiments of the present invention can be synthesized using standard synthetic techniques known to those of skill in the art. Compounds of the present invention can be synthesized using the general synthetic procedures set forth in Schemes I-II.
EXAMPLE 1
Thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl)ester
[0222]
Step 1: N,N-dimethyl-3-phenoxypropan-1-amine
[0223]
[0224] Into a 5 L 3-necked round-bottom flask was placed a solution of 1-(3-bromopropoxy)benzene (250 g, 1.16 mol) in THF (600 ml). To this was added dimethylamine in water (1 L 33%). To the mixture was added KOH (200 g, 4.46 mol). The resulting solution was allowed to react, with stirring, for 5 hours while the temperature was maintained at room temperature. The reaction progress was monitored by TLC (EtOAc/PE=1:3). The resulting solution was extracted five times with 200 ml of EtOAc and the organic layers combined. The filtrate was concentrated by evaporation under vacuum using a rotary evaporator. This resulted in 200 g of crude N,N-dimethyl-3-phenoxypropan-1-amine as light yellow oil.
Step 2: 4-[3-(dimethylamino)propoxy]benzenesulfonyl chloride
[0225]
[0226] Into a 2 L 3-necked roundbottom flask, was placed a solution of N,N-dimethyl-3-phenoxypropan-1-amine (200 g, 1.17 mol) in DCM (1 L). HCl (gas) was introduced with a tube for 2 hours while the temperature was maintained at 0° C. The resulting reaction was concentrated by evaporation under vacuum using a rotary evaporator. This resulted in 240 g of the HCl salt of N,N-dimethyl-3-phenoxypropan-1-amine as white solid.
[0227] Into a 1 L 3-necked roundbottom flask, was placed the HCl salt of N,N-dimethyl-3-phenoxypropan-1-amine (100 g, 558.66 mmol) and DCM (250 ml) added. This was followed by the dropwise addition of a solution of chlorosulfonic acid (143 g, 1.23 mol) in DCM (250 ml), while cooling to a temperature of −10° C. over a period of 1 hour. The resulting solution was allowed to react, with stirring, for 1 hour while the temperature was maintained at −10° C. in a bath of H 2 O/ice. The resulting mixture was extracted with 500 ml of DCM. The final product was purified by recrystallization from MeOH. This resulted in 100 g (73%) of 4-(3-(dimethylamino)propoxy)benzenesulfonic acid hydrochloride as a white solid.
[0228] Into a 500 ml roundbottom flask, was placed 4-(3-(dimethylamino)propoxy)benzenesulfonic acid hydrochloride (100 g, 338.18 mmol). To the mixture was added thionyl chloride (400 ml). The resulting solution was allowed to react, with stirring, for 2 hours while the temperature was maintained at reflux in an oil bath. The mixture was concentrated by evaporation under vacuum using a rotary evaporator. This resulted in 106 g (100%) of 4-(3-(dimethylamino)propoxy)benzene-1-sulfonyl chloride hydrochloride as a white solid. 1 H-NMR (400 MHz, DMSO) δ 7.97 (m, 2H), 7.06 (m, 2H), 4.25 (m, 2H), 3.28 (m, 2H), 2.90(s, 6H), 2.45 (m, 2H).
Step 3: N-(5-Acetyl-pyridin-2-yl)-4-(3-dimethylamino-propoxy)-benzenesulfonamide
[0229]
[0230] The flask was charged with 1-(6-amino-pyridin-3-yl)-ethanone (100 g, 0.74 mol. Ref: J. Med. Chem. 1973, 16 (8), 959-961) and was purged with nitrogen. To this was added 500 mL pyridine, and the mixture was heated to 60° C.; a pale amber solution was obtained. To it was added 230 g 4-[3-(dimethylamino)propoxy]benzenesulfonyl chloride (230 g, 0.74 mol) in portions over the course of one hour. After the addition was complete the mixture was heated to 60° C. for 90 minutes. It was allowed to cool to 35° C., and was then poured into a vigorously stirred mixture of 2L ethyl acetate and 1170 g dibasic potassium phosphate dissolved in 2 L water. The mixture was stirred for 15 minutes. The resulting precipitate was collected by filtration. It was washed with 2×1 L ethyl acetate and air dried to give 330 g of crude tan solid. 1 H-NMR (400 MHz, DMSO) δ 8.60 (s, 1H), 7.96 (d, 1H), 7.77 (d, 2H), 6.95-7.00 (m, 3H), 4.02 (t, 2H), 2.60 (t, 2H), 2.42 (s, 3H), 2.33 (s, 6H), 1.84-1.96 (m, 2H); [M+H] + 378.
Step 4: Thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester
[0231]
[0232] The flask was purged with nitrogen and charged with N-(5-Acetyl-pyridin-2-yl)-4-(3-dimethylamino-propoxy)-benzenesulfonamide (100 g, 0.265 mol) and 400 mL of dimethylformamide. Stirring was begun, and to it was added dropwise 98 mL of 32% HBr in acetic acid (0.53 mol). During the course of the addition the temperature rose to 45° C. To this was added in one portion pyrrolidone hydrotribromide (130 g, 0.262 mol). After the addition was complete the mixture was heated to 50° C. for 1 hour. The mixture was allowed to cool to 35° C. and to it was added potassium thioacetate (60.5 g, 0.53 mol) in one portion. The resulting mixture was stirred at room temperature for one hour. It was then filtered through a medium porosity frit to remove inorganic salts and the filtrate was poured into 2 L of isopropanol. This cloudy mixture was placed in a −20° C. freezer overnight. It was then allowed to stand at room temperature for 30 minutes and the clear, pale yellow supernatant was decanted away. The insoluble residue was suspended in 500 mL dichloromethane and vigorously stirred. To it was added a solution of dibasic potassium phosphate trihydrate (140 g, 0.53 mol) in 700 mL of water. The mixture was stirred for 15 minutes; most of the desired material precipitated from solution and adhered to the walls of the vessel. The aqueous layer was removed and extracted with dichloromethane. The combined organic extracts and insoluble residue were loaded on a plug of 900 g dry silica and eluted with 1 L fractions of 20% methanol in dichloromethane. Fractions 3-20 were concentrated to give thioacetic acid S-(2-{6-[4-(3-dimethylamino-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester as a tan solid (32.1 g, 27%). 1 H-NMR (400 MHz, DMSO) δ 8.66 (s, 1H), 7.94 (d, 1H), 7.77 (d, 2H), 6.98 (d, 2H), 6.90 (d, 1H), 4.34 (s, 2H), 4.03 (t, 2H), 2.68 (t, 2H), 2.40 (s, 6H), 2.33 (s, 3H), 1.88-1.98 (m, 2H); [M+H] + 452.
EXAMPLE 2
[0233]
Thioacetic acid S-(2-{6-[4-(2-dimethylamino-ethoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester
Step 1: N-(5-Acetyl-pyridin-2-yl)-4-iodo-benzenesulfonamide
[0234]
[0235] 4-Iodo-benzenesulfonyl chloride (83 g, 274 mmol, 1 eq) was added over a period of 1 min to 1-(6-amino-pyridin-3-yl)-ethanone (42 g, 301 mmol, 1.1 eq) dissolved in pyridine (350 mL). The resulting mixture was heated to 60° C. for 90 min with vigorous stirring and then cooled to room temperature. The reaction mixture was then poured (over a period of 1 min) into stirring 2N HCl (2.6 L). The off-white slurry was stirred for 1 h and filtered to give an off-white solid which was then triturated in MeOH (1.2 L) for 1 h, filtered, triturated further in DCM (200 mL) for 30 min, filtered, and dried to afford 94 g (85%) of N-(5-Acetyl-pyridin-2-yl)-4-iodo-benzenesulfonamide as an off-white solid. 1 H-NMR (400 MHz, DMSO-d 6 ) δ 8.60 (s, 1H), 8.15 (d, 1H), 7.93 (d, 2H), 7.66 (d, 2H), 7.22 (d, 1H), 2.48 (s, 3H); [M+H] + 403.
Step 2: N-(5-Acetyl-pyridin-2-yl)-4-(2-dimethylamino-ethoxy)-benzenesulfonamide
[0236]
[0237] N-(5-Acetyl-pyridin-2-yl)-4-iodo-benzenesulfonamide (4.0 g, 10 mmol, 1 eq), copper(I) iodide (95 mg, 0.50 mmol, 0.05 eq), 1,10-phenanthroline (180 mg, 1.0 mmol, 0.1 eq), and cesium carbonate (8.1 g, 25 mmol, 2.5 eq) were combined. Then, 2-dimethylamino-ethanol (20 mL, 170 mmol, 17 eq) was added. The dark heterogeneous reaction mixture was stirred vigorously and heated at 120° C. for 16 h. The reaction mixture was cooled to 35° C. and poured into a separation funnel containing 2.8 N pH 8.2 phosphate buffer (60 mL) and DCM (120 mL). Note: the 60 mL phosphate buffer aqueous solution contained K 2 HPO 4 (25 g, 140 mmol) and KH 2 PO 4 (2.4 g, 17 mmol). After agitation, the phases were allowed to separate. The organic layer was isolated and concentrated onto 20 g of silica. Fractions containing the desired product from the chromatography (using 120 g of silica and a 5% MeOH/DCM to 20% MeOH/DCM step gradient) were concentrated to a residue. The residue was taken up in MeOH (20 mL) and triturated for 1 h which induced an off-white precipitation. The off-white precipitation/slurry was filtered, and the solid dried to afford 1.5 g (40%) of N-(5-Acetyl-pyridin-2-yl)-4-(2-dimethylamino-ethoxy)-benzenesulfonamide as an off-white solid. 1 H-NMR (400 MHz, DMSO-d 6 ) δ 8.62 (s, 1H), 8.03 (d, 1H), 7.81 (d, 2H), 7.00-7.10 (m, 3H), 4.11 (t, 2H), 2.73 (t, 2H), 2.45 (s, 3H), 2.27 (s, 6H); [M+H] + 364.
Step 3: Thioacetic acid S-(2-{6-[4-(2-dimethylamino-ethoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester
[0238]
[0239] N-(5-Acetyl-pyridin-2-yl)-4-(2-dimethylamino-ethoxy)-benzenesufonamide (420 mg, 1.1 mmol, 1 eq) was dissolved with DMF (5 mL). THF (1 mL) was then added to the clear solution. The solution was cooled to 15° C. in an ice bath. Then, 33% HBr-AcOH (1.5 mL) was added to the stirred solution. The ice bath was removed and pyrrolidone hydrotribromide (480 mg, 1.2 mmol, 1.1 eq) was added in one lot. The resulting solution was stirred at 40° C. for 2 h. At this time, the red-colored reaction solution was poured into a separation funnel containing 2.8 N pH 8.2 phosphate buffer (12 mL) and DCM (24 mL). Note: the 12 mL phosphate buffer aqueous solution contained K 2 HPO 4 (5.1 g, 29 mmol) and KH 2 PO 4 (0.49 g, 3.5 mmol). The organic layer was isolated and concentrated to give the bromide as a dark, DMF-containing residue. MeOH (12 mL) and potassium thioacetate (150 mg, 1.3 mmol, 1.2 eq) were then added and the mixture was stirred for 2 h. The reaction mixture was concentrated onto 3 g of silica. Chromatography (using 20 g of silica and a 0% MeOH/DCM to 20% MeOH/DCM gradient) gave 350 mg (70%) of thioacetic acid S-(2-{6-[4-(2-dimethylamino-ethoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester as an off-white solid. Taking up the free base in DCM, and adding 1.1 eq of HCl (0.23 mL of 4M HCl in dioxane) and subsequent concentration, followed by drying overnight under vacuum, gave 350 mg of the HCl salt as an off-white solid. 1 H NMR (400 MHz, 20% MeOD/CDCl 3 ) δ 8.61 (s, 1H), 7.98 (d, 1H), 7.76 (d, 2H), 7.07 (d, 1H), 6.80 (d, 2H), 3.9-4.1 (m, 6H), 2.2-2.3 (m, 9H). [M+H] + 438.
EXAMPLE 3
[0240]
Thioacetic acid S-(2-{6-[4-(3-dimethylamino-2,2-dimethyl-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester
[0241] Thioacetic acid S-(2-{6-[4-(3-dimethylamino-2,2-dimethyl-propoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester was synthesized as described in EXAMPLE 2 using N-(5-acetyl-pyridin-2-yl)-4-iodo-benzenesulfonamide and 3-dimethylamino-2,2-dimethyl-propan-1-ol as starting materials. 1 H NMR (400 MHz, CD 3 OD) δ 8.72 (s, 1H), 8.18 (d, 1H), 7.97 (d, 2H), 7.21 (d, 1H), 7.14 (d, 2H), 4.32 (s, 2H), 3.96 (s, 2H), 2.96 (s, 6H), 2.37 (s, 3H), 2.30 (s, 2H), 1.21 (s, 6H). LCMS: 481 (M+1).
EXAMPLE 4
Thioacetic acid S-(2-{6-[4-(4-dimethylamino-butoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester
[0242]
[0243] Thioacetic acid S-(2-{6-[4-(4-dimethylamino-butoxy)-benzenesulfonylamino]-pyridin-3-yl}-2-oxo-ethyl) ester was synthesized as described in EXAMPLE 2 using N-(5-acetyl-pyridin-2-yl)-4-iodo-benzenesulfonamide and 4-dimethylamino-butan-1-ol as starting materials. 1 H NMR (400 MHz, DMSO-d 6 ) δ 8.74 (s, 1H), 8.17 (d, 1H), 7.86 (d, 2H), 7.17 (d, 1H), 7.08 (d, 2H), 4.42 (s, 2H), 4.03 (s, 2H), 3.09 (s, 2H), 2.73 (s, 6H), 2.33 (s, 3H), 1.6-1.8 (m, 4H). LCMS: 466 (M+1) + .
[0244] The following compounds can generally be made using the methods described above. It is expected that these compounds when made will have activity similar to those that have been made in the examples above.
[0245] The activity of the above mentioned Examples as HDAC inhibitors has generally been shown by the following assays. The other compounds listed above, which may not yet been made or tested, are predicted to generally have activity in these assays as well.
Inhibition Assays
[0000] 1) In Vitro HDAC-Inhibition Assay:
[0246] This assay measures a compound's ability to inhibit acetyl-lysine deacetylation in vitro and was used as both a primary screening method as well as for IC50 determinations of confirmed inhibitors. The assay is performed in vitro using an HDAC enzyme source (e.g. partially purified nuclear extract or immunopurified HDAC complexes) and a proprietary fluorescent substrate/developer system (HDAC Quantizyme Fluor de Lys Fluorescent Activity Assay, BIOMOL). The assay is run in 1,536-well Greiner white-bottom plates using the following volumes and order of addition:
[0247] Step 1: Enzyme (2.5 μL) source added to plate (from refrigerated container)
[0248] Step 2: Compounds (50 nL) added with pin transfer device
[0249] Step 3: Fluor de Lys (2.5 μL) substrate added, incubate at RT, 30 minutes
[0250] Step 4: Developer (5 μL) solution is added (containing TSA), to stop reaction
[0251] Step 5: Plate Reader—data collection
[0252] The deacetylated fluorophore is excited with 360 nm light and the emitted light (460 nm) is detected on an automated fluorometric plate reader (Aquest, Molecular Devices).
[0000] 2) Cellular Histone Hyperacetylation Assays:
[0253] These two secondary assays evaluates a compound's ability to inhibit HDAC in cells by measuring cellular histone acetylation levels. The cytoblot facilitates quantitative EC50 information for cellular HDAC inhibition. Transformed cell lines (e.g. HeLa, A549, MCF-7) are cultured under standard media and culture conditions prior to plating.
[0000] For Cytoblot:
[0254] Cells (approx. 2,500/well) are allowed to adhere 10-24 hours to wells of a 384-well Greiner PS assay plate in media containing 1-5% serum. Cells are treated with appropriate compound and specific concentrations for 0 to 24 hours. Cells are washed once with PBS (60 μL) and then fixed (95% ethanol, 5% acetic acid or 2% PFA) for 1 minute at RT (30 μL). Cells are blocked with 1% BSA for 1 hour and washed and stained with antibody (e.g. anti-Acetylated Histone H3, Upstate Biotechnology), followed by washing and incubation with an appropriate secondary antibody conjugated to HRP or fluorophore. For luminescence assays, signal is generated using Luminol substrate (Santa Cruz Biotechnology) and detected using an Aquest plate reader (Molecular Devices).
[0000] For Immunoblot:
[0255] Cells (4×10 5 /well) are plated into Corning 6-well dish and allowed to adhere overnight. Cells are treated with compound at appropriate concentration for 12-18 hours at 37° C. Cells are washed with PBS on ice. Cells are dislodged with rubber policeman and lysed in buffer containing 25 mM Tris, pH7.6; 150 mM NaCl, 25 mM MgCl 2 , 1% Tween-20, and nuclei collected by centrifugation (7500 g). Nuclei are washed once in 25 mM Tris, pH7.6; 10 mM EDTA, collected by centrifugation (7500 g). Supernatant is removed and histones are extracted using 0.4 M HCl. Samples are centrifuged at 14000 g and supernatants are precipitated in 1 ml cold acetone. The histone pellet is dissolved in water and histones are separated and analyzed by SDS-PAGE Coomassie and immunoblotting (anti-acetylated histone antibodies, Upstate Biotechnology) using standard techniques.
[0000] 3) Differential Cytotoxicity Assay:
[0256] HDAC inhibitors display differential cytotoxicity toward certain transformed cell lines. Cells are cultured according to standard ATCC recommended conditions that are appropriate to each cell type. Compounds were tested for their ability to kill different cell types (normal and transformed) using the ATPlite luminescence ATP detection assay system (Perkin Elmer). Assays are run in either 384-well or 1536-well Greiner PS plates. Cells (30 μL or 5 μL, respectively) are dispensed using either multichannel pipette for 384-well plates, or proprietary Kalypsys bulk liquid dispenser for 1536-well plates. Compounds added using proprietary pin-transfer device (500 nL or 5 nL) and incubated 5 to 30 hours prior to analysis. Luminescence is measured using Aquest plate reader (Molecular Devices).
[0257] The activity of Examples 1-4 as HDAC inhibitors is shown in Table 1 below.
TABLE 1 In vitro IC 50 (μM) Cellular IC 50 (μM) + indicates <1 + indicates <1 Example No. − indicates >1 − indicates >1 1 + + 2 + + 3 + + 4 + +
[0258] All references cited above are incorporated herein by reference in their entirety.
[0259] From the foregoing description, one skilled in the art can easily ascertain the essential characteristics of this invention, and without departing from the spirit and scope thereof, can make various changes and modifications of the invention to adapt it to various usages and conditions.
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Disclosed herein are carbonyl compounds of having the structural formula:
or a pharmaceutically acceptable salt, ester, or prodrug thereof, Methods and compositions are disclosed for treating disease states including, but not limited to cancers, autoimmune diseases, tissue damage, central nervous system disorders, neurodegenerative disorders, fibrosis, bone disorders, polyglutamine-repeat disorders, anemias, thalassemias, inflammatory conditions, cardiovascular conditions, and disorders in which angiogenesis play a role in pathogenesis, using the compounds of the invention. In addition, methods of modulating the activity of histone deacetylase (HDAC) are also disclosed.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This application is directed to the art of composite brake shoes.
[0003] 2. Description of Related Art
[0004] Railcars are supported and guided by steel wheels. The treads at the outer circumference of the wheels ride over steel rails. Railcar brakes comprise brake shoes that are brought into frictional engagement with the wheel treads. The brake shoes are supported by brake heads which, in turn, are movably supported by the brake rigging comprised of a system of levers and a pneumatic cylinder. Brake shoes are comprised of various materials that are selected for their frictional characteristics and for the effect on the wear life of the wheel treads. Many brake shoes are composites of materials having different characteristics. In typical composite brakes shoes, materials of differing frictional characteristics bear upon the wheel tread during braking. This may be achieved by placing inserts of a different material into the friction face of the shoe comprised of the principal brake shoe material.
[0005] Standard railway brake shoes in North America are produced with metal backing plates for support of the friction material and for attachment and retention of the brake shoes to the brake heads. Elsewhere in the world, brake shoes are produced without metal backing plates and normally include a skeletal wire frame. One type of railway brake shoe also includes a metallic insert solidly affixed by welding to the metal backing plate before the brake pad is formed, for example, by molding, onto the backing plate. See U.S. Pat. No. 6,241,058 entitled “Brake Shoe with Insert Bonded to Backing Plate.” Recently, metallic inserts have been introduced into brake shoes without the metal backings as taught in PCT/US2007/069854 entitled “Railway Brake Shoe.”
[0006] The brake shoe friction material often comprises a blend of abrasive materials, organic and inorganic filler materials, and resins. The metallic insert may be selected to provide beneficial treatment of the rolling surface of the wheel.
[0007] Fiber reinforced resilient backing layers between the friction material and metal backing plates have been suggested to attenuate sound. See U.S. Pat. No. 4,371,631 entitled “Backing Plate Composition for Brake Shoes.”
SUMMARY OF THE INVENTION
[0008] It is an advantage, according to this invention, to provide structural reinforcement at side layers of a brake shoe to reduce the formation and propagation of cracks.
[0009] Brake shoes have a friction surface which, during braking, bears on the convex rolling surface of the railcar wheel. The rolling surface of the wheel is a surface of rotation that may be a convex-conical surface or a combination of convex-conical and cylindrical surfaces or other surfaces of rotation. The surface of the brake shoe has a concave surface of rotation that matches a portion of the convex surface of the wheel. These surfaces of rotation are defined by a generatrix (not necessarily straight line) rotated around an axis which is defined by the wheel axle. Thus, the friction surface of the brake shoe has a generally axial and a circumferential extent and the brake shoe has a radial thickness moving away from the friction surface. The features of the brake shoes, according to various embodiments of this invention, will be described herein with reference to the generally axial, circumferential and radial directions.
[0010] Briefly, according to one embodiment of this invention, a brake shoe with or without a metal backing is provided. The brake shoe is defined by a friction surface for bearing upon a wheel tread and a radially opposed back surface for being placed in contact with and secured to a brake head and two side surfaces that extend between the friction surface and the back surface. The brake shoe has a metal insert comprising two spaced bodies having faces lying in the friction surface of the brake shoe. The spaced bodies extend radially away from the friction surface and to the back surface of the brake shoe. The brake shoe is comprised of molded friction material comprising a blend of abrasive materials, fillers, and resin. Along at least a portion of at least one side surface adjacent the spaced metal insert bodies, there is a layer of fiber-reinforced material. The fiber-reinforced material may be molded friction material reinforced with fibers.
[0011] According to this invention, the sides of the brake shoe are strengthened to reduce cracks due to thermal or mechanical stresses during braking by adding fiber/composition material to the sides of the brake shoes during the molding process. During the molding process, heat and pressure cause the fiber/composition material to be integrally molded and adhered to the friction material comprising the bulk of the brake shoe with which it is compatible.
[0012] When used with brake shoes having metal inserts and when located adjacent to the metal inserts, the reinforcement layers along the side surfaces are particularly effective in preventing formation and propagation of cracks between the molded friction material and the metal inserts.
[0013] Preferably, the fiber material may comprise woven or stitched fabric of fiberglass, aramid fibers, cotton fibers etc. impregnated with a phenolic or other resin. The composition of the reinforcement layers must be selected so that the reinforcement layers wear at substantially the same rate as the bulk friction composition.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Further features and other objects and advantages will become apparent from the following detailed description of preferred embodiments made with reference to the drawings in which:
[0015] FIGS. 1 , 2 , and 3 are back, side, and friction face views of a brake shoe having a metal insert;
[0016] FIG. 4 is a perspective view of a brake shoe with a partial side reinforcement layer; and
[0017] FIG. 5 is a perspective view of a brake shoe with a full side reinforcement layer.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0018] The function of a composition railway brake shoe is to provide braking effort in the form of friction generating a retarding force on the rolling surfaces of the wheels of a railcar. Referring to FIGS. 1 to 5 , the brake shoe structure is typically an arc-shaped block designed with one friction surface 12 to fit against the circumference of the wheel and at its radially spaced back surface 14 to be mounted to a supporting member of the brake system which applies force to the brake shoe during braking. Extending between the friction surface 12 and back surface 14 are side surfaces 16 . The brake shoe may include a metal backing plate on or embedded in its back surface for attachment to the supporting member of the brake system. The brake shoe may include metal inserts 10 and 11 which project through the thickness of the composition material to provide improved wearability or conditioning of the wheel surface, and/or to improve rolling adhesion between the railcar wheel and rails.
[0019] Due to several factors, stresses are developed on various specific locations of the brake shoe structure that can cause cracking or breakage of the brake shoe structure during use. The factors may include the following: a) the curved shape of the brake shoe, b) discontinuities between the composition and the metal insert or metal backing plate, c) high normal application forces and tangential friction forces occurring during braking, d) cyclical vibration and shock loadings during brake release, e) irregular fit between the friction surface of the brake shoe and the wheel, and f) non-uniform force distribution due to irregular mating between the back surface of the brake shoe and the supporting member of the brake system.
[0020] Cracks in the back of the brake shoe which develop due to various stress factors may be superficial or they can represent significant safety issues having the potential for breakage and loss of function.
[0021] It is an advantage of this invention to reduce the likelihood of breakage and loss of function by reinforcing the side surface layer of the brake shoe structure.
[0022] In one embodiment according to this invention, side reinforcement layers are prepared in advance of molding the brake shoe. The reinforcement layers are composed of a resilient composite material that encapsulates one or more layers of fiber reinforcement and are compatible with the bulk composition braking material of the brake block. The reinforcement layers are made integral with the brake block by positioning the reinforcing layers in the mold prior to molding the brake block. According to another embodiment, sheets of fibrous material impregnated with resin may be bonded to the side surface of the brake shoe either during or after the brake shoe molding process.
[0023] Having thus defined my invention in the detail and particularity required by the Patent Laws, what is desired protected by Letters Patent is set forth in the following claims.
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A molded brake shoe formed of friction material with or without a metal backing. Along at least a portion of at least one side surface of the brake shoe there is a layer of the molded friction material reinforced with a fiber.
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BACKGROUND OF THE INVENTION
Charged species in solution or suspension in a liquid will migrate under the influence of an applied electric field in a phenomenon known as electrophoresis. Different species have different electrophoretic mobilities, providing a mechanism for separating different species. Coupling this separation means with a detecting means gives an analytical technique known as capillary zone electrophoresis.
Electroosmosis is the flow of liquid, generally a polar liquid, in contact with a porous solid, under the influence of an applied electric field. Electroosmosis has been attributed to the formation of an electric double layer at the solid/liquid interface. Under the influence of an electric field parallel to that interface, a portion of the liquid's diffuse layer moves, because of the electric forces acting on the excess ionic charge in that layer, and a shear plane is set up at some distance from the interface. A constant flow rate is reached when the force exerted on the ions (and thus on the liquid as a whole) is balanced by the frictional forces arising from the viscosity of the liquid. The electric potential at the shear plane is called the zeta potential, represented by z or the Greek letter "zeta."
The linear velocity, v, of the liquid under the influence of an applied electric field E is approximately
v=(e/h)E z (1)
where e is the dielectric constant of the liquid, and h is the viscosity of the liquid.
Thus v is proportional (or approximately proportional) to the zeta potential, z. The magnitude of the zeta potential depends on, among other things, the particular liquid, the nature of the solid surface, and the concentrations of different species in the liquid. Polar solvents, such as water, can give rise to zeta potentials of as much 100 mV in contact with either polar or non-polar surfaces.
Electroosmosis can either augment or interfere with capillary electrophoresis. In can interfere because electroosmotic mobility is typically greater than are electrophoretic mobilities, limiting the time available for electrophoretic processes to separate different species before electroosmosis flushes the species out of the capillary.
One method to control the rate of electroosmosis is to change the voltage applied across the length of the capillary, but such a change also affects the rate of electrophoresis, and will not significantly affect the overall degree of electrophoretic separation. Other methods of controlling the rate of electroosmosis are to change the concentrations of species in solution or suspension, to change the pH, or to change the nature of the material forming the inner layer of the capillary. None of these methods is flexible or capable or rapid change, and each has other disadvantages as well.
There have been a number of recent efforts to make chemical sensors using microfabrication techniques. Most microsensors fabricated to data have used a two-step detection means. In the first step, chemical selectivity is accomplished by means of a chemical transformation, or by physisorption onto a chemically selective coating. In the second step, a physical consequence of the first step--e.g., a release of heat, a change in optical absorption, etc.--is converted to an electrical signal by means of a suitable microtransducer. Examples of chemical microsensors are the ISFET and the CHEMFET.
In conventional chemical sensors, the analyte is measured in the presence of other species. The selectivity component of the sensor ideally should respond only to the analyte. An alternative means of chemical analysis is first to separate the analyte from background species, and then to sense it with the detector. The detector in such a case need not be selective. An example of this type of chemical sensor is the micro-gas chromatograph developed by Terry et al., "A Gas Chromatographic Air Analyzer Fabricated on a Silicon Wafer," IEEE Trans. Electron Devices, Vol. ED-26, pp. 1880-86 (1979). Such chemical sensors may be called separation-based chemical microsensors. In addition to other factors favoring miniaturization, chromatographic systems also benefit from scaling laws--generally a decrease in column diameter results in an increased separation efficiency per unit length, or faster separations with short columns.
In capillary electrophoresis, a buffer-filled capillary is placed between two buffer reservoirs, and a potential field is applied across this capillary. The electric field creates an electroosmotic flow of buffer, generally toward the cathode. The electric field also causes electrophoretic flow of ionic solutes. The electrophoretic flow will generally be at a different rate from that of the electroosmotic flow. The difference between the electrophoretic mobilities of the solutes causes their separation. The separated species may be detected when they reach the cathode or anode, typically the cathode. Ewing et al., "Capillary Electrophoresis," Analytical Chemistry, Vol. 61, No. 4, pp. 292A-303A (1989).
A disadvantage of existing methods of capillary electrophoresis is the fact that the rate of electroosmotic flow is often high enough, compared to the electrophoretic mobilities, that electroosmotic flow carries the species out of the capillary before adequate separation of the species occurs. It is known that maximum resolution results when electroosmotic mobility just balances electrophoretic mobility. It has previously been though that such an approach required a lengthy analysis time. See Ewing et al., supra, at p. 298A; Jorgenson et al., "Zone Electrophoresis in Open-Tubular Glass Capillaries," Anal. Chem. Vol. 53, pp. 1298-1302 (1981). The desirability of thus tuning electroosmosis to achieve a high-resolution separation, and then re-tuning the electroosmotic flow to sweep separated components to a detector, has been recognized in the art. See Lauer et al., "Zone Electrophoresis in Open-Tubular Capillaries--Recent Advances," Trends in Analytical Chemistry, vol. 5, no. 1, pp. 11-15 (1986), at p. 13. Despite this recognition, to the knowledge of the inventor there has been nor previously reported means for controlling the rate of electroosmosis which is simultaneously flexible, capable of rapid response, and capable of changing the rate of electroosmosis independently of the rate of electrophoresis.
Because the rate of electroosmotic flow is proportional to the zeta potential, the rate of electroosmotic flow may be controlled or even stopped by adjusting the zeta potential, preferably without changing the electric potential across the length of the capillary. But existing method of controlling the zeta potential having significant disadvantages. These methods include changing the concentrations of species in solution or suspension, to change the pH, or to change the nature of the material forming the inner layer of the capillary. None of these methods is flexible or capable or rapid change, and each has other disadvantages as well. For example, a zero zeta potential may be desired to eliminate electroosmosis, so that only electrophoresis occurs. In a silica capillary, an approximately zero zeta potential may be achieved with a pH of 2-3; but such an acidic environment denatures many proteins. See Jorgenson et al., supra, at p. 1301; McCormick, "Capillary Zone Electrophoretic Separation of Peptides and Proteins Using Low pH Buffers in Modified Silica Capillaries," Anal. Chem., Vol. 60, pp. 2322-28 (1988).
It has been observed that adding micelles to the liquid can allow the separation of neutral species as well as charged ones: A micelle may incorporate a neutral species into its interior, while the charge on the micelle's surface causes the micelle-neutral species complex to act as a charged species in the electrophoresis, permitting separations. See Terabe et al., "Electrokinetic Separations with Micellar Solutions and Open-Tubular Capillaries, " Anal. Chem., vol. 56, pp. 111-13 (1984); and Terabe et al. "Electrokinetic Chromatography with Micellar Solution and Open-Tubular Capillary," Anal. Chem., vol. 57, pp. 834-41 (1985); both of which are incorporated by reference.
SUMMARY OF THE INVENTION
Field effect electroosmosis, a novel means of controlling the rate of electroosmosis due to a first electric potential, has been discovered in which a second electric potential is applied between the electrically insulating walls of a capillary and the liquid. The second electric potential changes the charge on the wall of the capillary, and thus allows manipulation of the zeta potential within the capillary. Manipulation of the zeta potential in this manner permits flexibly and rapidly controlling the rate of electroosmosis independently of the rate of electrophoresis.
The zeta potential becomes a function of, among other things, the voltage applied between the insulating capillary walls and the liquid, the pH of the electrolyte, and the concentrations of other ions in the electrolyte. By adjusting these factors, particularly the voltage between the capillary walls and the liquid, the zeta potential may be manipulated to a degree not previously possible. By controlling this applied voltage, the zeta potential may be made uniform throughout the capillary; or it may be made to be zero throughout the capillary; or it may be made to vary in a chosen manner across the length of the capillary. These manipulations of the zeta potential may cause electroosmosis to stop, or may be used otherwise to control the rate of electroosmosis.
If the rate of electroosmosis is adjusted to be equal and opposite to the rate of electrophoresis of a certain species, that species will become essentially immobile within the capillary, so that it becomes possible to improve resolution, and to separate species which have very close electrophoretic mobilities.
A device applying this field-effect electroosmosis phenomenon is called a MIEEKFED, a "Metal-Insulator-Electrolyte-Electrokinetic Field-Effect Device." A MIEEKFED in electrokinetic applications is analogous is some ways to a conventional MOSFET-type transistor in electronic applications. In a MIEEKFED, the electrolyte flow may be controlled, while in a MOSFET the electric current flow may be controlled--in either case, by means of an electric field applied perpendicular to the respective flow.
In a conventional MOSFET, an electric potential difference applied between the gate electrode and the substrate causes a change in the electric field orthogonal to the SiO 2 --Si interface, resulting in modulation of the channel conductance. By replacing the silicon with an electrolyte which is free to flow, a MIEEKFED results. The voltage at the outer surface of the double layer controls the velocity of the electrolyte flow.
A MIEEKFED, which may be thought of as a field effect electrokinetic transistor, adds a new dimension to capillary electrophoresis separation-based sensors. A MIEEKFED can improve separations between different species whose mobilities would otherwise be very close using conventional techniques of capillary electrophoresis.
Applications of MIEEKFED's include capillary electrophoresis and other separation-based sensors. Capillary electrophoresis may be conducted with no electroosmotic flow by selecting the applied field to produce a zero zeta potential. This zero zeta potential may be flexibly achieved with or without altering the pH, the concentration of the electrolyte, or the inner layer of the capillary. A MIEEKFED is capable of rapidly and flexibly changing the zeta potential as a function of time.
Using a MIEEKFED in a capillary electrophoresis apparatus results in a number of advantages. The zeta potential, and therefore the rate of electroosmosis, may be flexibly controlled without unwanted restrictions on pH, electrolyte concentration, or the inner layer of the capillary. This degree, of flexible control allows improved electrophoretic separation of different species with close electrophoretic mobilities, which can otherwise be difficult to separate. Such a device built in accordance with the present invention can also be used to reduce the degree of "tailing" commonly observed in capillary electrophoresis of macromolecules. The tailing can be reduced by using a MIEEKFED to create a low, and preferably uniform, zeta potential.
The MIEEKFED has great potential for miniaturization, particularly in light of recent advances in the technology of micro-machining silicon. See Peterson, "Silicon as a Mechanical Material," Proceedings of the IEEE, Vol. 70, No. 5, pp. 420-457 (1982), which is incorporated by reference.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1a and 1b illustrates a perspective view and a plan view of a MIEEKFED.
FIG. 2 illustrates computer calculations of the zeta potential in a MIEEKFED as a function of applied voltage, at different pH values, at a constant concentration of KC1.
FIG. 3 illustrates computer calculations of the zeta potential in a MIEEKFED as a function of applied voltage, at different KC1 concentrations and a constant pH.
FIG. 4 illustrates MIEEKFED with an electric circuit capable of creating a constant zeta potential.
FIG. 5a and 5b illustrates a capillary electrophoresis apparatus incorporating a MIEEKFED.
DETAILED DESCRIPTION OF THE INVENTION
A physical embodiment of the present invention has not been constructed to date--however, computer simulations have been most promising.
A MIEEKFED comprises an insulating capillary having an inner bore, and coated on the outside with a conducting layer; or alternatively, a conducting capillary coated on the inside with an insulating layer. Voltages are applied both across the length of the capillary, and "perpendicular" to the capillary--meaning that the voltage is applied between the liquid and the conducting layer. Although a capillary is preferred, the present invention should work in other shapes of insulators having bores through them.
In a conventional MOSFET, an electric potential difference applied between the gate electrode and the substrate causes a change in the electric field orthogonal to the SiO 2 --Si interface, resulting in modulation of the channel conductance. By replacing the silicon with and electrolyte which is free to flow, the MIEEKFED illustrated in FIG. 1 results. FIG. 1 illustrates a perspective view and a plan view of a MIEEKFED 1. A metal layer 2 surrounds and is in contact with insulator 3, which is a capillary having a bore through it. The bore of the capillary contains at least a part of electrolyte 4. Electrolyte 4 will typically comprise a polar liquid, such a water; may also comprise one or more ions; may also comprise one or more compounds in suspension or solution; and may also comprise one or more micelles. A first voltage V d is applied across the ends of the capillary between anode 5 and cathode 6. A second voltage V G is applied between electrode 7 and cathode 6. At the interface of insulator 3 and electrolyte 4, a double layer 8 is formed. The voltage at the outer surface of the double layer controls the velocity of electrolyte flow in the capillary.
A suitable material for the insulator is silica, or another insulating material with a high dielectric breakdown, preferably greater than 1 megavolt/cm, most preferably greater than 5 megavolt/cm, and is preferably silica, because of silica's high dielectric breakdown and existing micromachining techniques for silica.
Suitable materials for the conductor include materials of high conductivity which may readily be deposited on the insulator with a good electronic match, preferably aluminum or copper. The conducting layer not necessarily be a metal, although the expectation that it will usually be a metal is the reason for the initial "M" in the acronym MIEEKFED.
The thickness of the insulator is determined by the range of voltages which may practically be applied. Uniformity in thickness is desirable. There are competing considerations in determining the optimal thickness of the insulator layer. On the one hand, the thinner the layer, the smaller the voltage needed. On the other hand, it is difficult to fabricate very thin capillaries with uniform thickness, and such thin capillaries tend to be fragile. A compromise between these competing consideration must be reached. A preferred range for the insulator thickness in the case of silica will be 1-100 micron. The range 40-100 micron is pratical to fabricate by traditional means; below that range may be achieved by silicon micromachining techniques. The maximum perpendicular voltage that may be applied across the insulator is determined by the dielectric breakdown of the insulator. For silica, this breakdown occurs at a field of about 5-10 megavolt/cm.
Suitable methods for manufacturing the insulating capillary include redrawing, for thicknesses down to about 40 microns; thinner capillaries may be made through silicon micromachining techniques. See Petersen, supra, which is incorporated by reference. Suitable methods for manufacturing the conductive coating include chemical vapor diposition, and sputtering.
FIGS. 2 and 3 illustrate computer calculations of the zeta potential as a function of V G for a 1-micron thick silica capillary, at different pH's, and at different concentrations n o of KC1 in water, respectively. In these Figures, V G ranges from -300 to +300 volts, which corresponds to a maximum electric field of 3×10 6 V/cm, below the dielectric breakdown range for SiO 2 of about 5×10 6 to about 1×10 7 V/cm. In FIG. 2, the concentration of KC1 in water is constant at 0.005 molar. In FIG. 3, the pH is constant at pH=3. Note that changing V G results in changing both the magnitude and the polarity of the zeta potential. Also note that when V G is close to zero, an incremental change in V G causes a greater change in the zeta potential than does the same incremental change when V G is larger. It is also apparent from FIG. 3 that a larger change in the zeta potential results from the same change in V G at lower ionic concentrations than at higher ionic concentrations.
The dependence of the zeta function on V G is complicated, and may either be observed empirically, or estimated through computer calculations as shown in FIGS. 2 and 3. This dependence may be written as
V.sub.G =f(z)
(V.sub.d =0)
or
z=f -1 (V G )
(V.sub.d =0)
In a MIEEKFED, a second voltage V d is applied across the length of a capillary of length L, so z is a function of distance x along the capillary as well: ##EQU1## Substituting equation (2) into equation (1), and substituting V d/L for E, gives the field-effect electroosmosis velocity: ##EQU2##
Equation (3) suggests that the velocity varies with distance; but because a liquid is essentially incompressible, the true velocity should be approximately equal to the average value of the above expression for v(x) over the range x=0 to x=L.
In a short capillary, a small potential will suffice to move the electrolyte, so it is feasible to have V d <<V G . In this case, equation 3 may be approximated: ##EQU3##
The zeta potential along the length of the capillary can be made constant through the use of a circuit such as that illustrated in FIG. 4. The zeta potential will be constant at f -1 (V G -V d ).
In FIG. 4, compared to FIG. 1, the position of electrode 7 is changed, and resistive layer 9 has replaced metal layer 2. A new voltage V G -V d has also supplied to one end of the capillary bore. Suitable methods for making resistive layer 9 include growing a resistive layer on the insulator by sputtering or chemical vapor deposition, or by growing silica on silicon on a microchip, as for example, by the technique of Petersen, supra, which is incorporated by reference. Using an appropriate value of V G -V d , a constant zeta potential of any chosen magnitude may be chosen (within the limits imposed by the thickness and the dielectric breakdown of the insulator). In particular a zero zeta potential, and thus zero electroosmosis, may be achieved using the circuit of FIG. 4 and selecting appropriate V G and V d . This result can be achieved without narrow limits on concentrations, pH's, or particular insulator materials, as has previously been the case.
More generally, an electroosmotic velocity v may be obtained, using the circuit of FIG. 4, from equation (3) by selecting ##EQU4##
Thus, for example, it might be desirable to separate and detect three species, A, B, and C of very close rates of electrophoresis, v A , v B , and v C , respectively, where v A <v B <v C . This result may be achieved using the capillary electrophoresis apparatus of FIG. 5. This apparatus incorporates the MIEEKFED 1 of FIG. 4, a buffer reservoir 10 feeding MIEEKFED 1, and a detector 11 for detecting components injected into MIEEKFED 1 as they exit the capillary.
Selecting V G -V d to give an electroosmosis rate equal to -v B , species B will be essentially immobile in the capillary, while species A will move slowly towards the anode 5, and species C will move slowly toward the cathode 6, and be detected by detector 11. "Tuning" the voltages applied as a function of time can subsequently cause species B, and finally species A, to reach detector 11. Using conventional means of capillary electrophoresis chromatography, it can be difficult to separate species with very close electrophoresis mobilities. The MIEEKFED allows flexibly "tuning" the rate of electroosmosis to counterbalance electrophoresis, and to achieve better separations than would otherwise be possible in capillary electrophoresis, over a broader range of concentrations, pH's, insulator materials, etc.
Another application of the present invention is to reduce the degree of "tailing" commonly seen in capillary electrophoresis of macromolecules. Tailing is reduced by reducing the zeta potential in the capillary. Thus tailing can be controlled by using a MIEEKFED to create a very low, and preferably uniform, zeta potential.
Higher resolution, but slower speed, results from a lower zeta potential. On the other hand, a higher zeta potential results in lower resolution, but faster response times. The more dilute the concentration, the greater is the degree of control over the zeta potential. See FIG. 3.
Microfabrication techniques such as those of Petersen, above, are well suited for making MIEEKFED's, because of the need for thin layers in a MIEEKFED. One possibility is that of performing multiple capillary electrophoresis on a single chip, having several capillaries "tuned" to different species, and acting simultaneously in parallel.
Separations of neutral species in a MIEEKFED may be performed with micelles, as described in the two Terabe references cited supra, both of which are incorporated by reference. A neutral species is considered to be "associated" with a micelle if it shows an affinity for the micelle, even though it may associate, dissociate, and reassociate from time to time. Different micelles may be used to separate different neutral species, or the same micelle--provided that the different neutral species have different affinities for that micelle.
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Apparatus and process for controlling the rate of electroosmosis due to a first electric potential in an electrically insulating capillary, in which a second electric potential is applied between the electrically insulating walls of the capillary and a liquid within the capillary. This second electric potential changes the charge on the wall of the capillary, and thus allows manipulation of the zeta potential within the capillary, and therefore the rate of electroosmosis.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates in general to the field of data processing systems and in particular to the field of automating the performance of selected processes within a data processing system. Still more particularly, the present invention relates to an improved method for automating the deferred performance of selected procedures within a data processing system.
2. Description of the Prior Art
The advent of powerful data processing systems has lead to an increasing amount of automation of processes which once required extensive human intervention. For example, it is not uncommon for long and complex data processing procedures to be initiated and run for long periods of time without requiring a computer user to periodically control the process.
However, a problem which continues to exist in even the most modern computer systems is centered in the fact that it is often necessary or desirable for a program or document to be initiated or transmitted at a time which is inconvenient for the computer user. Similarly, a process which requires multiple initiations over a period of time cannot be easily automated to reduce the amount of human intervention which is necessary.
It should therefore be apparent that a need exists for a method whereby a process or document may be automated to the extent that selected procedures may be initiated or transmitted automatically upon the occurrence of a selected deferral time.
SUMMARY OF THE INVENTION
It is therefore one object of the present invention to provide an improved data processing method.
It is another object of the present invention to provide an improved data processing method which permits the automation of selected data processing procedures.
It is yet another object of the present invention to provide an improved data processing method which permits the automating of deferred performance of selected procedures within a data processing system.
The foregoing objects are achieved as is now described. A desired deferral time is specified and associated with a particular document or process within a data processing system. Thereafter, the occurrence of the desired deferral time results in the automated processing of the associated document by the system. In one embodiment of the present invention a user may specify a particular date and time after which a response to a particular document is desired. The desired deferral time is then associated with the particular document in a distribution profile and utilized to either prompt a recipient to respond after the elapsing of the specified time or to automatically defer the transmission of the recipients response until the desired time has occurred. Similarly, a user may utilize this technique to chronologically order the fan out distribution of an electronic document by transmitting a list of the desired addressees and an associated desired deferral time for each such addressee to a transmission service. Thereafter, as each desired deferral time elapses the document is automatically transmitted to an associated addressee.
The above as well as additional objects, features, and advantages of the invention will become apparent in the following detailed description.
BRIEF DESCRIPTION OF THE DRAWING
The novel features believed characteristic of the invention are set forth in the appended claims. The invention itself however, as well as a preferred mode of use, further objects and advantages thereof, will best be understood by reference to the following detailed description of an illustrative embodiment when read in conjunction with the accompanying drawings, wherein:
FIG. 1 is a pictorial representation of a distributed data processing system which may be utilized to implement the method of the present invention;
FIG. 2 is a graphic depiction of a distribution profile which may be utilized to implement the method of the present invention;
FIG. 3 is a logic flowchart depicting the deferral of an electronic document process by means of the method of the present invention; and
FIG. 4 is a logic flowchart depicting the automated prompting of a deferred response to a document in accordance with the method of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
With reference now to the figures and in particular with reference to FIG. 1, there is depicted a pictorial representation of a data processing system 8 which may be utilized to implement the method of the present invention. As may be seen, data processing system 8 may include a plurality of networks, such as Local Area Networks (LAN) 10 and 32, each of which preferably includes a plurality of individual computers 12 and 30, respectively. Of course, those skilled in the art will appreciate that a plurality of Intelligent Work Stations (IWS) coupled to a host processor may be utilized for each such network.
As is common is such data processing systems, each individual computer may be coupled to a storage device 14 and/or a printer/output device 16. One or more such storage devices 14 may be utilized, in accordance with the method of the present invention, to store the various data processing procedures or documents which may be periodically accessed by a user within data processing system 8, and automated in a deferred manner in accordance with the method of the present invention. In a manner well known in the prior art, each such data processing procedure or document may be stored within a storage device 14 which is associated with a Resource Manager or Library Service, which is responsible for maintaining and updating all resource objects associated therewith.
Still referring to FIG. 1, it may be seen that data processing network 8 may also include multiple mainframe computers, such as mainframe computer 18, which may be preferably coupled to Local Area Network (LAN) 10 by means of communications link 22. Mainframe computer 18 may also be coupled to a storage device 20 which may serve as remote storage for Local Area Network (LAN) 10. Similarly, Local Area Network (LAN) 10 may be coupled via communications link 24 through a subsystem control unit/communications controller 27 and communications link 34 to a gateway server 28. Gateway server 28 is preferably an individual computer or Intelligent Work Station (IWS) which serves to link Local Area Network (LAN) 32 to Local Area Network (LAN) 10.
As discussed above with respect to Local Area Network (LAN) 32 and Local Area Network (LAN) 10, a plurality of data processing procedures or documents may be stored within storage device 20 and controlled by mainframe computer 18, as Resource Manager or Library Service for the data processing procedures and documents thus stored. Of course, those skilled in the art will appreciate that mainframe computer 18 may be located a great geographical distance from Local Area Network (LAN) 10 and similarly Local Area Network (LAN) 10 may be located a substantial distance from Local Area Network (LAN) 32. That is, Local Area Network (LAN) 32 may be located in California while Local Area Network (LAN) 10 may be located within Texas and mainframe computer 18 may be located in New York.
In known prior art systems of this type it is common for a user in one area of distributed data processes system 8 to transmit a process or document to a second user within a different portion of distributed data processing 8. Within the textual content of a document transmitted in this manner it is also common for one user to specify to a second user that a response is desired not later that a particular time; however, there exists no current procedure whereby a user may automatically defer the transmittal of such a document or the receipt of a response from the recipient until the occurrence of a specified deferral time.
It should therefore be apparent that it would be very helpful to have a system whereby a delay for a particular procedure or document may be automated within the data processing system, thereby greatly enhancing the efficiency of the data processing system.
Referring now to FIG. 2, there is depicted a graphic representation of a distribution profile which may be utilized to implement the method of the present invention. As is illustrated, a document 40 is depicted along with a distribution profile 44. Distribution profile 44 is preferably stored in association with document 40 and linked thereto via reference 42. Those skilled in the art will appreciate that reference 42 may comprise a flag or other reference stored within document 40.
As is illustrated, distribution profile 44 preferably includes multiple fields of information which may be utilized to characterize the distribution of document 40. Although multiple specific fields are depicted within FIG. 2 several of these fields are illustrative in nature and those skilled in the art will appreciate that additional fields or different fields may be utilized without departing from the spirit of the present invention.
As is depicted in FIG. 2, distribution profile 44 includes a field 46 which may be utilized to indicate the importance of document 40. Field 48 similarly may be utilized to indicate the type of service which may be utilized with document 40 and field 50 preferably indicates the attributes of the type of reply which is required for document 40.
Field 52 within distribution profile 44 may be utilized to indicate a classification for document 40, either a security classification or delivery classification, as desired by the system operator. Next, in accordance with an important feature of the present invention, field 54 within distribution profile 44 may be utilized to indicate whether or not document 40 has a deferred request associated therewith. That is, whether or not the user specifying document 40 has requested that the transmittal or processing of document 40 be deferred until the occurrence of a specified deferral time. Finally, field 56 within distribution profile 44 may be utilized to specify the date and time associated with the deferral request contained within field 54. That is, the user specifying document 40 may also specify within distribution profile 44 a specific date and time the occurrence of which will automatically process or distribute document 40.
With reference now to FIG. 3, there is depicted a logic flowchart illustrating the deferral of an electronic document process by means of the method of the present invention. As is depicted, the process begins at block 60 and thereafter passes to block 62 which illustrates the requesting of a document process. As utilized herein the term "document" shall mean a document or data processing procedure and the term "process"shall mean the actual processing of that procedure or the transmission of a document from one point of the data processing system to another location therein. Next, block 64 illustrates a determination of whether or not a deferral of the process has been requested and if not, block 66 illustrates the execution of that process. Thereafter, the procedure terminates, as illustrated in block 68.
However, in the event the determination illustrated in block 64 indicates that a deferral of the requested process has been requested, then block 70 illustrates a determination of whether or not an appropriate deferral service exists. Those skilled in the art will appreciate that the mere requesting of a deferral of a process will not be effective to defer that process unless the service or Resource Manager includes a procedure which will recognize the deferral request. In the event a deferral service does not exist then the process again returns to block 66 wherein the process is executed and thereafter the procedure terminates, as illustrated in block 68.
In the event a deferral of the requested process has been requested and a deferral service does exist, as determined in blocks 64 and 70, then block 72 depicts the setting of the execute time for the process in question to the desired deferral time. That is, the time at which the deferred process requested will automatically be executed by the system is set equal to the desired deferral time specified in the distribution profile (see FIG. 2). Next, as depicted in block 74 the request is transmitted to the deferral service. Block 76 next illustrates the deferring of the process. Finally, block 78 illustrates a determination of whether or not the current time is equal to the execute time and if not, the process returns iteratively to block 76 to await the point at which the current time will equal the execute time. At the point when the current time equals the execute time the process returns to block 66, wherein the requested process is executed. Thereafter, the process terminates as illustrated in block 68.
Upon reference to the foregoing those skilled in the art will appreciate that by establishing a deferral service in accordance with the method of the present invention a computer user may specify any process associated with a data processing procedure or document and defer the execution of that process until a specified deferral time has occurred. In this manner, a computer user may automate the chronologically ordered fan out distribution of a document by requesting transmittal of that document to a plurality of recipients while specifying desired deferral times for each recipient thus listed. In this manner the service may be utilized to automatically initiate transmittal of the specified document to each of the plurality of recipients at the deferral time requested by the transmitter. Similarly, the document process requested may simply be the transmittal of a response from the recipient of the document. In such a situation, a recipient who replies to a document which has been transmitted prior to the occurrence of the requested deferral time will find his or her reply being automatically deferred until the requested deferral time has occurred. Thereafter, the transmission service associated with the recipient will, in accordance with the method of the present invention, automatically transmit the reply in question to the originator of the document.
In this manner the transmission of a document by an original transmitter of a document or the transmission of a response by a recipient of a document may be automatically and efficiently deferred until the occurrence of a specified elapsed time. This technique permits the data processing system to accurately and efficiently order the procedure whereby documents are transmitted or responses to documents are received by a document originator.
Referring now to FIG. 4, there is depicted a logic flowchart illustrating the automated prompting of a desired response to a document in accordance with the method of the present invention. This technique is similar in nature to the method depicted within FIG. 3; however, it is specific in application to the prompting of a response from a recipient of a document transmitted within the data processing system.
As is illustrated, this process begins at block 80 thereafter passes to block 82 which illustrates the receipt of a document. Next, block 84 illustrates a determination of whether or not a reply deferral has been requested and if not, the process passes to block 86 and terminates.
In the event the determination depicted within block 84 indicates that a reply deferral has been requested, then block 88 illustrates the retrieval of the current time from the system clock. Next, block 90 illustrates a determination of whether or not the requested deferral time has elapsed. If not, the process returns iteratively to block 88 to once again determine the current time from the system clock. However, in the event the requested deferral time has elapsed, the process passes to block 92 which illustrates the prompting of the user to reply to the document previously received. Thereafter, the process returns to block 86 and terminates, as previously illustrated.
Upon reference to the foregoing to those skilled in the art will appreciate that the applicant has disclosed a method whereby a specified deferral time may be associated with a document or process and the processing of that document may be automatically deferred and then automatically initiated upon the occurrence of the specified deferral time. In this manner, the transmission of a document, a reply to that document or the prompting of a recipient to reply to a document may be automatically deferred until a selected time and thereafter initiated by the data processing system without the necessity of human intervention.
Although the invention has been described with reference to a specific embodiment, this description is not meant to be construed in a limiting sense. Various modifications of the disclosed embodiment as well as alternative embodiments of the invention 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 any such modifications or embodiments that fall within the true scope of the invention.
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A method is disclosed for automating a selected delay within a data processing procedure. A desired deferral time is specified and associated with a particular document or process within a data processing system. Thereafter, the occurrence of the desired deferral time results in the automated processing of the associated document by the system. In one embodiment of the present invention a user may specify a particular date and time after which a response to a particular document is desired. The desired deferral time is then associated with the particular document in a distribution profile and utilized to either prompt a recipient to respond after the elapse of the specified time or to automatically defer the transmission of the recipient's response until the desired time. Similarly, a user may utilize this technique to chronologically order the fan out distribution of a document by transmitting a list of desired addressees and an associated desired deferral time for each such addressee to a transmission service. Thereafter, as each desired deferral time elapses the document will automatically be transmitted by the transmission service to an associated addressee.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of Provisional application No. 61/870,767 Filed 27 Aug. 2013.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
REFERENCE TO SEQUENCE LISTING, A TABLE OR A COMPUTER PROGRAM LISTING COMPACT DISC APPENDIX
[0003] Not Applicable
BACKGROUND OF THE INVENTION
[0004] In many vehicles, such as motorcycles, which use handlebars for steering, the speed of the vehicle is controlled by a mounted rotatable accelerator sleeve unit that is fastened to the right end of the handlebar, which is usually wrapped with a rubber or plastic grip. This rotatable accelerator sleeve, which is commonly called a throttle, is directly coupled to the vehicle's throttle housing, which transfers the rotation of the sleeve into either 1 or more throttle cables or an electronic sensor. Thus, by rotating the accelerator sleeve, the engine in the vehicle will either accelerate, maintain or decelerate the speed of the vehicle, depending on the direction of the rotation.
[0005] For convenience and safety purposes, the throttle is typically designed, using a biased return spring, to rotate the throttle back to its resting position, which will maintain the vehicle's engine idle and prevent the vehicle from accelerating. Thus, to maintain a constant speed, the operator of the vehicle must hold the throttle firmly at a desired rotational position, overpowering the throttle's biased return springs. During a long distance motorcycle trip, for example, a motorcycle operator may become fatigued due to the efforts of holding the throttle in one steady position. Lack of motion in the arm, lack of circulation, numbness, vibration injuries because of vibrations from the road and the engine and many other factors can cause numerous injuries to the operator's hand, or even serious injury if the operator's hand falls asleep due to exhaustion, distracting the operator from focusing on the road.
[0006] Many devices and methods have been designed to allow an operator of a handlebar steered vehicle to maintain a desired cruising speed without requiring a constant force applied to the throttle by the operator. These devices may be referred to generally as motorcycle cruise controls and/or throttle lock devices.
[0007] Some devices require the owner of the vehicle to drill into their throttle housing to mount the device firmly to the throttle housing, which damages the vehicle's warranty. The use of these devices can be seen in U.S. Pat. Nos. 4,256,197 A, 4,137,793 A, 20100294077 A1.
[0008] One such device requires the owner of the vehicle to mount the device to the handlebar itself, taking up precious space on the handlebars, restricting the use of other safety gear such as hand guards and could block the operator's usage and view of the controls and dash displays. The use of such a device can be seen in U.S. Pat. No. 3,982,446 A.
[0009] Some devices require electricity to work properly. Such a device can be seen in U.S. Pat. No. 6,318,490 B1.
[0010] Another device fastens over the throttle's rubber/plastic grip but is not fixed in place. It can be moved, rotated and slide side to side by the operator during the operation of the vehicle. This device covers sections of the throttle grip, restricting the operator's full use of the grip, which was not intended by the manufacture of the vehicle and may easily be accidentally bumped by the operator, causing the vehicle to dramatically decelerate or accelerate with unintended consequences. The use of this device can be seen in U.S. Pat. No. 4,875,386 A.
[0011] One device simply covers sections of the throttle grip and restricts full use of the throttle. It takes away space for the operator's hand, especially when the operator is wearing riding gloves. The use of one such device can be seen in U.S. Pat. No. 3,982,446 A.
[0012] Another device is designed to disengage once the front brake lever is pulled. This is a safety concern for a motorist. If the device malfunctions, it will prevent the operator from using the front brakes, which, for a motorcycle, provides 75% of the vehicle's stopping power. Not only can the device malfunction and prevent the front brake from engaging, but the cruise control could be stuck in the “on” position and may not be overpowered by the operator. The use of this device can be seen in U.S. Pat. No. 6,820,710 B2.
[0013] Still, other devices mount to the bar end of the throttle grip and requires the operator to grab the device and rotate it in the direction of acceleration of the engine's throttle grip to engage the device. This can be extremely dangerous when operating the vehicle off-road with gloves on. The use of these devices can be seen in U.S. Pat. Nos. D593463 S1, D593462 S1, D593464 S1.
BRIEF SUMMARY OF THE INVENTION
[0014] The present invention provides a cruise control for any handlebar steered vehicle which uses a mounted rotatable accelerator sleeve unit, or the like, and throttle housing, or the like, to accelerate, maintain and decelerate the speed of the engine and vehicle. This invention allows the owner of the vehicle to install this cruise control directly onto the rotating plastic sleeve without needing to drill into their throttle housing, which could void any warranty on the vehicle, it does not mount to the handlebar itself, which gives the operator more space near the hand controls and dash displays, it functions without the need of an electronic connection, it has no direct connection to front brake which simplifies the construction and prevents any potential malfunction of the cruise control, which could in turn prevent the front brake from being used to slow down and stop the vehicle in an emergency, it does not engage by rotating the throttle, which will prevent the operator from accidentally engaging the cruise control while wearing gloves and/or riding off-road, and it does not cover the throttle's grip in any way.
[0015] More specifically, this cruise control can be mounted on a wide variety of mounted rotatable accelerator sleeves units with varying throttle sleeve diameters due to its unique use of the pivotable clamping arm, single body piece, body hinge and cinching bolt. With the use of serrated inner teeth on the clamp and body, this cruise control can securely mount to any average size accelerator sleeve. The mounting point for this invention is located next to the throttle housing, clamped onto the accelerator sleeve which protrudes from the throttle housing, between the throttle housing and the accelerator sleeve's rubber/plastic grip's flange or inner end. This will give the operator easy access to the cruise control with their thumb.
[0016] For vehicles with accelerator sleeves, cruising speeds are at different positions of rotation in relation to the handlebars, but all previously designed cruise controls stay in the same location in relation to the handlebars. While the operator's hand rotates to accelerate, maintain or decelerate the vehicle, the location of the fixed controls of the cruise control in relation to the operator's rotated hand has now changed dramatically, which hinders the use of the controls of the cruise control, causing distraction and discomfort to the operator as they try to reach for the controls of the cruise control and causes safety issues when the operator tries to engage or disengage the cruise control. With this invention, when the operator accelerates the engine and vehicle by rotating the accelerator sleeve, the entire invention rotates with the accelerator sleeve, holding the invention and its controls in perfect ergonomic positioning during the entire ride. If the operator chooses to slow the vehicle, they should disengage the cruise control, then re-engage the cruise control at a slower speed. Their hand will not need to awkwardly move to press, roll or otherwise engage/disengage the cruise control. This invention rotates naturally with the operator's hand, not distracting the driver or causing discomfort while they manipulate the controls of the cruise control. This invention is a great advantage for any operator's safety, which has never been seen in a handlebar steered vehicle cruise control before.
[0017] For further simplification from other cruise controls, this invention uses only one button to engage and disengage the cruise control. This button can be moved to engage the cruise control, then moved again to disengage the cruise control. When the button is moved to engage the cruise control, a small stopper in the side of the single body piece will protrude from the single body piece and press against the surface of the throttle housing, creating sufficient pressure between the throttle housing and the cruise control, which in turn causes sufficient friction to hold the accelerator sleeve from naturally rolling back to its resting position. At all times, this invention can be overridden by the operator to accelerate or decelerate the engine and vehicle. This may disengage the cruise control. When the button is moved to disengage the cruise control, the stopper will then retract into the single body piece, allowing free rotational movement of the accelerator sleeve without any friction. Once the cruise control is disengaged, the mechanism inside the single body piece will reset, so when it is moved again, it will engage the stopper and start the entire process over again.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
[0018] FIG. 1 is a sectional view of a rubber/plastic grip fixed to the rotatable accelerator sleeve which covers the end of the handlebar and is mounted to the throttle housing which attaches to the handlebar and has two throttle cables protruding from its housing.
[0019] FIG. 2 has a perspective view of FIG. 1 , viewed from the position of the vehicle's operator, where the rubber/plastic grip is covering the accelerator sleeve, which is covering the handlebar and attached to the throttle housing that has two throttle cables protruding out of the top.
[0020] FIG. 3 has a perspective view of FIG. 1 , viewed from the position of the vehicle's operator, which shows how this cruise control invention mounts to the rotatable accelerator sleeve unit, between the throttle housing and the rubber/plastic grip, with its control button protruding in an ergonomic position for the operator to use their thumb to engage and disengage the cruise control.
[0021] FIG. 4 is a side perspective view of the cruise control which shows the side of the invention that faces the throttle housing, with its rectangular protruding stopper, its single body piece which attaches to the pivotable clamp arm in two places, one with a hinge and a second with a nut and bolt which allows it to clamp to varying throttle sleeve diameters, and the control button which is properly extended in its resting position.
[0022] FIG. 5 is a side perspective view, similar to FIG. 4 but showing how the pivotable clamp arm can be cinched down to fit varying throttle sleeve diameters.
[0023] FIG. 6 is a side perspective view, similar to FIG. 4 but without the pivotable clamp arm attached to the single body piece by either the hinge nor the nut and bolt holes.
[0024] FIG. 7 is a side perspective view of the cruise control which shows the side of the invention that faces away from the throttle housing and towards the rubber/plastic grip. It shows how the single body piece and the pivotable clamp arm can fit between a very narrow gap between the throttle housing and the rubber/plastic grip.
[0025] FIG. 8 is a side perspective view, similar to FIG. 5 , showing the control button in its properly extended resting position.
[0026] FIG. 9 is a side perspective view, similar to FIG. 5 , but showing the control button in its fully compressed position which will either engage the stopper mechanism or disengage the stopper mechanism, compressing the control button will perform the opposite response of the stopper in its current position.
[0027] FIG. 10 is a perspective view, very similar to FIG. 3 but viewing the side of the invention which faces the throttle housing, showing the stopper fully disengaged and recessed into the single body piece and showing the bolt holes in the clamp arm. This perspective shows the thin vertical serrated walls on both the pivotable clamp arm and the body piece.
[0028] FIG. 11 is a perspective view, similar to FIG. 10 , but showing the stopper fully engaged and protruding out of the single body piece.
[0029] FIG. 12 is a perspective view of the invention from a short distance away from the end of the handlebar, where the cruise control is mounted to the throttle sleeve between the throttle housing and the rubber/plastic grip, where the mounted rotatable accelerator sleeve unit is at rest and rotated to a stop because of the biased springs pulling on the throttle cables.
[0030] FIG. 13 is a perspective view, similar to FIG. 12 , but showing the rotatable accelerator sleeve unit rotated back to a comfortable cruising position for the operator, with the stopper engaged, holding the throttle in place because of the friction between the throttle housing, the invention and the throttle sleeve, which now overpowers the springs in the throttle cables from rotating the throttle sleeve back to its resting position like in FIG. 12 .
DETAILED DESCRIPTION OF THE INVENTION
[0031] This invention 12 , illustrated in the accompanying drawings, is meant to be used as a cruise control 12 for a vehicle which is steered by handlebars 1 and accelerates, maintains and decelerates its speed with a mounted rotatable accelerator sleeve unit 9 , similar to a motorcycle. An example of this type of mounted rotatable accelerator sleeve unit 9 is shown in FIGS. 1-3 and 12 - 13 . In FIG. 1 the rubber/plastic grip 4 is fixed to the accelerator sleeve 5 which is mounted to the throttle housing 2 . The throttle housing 2 is mounted to the handlebars 1 , and has, in this example, two throttle cables 3 protruding out of the throttle housing 2 .
[0032] FIG. 2 shows the exposed segment of the accelerator sleeve 5 between the throttle housing 2 and the rubber/plastic grip 4 , which is where the invention 12 will be mounted. In FIG. 3 , the cruise control 12 is attached to the mounted rotatable accelerator sleeve unit 9 , and when combined 20 , shows where the invention 12 attaches to the accelerator sleeve 5 . FIG. 4 shows the pivotable clamping arm 10 , its outer hinge 14 and the sidewall of the bolt hole 15 . FIG. 4 shows the invention 12 in a position where the nut and bolt 16 have only been cinched down slightly, allowing the invention 12 to be mounted to accelerator sleeve 5 with a large diameter. FIG. 4 is a perspective view, viewing the side of the invention 12 that faces the throttle housing 2 . In this view, you can see how the stopper 18 is positioned in relation to the pivotable clamp arm 10 and the single button 8 . FIG. 5 shows the invention 12 with the nut and bolt 16 cinched tight to fit on an accelerator sleeve 5 with a narrow diameter. FIG. 6 shows the pivotable clamp 10 fully detached from the single body piece 11 and easily displays the inner part of the hinge 13 and the outer part of the hinge 14 .
[0033] FIG. 7 is a perspective view looking at the invention's 12 side which faces away from the throttle housing 2 . FIGS. 7 and 10 shows the pivotable clamp arm's 10 thinner vertical serrated wall 19 and the body piece's 11 vertical serrated wall 22 . The vertical serrated walls 19 and 22 are thinner than the overall width of the pivotable clamp arm 10 and the body piece 11 , allowing the clamp 10 and body piece 11 to mount in a very small segment of the accelerator sleeve 5 between the throttle housing 2 and the grip 4 .
[0034] FIG. 8 shows the single button 8 in its properly extended resting position. When this button 8 is pressed in by the operator's thumb, like in FIG. 9 , it will be forced back out by a spring-like mechanism housed within the single body piece 11 .
[0035] FIG. 10-11 show exactly how the stopper 18 protrudes and retracts from the single body piece 11 . FIG. 10 shows the stopper 18 completely recessed in the single body piece 11 , this is how the stopper 18 rests when the invention 12 is fully disengaged. FIG. 11 shows the stopper 18 protruding from the single body piece 11 , this is how the stopper 18 rests when the invention 12 is fully engaged.
[0036] FIG. 12 shows the combination 20 of the invention 12 attached to the mounted rotatable accelerator sleeve unit 9 , similar to FIG. 3 . The marker 21 at the end of the grip is showing the accelerator sleeve 5 in its rested state in FIG. 12 . FIG. 13 shows the invention 12 and the mounted rotatable accelerator sleeve unit 9 fully combined 20 but unlike in FIG. 12 where the accelerator sleeve 5 is at rest, FIG. 13 shows the accelerator sleeve 5 rotated back to give the operator a comfortable cruising speed, and the invention 12 is holding the mounted rotatable accelerator sleeve unit 9 in place. The marker 21 in FIG. 13 denotes the rotation of the mounted rotatable accelerator sleeve unit 9 and the cruise control 12 combined 20 .
[0037] This invention has many advantages over other types of motorcycle cruise controls and throttle locks due to its unique design and function. Some devices require the owner of the vehicle to drill into the throttle housing to mount the device, which may void the vehicle's warranty. Other devices require the owner of the vehicle to mount the device to the handlebar itself, taking up precious space on the handlebar, restricting the use of other safety gear such as hand guards and could block the operator's usage and view of the vehicle controls and dash display. Still, other devices require the owner of the vehicle to mount the device to the bar end of the handlebar, these types of throttle locks activate when the operator grips the device and rotates it as they rotate the throttle to accelerate. This is very dangerous and cumbersome for the rider, especially if they are wearing thick gloves and grab the device unintentionally, thus activating the device inadvertently. None of these previously mentioned devices, nor any others not mentioned here, function by rotating with the operator's hand and throttle as the operator accelerates the vehicle. All of the devices mentioned are mounted in place to either the handlebar, the throttle housing or some other non-rotating part, in order to hold the device as an anchor point. This causes a problem since the operator's hand doesn't remain in the same place while they rotate the throttle. Once they rotate the throttle, their hand will rotate away or towards the fixed controls of the cruise controls. The operator has to adjust their hand according to where the cruise control is located. Every time they change speeds, the controls for the cruise control will be in a different location.
[0038] My invention 12 is different. It rotates naturally with the operator's hand and the throttle 5 . With my invention 12 , the controls 8 of my cruise control 12 will move in unison with relation to the operator's hand as they rotate the throttle 5 between various speeds. This invention's 12 controls 8 will always be perfectly located in relation to wherever the operator places their hand and the throttle 5 . This is a great advantage for the operator since they will no longer need to slide their hand around the throttle 5 in order to manipulate the controls 8 of the cruise control 12 . My invention 12 does not have an anchor point attached to the handlebars 1 . My invention 12 doesn't need the owner to mount it to the throttle housing 2 , they simply tighten the clamp 10 and the body piece 11 to the rotatable accelerator sleeve 5 . My invention 12 does not cover any portion of the rubber/plastic grip 4 , it gives the operator full use of the grip 4 , as the manufacture intended.
[0039] All visible parts of this invention 12 , seen in all FIGS. can be fashioned out of any hard metal or plastic or the like by a CNC process, injection molding, die cast molding or any other parts building machine. The parts within the single body piece 11 , which are not visible in the FIGS., can be fashioned from similar materials by the same manufacturing processes common to machine shops and the like.
[0040] For proper use of this invention 12 on a vehicle, the operator must first detach the nut and bolt 16 and disjoint the outer hinge 14 from the inner hinge 13 , which will completely remove the clamp 10 from the single body piece 11 . The body piece 11 will then need to be positioned under the accelerator sleeve 5 between the throttle housing 2 and the grip 4 , as in FIG. 3 . Now, join the inner hinge 13 and the outer hinge 14 to connect the pivotable clamp arm 10 to the body piece 11 , then place the bolt 16 through the clamp's 10 bolt hole 15 and through the body piece's 11 bolt hole 17 , then cinch the clamp arm 10 down by tightening the nut and bolt 16 until sufficient pressure is made around the accelerator sleeve 5 between the clamp's 10 vertical serrated wall 19 and the body piece's 11 vertical serrated wall 22 . The cruise control 12 is now securely attached to the accelerator sleeve 5 and will not slide side to side or rotate around the accelerator sleeve 5 , but will move in conjunction with the accelerator sleeve 5 .
[0041] To operate the mounted rotatable accelerator sleeve unit 9 to accelerate the vehicle, the operator will need to rotate the accelerator sleeve 5 which in turn accelerates the speed of the engine and the vehicle, as well as turns the invention 12 in perfect rotational unity with the accelerator sleeve 5 , since the two parts are now attached to each other. Once the operator has reached the desired speed, they can simply use their thumb to press the button 8 in fully, which engages the invention 12 and forces the stopper 18 to protrude from the body piece 11 . Once the operator has fully pressed the button 8 in, the stopper 18 will be held in place by the mechanism inside the body piece 11 and the button 8 will automatically extend out of the body piece 11 back to its proper resting position. Now the cruise control 12 is fully engaged and holding the accelerator sleeve 5 in place by using the friction caused from the stopper 18 pressing against the throttle housing 2 . This friction is strong enough to resist the biased spring tension on the throttle cables 3 which is constantly trying to rotate the accelerator sleeve 5 back to its resting position, however, it is not strong enough to resist pressure the operator places on the accelerator sleeve 5 if they choose to override the cruise control 12 and accelerate or decelerate the vehicle with the cruise control 12 fully engaged.
[0042] When the operator chooses to disengage the cruise control 12 , they need to press the button 8 fully in to allow the mechanism inside of the body piece 11 to retract the stopper 18 into its recessed hole within the body piece 11 . Once the button 8 is fully pressed in and the stopper 18 has fully retracted, the button 8 will automatically extend out of the body piece 11 back to its resting position, ready to start the entire cycle over again.
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A cruise control for a vehicle having a mounted rotatable accelerator sleeve and throttle housing which is mounted to a handlebar. The cruise control mounts entirely to the accelerator sleeve and rotates in perfect unity with the throttle when it is rotated. The cruise control is mounted between the throttle housing and the rubber/plastic grip's inner end, directly onto the accelerator sleeve. When the single button of the cruise control is pressed, the cruise control engages and uses friction against the surface of the throttle housing to hold the throttle in place. The operator can force the throttle to rotate by overpowering the friction caused by the cruise control, or preferably, they can disengage the cruise control by pressing the single button again, resetting the cruise control to be engaged again by pressing the single button.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a head position detecting method and a disk device, and, in particular, to a head position detecting method and disk device in which a servo signal is detected in accordance with an area servo method.
Recently, as an information amount increases in an information-oriented society, increase of the storage capacity of a magnetic disk device and high-speed access to stored data are demanded. Therefore, for a magnetic disk, increase of BPI (Byte Per Inch: a unit for indicating a recording density) and improvement of TPI (Tracks Per Inch: a unit for indicating a track density) are requested.
However, in a magnetic disk device, when increasing TPI, a dead space between tracks decreases. When a dead space between tracks decreases, higher head position detecting accuracy is required.
In order to achieve higher head position detecting accuracy, it is necessary to detect a servo signal with high accuracy. For this purpose, a servo signal detecting method has been changed from a peak hold method to a so-called area servo method. In the peak hold method, the head position is detected from the peak value of a servo signal. In the area servo method, a servo signal waveform is integrated and the head position is detected from the integrated value.
2. Description of the Related Art
FIG. 1 shows a block diagram of one example of a magnetic disk device in the related art.
The magnetic disk device 1 causes magnetic heads 3 to approach magnetic disks 2, which are made of a magnetic substance and rotate in an arrow-A direction, and performs information recording and reproducing. In the magnetic disks, cylinders are previously set concentrically for fixing information recording and reproducing positions. The magnetic heads 3 are held at a projecting end of an arm 4. The other end of the arm 4 is held by an actuator 5. The actuator 5 rotates the arm 4 in an arrow-B direction about a shaft 5a, and performs position control so as to position the magnetic heads 3 at a desired cylinder.
Further, the signal reproduced as a result of the magnetic heads 3 scanning the magnetic disk 2 is supplied to a R/W (Read/Write) pre-amplifier 6. The R/W pre-amplifier 6 amplifies the signal reproduced by the magnetic heads 3, supplies the signal to an automatic gain control (AGC) amplifier 7, and, also, amplifies a recording signal to be recorded to the magnetic disks 2 and supplies the signal to the magnetic heads 3.
The AGC circuit 7 controls the amplitude of the main signal of the reproduced signal amplified by the R/W pre-amplifier 6 to be equal to or less than a fixed level. The output signal of the AGC circuit 7 is supplied to a signal detecting portion 8 and a servo detecting portion 9. The signal detecting portion 8 reads control information and data from the reproduced signal, converts it into digital information and supplies it to a CPU 10. The CPU 10 decodes the digital information read from the signal detecting portion and outputs it as reproduced data.
The servo detecting circuit 9 detects a servo portion of the output signal of the AGC amplifier 7, detects the current position of the magnetic heads 3 by a servo burst signal of the servo portion, generates an error signal and supplies it to the CPU 10.
In accordance with the error signal from the servo detecting portion 9, the CPU 10 generates a position control signal for controlling the position of the magnetic heads 3, and supplies the signal to a D/A (Digital/Analog) converter 11. The D/A converter 11 converts the position control signal supplied by the CPU 10 into an analog signal and supplies the signal to a driver 12. In accordance with the position control signal supplied by the D/A converter 11, the driver 12 generates a driving signal for driving the actuator 5, and supplies the signal to the actuator 5.
The actuator 5 rotates about the shaft 5a in accordance with the driving signal supplied by the driver 12, and rotates the arm 4 in the arrow-B direction. As a result of the rotation of the actuator 5, the magnetic heads 3 held at the projecting end of the arm 4 move in the arrow-B direction on the magnetic disks 2, and scan a desired cylinder on the magnetic disks 2.
FIGS. 2A and 2B show a data format of the magnetic disks. FIG. 2A shows a perspective view of the magnetic disk 2 and FIG. 2B shows a development of the cylinders.
As shown in FIG. 2A, the plurality of cylinders 21 are formed concentrically on the two sides of the magnetic disk 2. As shown in FIG. 2B, the servo portions 22 are formed with predetermined intervals in the cylinders 21 for recognizing the position of the magnetic heads 3 as a result of being read by the magnetic heads 3. Between the servo portions, data portions 23 for writing data thereto are formed.
At the time of recording and reproducing, the servo burst signal written in the servo portions 22 is reproduced by the magnetic heads 3, and, through the reproduced signal, the cylinder number at which the magnetic heads 3 currently scan and the position shift on the cylinder are recognized by the CPU 10.
FIG. 3 shows a data format of the servo portion of the magnetic disks.
The servo portion 22 includes an AGC portion 24 for fixing the signal reception level, a training pattern portion 25 for indicating the start of the servo information, a servo information portion 26 in which digital information such as the cylinder number and so forth are recorded and a servo burst portion 27 in which the servo burst signal for generating a tracking error signal is recorded.
As shown in FIG. 3, the servo burst portion 27 includes the servo burst signals S1, S2, which are formed to lie across adjacent cylinders, and the servo burst signals S3, S4, which are formed on respective cylinders. The servo burst signals S1, S2, S3 and S4 are formed successively in the direction in which the cylinders extend.
FIG. 4 shows a waveform of the servo burst signals reproduced by the magnetic heads. FIG. 4 shows the waveform of the reproduced signal obtained when, in FIG. 3, the magnetic head 3 scans an approximately central portion of the cylinder 21-1 in an arrow-C direction.
During the time from t0 through t1, the magnetic head 3 scans the servo burst signal S1. During this time, because the servo burst signal S1 is formed to lie across from the center of the cylinder 21-1 to the center of the cylinder 21-2, when the magnetic head 3 scans the center of the cylinder 21-1, the magnetic head 3 scans approximately half of the servo burst signal S1. Accordingly, the amplitude is approximately half in comparison to the case where the magnetic head 3 reproduces the servo burst signal with the entirety of the magnetic head 3.
Then, when, during the time from t1 through t2, the magnetic head 3 scans the cylinder 21-1 in the arrow-C direction, the magnetic head 3 scans the servo burst signal S2. During this time, because the servo burst signal S2 is formed to lie across from the center of the cylinder 21-3 to the center of the cylinder 21-1, when the magnetic head 3 scans the center of the cylinder 21-1, the magnetic head 3 scans approximately half of the servo burst signal S2. Accordingly, the amplitude is approximately half in comparison to the case where the magnetic head 3 reproduces the servo burst signal with the entirety of the magnetic head 3.
Then, when, during the time from t2 through t3, the magnetic head 3 scans the cylinder 21-1 in the arrow-C direction, the magnetic head 3 scans the servo burst signal S3. During this time, because the servo burst signal S3 is formed across the entire width of the cylinder 21-1, all of the signal reproduced by the magnetic head 3 is the servo burst signal, and the amplitude is maximum among the cases where the magnetic head 3 reproduces the servo burst signals.
Then, when, during the time from t3 through t4, the magnetic head 3 scans the cylinder 21-1 in the arrow-C direction, the magnetic head 3 scans between the servo burst signals S4. Accordingly, the servo burst signals S4 are not reproduced.
The reproduced signals of the servo burst signals as shown in FIG. 4 are supplied to the servo detecting portion 9 through the R/W pre-amplifier 6 and AGC amplifier 7. In order to accurately obtain the difference between the above-mentioned servo burst signal S1 and servo burst signal S2 which are formed across adjacent cylinders, the servo detecting portion 9 obtains the integrated values obtained from integrating the servo burst signal S1 and servo burst signal S2.
FIG. 5 shows a block diagram of one example of the servo detecting portion in the related art.
The servo detecting portion 9 includes a full-wave rectifier 31 which performs full-wave rectification on the output servo burst signal of the AGC amplifier 7, an integrating circuit 32 which integrates the servo burst signal which has undergone the full-wave rectification in the full-wave rectifier 31, an A/D converter 33 which converts the integrated value obtained from the integrating circuit 32 into the digital data, a zero-crossing detector 34 which detects the zero-crossing points of the output servo burst signal of the AGC amplifier 7 and an integration control circuit 35 which counts the zero-crossing points detected by the zero-crossing detector 34 and controls the integrating circuit 32 so that the integrating circuit 32 holds the integrated value when the count becomes a previously set count value.
FIG. 6 shows a block diagram of the integrating circuit in the related art.
The integrating circuit 32 includes a capacitor Cap which stores the servo burst signal which has undergone the full-wave rectification in the full-wave rectifier 31 and a holding circuit 36 which holds the charged voltage stored in the capacitor Cap.
The CPU 10 and the integration control circuit 35 are connected to the holding circuit 36, and the holding circuit 36 discharges the charged voltage held in the capacitor Cap and holds the charged voltage of the capacitor Cap. In response to a start control signal from the CPU 10, the holding circuit 36 discharges the capacitor Cap and charges the servo burst signal in the capacitor Cap.
The start control signal from the CPU 10 is also supplied to the integration control circuit 35 and resetting of the zero-crossing point count value is performed. The integration control circuit 35 is reset by the start control signal from the CPU 10, counting is started, and the integration control circuit 35 causes the holding circuit 36 to hold the charged voltage of the capacitor Cap when the count becomes the predetermined count value.
FIGS. 7A, 7B and 7C show an operation explanation drawing. FIG. 7A shows the servo burst signal, FIG. 7B shows the zero-crossing count value and FIG. 7C shows the charged voltage of the capacitor Cap.
When the start control signal is output from the CPU 10 at the time t0, the capacitor Cap is discharged, the charged voltage of the capacitor Cap becomes zero as shown in FIG. 7C, the integration control circuit 35 is reset as shown in FIG. 7B and the zero-crossing point-count value of the servo burst signal is caused to be zero.
Then, when the servo burst signal passes the zero-crossing point at the time t1 as shown in FIG. 7A, the count value of the integration control circuit 35 is incremented and becomes `1`. Similarly, at the times from t2 through t10, the servo burst signal crosses zero, and the count value of the integration control circuit 35 is incremented. During the time, the capacitor Cap is charged with the signal obtained from performing full-wave rectification on the servo burst signal shown in FIG. 7A, and the charged voltage thereof increases as shown in FIG. 7C.
When the count value of the integration control circuit 35 becomes the predetermined count value `10` at the time t10, the integration control circuit 35 controls the holding circuit 36 so that the charging of the capacitor Cap is stopped. Further, the integration control circuit 35 causes the holding circuit 36 to hold the charged voltage of this time. The charged voltage V1 held in the holding circuit 36 is converted into the digital data by the A/D converter 33 and is supplied to the CPU 10.
In accordance with the difference between the integrated values of the servo burst signal S1 and the servo burst signal S2, the CPU 10 generates an error signal for controlling the position of the magnetic head 3 so that the magnetic head 3 scans the center of the desired cylinder 21-1.
However, in the servo detecting circuit, using the area servo method, of the magnetic disk device in the related art, when noises occur around the zero-crossing point of the servo burst signal as indicated by broken lines around the times t11, t5 and t12 of FIG. 7A, the noises are counted as the zero-crossing points as indicated by (5) and (7) in FIG. 7B, the peak number of the burst signal to be integrated increases and the count value of the integration control circuit becomes `10` at the time t8. Accordingly, although the integration by the capacitor Cap should be stopped at the time t10, the integration is stopped at the time t8. As a result, the integrated value V2, of the integration period shorter by the time (t10-t8) than that of the integrated value V1 of the normal case, is detected.
Thus, due to the noises, variation occurs in the integrated value of the servo burst signal, the accurate on-track condition cannot be detected, the head cannot be positioned accurately, and so forth. Thus, a problem occurs.
Further, in the servo circuit, using the area servo method, of the magnetic disk device in the related art, the capacitance for charging the servo burst signal is fixed. The waveforms of the read servo burst signals are different between the case of the position of the magnetic head being on the inner side of the magnetic disk and the case of the position of the magnetic head being on the outer side of the magnetic disk.
FIG. 8 shows waveforms of the servo burst signals of the inner side and outer side of the magnetic disk.
In FIG. 8, the solid line indicates the waveform of the servo burst signal of the inner side and the broken line indicates the waveform of the servo burst signal of the outer side.
Because recording density of the magnetic disk is different between the inner side and outer side of the magnetic disk, a difference occurs in the half-value widths W 50 of the reproduced servo burst signals. When recording density is maximum in the inner side, the half-value width W 50 of the servo burst signal in the outer side decreases and the waveform is distorted as indicated by the broken line in the figure.
Accordingly, in the outer side of the magnetic disk, the integrated value of the servo burst signal is smaller than that of the inner side by the amount indicated by the broken-line hatching in FIG. 8. When the integrated value of the servo burst signal becomes smaller, change of the integrated value for the position of the magnetic head becomes smaller. Thereby, the difference of the integrated value of the burst signal for the change amount becomes smaller and sensitivity for position shift of the magnetic head is lowered. As a result, head positioning cannot be performed accurately and so forth. Thus, a problem occurs.
SUMMARY OF THE INVENTION
The present invention has been devised in consideration of the above-mentioned problems. An object of the present invention is to provide a head position detecting method and a disk device in which, by accurately detecting the servo burst signal, head positioning can be accurately performed.
A first head position detecting method according to the present invention is a method in which a servo signal previously written on a disk is read through a head, the servo signal read through the head is integrated for a predetermined number of zero-crossing points of the servo signal, and, based on information obtained from the integration, the position of the head on the disk is detected,
wherein the servo signal is detected, a noise component which varies the servo signal across the zero-crossing point of the servo signal is removed, and a period of the integration is determined as a result of counting the zero-crossing points of the servo signal from which the noise component has been removed.
In this method, the servo signal is detected, a noise component which varies the servo signal across the zero-crossing point of the servo signal is removed, and the zero-crossing points are detected by counting the zero-crossing points of the servo signal from which the noise component has been removed. Thereby, noises are prevented from being counted as the zero-crossing points. Accordingly, the servo signal integration period can be precisely detected, and thereby, the position of the head on the disk can be precisely detected.
A second head position detecting method according to the present invention is a method in which a servo signal previously written on a disk is read through a head, the servo signal read through the head is integrated for a predetermined number of zero-crossing points of the servo signal, and, based on information obtained from the integration, the position of the head on the disk is detected,
wherein:
the zero-crossing points of the servo signal are detected, the zero-crossing points are counted, and the time since the detection of the zero-crossing points of the servo signal was started is measured; and
when the measured time has reached or exceeded a predetermined time which is shorter than a time from a time at which count of the zero-crossing points of the servo signal was started to a time at which the count reaches a predetermined count value, and also, when the number of the detected zero-crossing points has reached the predetermined count value, the servo signal integration operation is stopped.
In this method, even if noises in the servo signal are counted as the zero-crossing points and the count value has reached the predetermined count value within the predetermined time, stopping of the integration is not allowed until the predetermined time elapses. Accordingly, the integrated value which is less than is necessary is prevented from being detected. Thereby, influence of noises or the like can be reduced and the position of the head on the disk can be precisely detected.
A third head position detecting method according to the present invention is a method in which a servo signal previously written on a disk is read through a head, the servo signal read through the head is integrated for a predetermined number of zero-crossing points of the servo signal, and, based on information obtained from the integration, the position of the head on the disk is detected,
wherein:
the zero-crossing points of the servo signal are detected, the zero-crossing points are counted, and the time since the detection of the zero-crossing points of the servo signal was started is measured; and
when the measured time has reached a predetermined time which is longer than a time from a time at which count of the zero-crossing points of the servo signal was started to a time at which the count reaches a predetermined count value, the servo signal integration operation is stopped.
In this method, even if the zero-crossing points are not counted due to erroneous counting and the integration is not stopped although it is the time the integration should be stopped, the integration is stopped when the predetermined time, which is longer than the time at which the count value reaches the predetermined value, elapses. Accordingly, the integrated value which is more than is necessary is prevented from being detected. Thereby, influence of erroneous counting or the like can be reduced and the position of the head on the disk can be precisely detected.
A fourth head position detecting method is a method in which a servo signal previously written on a disk is read through a head, and, based on information obtained from integrating the servo signal read through the head, the position of the head on the disk is detected,
wherein, in accordance with a position at which the head detects the servo signal on the disk, integration sensitivity is controlled so that the inclination of the servo signal integrated value is fixed.
In this method, the integration sensitivity is controlled in accordance with a position of the head on the disk so that the inclination of the integrated value of the servo signal is fixed. Thereby, in a case of a hard disk drive where the half-value widths W 50 of the servo signals detected through the head vary between an inner portion and an outer portion of the disk, the integrated values thereof can be approximately fixed. Accordingly, control sensitivity can be fixed between the inner portion and the outer portion of the disk.
A fifth head position detecting method is a method in which a noise component which varies the servo signal across the zero-crossing point of the detected servo signal is removed, and the position of the head is detected as a result of integrating the servo signal from which the noise component was removed. This method also includes the features of the above-described second and third head position detecting methods.
In this method, the servo signal is detected, a noise component which varies the servo signal across the zero-crossing point of the servo signal is removed, and the zero-crossing points are detected by counting the zero-crossing points of the servo signal from which the noise component has been removed. Thereby, noises are prevented from being counted as the zero-crossing points. Accordingly, the servo signal integration period can be precisely detected, and thereby, the position of the head on the disk can be precisely detected. Further, even if noises cannot be sufficiently removed and the count value has reached the predetermined count value within the predetermined time, stopping of the integration is not allowed until the predetermined time elapses. Accordingly, the integrated value which is less than is necessary is prevented from being detected. Thereby, influence of noises or the like can be reduced and the position of the head on the disk can be precisely detected. Further, even if the zero-crossing points are not counted due to erroneous counting and the integration is not stopped although it is the time the integration should be stopped, the integration is stopped when the predetermined time, which is longer than the time at which the count value reaches the predetermined value, elapses. Accordingly, the integrated value which is more than is necessary is prevented from being detected. Thereby, influence of erroneous counting or the like can be reduced and the position of the head on the disk can be precisely detected.
A sixth head position detecting method is a method in which, when the servo signal read through the head is integrated, in accordance with a position at which the head detects the servo signal on the disk, integration sensitivity is controlled so that the inclination of the servo signal integrated value is fixed.
In this method, the integration sensitivity is controlled in accordance with a position of the head on the disk so that the inclination of the integrated value of the servo signal is fixed. Thereby, in a case of a hard disk drive where the half-value widths W 50 of the servo signals detected through the head vary between an inner portion and an outer portion of the disk, the integrated values thereof can be approximately fixed. Accordingly, control sensitivity can be fixed between the inner portion and the outer portion of the disk.
A first disk device is a device comprising: signal detecting means for detecting a signal previously written on a disk; a zero-crossing counter for counting zero-crossing points of a servo signal, of the signal detected by the signal detecting means, by which the position of the head is detected; an integrating circuit for integrating the servo signal until the count value of the zero-crossing counter reaches a predetermined count value; and control means for controlling the position of the head on the disk based on the integrated value integrated by the integrating circuit,
wherein the disk device further comprises a filter, provided between the signal detecting means and the zero-crossing counter, for removing a noise component, which varies across the zero-crossing point, from the servo signal supplied by the signal detecting means, and supplying the resulting signal to the zero-crossing counter.
In this device, a noise component which varies the servo signal across the zero-crossing point of the servo signal is removed by the filter, and the zero-crossing points are detected by counting the zero-crossing points of the servo signal from which the noise component has been removed. Thereby, noises are prevented from being counted as the zero-crossing points. Accordingly, the servo signal integration period can be precisely detected, and thereby, the position of the head on the disk can be precisely detected.
A second disk device is a device comprising: signal detecting means for detecting a signal previously written on a disk; a zero-crossing counter for counting zero-crossing points of a servo signal, of the signal detected by the signal detecting means, by which the position of the head is detected; an integrating circuit for integrating the servo signal until the count value of the zero-crossing counter reaches a predetermined count value; and control means for controlling the position of the head on the disk based on the integrated value integrated by the integrating circuit,
wherein the disk device further comprises:
time measuring means for measuring a time since counting of the zero-crossing counter was started; and
integration stopping control means for stopping the servo signal integration operation when the measured time of the time measuring means has reached or exceeded a predetermined time which is shorter than a time from a time at which count of the zero-crossing points of the servo signal was started to a time at which the count reaches a predetermined count value, and also, when the number of the detected zero-crossing points has reached the predetermined count value.
In this device, the integration stopping control means stops the integration operation of the integrating circuit when the measured time of the time measuring means becomes the predetermined time which is close to the time at which the count value of the zero-crossing points of the servo signal becomes the predetermined count value, and also, when the count value of the zero-crossing counter becomes the predetermined count value. Thereby, even if noises of the servo signal are counted as the zero-crossing points and the count value has reached the predetermined count value within the predetermined time, stopping of the integration is not allowed until the predetermined time elapses. Accordingly, the integrated value which is less than is necessary is prevented from being detected. Thereby, influence of noises or the like can be reduced and the position of the head on the disk can be precisely detected.
A third disk device is a device comprising: signal detecting means for detecting a signal previously written on a disk; a zero-crossing counter for counting zero-crossing points of a servo signal, of the signal detected by the signal detecting means, by which the position of the head is detected; an integrating circuit for integrating the servo signal until the count value of the zero-crossing counter reaches a predetermined count value; and control means for controlling the position of the head on the disk based on the integrated value integrated by the integrating circuit,
wherein the disk device further comprises:
time measuring means for measuring a time since counting of the zero-crossing counter was started; and
integration stopping control means for stopping the servo signal integration operation when the measured time has reached a predetermined time which is longer than a time from a time at which count of the zero-crossing points of the servo signal was started to a time at which the count reaches a predetermined count value.
In this device, the integration stopping control means stops the servo signal integration operation when the measured time has reached the predetermined time which is longer than the time from the time at which count of the zero-crossing points of the servo signal was started to the time at which the count reaches the predetermined count value. Thereby, even if the zero-crossing points are not counted due to erroneous counting and the integration is not stopped although it is the time the integration should be stopped, the integration is stopped when the predetermined time, which is longer than the time at which the count value reaches the predetermined value, elapses. Accordingly, the integrated value which is more than is necessary is prevented from being detected. Thereby, influence of erroneous counting or the like can be reduced and the position of the head on the disk can be precisely detected.
A fourth disk device is a device obtained from modifying the above-described second or third disk device, further comprising a filter, provided between the signal detecting means and the zero-crossing counter, for removing a noise component, which varies across the zero-crossing point, from the servo signal supplied by the signal detecting means, and supplying the resulting signal to the zero-crossing counter.
In this device, a noise component which varies across the zero-crossing point of the servo signal is removed by the filter. Thereby, noises are prevented from being counted as the zero-crossing points. Accordingly, the servo signal integration period can be precisely detected, and thereby, the position of the head on the disk can be precisely detected.
A fifth disk device is a device comprising: signal detecting means for detecting a signal previously written on a disk; a zero-crossing counter for counting zero-crossing points of a servo signal, of the signal detected by the signal detecting means, by which the position of the head is detected; an integrating circuit for integrating the servo signal until the count value of the zero-crossing counter reaches a predetermined count value; and control means for controlling the position of the head on the disk based on the integrated value integrated by the integrating circuit,
wherein the disk device further comprises integration sensitivity control means for controlling integration sensitivity so that the inclination of the servo signal integrated value is fixed, in accordance with a position at which the head detects the servo signal on the disk.
In this device, the integration sensitivity is controlled in accordance with a position of the head on the disk so that the inclination of the integrated value of the servo signal is fixed. Thereby, in a case of a hard disk drive where the half-value widths W 50 of the servo signals detected through the head vary between an inner portion and an outer portion of the disk, the integrated values thereof can be approximately fixed. Accordingly, control sensitivity can be fixed between the inner portion and the outer portion of the disk.
A sixth disk device is the device including the features of the above-described first, second, third and fourth disk devices, in which the disk device further comprises integration sensitivity control means for controlling integration sensitivity so that the inclination of the servo signal integrated value is fixed, in accordance with a position at which the head detects the servo signal on the disk.
In this device, in addition to reducing influence of noises and erroneous counting, head positioning precision can be uniform between an inner portion and an outer portion of the disk.
A seventh disk device is a device obtained from modifying the above-described fifth or sixth disk device, in which:
the integrating circuit comprises charge storing means which is charged with the servo signal; and
the integration sensitivity control means controls capacitance of the charge storing means in accordance with a position at which the head detects the servo signal on the disk.
In this device, the inclination of the integrated value of the servo signal is fixed as a result of controlling the capacitance of the charge storing means in accordance with a position of the head on the disk. Thereby, head positioning precision can be uniform between an inner portion and an outer portion of the disk.
An eighth disk device is a device obtained from modifying the above-described seventh disk device, in which:
the charge storing means comprises a plurality of capacitors having different capacitances; and
the integration sensitivity control means performs switching of connection of the plurality of capacitors, in accordance with a position at which the head detects the servo signal on the disk, so as to control the capacitance of the charge storing means.
In this device, the charge storing means includes the plurality of capacitors having different capacitances, and a desired capacitance can be selected by switching connection of the plurality of capacitors in accordance with the servo signal detected position. Thereby, the inclination of the integrated value of the servo signal can be fixed. Thereby, head positioning precision can be uniform between an inner portion and an outer portion of the disk.
A ninth disk device is a device obtained from modifying the above-described fourth, fifth, sixth or seventh disk device, in which:
the integrating circuit comprises a capacitor which is charged with a charging current; and
the integration sensitivity control means controls the charging current of the capacitor in accordance with a position at which the head detects the servo signal on the disk.
In this device, the inclination of the integrated value of the servo signal can be fixed by controlling the charging current of the capacitor in accordance with a position at which the head detects the servo signal on the disk. Accordingly, head positioning precision can be uniform between an inner portion and an outer portion of the disk.
A tenth disk device is a disk device obtained from modifying the above-described ninth disk device, in which the integration sensitivity control means generates the charging current in accordance with the servo signal and supplies the charging current to the capacitor, and comprises a charging pump circuit for controlling the charging current in accordance with a position at which the head detects the servo signal on the disk.
In this device, the inclination of the integrated value of the servo signal can be fixed as a result of controlling the gain of the charging current with respect to the servo signal in the charging pump circuit. Accordingly, head positioning precision can be uniform between an inner portion and an outer portion of the disk.
Other objects and further features of the present invention will become more apparent from the following detailed description when read in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a block diagram of one example of a magnetic disk device in the related art;
FIGS. 2A and 2B show a data format of a magnetic disk;
FIG. 3 shows a data format of a servo portion of the magnetic disk;
FIG. 4 shows a waveform of a reproduced signal when servo burst signals are reproduced through a magnetic head;
FIG. 5 shows a block diagram of one example of a servo detecting portion in the related art;
FIG. 6 shows a block diagram of one example of an integrating circuit in the related art;
FIGS. 7A, 7B and 7C show an operation explanation drawing of the servo detecting portion in the related art;
FIG. 8 shows waveforms of the servo burst signals of an inner side and an outer side of the magnetic disk;
FIG. 9 shows a block diagram of one embodiment of the present invention;
FIG. 10 shows a block diagram of a servo detecting portion in the embodiment of the present invention;
FIG. 11 shows a block diagram of an integrating circuit in the embodiment of the present invention;
FIG. 12 shows a flowchart of capacitor switching processing of a CPU in the embodiment of the present invention;
FIG. 13 shows a block diagram of a variant example of the integrating circuit in the embodiment of the present invention;
FIG. 14 shows a flowchart of charging current control processing of the CPU when the integrating circuit in the variant example of the embodiment of the present invention is used;
FIG. 15 shows a flowchart of the servo processing of the CPU in the embodiment of the present invention;
FIGS. 16A, 16B and 16C show an operation explanation drawing of a timer circuit in the embodiment of the present invention; and
FIGS. 17A, 17B and 17C show an operation explanation drawing of a variant example of the timer circuit in the embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 9 shows a block diagram of one embodiment of the present invention. In the figure, the same reference numerals are given to the parts the same as those of FIG. 1, and descriptions thereof will be omitted.
The embodiment is obtained as a result of applying a servo signal detecting method according to the present invention to a hard disk drive (HDD).
A servo detecting portion 101 of a hard disk drive 100 in the embodiment is a circuit which detects the integrated values of the servo burst signals and generates a tracking error signal from the difference of the servo burst signals. The servo detecting portion 101 removes high-frequency noises, which affect the detection of zero-crossing points, from the servo burst signals, and limits the period of the servo burst signal so as to prevent erroneous detection of the servo burst signal.
FIG. 10 shows a block diagram of the servo detecting portion 101 in the embodiment of the present invention. In the figure, the same reference numerals are given to the parts the same as those of FIG. 5, and descriptions thereof will be omitted.
The output signal of the AGC amplifier is supplied to the servo detecting portion 101 of the embodiment. In the servo detecting portion 101, the output signal of the AGC amplifier 7 is supplied to a low-pass filter 111 for removing the noises.
Assuming that the frequency of the servo burst signal is approximately from 7 through 8 MHz, the characteristic of the low-pass filter 111 is set so as not to pass the signals of frequencies equal to or higher than 20 MHz which is on the order of double the frequency of the servo burst signal. By this low-pass filter 111, the waveform of the servo burst signal is not distorted, the noise components are removed, and the servo burst signal is supplied to the zero-crossing detector 34. Accordingly, it is prevented that the zero-crossing detector 34 erroneously detects the noise components as zero-crossing points.
The signal from which the noise components have been removed by the low-pass filter 111 is supplied to the full-wave rectifier 31 and the zero-crossing detector 34. The full-wave rectifier 31 performs full-wave rectification on the signal supplied by the low-pass filter 111. The zero-crossing detector 34 detects zero-crossing points of the signal supplied by the low-pass filter 111. The signal which has undergone the full-wave rectification is supplied to an integrating circuit 112. The integrating circuit 112 causes the signal having undergone the full-wave rectification to change a capacitor, and thereby detects the integrated value of the servo burst signal. The integrated value is converted into digital data by the A/D converter 33, and then the digital data is supplied to a CPU 102.
The details of the integrating circuit 112 will now be described with reference to a figure.
FIG. 11 shows a block diagram of the integrating circuit in the embodiment of the present invention.
The integrating circuit 112 in the embodiment includes two capacitors C1 and C2 having different capacitances, a switching circuit 121 which selects the capacitor to be charged between the capacitors C1 and C2, and a holding circuit 122 which holds the charged voltage of the capacitor selected by the switching circuit 121.
The capacitance of the capacitor C1 is set to be larger than that of the capacitor C2, the capacitor C1 being selected when the position of the magnetic head 3 is on an inner side of a predetermined position of the magnetic disk 2. The capacitance of the capacitor C2 is set to be smaller than that of the capacitor C1, the capacitor C2 being selected when the position of the magnetic head 3 is on an outer side of the predetermined position of the magnetic disk 2.
A switching control signal is supplied to the switching circuit 121 from the CPU 102. In accordance with the switching control signal supplied from the CPU 102, the connection of the switching circuit 121 is changed between the capacitors C1 and C2.
The CPU 102 generates the switching control signal by capacitance switching processing performed in accordance with a cylinder number detection result.
FIG. 12 shows a flowchart of the capacitance switching processing of the CPU of the embodiment of the present invention.
The CPU 102 monitors the signal from the signal detecting portion 8, and, when detecting a servo portion reading shown in the figure, performs the capacitance switching processing. The CPU 102 recognizes cylinder number information Sa supplied by the signal detecting portion 8 (in steps S1-1, S1-2).
When recognizing the cylinder number information Sa in the step S1-2, the CPU 102 compares the recognized cylinder number information Sa with a previously set boundary cylinder number S0 which divides the outer side and the inner side of the magnetic disk 2 (in a step S1-3).
When the recognized cylinder number Sa is smaller than the boundary cylinder number S0 in the step S1-3, the CPU 102 determines that the magnetic head 2 is located on the inner side of the magnetic disk 2, and generates the switching control signal which controls the switching circuit 121 so that the capacitor C1 is connected (in a step S1-4).
When the recognized cylinder number Sa is larger than the boundary cylinder number S0 in the step S1-3, the CPU 102 determines that the magnetic head 2 is located on the outer side of the magnetic disk 2, and generates the switching control signal which controls the switching circuit 121 so that the capacitor C2 is connected (in a step S1-5).
Thus, by the capacitance switching processing by the CPU 102, it is determined whether the magnetic head 3 is currently present on the inner side or the outer side of the magnetic disk 2, in accordance with the cylinder number information stored in the servo portion of the magnetic disk 2 which the magnetic head 3 currently scans. Then, the switching control signal in accordance with the position of the magnetic head 3 is supplied to the switching circuit 121. In accordance with the switching control signal from the CPU 102, the switching circuit selects either the large-capacitance capacitor C1 or the small-capacitance capacitor C2.
Thus, when the magnetic head 3 is located on the inner side of the magnetic disk 2, the large-capacitance capacitor C1 is connected, and when the magnetic head 3 is located on the outer side of the magnetic disk 2, the small-capacitance capacitor C2 is connected.
Thereby, for the inner side of the magnetic disk in which the half-value width of the reproduced signal by the magnetic head 3 is large as shown in FIG. 8, the servo burst signal charges the capacitor C1 which has the capacitance larger than that for the outer side, and the integrated value is obtained. For the outer side of the magnetic disk 2 in which the half-value width of the reproduced signal by the magnetic head 3 is small as shown in FIG. 8, the servo burst signal charges the capacitor C2 which has the capacitance smaller than that for the inner side, and the integrated value is obtained. Accordingly, by performing setting so that no difference occurs between the integrated values for the inner side and outer side of the magnetic disk 2, it is possible that the position control sensitivities for the inner side and outer side of the magnetic disk 2 are approximately equal. Thereby, through the entire surface of the magnetic disk 2, the magnetic head 3 position control sensitivity can be fixed.
In the above-described integrating circuit 112, the inclination of the integrated value is fixed independent of the inner side and outer side of the magnetic disk by the switching of the capacitors C1 and C2 of the different capacitances. However, it can also be considered that the integrated value is fixed by changing charging current in accordance with the position of the magnetic head 3 on the magnetic disk 2 with a capacitor of a fixed capacitance.
FIG. 13 shows a block diagram of a variant example of the integrating circuit in the embodiment of the present invention. In the figure, the same reference numerals are given to the parts the same as those of FIG. 11, and descriptions thereof will be omitted.
In the integrating circuit 123 in the variant example, the capacitance of a capacitor C0 is fixed, and the current in accordance with the output signal of the full-wave rectifier is supplied to the capacitor C0 by a charging pump circuit 124. The output current gain of the charging pump circuit 124 for the output signal of the full-wave rectifier 31 changes in accordance with instruction information from the CPU 102. The instruction information of the CPU 102 is converted into an analog signal by a DA converter 125 and is supplied to the charging pump circuit 124.
FIG. 14 shows a flowchart of charging current control processing of the CPU when the integrating circuit in the variant example of the embodiment of the present invention is used.
The CPU 102 monitors the signal from the signal detecting portion 8, and, when detecting the servo portion reading shown in the figure, performs the charging current control processing. The CPU 102 recognizes cylinder number information Sa supplied by the signal detecting portion 8 (in steps S2-1, S2-2).
When recognizing the cylinder number information Sa in the step S2-2, the CPU 102 reads charging current information which was previously set inside and supplies it to the D/A converter (in a step 2-3).
The charging current information was set in accordance with the half-value width W 50 of the reproduced signal of the servo burst portion, and was set so that a charging current supplied to the capacitor C0 from the charging pump circuit 124 is larger for a magnetic disk inner-side cylinder number.
The D/A converter 125 converts the charging current information supplied from the CPU 102 into the analog signal and supplies it to the charging pump circuit 124.
The charging pump circuit 124 amplifies the output signal of the full-wave rectifier with the gain which is in accordance with the charging current information from the CPU 102, and supplies the thus-obtained charging current to the capacitor CO.
Thus, the inclination of the integrated value of the servo burst portion can be fixed independent of the position of the magnetic head 3 on the magnetic disk 2. Thereby, it is possible that the position control sensitivities for the inner side and outer side of the magnetic disk 2 can be approximately equal. Accordingly, through the entire surface of the magnetic disk 2, the magnetic head 3 position control sensitivity can be fixed.
The integrated values of the servo burst signals detected by the integrating circuits 112, 123 shown in FIG. 11, FIG. 13 are supplied to the A/D converter 33.
The A/D converter 33 converts the analog integrated value, detected by the integrating circuit 112, into the digital data, and supplies it to the CPU 102.
The CPU 102 controls the position of the magnetic head 3 with respect to the magnetic disk 2 and thus performs servo processing based on the digital information supplied from the A/D converter 125.
FIG. 15 shows a flowchart of the servo processing of the CPU in the embodiment of the present invention.
In the servo processing, the CPU 102 obtains from the A/D converter 33 the digital information corresponding to the integrated value of the first servo burst signal S1 shown in FIG. 3, and holds it (in a step S3-1).
The CPU 102 then obtains from the A/D converter 33 the digital information corresponding to the integrated value of the second servo burst signal S2, arranged subsequent to the first servo burst signal S1, shown in FIG. 3, and holds it (in a step S32).
The CPU 102 detects the difference between the integrated value of the first servo burst signal S1 obtained and held in the step S2-1 and the integrated value of the second servo burst signal S2 obtained and held in the step S2-2, and produces a head position control signal in accordance with the difference between the integrated value of the first servo burst signal S1 and the integrated value of the second servo burst signal S2 (in steps S3-3, S3-4).
The CPU 102 supplies the head position control signal, produced in the step S304, to the D/A converter 11, and finishes the servo processing (in S3-5).
The D/A converter 11 converts the head position control signal, supplied from the CPU 102, into an analog signal, and supplies it to the driver 12 which drives the actuator 5. In accordance with the head position control signal supplied from the D/A converter 11, the driver 12 corrects the driving signal which drives the actuator 5.
The driving signal, produced by the driver 12, is supplied to the actuator 5. The actuator 5 rotates in accordance with the driving signal supplied from the driver 12, and moves the magnetic head 3 in the inner and outer directions of the magnetic disk 2.
Thus, the first and second servo burst signals S1, S2, which are arranged in the boundary portions between the cylinder which the magnetic head 3 currently scans and the adjacent cylinders, are detected. Then, in accordance with the difference between the integrated values thereof, the magnetic head 3 is controlled so that the difference between the integrated values of the first and second servo burst signals S1, S2 becomes zero. That is, the magnetic head 3 is controlled so that the magnetic head 3 scans the center line of the desired cylinder.
Returning to FIG. 10, a zero-crossing counter 113 and a timer circuit 114 will now be described.
In the servo detecting portion 101, the output signal of the low-pass filter 111 is supplied to the integrating circuit 112 through the full-wave rectifier 31, is integrated, and also is supplied to the zero-crossing detector 34 and is used for controlling the integrating period of the integrating circuit 112.
The zero-crossing detector 34 detects the zero-crossing points of the signal supplied from the low-pass filter 111, and generates a one-shot pulse at the zero-crossing point.
The one-shot pulse generated at the zero-crossing point is supplied to the zero-crossing counter 113. The zero-crossing counter 113 counts the one-shot pulses, generated at the zero-crossing points, supplied from the zero-crossing detector 34. At this time, the zero-crossing counter is reset by the start control signal supplied from the CPU 102 and raises an output signal level to a high level.
When the count value has reached a previously set predetermined count value, the zero-crossing counter 113 inverts the output signal level to a low level.
The count value of the zero-crossing counter 113 is supplied to the timer circuit 114. The start control signal, which is the same as that supplied to the zero-crossing counter 113, is supplied to the timer circuit 114 from the CPU 102. The timer circuit 114 is reset in synchronization with the zero-crossing counter 113 by the start control signal, and performs time measurement of a predetermined time. The timer circuit 114 allows outputting of the output signal of the zero-crossing counter 113 after the predetermined time has elapsed.
FIGS. 16A, 16B and 16C show an operation explanation drawing of the timer circuit in the embodiment of the present invention. FIG. 16A shows the reproduced signal waveform of the servo burst portion which has undergone full-wave rectification of the full-wave rectifier 31. FIG. 16B shows the charged voltage waveform of the capacitor C1 or C2. FIG. 16C shows the output signal waveform of the timer circuit 114.
When the servo burst portion is detected at the time t1, the start control signal is supplied from the CPU 102 to the holding circuit 122, zero-crossing counter 113 and timer circuit 114. In response to the start control signal, the holding circuit 122 discharges the capacitor C1 or C2, and also, resets the held integrated value. Thereby, the charged voltage of the capacitor C1 or C2 is `0` as shown in FIG. 16B.
Then, when the signal, obtained from performing full-wave rectification on the reproduced signal of the servo burst portion, is supplied to the integrating circuit 112 from the full-wave rectifier 31, as shown in FIG. 16A, the capacitor C1 or C2 of the integrating circuit 112 is charged by the output signal of the full-wave rectifier 31. Thereby, as shown in FIG. 16B, the capacitor C1 or C2 is gradually charged by the reproduced signal of the servo burst portion.
The zero-crossing counter 113 is reset at the time t1 in response to the start control signal from the CPU 102, and the output signal level is caused to be the high level. Then, the zero-crossing counter 113 counts the zero-crossing points, of the reproduced signal of the servo burst portion, detected by the zero-crossing detector 34. After counting the zero-crossing points to a predetermined number, for example, `10`, the zero-crossing counter 113 inverts the output signal level from the high level to the low level.
The timer circuit 114 is reset at the time t1 in response to the start control signal from the CPU 102, and measures time until the time t2 which is the time after a predetermined time T0 has elapsed. After the predetermined time T0 has elapsed, the timer circuit 114 allows outputting of the output signal of the zero-crossing counter 113. The predetermined time T0 is set to be the time which is shorter than the time which is required for the count value to become the predetermined number when the zero-crossing points are counted in the normal case.
Thereby, even if the zero-crossing points have reached the predetermined count value at the time t3 and the output signal level of the zero-crossing counter 113 becomes the low level, because the time measurement of the timer circuit 114 has not measured the predetermined time T0 from the time t1, the output signal level supplied to the integrating circuit 112 from the timer circuit 114 is maintained at the high level. At the time t2 after the measured time of the timer circuit 114 has reached the predetermined time measurement time T0, the output signal level is caused to be the low level.
Further, after the measured time of the timer 114 since the reproduced signal of the servo burst portion was supplied has reached the predetermined time T0, the output signal of the zero-crossing counter 113 is supplied to the integrating circuit 112. At this time, when the count value of the zero-crossing counter 113 has not reached the predetermined count value, the level of the output signal of the zero-crossing counter 113 is the high level and thus the signal supplied to the integrating circuit 112 is the high level.
When the count value of the zero-crossing points of the zero-crossing counter 113 has reached the predetermined count value at the time t4, the level of the output signal of the zero-crossing counter 113 is inverted into the low level. Accordingly, at the time t4, the signal supplied to the integrating circuit 112 is inverted into the low level.
The output signal from the timer circuit 114 is supplied to the holding circuit 122 of the integrating circuit 112. The holding circuit 122 of the integrating circuit 112 receives the charged voltage of the capacitor C1 or C2 and holds it when the level of the output signal from the timer circuit 114 is the high level. When the level of the output signal from the timer circuit 114 is the low level, the holding circuit 122 disconnects the connection with the capacitor C1 or C2 and holds the charged voltage when the output signal level has become the low level.
Thus, even if the count value of the zero-crossing points of the reproduced signal of the servo burst portion varies due to noises or the like and the zero-crossing points which should be counted are not counted, the charged voltage of the capacitor C1 or C2 of the integrating circuit 112 is held by the holding circuit 122 until the time reaches in the proximity of the time of the correct count value. As a result, the integrated value for approximately the servo burst portion can be detected.
When the zero-crossing points of the reproduced signal of the servo burst portion are correctly counted, the time measurement of the timer circuit 114 is finished immediately before the zero-crossing point of the correct count value. When the counting has been finished, the charged voltage of the capacitor C1 or C2 is held by the holding circuit 122. Accordingly, the integrated value of the servo burst portion can be accurately detected.
In the embodiment, the zero-crossing counter 113 manages the count value of the zero-crossing points to be counted, the timer circuit 114 manages the time at which the count value of the zero-crossing points of the reproduced signal of the servo burst portion should reach the predetermined count value, and the time of detecting the charged voltage of the capacitor C1 or C2 of the integrating circuit 112 is controlled. Thereby, the integrated value of the servo burst portion can be accurately detected, and thereby, scanning of the cylinder by the magnetic head 3 can be accurately performed.
In the embodiment, the timer circuit 114 performs control so that, after the predetermined time T0 has elapsed since the integration was started, the integrating circuit 112 is stopped by the output of the zero-crossing counter 113. Further, it can also be considered that integration finish time is set and excess integration due to erroneous counting of the like is prevented.
FIGS. 17A, 17B and 17C show an operation explanation drawing of a variant example of the timer circuit in the embodiment of the present invention. FIG. 17A shows the reproduced signal waveform of the servo burst portion which has undergone full-wave rectification of the full-wave rectifier 31. FIG. 17B shows the charged voltage waveform of the capacitor C1 or C2. FIG. 17C shows an output signal allowing waveform of the timer circuit 114.
When the servo burst portion is detected at the time t1, the start control signal is supplied from the CPU 102 to the holding circuit 122, zero-crossing counter 113 and timer circuit 114. In response to the start control signal, the holding circuit 122 discharges the capacitor C1 or C2 and resets the held integrated value. Thereby, the charged voltage of the capacitor C1 or C2 is `0` as shown in FIG. 17B.
Then, when the signal, obtained from performing full-wave rectification on the reproduced signal of the servo burst portion, is supplied to the integrating circuit 112 from the full-wave rectifier 31, as shown in FIG. 17A, the capacitor C1 or C2 of the integrating circuit 112 is charged by the output signal of the full-wave rectifier 31. Thereby, as shown in FIG. 17B, the capacitor C1 or C2 is gradually charged by the reproduced signal of the servo burst portion.
The zero-crossing counter 113 is reset at the time t1 in response to the start control signal from the CPU 102, and the output signal level is caused to be the high level. Then, the zero-crossing counter 113 counts the zero-crossing points, of the reproduced signal of the servo burst portion, detected by the zero-crossing detector 34. After counting the zero-crossing points to a predetermined number, for example, `10`, the zero-crossing counter 113 inverts the output signal level from the high level to the low level.
The timer circuit 114 is reset at the time t1 in response to the start control signal from the CPU 102, and starts time measurement. The timer circuit 114 maintains the level of the signal, which is supplied to the integrating circuit 112, to be the high level until the time t2 at which the measured time has reached a previously set first time T1, and maintains the same to be the low level after the time t3 at which the measured time has reached a previously set second time T2. Further, the timer circuit 114 allows supplying of the output signal of the zero-crossing counter 113 to the integrating circuit 112 during the time T0 from the time after the time T1 has elapsed to the time after the time T2 has elapsed since the timer circuit 114 was reset.
The first time T1 is set to a time which is shorter than the time which is required for the count value to reach the predetermined value when the zero-crossing points are counted in the normal case. The second time T2 is set to a time which is longer than the time which is required for the count value to reach the predetermined value when the zero-crossing points are counted in the normal case.
Accordingly, even if the count value of the zero-crossing points has reached the predetermined count value at the time t4 and the level of the output signal of the zero-crossing counter 113 becomes the low level, because the measured time of the timer circuit 114 from the time t1 has not reached the predetermined time T1, the level of the output signal supplied from the timer circuit 114 to the integrating circuit 112 is maintained to be the high level. At the time t2 at which the measured time of the timer circuit 114 has reached the time T1, the level of the output signal supplied from the timer circuit 114 to the integrating circuit 112 is caused to be the low level, and the integration operation of the integrating circuit 112 is stopped.
After the measured time of the timer circuit 114 since the reproduced signal of the servo burst portion was supplied has reached the first time T1, the output signal of the zero-crossing counter 113 is supplied to the integrating circuit 112. Therefore, when the count value of the zero-crossing points of the zero-crossing counter 113 has not reached the predetermined value, the level of the output signal of the zero-crossing counter 113 is the high level. Accordingly, the level of the signal supplied to the integrating circuit 112 is maintained to be the high level. When the count value of the zero-crossing points of the zero-crossing counter 113 has reached the predetermined count value at the time t5, the level of the output signal of the zero-crossing counter 113 is inverted into the low level. Accordingly, the level of the signal supplied to the integrating circuit 112 at the time t5 is inverted to the low level. Thereby, the integration operation of the integrating circuit 112 is stopped.
At the time t3 at which the measured time of the timer circuit 114 since the reproduced signal of the servo burst portion was supplied has reached the second time T2, the level of the signal supplied to the integrating circuit 112 is forcibly caused to be the low level independent of the output signal of the zero-crossing counter 113. Thereby, the integration operation of the integrating circuit 112 is stopped.
In the embodiment, when it is the time t3 at which the measured time of the timer circuit 114 has reached the second time T2, the level of the signal supplied to the integrating circuit 112 is forcibly caused to be the low level independent of the output signal of the zero-crossing counter 113. Thereby, the integration operation of the integrating circuit 112 is stopped. Accordingly, even if there are the zero-crossing points which are not counted by the zero-crossing counter 113 due to erroneous counting or the like, the integration operation of the integrating circuit 112 can be stopped when the measured time of the timer circuit 112 has reached the second time T2 at which the-count value of the zero-crossing points are considerably deviated from the previously set predetermined count value. Thereby, it is possible to prevent the integrating circuit 112 from performing more integration operation than is necessary. Accordingly, considerable deviation of the integrated value of the servo burst signal does not occur, and the precise servo operation can be performed.
The present invention is not limited to the above-described embodiment and variant examples, and variations and modifications may be made without departing from the scope of the present invention claimed in the following claims.
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A noise component is eliminated from a servo signal recorded on a recording medium and read by a head. A number of times that a noise eliminated servo signal crosses zero-cross points is counted in order to determine an integration period based on the number of times. The noise-eliminated servo signal is integrated for the integration period, an integrated value thus obtained indicating a position of the head.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
Trisodium carboxymethyloxysuccinate has recently been disclosed as a builder salt to enhance the cleaning power of detergent surfactants, and to replace detergent builder phosphates in cleaning compositions, as set forth in U.S. Pat. No. 3,692,685, assigned to the instant assignee, and incorporated herein by reference.
As explained in the aforesaid patent, the carboxymethyloxysuccinates are biodegradable and non-eutrophying and are excellent substitutes for the established detergent builder polyphosphates which are suspected of being a factor in the eutrophication of lakes, etc. However, the level of fabric detergency to which the consumer has become accustomed from the use of polyphosphate-built detergents is not quite reached in the overall use of trisodium carboxymethyloxy-succinate as a replacement for polyphosphates. Typical of the comparative efficacy are the results shown in a series of experiments designated as Examples 1-10 in the aforesaid U.S. Pat. No. 3,692,685. In this series the detergent effect of the trisodium carboxymethyloxysuccinate-built detergent compositions is shown to vary from 82 to 97% of the detergency of a comparative sodium tripolyphosphate-built detergent composition. The data also indicate that the detergency-enhancing effect of trisodium carboxymethyloxysuccinate is greater on some detergent species than on others.
Sodium citrate has also been suggested as a builder substitute for polyphosphates in detergent compositions. However, sodium citrate possesses the disadvantage that it reacts with sodium hypochlorite at pH levels below about 8.5 where significant amounts of the hypochlorous acid species are present. This disadvantage becomes evident in home laundering since in many instances wherein the soil on the fabric being washed is acidic, the pH of the wash solution drops below 8.5, causing the citrate to become reactive towards any hypochlorite bleach that may be added and thereby, impairing the bleaching efficiency and detergency of the washing operation.
Carboxymethyloxysuccinic acid and its salts, on the other hand, are stable towards hypochlorite in both acidic and alkaline solution and, for this reason, the compositions of the present invention are useful for cleaning fabrics and, particularly in acidic media, for the cleaning and sanitizing of metal surfaces and other hard surfaces such as walls and floors.
2. Discussion of the Prior Art
Trisodium carboxymethyloxysuccinate, a method for its preparation, and its properties as a detergent builder are extensively discussed in U.S. Pat. No. 3,692,685. Example 11 of this patent discloses a dishwashing composition containing 43.0% trisodium carboxymethyloxysuccinate with 21.0% chlorinated trisodium phosphate.
Chlorinated compounds of the type referred to in the instant specification as chlorine-releasing agents, which liberate elemental chlorine under the conditions of use set forth herein, are well known in the detergent, bleaching and sanitizing arts. Disclosures of typical chlorine-releasing agents, preparative procedures, and uses in combination with certain detergents and additives may be found collectively in the following list of patents, which is by no means exhaustive.
______________________________________U.S. Pat. Nos. 1,555,474; 1,950,956; 1,965,304; 2,929,816; 3,035,054; 3,035,056; 3,035,057; 3,110,677; 3,112,274; 3,346,502.______________________________________
Chlorine-releasing agents are disclosed in the ACS Monograph entitled "Chlorine -- Its Manufacture, Properties and Uses" by Sconce, published by Reinhold in 1962.
Oxygen-releasing compounds are disclosed in the following patents.
______________________________________U.S. Pat. Nos. 2,706,178; 2,955,086; 3,075,921; 3,131,995.______________________________________
Activators for peroxy compounds are disclosed in the following patents.
______________________________________U.S. Pat. Nos. 2,955,905 3,177,148 3,211,658 3,245,913 3,398,096German Pat. No. 1,018,181French Pat. No. 1,199,123Great Britain Pat. No. 984,459Great Britain Pat. No. 1,025,791______________________________________
U.S. Pat. No. 3,306,858 discloses a method for incorporating a nonionic detergent and a chlorine-releasing agent together in the same detergent compositions. The method comprises absorbing the nonionic detergent on a particulate carrier, for example a polyphosphate, followed by coating with a sodium silicate solution. The coated particles are dried or further mixed with an inorganic salt to absorb excess moisture. Following the foregoing encapsulation procedure, the encapsulated particles are mixed with particles of a chlorine-releasing agent.
U.S. Pat. No. 3,717,580 discloses that excess hypochlorite remaining after a sanitizing procedure can be destroyed by contact with citric acid, a compound isomeric with carboxymethyloxysuccinic acid. While this is an advantage when hypochlorite is used on hard surfaces, it is a disadvantage when citrate is used as the detergent builder in the washing of fabrics and hypochlorite bleach is added to the wash, particularly since citric acid and hypochlorites are more reactive in solution if the pH is below about 8.
SUMMARY OF THE INVENTION
It has now been discovered that the fabric detergency of a trisodium carboxymethyloxysuccinate-built detergent composition can be made to equal or exceed that of a corresponding tripolyphosphate-built detergent composition by the inclusion therewith of a chlorine-releasing agent or an appropriately activated oxygen-releasing agent.
It has also been discovered that, contrary to the property of sodium citrate, a detergent builder isomeric with trisodium carboxymethyloxysuccinate, of reacting with sodium hypochlorite, particularly at pH 7, trisodium carboxymethyloxysuccinate is unreactive under the same conditions.
It is accordingly an object of the present invention to improve the detergency of a trisodium carboxymethyloxysuccinate-built detergent composition.
It is another object of the invention to provide a built detergent composition wherein the builder is non-eutrophying to overcome the disadvantage of polyphosphates, and is unreactive toward hypochlorites, to overcome the disadvantage of citrate builders.
It is a further object of the invention to provide a composition suitable for cleaning metal surfaces, such as food processing equipment, and other hard surfaces such as walls and floors, in acidic media.
The aforementioned improvement in detergency is accomplished by the inclusion of a chlorine-releasing agent or an oxygen-releasing agent with the carboxymethyloxysuccinate-built detergent composition as more fully described hereinbelow.
DETAILED DESCRIPTION OF THE INVENTION
As a first embodiment, the invention broadly contemplates a builder combination suitable for use in detergent compositions comprising a mixture of an alkali metal chlorine-releasing or oxygen-releasing compound and a polycarboxy salt having the general formula ##STR1##
Wherein M is hydrogen or an alkali metal, calcium or magnesium water-solubilizing cation, or mixtures thereof, and x is an integer having a value equal to the valence of M. A useful calcium salt has the formula ##STR2##
The term "alkali metal" includes sodium, potassium and lithium. The two first-named alkali-metal cations are preferred. In instances wherein stains or soils containing heavy metal compounds such as iron compounds are to be removed as part of the cleaning operation, the alkaline earth metal salts of carboxymethyloxysuccinic acid may advantageously be employed since these are prepared as precursors in the manufacture of the alkali metal salts of carboxymethyloxysuccinic acid and, moreover, readily exchange their alkaline earth metal cations for the heavy metal cations.
In a second embodiment, the invention provides a particulate or liquid detergent composition comprising a quaternary ammonium detergent or a substantially nitrogen-free anionic detergent, trisodium carboxymethyloxysuccinate, and a compound to release chlorine or oxygen as hereinafter defined.
In a third embodiment the invention contemplates solutions containing the aforementioned combination at concentrations normally used for washing fabrics in automatic machines. Usually such solutions will contain
i. about 200 ppm to about 2000 ppm of an anionic or a quaternary ammonium nonsoap surfactant having detergent properties, or mixtures thereof,
ii. about 50 ppm to about 300 ppm of a chlorine-releasing agent,
iii. about 200 ppm to about 2000 ppm of a polycarboxy salt having the general formula ##STR3## wherein M is hydrogen or an alkali metal, calcium or magnesium cation, and x is the valence of M, and
iv. water as essentially the balance of the formulation.
The structural formula set forth hereinabove includes a conventional representation of the cation portion of the molecule, although it will be understood that when the cation is calcium or magnesium, having a valence of 2, each calcium or magnesium cation may be associated with any two carboxyl groups on the same anion or with two carboxyl groups on different anions.
The compositions of the invention are useful under both acidic and alkaline conditions, specifically within the pH range of about 3 to about 12.
By the term "chlorine-releasing agent" as used herein is meant any inorganic or organic compound having chlorine in its molecule and which is capable of having its chlorine liberated as elemental chlorine to form hypochlorous acid or its salts under the conditions usually employed for detergent, bleaching or sanitizing purposes.
A non-limiting list of chlorine-releasing agents suitable for use in the present invention includes:
hypochlorous acid,
sodium hypochlorite,
lithium hypochlorite,
calcium hypochlorite,
chlorinated trisodium phosphate,
monochloramine
dichloramine,
sodium dichloroisocyanurate,
potassium dichloroisocyanurate,
dichlorocyanuric acid,
trichloroisocyanuric acid,
[(monotrichloro)-tetra(monopotassium dichloro)]pentaisocyanurate,
1,3-dichloro-5,5-dimethylhydantoin,
N,n'-dichlorobenzoyleneurea,
para-toluene sulfondichloramide,
N,n-dichloroazodicarbonamide,
trichloromelamine,
N-chloroammeline,
N-chlorosuccinimide,
N-chloroacetylurea,
N,n'-dichlorobiuret,
chlorinated dicyandiamide,
sodium salt of N-chloro-p-toluenesulfonamide.
By the term "oxygen-releasing agent" as used herein is meant any inorganic or organic peroxy compound capable of having its oxygen released as elemental oxygen or as hydrogen peroxide or its salts under the conditions usually employed for washing, bleaching or sanitizing. The oxygen-releasing agents may require an activator or promoter to aid in the release of oxygen, particularly when employed at the temperatures not substantially higher than those typically encountered in automatic washing machines, e.g., about 120° to about 140° F.
A non-limiting list of oxygen-releasing compounds suitable for use in the present invention includes:
sodium perborate,
sodium percarbonate (sodium carbonate peroxide)-2Na 2 CO 3 .3H 2 O 2 ,
sodium perborosilicate,
sodium dipersulfate,
diperisophthalic acid and salts thereof,
peroxybenzoic acid, and the 2-chloro, 3-chloro, 4-chloro, 3-methyl, 4-methyl, 2-nitro, 3-nitro,
4-nitro, 4-methoxy, 4-isopropyl, 4-tert-butyl,
4-cyano, and the 2,4-dichloro derivatives thereof, as disclosed in U.S. Pat. No. 3,075,921.
Activators for enhancing the bleaching action of water-soluble inorganic percompounds may be one wherein a transition element in the periodic system is added to a powdered carrier selected from the groups consisting of water-insoluble or hardly soluble compounds of Zn, Cd, Ca, Mg, Al, Sn, Be, Ti, Sb, Bi and SiO 2 .
The foregoing activators are disclosed in U.S. Pat. No. 3,398,096.
Other suitable activators are diacylorganoamides disclosed in U.S. Pat. No. 3,177,148, including
N-acetyl anthranil,
N,n-diacetyl-5,5-dimethylhydantoin
N,n-diacetylaniline
N,n-diacetyl-p-toluidine
N,n-diacetyl-p-chloroaniline
N,n-dibutyrylaniline
Dibenzanilide
N-acetyl caprolactam
N,n'-diacetylbarbitone
N-acetyl phthalimide
N-acetyl saccharin
The method for preparing trisodium carboxymethyloxysuccinate is described in the aforementioned U.S. Pat. No. 3,692,685. The salt may be prepared by reacting together maleic acid, glycolic acid and calcium hydroxide, or other divalent metal hydroxide, in water at reflux temperatures, cooling, adding sodium carbonate, and filtering to remove the resulting divalent metal carbonate.
Carboxymethyloxysuccinic acid and its salts are stable toward chlorine-releasing and oxygen-releasing agents.
The detergent suitable for use with the builder combination of the invention is any detergent species that is compatible with the chlorine- or oxygen-releasing agent.
Among the detergent species adversely affected by the chlorine-releasing agents are the anionic detergents having nitrogen or substantial unsaturation in the molecule, and most nonionics.
However, nonionic detergents that have a low weight-percentage of hydroxyl groups in the molecule and additionally are nitrogen-free are stable toward chlorine-releasing agents, and may be employed in the compositions of the present invention, being especially useful when the composition is in particulate form. Stable nonionics within the above description are the Pluronics (trade mark of the Wyandotte Chemicals Corporation) formed by condensing propylene oxide with propylene glycol to a molecular weight of about 600-2500 to form a base, followed by condensing ethylene oxide to this base to the extent of about 20% to about 90% by weight, total molecule basis. Suitable non-ionic species of this type are disclosed in U.S. Pat. Nos. 2,674,619 and 2,677,700. Other useful nonionics are disclosed in U.S. Pat. No. 3,048,548.
The lower molecular weight nonionic detergent species may be used if the compositions are freshly prepared before use. Nonionics falling within this category are the ethoxylated alkyl phenols having 6-12 carbon atoms in the alkyl portion, which may be straight or branched, and having 6-25 molar proportions of ethylene oxide, and ethoxylates of alkanols having 8-18 carbon atoms per molecule and 5-30 molar proportions of ethylene oxide wherein the ethylene oxide content is at least about 52% by weight.
Specific nonionic species falling within the above classes are: branched-chain nonyl phenol condensed with 8-14 molar proportions of ethylene oxide, a mixed C 11 -C 15 secondary alcohol condensed with 9-14 molar proportions of ethylene oxide, a mixed C 14 -C 15 alcohol made by the Oxo process condensed with 9-12 molar proportions of ethylene oxide, a mixture of 65% C 14 and 35% C 15 synthetic straight chain primary alcohols condensed with 9-15 molar proportions of ethylene oxide, or the mixed fatty alcohols (predominantly of 12 and 14 carbon chain length) derived from coconut oil condensed with about 10 to about 30 molar proportions of ethylene oxide.
Among the suitable anionics there may be mentioned the alkylarylsulfonates, more specifically the alkylbenzenesulfonates wherein the alkyl group is a straight chain having about 11 to about 15 carbon atoms or mixtures thereof, and the sulfonated phenyl group is randomly positioned along the alkyl chain. The alkylbenzenesulfonates may have a branched alkyl group of about 9 to about 15 carbon atoms, or mixtures thereof, such as may be derived from polypropylene and described in U.S. Pat. Nos. 2,477,382 and 2,477,383. Also useful are the alkylbenzenesulfonates described in U.S. Pat. Nos. 2,390,295, 3,320,174 and in Nos. 2,712,530 and 2,723,240.
The alkyl sulfate salts are useful in the practice of the invention, particularly the sodium alkyl sulfates wherein the alkyl group is straight or branched, substantially saturated, and has about 12 to about 18 carbon atoms, but may have as low as 6 carbon atoms in admixture with longer chain lengths, for example when the alkyl group is a mixture derived from coconut oil, palm kernel oil, or other tropical nut oil.
Useful detergents include the alkanesulfonates having about 8 to about 18 carbon atoms, preferably about 10 to about 14 carbon atoms. The alkanesulfonates may be prepared by methods known in the art, for example as described in U.S. Pat. No. 3,541,140.
The disodium salts of alpha-sulfonated fatty acids may be employed, or a methyl or ethyl ester thereof as disclosed in U.S. Pat. No. 3,338,838.
The alkali-metal acyl isethionates having about 12 to about 18 carbon atoms in the acyl groups may be used. Suitable preparatory procedures for the acyl isethionates may be found in U.S. Pat. Nos. 3,320,292, 3,376,229, 3,151,136, 3,383,396, 3,420,857 and 3,420,858.
A suitable anionic mixture comprises about equal parts by weight of
i. a sodium salt of a sulfated condensate of an aliphatic monohydric alkanol having about 12-14 carbon atoms and an average of about 3 molar proportions of ethylene oxide, and
ii. sodium alkylbenzenesulfonate wherein the benzene ring is randomly positioned along a linear alkyl group having an average of about 13 carbon atoms.
If desired the detergent component may be a quaternary ammonium compound, for example
cetyltrimethylammonium bromide
dodecyldimethylbenzylammonium chloride
tetradecyldimethylethylbenzylammonium chloride
carboxymethyldimethyltetradecylammonium choride
carboxymethyldimethyloctadecylammonium chloride
1,1'-oxybis[N-tetramethylene-N-carboxymethylpiperidinium chloride]
1,1'ethylenebis[N-oxyethylene-N-carboxymethylpiperidinium chloride]
benzyl dibutyl-2-[2,3,4,6-tetrachlorophenoxy)ethoxy]-ethyl ammonium chloride
diisobutylphenoxyethoxyethyldimethylbenzylammonium chloride
diisobutylcresoxyethoxyethyldimethylbenzylammonium chloride
N-methyl-N-(2-hydroxyethyl)-N-(2-hydroxydodecyl)-N-benzyl ammonium chloride
Stearyl trimethylammonium bromide
Lauryldimethylchlorethoxyethylammonium chloride
Alkyl (C 8 -C 18 )dimethyl(3,4-dichlorobenzyl)ammonium chloride
Lauryl pyridinium bromide
Lauryl isoquinolinium bromide
N(lauroyloxyethylaminoformylmethyl)pyridinium chloride
Betaines, such as beta(hexadecyldiethylammonio)propionate, and
Sultaines, such as 3-(tetradecyldimethylammonio)ethane-1-sulfonate.
Other detergent adjuncts having detergent-building properties may be present in the compositions of the invention in minor amounts relative to the aforesaid carboxymethyloxysuccinate. For example, there may be present sodium carbonate, sodium silicate, condensed phosphates, orthophosphates, borates, tetrasodium oxydisuccinate, starch- or cellulose-derived polycarboxylates, polyacrylates, soil-suspending agents, hydrotropes, corrosion inhibitors, dyes, perfumes, optical brighteners, fillers, suds boosters, suds depressants, anticaking agents, alkaline compounds, buffers, and the like.
In accordance with one aspect of the invention there may be prepared a mixture of about 50% to about 95% of trisodium carboxymethyloxysuccinate and about 5% to about 15% of a chlorine-releasing or oxygen-releasing agent, the mixture being in dry particulate form, and suitable for use as a builder combination in conjunction with a detergent. Expressed as weight ratios, about 0.05 part to about 1 part by weight of chlorine-releasing agent may be employed in combination with 1 part by weight of trisodium carboxymethyloxysuccinate. A useful ratio is about 0.2 to 1 respectively, by weight.
A detergent of the types disclosed hereinbefore may be admixed with the aforementioned builder mixture in liquid or particulate forms of the products of the invention. Liquid forms may contain
______________________________________ Percent or parts by weight______________________________________ Broad Preferred______________________________________Anionic or quaternary ammonium 10-35 15-25nonsoap surfactantCarboxymethyloxysuccinic acid 10-50 25-35or salt thereofChlorine-releasing or oxygen- 2-5 2-4releasing agentWater 35-78 40-58______________________________________
More specifically, liquid forms may comprise:
i. About 10% to about 35% of an anionic or a quaternary ammonium nonsoap surfactant having detergent properties, or mixtures thereof,
ii. about 10% to about 50% of a polycarboxy salt having the general formula ##STR4## wherein M is hydrogen or an alkali metal cation,
iii. about 2% to about 5% of a hypochlorite selected from the group consisting of alkali-metal hypochlorite and hypochlorous acid,
iv. about 35% to about 78% water.
Particulate forms may contain
______________________________________ Percent or parts by weight______________________________________ Broad Preferred______________________________________Anionic or quaternary ammonium 10-40 15-30nonsoap surfactantTrisodium carboxymethyloxy- 25-60 30-45succinateChlorine-releasing or oxygen- 5-15 7-12releasing agentWater 5-15 7-10______________________________________
The chlorine-releasing or oxygen-releasing agent will be selected with due regard to their effect on the detergent species contemplated for use therewith, and with due regard to the form of the product. When employed in particulate form, the chlorine-releasing or oxygen-releasing agent may be encapsulated to increase storage stability.
For a better understanding of the invention, reference is made to the following examples, which are illustrative but not limitative of the invention.
EXAMPLE 1
The following example demonstrates the improvement in detergency obtained when sodium hypochlorite is employed in conjunction with trisodium carboxymethyloxysuccinate for fabric washing. To conduct the detergency test, there is placed in the cup of a Terg-O-Tometer 1000 ml of a 180 ppm-hardness water solution of 1.0 gram of trisodium carboxymethyloxysuccinate, 0.89 gram of sodium alkylbenzenesulfonate containing 43% active matter, 0.43 gram of sodium silicate solution (RU type, ratio of SiO 2 to Na 2 O = 2.4; 46.8% solids) at a temperature of 120° F. Next is added 3.7 ml of a 5.25% solution of sodium hypochlorite, and the pH adjusted to 10.0. Following this there are added four swatches of Dacron/cotton fabric measuring 41/2 by 6 inches each, soiled with vacuum cleaner dust. The Terg-O-Tometer is operated for 10 minutes at 90 oscillations of the paddle per minute. The cloths are then rinsed once for one minute in 1 liter of 180 ppm water at 100°-120° F, dried by tumbling at about 110° F, and the detergency measured by determining the reflectance in a Gardner Automatic Color Difference Meter, Model AC-3. The detergency is expressed in DU's, which is a figure obtained by subtracting the reading of the unwashed cloth from the reading of the washed cloth. The quantities of components mentioned above represent 50% by weight of trisodium carboxymethyloxysuccinate, 18% by weight of sodium alkyl (av. 13 carbon atoms) benzenesulfonate, 10% sodium silicate solids, and 10% sodium hypochlorite solids, basis of a complete detergent composition added at 0.2% in the wash solution. The foregoing figures total 88% of a complete detergent composition. The balance, i.e. 12%, is water.
A control test is conducted as above but without the hypochlorite, and a comparable pair of tests is made in which sodium tripolyphosphate is substituted for trisodium carboxymethyloxysuccinate. The results set forth in Table I below, clearly show (1) that sodium hypochlorite improves the detergency of a detergent composition built with trisodium carboxymethyloxysuccinate to exceed the detergency of a corresponding detergent composition built with sodium tripolyphosphate, and (2) that sodium hypochlorite has a greater detergent-enhancing effect on trisodium carboxymethyloxysuccinate than on sodium tripolyphosphate.
Table I______________________________________Component Percent by Weight______________________________________ A B C D______________________________________Sodium alkylbenzenesulfonate 18 18 18 18Trisodium carboxymethyloxy- 50 50 -- --succinateSodium tripolyphosphate -- -- 50 50Sodium silicate solids 10 10 10 10Sodium hypochlorite* -- 10 -- 10Water 22 12 22 12______________________________________ 100 100 100 100Detergency, D.U. 24.0 35.0 27.0 36.2______________________________________ *10% sodium hypochlorite provides 200 ppm NaOCl in the wash solution.
EXAMPLE 2
The following is a liquid detergent composition within the invention.
______________________________________ Percent by Weight______________________________________Sodium salt of a sulfate condensate of an aliphatic monohydric alkanol having about 12-14 carbon atoms and an average of about 3 molar proportions of ethylene oxide 20.0Trisodium carboxymethyloxysuccinate 25.0Sodium xylenesulfonate 5.0Sodium hypochlorite 4.0Dimethyl dodecyl amine oxide 5.0Sodium silicate solids, ratio of SiO.sub.2 to Na.sub.2 O = 2.0 10.0NaOH q.s. to pH 11.0 and water q.s. to 100% 31.0______________________________________ 100.0______________________________________
EXAMPLE 3
Following is a particulate detergent within the invention.
______________________________________ Percent by Weight______________________________________Sodium alkylbenzenesulfonate.sup.(a) 20.0Trisodium carboxymethyloxysuccinate 48.0Sodium silicate solids.sup.(b) 6.0Sodium toluenesulfonate 2.0Optical brightener 0.1Water 8.9Encapsulated potassium dichloroisocyanurate 15.0______________________________________ 100.0______________________________________ .sup.(a) the alkyl groups are linear with an average of about 13 carbon atoms and the benzene ring is randomly positioned on the secondary positions along the alkyl chains. .sup.(b) RU-type sodium silicate having an SiO.sub.2 :Na.sub.2 O ratio of 2.4.
To prepare the foregoing composition, all of the components except the potassium dichloroisocyanurate are mixed in a crutcher and spray dried by means well known in the art. Eighty-five parts by weight of the spray-dried composition in particulate form are mixed with 15 parts by weight of encapsulated potassium dichloroisocyanurate of which 331/3% is encapsulating material, i.e., sodium stearate.
EXAMPLE 4
Following is a quaternary ammonium detergent composition within the invention.
______________________________________ Percent by Weight______________________________________Cetyltrimethylammonium bromide 20.0Trisodium carboxymethyloxysuccinate 50.0Chlorinated trisodium phosphate 10.0Sodium metasilicate 10.0Sodium sulfate 10.0______________________________________ 100.0______________________________________
The components, each in particulate form, are conveniently mixed together to form a particulate composition.
EXAMPLE 5
The following mixtures are suitable as builder combinations for use with an anionic or quaternary ammonium detergent.
__________________________________________________________________________ Parts by Weight A B C D E F G H I__________________________________________________________________________Trisodium carboxy-methyloxysuccinate 1 1 1 1 1 1 1 1 1Sodium hypochlorite 0.05 1 -- -- -- -- -- -- --Para-toluenesulfon-dichloramide -- -- 1 -- -- -- -- -- --1,3-dichloro-5,5-di-methylhydantoin -- -- -- 0.5 -- -- -- -- --Calcium hypochlorite -- -- -- -- 0.05 -- -- -- --N-chloroammeline -- -- -- -- -- 1 -- -- --N-chlorosuccinimide -- -- -- -- -- -- 0.4 -- --N,N'-dichlorobiuret -- -- -- -- -- -- -- 0.2 --Chlorinated dicyan-diamide -- -- -- -- -- -- -- -- 1__________________________________________________________________________
EXAMPLE 6
A liquid composition in accordance with the invention is prepared in the following manner.
16.65 grams of trisodium carboxymethyloxysuccinate pentahydrate having 72.2% active material are dissolved in 25.19 grams of a liquid commercial household hypochlorite bleach containing 4.74% NaOCl, resulting in the following final composition.
______________________________________ Percent by Weight______________________________________Trisodium carboxymethyloxysuccinate 28.73NaOCl 2.85Water 68.42______________________________________ 100.00______________________________________
EXAMPLE 7
A liquid composition is prepared in the manner of Example 6 except that the carboxymethyloxysuccinate is the tripotassium salt in anhydrous form. The product has the composition:
______________________________________ Percent by Weight______________________________________Potassium carboxymethyloxysuccinate 47.51NaOCl 2.48Water 50.01______________________________________ 100.00______________________________________
EXAMPLE 8
The following compositions are prepared at washing concentrations, i.e., aqueous solutions of 0.2% whole built detergent composition.
__________________________________________________________________________ Percent By Weight A B C D E F G H__________________________________________________________________________Trisodium carboxymethyloxy-succinate 25 25 30 30 60 60 60 60Sodium tetradecanesulfonate -- 20 -- -- -- -- -- 5Sodium acyl isethionate.sup.(a) -- -- 10 -- -- -- -- --Sodium dodecyl sulfate -- -- -- 15 -- -- 10 --Potassium alkylbenzenesul-fonate.sup.(b) 40 -- -- -- -- -- 10 --Disodium alpha-sulfo-alkanoate.sup.(a) -- -- -- -- 20 -- -- 10N-methyl-N-(2-hydroxyethyl)-N-(2-hydroxy-dodecyl)-N-benzylammonium chloride -- -- -- -- -- 15 -- --Lithium hypochlorite 10 -- -- -- -- -- -- 10Potassium dichloroiso-cyanurate -- 5 -- -- -- 10 5 --N,N-dichlorobenzoyleneurea -- -- 10 -- -- -- -- --Para-toluenesulfondichlor-amide -- -- -- 15 -- -- -- --N-chloro-acetylurea -- -- -- -- 15 -- -- --Sodium meta silicate -- 10 -- -- -- -- -- --Sodium carbonate 5 -- 10 -- -- -- -- --Water 20 40 40 40 5 15 15 15__________________________________________________________________________ 100 100 100 100 100 100 100 100pH at washing concentration 12 10 9 11 9 10 9 12__________________________________________________________________________ .sup.(a) derived from coconut oil fatty acids. .sup.(b) the alkyl groups are linear with an average of about 13 carbon atoms and the benzene ring is randomly positioned on the secondary positions along the alkyl chains.
The foregoing components, except the water, are separately added to one liter of water at 180 ppm hardness as CaCO 3 (2/3 Ca + + , 1/3 Mg + + ) in proportions to provide a washing concentration of 0.2%, whole composition basis. The pH is adjusted, where necessary, to the levels shown.
EXAMPLE 9
A solution containing 0.04 gram of sodium alkylbenzenesulfonate.sup.(a), 0.10 gram of sodium carboxymethyloxysuccinate, 0.02 gram sodium hypochlorite, per 100 grams of solution, is employed to wash the mildewed surface of a painted wall. The wall is cleaned, and the mildew discoloration removed by the washing process.
EXAMPLE 10
The following composition is prepared.
______________________________________ Percent By Weight______________________________________Carboxymethyloxysuccinic acid 25Hypochlorous acid 4Potassium dodecylbenzenesulfonate 10Water 61______________________________________ 100pH 3______________________________________
The foregoing composition is advantageously prepared, or acidified to the desired pH level, shortly before use, since the hypochlorous acid component is unstable in aqueous acidic solution.
Having described the invention, persons skilled in the art will be aware of modifications not specifically set forth herein, and the invention is to be limited only within the scope of the appended claims.
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A mixture of an alkali metal or alkaline earth carboxymethyloxysuccinate and a chlorine-releasing agent or an appropriately activated oxygen-releasing agent provides a builder combination suitable for use in detergent compositions to improve the detergency over that obtained when the carboxymethyloxysuccinate is the sole builder. The compositions are also useful in acidic solutions and have utility for the cleaning of metal and other hard surfaces.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims the right of foreign priority with respect to Application No. U.S. 60/679,884, filed May 12, 2005, in United States of America, the disclosure of which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to a non-welded, structural connection system with moment resisting capability that can be used in a pony-truss bridge system or in diverse areas of architectural design, engineering, fabrication, and field erection structures using tubular members.
BACKGROUND OF THE INVENTION
[0003] Transportable and assemblable bridges are known which can provide a path for pedestrian, bicycles, light or heavy vehicles, across and over obstacles such as rivers and ravines. Some example of previous invention of prefabricated unit construction modular bridging systems may be found in U.S. Pat. Nos. 4,912,795/5,414,885/6,009,586/4,965,903/6,308,357/6,631,530 and 5,924,152.
[0004] Most of the time, fusion welding is employed to assemble such structures. However, it is well known in literature that aluminum fusion welding partially anneals the weld zone by creating a heat-affected-zone on the base metal which decreases its ultimate and yield strengths (example can be read in Dispersoid-Free Zones in the Heat-Affected Zone of Aluminum Alloy Welds—B. C. MEYER, H. DOYEN, D. EMANOWSKI, G. TEMPUS, T. HIRSCH, and P. MAYR). The present invention allows the fabrication of such structure using the full strength of aluminum because no welding for the main bearing structure would be required anymore. As an additional feature, the invention could allow anodizing, bake paint finished and easy transportation of all components to the erection site. The fabrication of all components could also be made by numerically controlled technologies that could increase accuracy as well as minimizing the fabrication time. Most of these additional features are not always possible for conventional aluminum welded structures since large structures request special transportation or would not fit into anodizing baths or on automated bake paint lines.
[0005] Another important advantage is that the invention allows all elements to be joined quickly together on site with a minimum of fasteners to form a bridge of the required length and strength within the overall limitations of the system whether it is made of aluminum, steel or other suitable material.
OBJECTS OF THE INVENTION
[0006] It is an object of the present invention to provide a mean to build transportable bridges which can be easily and readily transported in pieces by, for example, trucks, boats, aircrafts or helicopters.
[0007] It is a further object of the present invention to design such bridge pieces so that they may be carried or parachuted into the desired location.
[0008] It is yet another object of the present invention to allow for the bridge to be assembled as a self-supporting, projecting structure by relatively few people without using special equipment.
[0009] The invention can achieve one or more of the following advantages:
Avoiding the creation of a heat-affected-zone for the main bearing elements; No certified welders are required to assemble the structure; Very long span possible due to the light weight of aluminum; Allowing architectural finishes such as anodizing, bake paint finishes and others; Pre-engineered structures that minimize the engineering design costs; Off-the-shelf elements that allow a structure to be shipped within few working days compared to weeks or months for a regular welded structure; Pre-fabricated elements with numeric controlled technologies reduces labour costs and poor accuracy; Decreasing assembly costs because the structure can be assembled quickly with minimal labour as well as a minimum number of fasteners; Ease of transportation (or exportation) allows all elements to be shipped on regular bundles or pallets independently of the final size of the complete structure.
[0019] The invention is especially advantageous for use in the construction of structures made from aluminum.
[0020] Other and further objects and advantages of the present invention will be obvious upon an understanding of the illustrative embodiments about to be described or will be indicated in the appended claims, and various advantages not referred to herein will occur to one skilled in the art upon employment of the invention in practice.
SUMMARY OF THE INVENTION
[0021] There is, therefore, provided in the practice of this invention a connection system with moment resisting capability, a novel framing element and a method of assembling same.
[0022] The present invention relates to a novel connection system with moment resisting capability being used, but not limited to, in a pony-truss bridge which can be assembled from individual prefabricated or off-the-shelf components.
[0023] Such structure may be constructed quickly to meet variation of spans or widths as well as to provide temporary or permanent access to all individuals, light vehicles and bicycles between two areas of different elevation or across and over obstacles or may be used as a walkway system to be cantilevered from the existing bridge structure, thereby providing suitable walkway widths on both sides of a bridge without reducing the width of existing traffic lanes.
[0024] The connection system can be attached to the tension chord of a pony-truss bridge to resist bending moment such as required for the top chord stability (top chord stability criteria utilizing elastic lateral restraints—TV Galambos, Timoshenko). To assemble the connection system, three or more multi-hollow members are slid into female node cavities and preferably locked in place utilizing a fastener, usually a bolt, that goes through their neutral axis. The framing elements are positioned accurately into the node's cavities according to fabrication accuracy which may be done by numeric controlled technologies. The framing member attachment or fastener means is preferably done within the area of its neutral axis by typically, but not limited to, a bolt that acts to absorb the tensile forces exerted on to the system without compromising the node connection. Once the member is in place, it can be secured by a bolt, a threaded rod or any other means that will keep the member into place ideally, but not limited to, within the neutral axis region. The external wall of the element has a friction contact with the internal side cavity which will resist the compression forces or bending moments exerted onto the element therefore it can transfer such forces or moment to the node without compromising the node connection.
[0025] A given connection system is comprised of a joint or node and associated interlinked members to be used in pony-truss bridges system or any other applicable engineered structures. A preferred embodiment of the connection system employs custom aluminum extruded hollow elements and a node and bolts or rods to secure elements to the node.
[0026] Pony-truss bridge or other structures may be wholly or partially constructed using the moment resisting connectors in accordance with the invention. Such a structure is comprised of a plurality of framing elements, joint or node connectors, and attachment means.
[0027] To assemble a structure with the use of the invention, some members are positioned into the node's cavities given at the same time the final alignment due to the perfect fit inside the cavity while another member, generally a chord, is liked onto the channel's node. Ideally, all members are secured with fasteners while some have only one fastener that goes through their neutral axis and another one, generally the chord, has at least two bolts that secure it through the node's channel. For ease of reference, every time the word <<cavity>> is used hereinafter, it is to be understood a cavity with a specific depth to confer moment resisting capability. This depth can be determined with calculation, benchmark tests or other known means.
[0028] An example of a structure using the invention is a transportable bridge or other similar structure having two longitudinal vertical trusses, comprising: plural bridge elements connected to each other by rigid nodes on a chord. The structure includes: a decking extending across a width of the bridge and having an horizontal triangular or Vierendeel truss depending on the lateral forces being acting on the structure (usually created by wind loads). Each vertical truss of the structure (main carrying members) resists gravity live and dead loads and brings sufficient stiffness to limit the deflection in conjunction of acting as a guard-rail. When the invention is being used for a pony-truss bridge system both vertical trusses have a bottom chord and an oppositely disposed top chord, the lower chord portion of the truss being connected to the transversals usually also made of a multi-hollow beams and multi-hollow diagonal struts by the rigid node herein named connection system.
[0029] The bridge vertical trusses, and thus the main load carrying members of the bridge, has essentially five different components: the top and bottom chords, the diagonals struts and/or vertical posts, the top connector (superior node) and the bottom connector (inferior node) which one connect both vertical trusses by horizontal floor members. These horizontal members can support what is called stringers located underneath a decking. The decking can be however made of different type of material but preferably, it could be made of a material having a low specific mass, for example composites or aluminum. The triangular trusses are dimensioned to reduce their size and corresponding weight. Consequently, the decking and the triangular trusses can be made so light that eventually the bridge structure could land on floating dock without the necessity to add additional buoyancy to it. Eventually the reduced weight of the individual components could allow the bridge to be manually assembled and carried by relatively few people.
[0030] When assembled, the bridge has a half-through shape, and consists essentially of longitudinally extending main support vertical trusses, and a decking.
[0031] The connection system being used as a moment resisting connector for the half-through bridge structure that can be eventually used to construct footbridges, golf course bridges, skywalks, overpasses, vehicular access bridges, bicycle path bridge, trail bridges, recreational bridges, walkways and so.
[0032] Further, freeway overpasses and underpasses built in the last decades frequently lack adequate walkways in situations where pedestrians or bicycles are permitted. In many communities, such barriers prevent pedestrian/bicycles access between neighborhoods, schools, and employment centers. In such cases the invention could serve to construct bridges that can be placed on the side of existing narrow bridges to give better access to the communities.
[0033] To eliminate excessive free play between the connected components when the bridge is assembled, the triangular trusses are interlockingly connected with each other. The interlocking connection includes at least one fastener that goes through the neutral axis of the diagonal and/or vertical struts, transversal beams as well as a minimum of fasteners to hold the connector to the bottom chord of the truss. Fasteners that secure the struts to the connector act in tension while fasteners that hold the connector to the chords act in shear. Further, the top chord is linked to the diagonal and/or vertical struts with the mean of a pin connection working in shear.
[0034] A lubricant can be disposed at the interface of the connection of framing elements and node connectors to allow an easier disassembling if the bridge is temporarily installed.
[0035] The invention will be described below in greater detail in connection with embodiments thereof that are illustrated in the drawing figures.
[0036] The features of the present invention which are believed to be novel are set forth with particularity in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] A preferred embodiment of the present invention will be described in greater detail below with reference to the following drawings, in which:
[0038] FIG. 1 is a perspective view of a fully assembled modular bridge in accordance with the present invention.
[0039] FIG. 2 is a perspective view of the main carrying members of the bridge shown in FIG. 1 prior to installation of floor boards, fencing and stringers;
[0040] FIG. 3 is an exploded perspective view of the bridge understructure shown in FIG. 2 ;
[0041] FIG. 4 is an exploded perspective view of the bridge shown in FIG. 1 including floor boards, fencing and stringers;
[0042] FIG. 5 is a perspective view of a splice in the bridge of FIG. 2 ;
[0043] FIG. 6 is a exploded perspective view of the connection system with moment resisting capability shown in all previous figures ( FIGS. 1 , 2 , 3 , 4 & 5 );
[0044] FIG. 7 is an elevation view of the connection system shown in FIG. 6 when fully assembled;
[0045] FIG. 8 is a section view along lines A-A in FIG. 7 when fully assembled;
[0046] FIG. 9 is a section view along lines B-B in FIG. 7 when fully assembled;
[0047] FIG. 10 is a section view of along lines C-C in FIG. 9 when fully assembled;
[0048] FIG. 11 is a exploded perspective view of the compression chord connector shown in FIGS. 1 , 2 , 3 , 4 & 5 ;
[0049] FIG. 12 a section view of the superior connector shown in FIG. 11 when fully assembled;
[0050] FIG. 14 is a section view along lines D-D in FIG. 12 when fully assembled.
[0051] FIG. 15 is an elevation view of the inferior node connector with moment resisting capabilities;
[0052] FIG. 16 is an elevation view of the superior node connector;
[0053] FIG. 17 is a section view of the diagonal/vertical struts and transversals;
[0054] FIG. 18 is an alternative for the inferior connector element. It is therefore possible that the struts to be made of a hollow section, usually circular, and the tension forces can be taken by a rod that is independently located near the strut neutral axis.
[0055] FIG. 19 is a section view along lines E-E in FIG. 18 when fully assembled;
[0056] FIG. 20 is another alternative for the inferior connector element. It is therefore possible that the struts to be made of a hollow section, usually circular, and the tension forces can be taken by an insert located inside the hollow section.
[0057] FIG. 21 is a section view along lines F-F in FIG. 20 when fully assembled;
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0058] Turning to FIG. 1 , a modular pedestrian bridge 1 is shown comprising a plurality of individual elements connected to each other by the mean of node connectors 4 and 7 . Fencing 20 connect to the vertical trusses on the inside as shown or eventually on the outside. A decking 21 , or eventually floor boards, is placed on top of the stringers (not shown) and acts as a floor to be walked on. Ends of the bridge, when installed, are connected to respective end footings (not shown) via respective anchors (not shown).
[0059] The modular sections of fencing 20 may be fabricated to any suitable length. Typical sections contemplated are 5 feet, 10 feet, 15 or 20 feet in length.
[0060] FIG. 2 shows the bridge in FIG. 1 prior to installation of the decking and stringers. As can be seen from FIG. 2 , both vertical trusses are linked to each other via a plurality of transversals 3 and diagonals 5 extending there between.
[0061] FIG. 3 illustrates an exploded view of the main bearing structure comprising a plurality of linear elements such as two tension chords 8 , two compression chords 1 , a plurality of diagonals 2 , transversals 3 , floor diagonals 5 all connected to each other by the mean of top node connectors 7 and bottom node connectors 4 .
[0062] Next, as shown with reference to FIG. 4 , longitudinal stringers 22 are placed and secured on top of the transversals 3 . A decking is secured to the stringers via fasteners (not shown). A fencing system 20 (optional) can be attached to the vertical main load carrying trusses.
[0063] Turning to FIG. 5 , successive ones of the vertical trusses are shown comprising top and bottom chord members 1 and 8 connected via splices 30 and 31 . Diagonal members 2 provide additional support.
[0064] The bottom node connector is shown in greater detail with reference to FIG. 6 comprising diagonals 2 , tension chord 8 , floor diagonals 5 , transversals beams 3 and a node connector 4 that have the ability to transfer bending moments. The diagonals and transversals are inserted into corresponding cavities thereby 41 at the distal ends of the diagonals and transversals members 2 and 3 . Ideally, the diagonals and transversals have tapered ends for insertion into corresponding ones of the cavities. Their ends can be milled, turned, swaged or bring to this particular shape by the mean of any way. The cavities however could be or not to be of a similar corresponding shape depending on temporary or permanent use of the structure (vertical or tapered inside wall of cavities). The best way to secure such diagonals and transversals inside the node connector could be done by the use of a bolt that is screwed inside the internal region 42 of the multi-hollow cavity extruded tube as shown in FIG. 17 and as shown in greater detail with reference to FIGS. 8 and 10 . The node connector is attached to the tension chord by a pair of bolts 34 and nuts 35 through two like pairs of holes adapted to align the node 4 and the chord 8 . Both floor diagonals attach to the node connector with bolts 32 and nuts 33 .
[0065] The node connector form a solid and extremely stable connection between the hollow tubing chord members 8 , the transversal beam 3 and the diagonals 2 for maintaining structural integrity throughout the chord members 8 , thereby overcoming lateral stability problems inherent in half through (pony) bridge. As shown with reference to FIG. 6 , bolts that are used to secure diagonals and transversals are hidden so they cannot be unscrewed while the node is attached to the chord providing additional safety against thief or sabotage. Additionally, anti thief nuts can be used instead of regular nuts to secure the node connector to the chord 35 . The resulting connector is in a visually attractive appearance.
[0066] Turning now to FIGS. 7 , 8 , 9 and 10 , the first figure is an elevation view from the inside of the bridge. Element 3 is the transversal hollow beam and elements 5 are the diagonal bracings to resist any horizontal loading act on the projected area of the bridge structure. Elements 2 are the diagonals that support the compression chord (not shown). They mainly resist tension and compression forces but they also transfer some bending moment to the floor beams as well as they transfer torsion to the tension chord 8 since they stabilize the compression chord which one tend to buckle. FIG. 8 shows a view along lines A-A in FIG. 7 . As it can be seen a fastener 36 , generally a bolt, secures the floor beam 3 into the node 4 cavity. Bolt 34 secure the node 4 to the tension chord 8 . FIG. 9 shows a view along lines B-B in FIG. 7 . FIG. 10 shows a view along lines C-C in FIG. 9 . Once again we find two fasteners, generally bolts, to secure both diagonal members 2 into the node 4 cavities.
[0067] As shown best with reference to FIG. 11 , the exploded view of the compression node connector shows two diagonals 2 , two superior node connectors 7 , a compression chord 1 and their associated fasteners 36 , 37 and 38 , generally bolts. The diagonals 2 are linked to the superior nodes generally by the mean of one bolt 36 screwed into their neutral axis. The superior node connectors are however linked to the compression chord by the mean of a bolt 37 that fits into a hole in the compression chord 1 . The bolt 37 is secured in place with a nut 38 or preferably with an antitheft nut (not shown).
[0068] FIG. 12 shows a sectional view from the compression chord 1 . It is therefore acknowledge that the bolt 37 works in shear while the fasteners (not shown) that secure the diagonal 2 on the superior node 7 works in tension.
[0069] FIG. 14 shows a view along lines D-D in FIG. 12 . As it is shown fasteners, generally bolts 36 , secure the diagonals 2 on the superior node 7 . A fastener 37 goes through a hole in the compression chord 1 .
[0070] FIG. 15 shows the moment resisting node connector 4 while FIG. 16 shows the superior node connector which one are generally liked to a multi-hollow extruded shape as it is shown in FIG. 17 . Even if the cylindrical framing element 2 , 3 has been shown having a circular section, it is to be noted that the section of the framing element could have any other suitable section such as, for example curved section (e.g. ellipsoidal) or polygonal section (e.g. square, triangular or else).
[0071] FIG. 18 shows a possible alternative to the use of a multi-hollow section shown in FIG. 17 . It is therefore possible to use, but not preferred, a regular hollow shape that could be secured into the node cavities by the mean of a rod partially or completely threaded. FIG. 19 shown a view along lines E-E in FIG. 18 . A rod 39 can run on or near the neutral axis of a tube. A nut 40 can give a pre-tension to maintain the tube inside the cavity with adequate pressure.
[0072] In addition to the alternative shown in FIG. 18 , FIG. 20 shows another alternative that could be possible, but not necessary desired, as it could allow the element 9 (a hollow section) to be secured into place with the mean of a threaded insert 44 as shown in FIG. 21 that would fit the inside of the element 9 . The insert 44 could be maintained inside the element 9 by the mean of welding or by any other mean.
[0073] FIG. 21 is a view along lines F-F in FIG. 20 and it shows the insert that could be achieved to secure in place the element 9 into place with a fastener 43 , generally a bolt.
[0074] Thus, in final assembly the center load of diagonals or verticals are supported equally by horizontal or tapered wall when the elements work in compression or by the mean of the fasteners, generally bolts, when the diagonals or verticals work in tension. The transversals however transfer their moment to the node with the friction applied along the internal walls.
[0075] Accordingly, a maximum dimension of transversals 3 and diagonals 2 may be accommodated irrespective of the width and length of the bridge. By way of contrast, know prior art transversals or diagonals connections require multiple welds, generally fillet weld type, which one are not desired since it weak the base material when aluminum is employed for such structure.
[0076] Accordingly, an important aspect of the present invention is the improved mechanical properties because of avoiding welding of the main structural members. The connector acts as a rigid node able to carry and transfer tension, compression, torsional and bending moments provided by usually only one interlocking fastener running through the neutral axis of diagonals/verticals and transversals.
[0077] Preferably, all metallic structural components of the pedestrian bridge in FIG. 1 in accordance with present invention are made of aluminum with the possibility to hard anodize each individual element, for forming an aesthetically pleasing and scratch resistant surface.
[0078] Other embodiments and variations of the present invention are contemplated.
[0079] For example, the connector of the present invention may be advantageously applied to virtually any structures using standard or custom hollow tubing. To that end, the inventive moment resisting connector could be used in such diverse applications as furniture construction, building construction, fencing, bridges, towers, flag post bases, gantry of motorway etc., any of which may be fabricated from stainless steel, plastic, steel or other suitable material.
[0080] Furthermore, whereas the preferred embodiment of the tapered end element which may usually be milled, swaged or turned by numeric controlled technologies, it is contemplated that end portions of the elements 2 and 3 may also be strait.
[0081] As a further alternative, the node configuration may be fabricated via specialized machining tools from a solid block or cast from metal or eventually made of composites.
[0082] Moreover, whereas the preferred embodiment discloses a structural connection for use with multi-hollow cross-sectional elements 2 and 3 in FIG. 17 , it is contemplated that the cooperating element and cavity aspect of the present invention may be applied equally to hollow tubing sections having square, circular or other cross-section.
[0083] All such embodiments or variations are believed to be within a sphere and scope of the present invention as defined by the claims appended hereto.
[0084] Although preferred embodiments of the invention have been described in detail herein and illustrated in the accompanying figures, it is to be understood that the invention is not limited to these precise embodiments and that various changes and modifications may be effected therein without departing from the scope or spirit of the present invention. For example, the node resisting joint and system of the invention may be used to construct roofs and other structures using nodes to join elongated members.
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The present invention is directed toward a novel moment resisting connection system, for use, but not limited to, with a pony-truss bridge system. The connection system comprises multi-hollow sections that can be, but are not limited to, extruded aluminum and a joint or node connector that can be casted, milled, forged or made by any other means.
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SUMMARY OF THE INVENTION
The new variety of Hybrid Tea rose plant was created by artificial pollination wherein two parents were crossed which previously had been studied in the hope that they would contribute the desired characteristics. The female parent (i.e., the seed parent) was an unnamed uncommercialized seedling. The male parent (i.e., the pollen parent) was the `Krilamy` variety (non-patented in the United States). The parentage of the new variety can be summarized as follows:
Unnamed Seedling×`Krilamy`.
The seeds resulting from the above pollination were sown and 240 small plantlets were obtained which were physically and biologically different from each other. Selective study resulted in the identification of a single plant of the new variety.
It was found through careful study that the new variety of the present invention exhibits the following combination of characteristics:
(a) from a physical point of view forms green mature wood, assumes a bushy to upright growth habit, forms large ovate buds, and forms attractive long-lasting flowers that are pink striped with white and have consistent petals, and
(b) from the biological point of view forms vigorous vegetation, produces flowers in abundance on a nearly continuous basis, exhibits the ability readily to be forced, and is resistant to diseases when grown under greenhouse conditions.
The new variety well meets the needs of the horticultural industry and is particularly well suited for growing in the greenhouse for the production of attractive very long-lasting cut flowers that are pink striped with white.
The new variety can be readily distinguished from other varieties in view of the combination of characteristics described herein. It exhibits very long and straight stems, rigid and straight peduncles, a propensity to be forced under greenhouse growing conditions, and a long vase life for its distinctive pink striped with white blossoms.
The new variety has been found to undergo asexual propagation and can be readily reproduced by conventional routes, such as budding (i.e., eye grafting). This asexual reproduction by budding as performed at Hyeres, France, has demonstrated that the characteristics of the new variety are strictly transmissible from one generation to another and are firmly fixed.
The new variety has been named the `Delstricycla` variety.
BRIEF DESCRIPTION OF THE PHOTOGRAPH
The accompanying photograph shows as nearly true as it is reasonably possible to make the same in a color illustration of this character typical specimens of the plant parts of the new variety. The rose plants of the new variety were grown under glass in the South of France.
FIG. 1 -- illustrates a specimen of a main branch;
FIG. 2 -- illustrates a specimen of a flowering stem;
FIG. 3 -- illustrates a specimen of a young shoot;
FIG. 4 -- illustrates specimens of a leaf with three leaflets -- plan view -- upper surface;
FIG. 5 -- illustrates a specimen of a leaf with five leaflets -- plan view -- upper surface;
FIG. 6 -- illustrates a specimen of a leaf with seven leaflets -- plan view -- upper surface;
FIG. 7 -- illustrates a specimen of a leaf with seven leaflets -- plan view -- under surface;
FIG. 8 -- illustrates a specimen of a floral bud at the opening of the sepals;
FIG. 9 -- illustrates a specimen of a floral bud at a more advanced stage than illustrated in FIG. 8;
FIG. 10 -- illustrates a specimen of a floral bud at a more advanced stage than illustrated in FIG. 9;
FIG. 11 -- illustrates a specimen of a floral bud at the opening of the petals;
FIG. 12 -- illustrates a specimen of a floral bud in a more advanced stage of opening than as illustrated in FIG. 11;
FIG. 13 -- illustrates a specimen of a floral bud at a more advanced stage of opening than as illustrated in FIG. 12;
FIG. 14 -- illustrates a specimen of a flower as the opening progresses;
FIG. 15 -- illustrates a specimen of an open flower-plan view -- reverse;
FIG. 16 -- illustrates a specimen of an open flower -- plan view -- obverse;
FIG. 17 -- illustrates a specimen of a fully open flower -- plan view -- reverse;
FIG. 18 -- illustrates a specimen of a fully open flower-plan view -- obverse;
FIG. 19 -- illustrates a specimen of a floral receptacle showing the arrangement of the stamens and pistils; and
FIG. 20 -- illustrates a specimen of a floral receptacle showing the arrangement of the pistils (stamens removed).
DETAILED DESCRIPTION
The chart used in the identification of the colors is that of The Royal Horticultural Society (R.H.S. Colour Chart). The description is based on the observation of plants grown under glass in the South of France. The coloration in common terms sometimes also is provided.
Class: Hybrid Tea.
Plant:
Height.--Plants which were pruned to a height of 80 cm. produce floral stems having a length of approximately 50 to 90 cm., and an average length of approximately 70 cm.
Habit.--Bushy to upright.
Branches:
Color.--Young shoots: When approximately 20 cm. long, exhibit a purple coloration, Greyed-Purple Group 183B at the tip changing to green, Yellow-Green Group 146C. Floral stems: Yellow-Green Group 146B. Mature wood: Yellow-Green Group 146A.
Thorns.--Configuration: Flat on the upper edge and concave on the under edge. Quantity, length and frequency: On a typical floral stem having a length of 10 cm., there commonly are approximately 3 small prickles <5 mm., and approximately 5 to 7 longer prickles >5 mm. On mature wood having a length of 10 cm., there commonly are approximately 15 to 18 pickles <5 mm. and approximately 5 to 7 longer pickles >5 mm. The length commonly is approximately 8 mm. on average on floral stems and approximately 9 mm. on average on mature wood. In each instance, the lengths commonly range from 1 to 11 mm. Color: On young shoots of approximately 30 cm. in length, the thorns are Greyed-Purple Group 183C to 183D, on floral stems the coloration of the thorns are Greyed-Yellow Group 162D with some reddish coloration, and on mature wood the thorns are Greyed-Orange Group 177B (Havana brown).
Leaves.--Number: Typical for the class. Size: Medium to large. Stipules: Adnate, small, and typical for the class.
Leaflets.--Number: Sometimes 3, and primarily 5 and 7. Size: Medium to large. Shape: Obtuse to rounded at the base of the terminal leaflet, slightly convex in cross section, and commonly possess weak margin undulation. Serration: Present, single, irregular, and very small. General appearance: Thin and weak with slight glossiness on the upper surface. Petiole: The inner surface is grooved with non-glandular edges. Petiole color on young shoot: Purple with green coloration on the inner surface and Yellow-Green Group 146D on the outer surface. Petiole color on floral stem: Bronze with green coloration on the inner surface and Yellow-Green Group 146D on the outer surface. Petiole color on mature wood: Yellow-Green Group 146D on inner surface, and Yellow-Green Group 146D on the outer surface. Petiole length of terminal leaflet: Approximately 12 to 19 mm., approximately 16 mm. on average, with a standard deviation of 2 mm. on a leaf of five leaflets. Terminal leaflet length: Approximately 45 to 100 mm., approximately 68 mm. on average, with a standard deviation of 10 mm. Terminal leaflet width: Approximately 33 to 55 mm., approximately 50 mm. on average, with a standard deviation of 5 mm. Terminal leaflet shape at base: Obtuse to rounded. Leaflet color of young shoot: On the upper surface Greyed-Purple Group 183B with some green coloration on the first leaves, and then green with reddish coloration on the margin changing to Yellow-Green Group 146B, and on the under surface Greyed-Purple Group 183B on the first leaves, and then purple with greenish coloration changing to Yellow-Green Group 147C. Leaflet color on floral stem: Yellow-Green Group 147A on the upper surface and Yellow-Green Group 148B on the under surface. Leaflet color of mature wood: Yellow-Green Group 147A on the upper surface, and Yellow-Green Group 148B on the under surface.
Inflorescence:
Number of flowers.--Generally one to five per stem as the auxiliary buds form flowers when grown under forced greenhouse conditions.
Peduncle.--Erect, stiff, Yellow-Green Group 146A with no hairs, commonly approximately 11 to 15 cm. in length (approximately 12 cm. in length on average).
Sepals.--Configuration: Two sepals commonly possess no extensions, and three sepals commonly possess extensions. The sepal length commonly ranges from approximately 30 to 60 mm. on average. Color: Yellow-Green Group 146B to 146C on the upper surface and Yellow-Green Group 146A to 146B on the under surface.
Buds.--Shape: Ovate. Size before calyx breaks: The bud lengths are approximately 21 to 30 mm., with an average length of approximately 23 mm. Color as calyx breaks: Red-Purple Group 60A striped with greenish-cream coloration. Size after calyx breaks: The bud lengths are approximately 44 to 60 mm., with an average length of approximately 47 mm. Color after calyx breaks: Inside: Red-Purple Group 63B to 63C and irregularly striped with white. Outside: Red-Purple Group 63A to 63B and irregularly striped with white.
Flower.--Time: Nearly continuously flowering. Shape: Double. Form: Round to irregularly rounded when viewed from above, flattened at the upper part when viewed from the side, and flattened convex at the lower part when viewed from the side. Diameter: Medium to large, approximately 9.2 to 11.8 cm., and approximately 10 cm. on average, with a standard deviation of 0.8 cm. Petal number: Commonly approximately 30 to 38, and an average of approximately 35. Petal size (second row from outside): The length is approximately 43 to 54 mm., a mean of approximately 51 mm., and a standard deviation of 2 mm.; and the width is approximately 46 to 52 mm., a mean of approximately 50 mm., and a standard deviation of 2 mm. Petal shape: Nearly rounded with medium reflexing of the margin and medium undulation of the margin. Petal color: The following description of a nearly fully open flower was made while observing a rose grown in the greenhouse during May which had been undergoing opening for two days. Petal color (middle zone): On the inner surface Red-Purple Group 63C to 63D towards the point of attachment an sometimes pink with irregular white stripes, and on the outer surface Red-Purple Group 63B to 63C and sometimes pink with irregular white stripes. Petal color (marginal zone): On the inner surface Red-Purple Group 63A to 63B and sometimes deeper Red-Purple Group 61B depending on the weather and sometimes irregular stripes of White Group 155B and sometimes pink with white, and on the outer surface Red-Purple Group 63C and sometimes irregular stripes of White Group 155B and sometimes pink with white. Petal spot at base: Small in size. Color of spot inner side: Yellow Group 3C. Color of spot outer side: Yellow-Green Group 150C. Stamens: Approximately 80 in number and are somewhat regularly arranged around the pistils. Filaments: Medium in length and Yellow Group 6C in coloration. Anthers: Medium in size, each opens at approximately the same time, and the immature coloration is Yellow Group 12B. Pollen: Normal in quantity and Yellow Group 4D in coloration. Pistils: Approximately 60 in number. Styles: Medium in length and Yellow-Green Group 154D in coloration. Stigmas: Yellow-Orange Group 14C, and generally are present at the same level as the anthers. Hips: No hips have been observed to date under greenhouse growing conditions. Seeds: None to date. Petal drop: Petals detach cleanly. Fragrance: None. Productivity: Under standard greenhouse growing conditions in the South of France commonly produces approximately 130 to 150 flowers per square meter per year. Lasting quality: Very good. When cut and placed in a vase, the flowers commonly last approximately 8 days. When present on the plant, the flowers commonly last approximately 8 to 10 days.
Development:
Vegetation.--Vigorous.
Blooming.--Abundant and almost continuous.
Aptitude to forcing.--Good.
Resistance to diseases.--Good under greenhouse conditions, and is sensitive to powdery mildew when grown outdoors.
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A new and distinct variety of Hybrid Tea rose plant is provided that abundantly and nearly continuously forms attractive double flowers which are pink striped with white. The plant is well suited for cut flower production in the greenhouse. This blossom coloration is believed to be unique for greenhouse roses. The buds are large and ovate in configuration. The flowers exhibit a good vase life and possess petals that detach cleanly. The plant exhibits a bushy to upright growth habit, forms long straight stems and straight peduncles and forms vigorous vegetation. Additionally, the plant is resistant to diseases when grown under greenhouse conditions.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from Japanese Patent Application No. 2010-082794 filed on Mar. 31, 2010, the entire contents of which are incorporated herein by reference.
TECHNICAL FIELD
[0002] Aspects of the present invention relates to a printing apparatus, particularly to a printing apparatus and a storing medium for storing a printing program, which can correct printing positions and printing densities.
BACKGROUND
[0003] There has been proposed a related-art printing apparatus which equips an image correction function that measures the deviation amount of a position and a density of a formed image and corrects the position and the density to reduce the measured deviation amount. When the image correction function is executed frequently, the quality of the image can be ensured. However, there are disadvantages such as a user has to wait for a long time or consumption of ink and toner is increased, due to especially the measurement of the deviation amount.
[0004] Therefore, in the related-art printing apparatus, when a predetermined correction execution condition is satisfied, for example, when a number of pages copied or a time elapsed after a previous image correction function was executed exceeds a predetermined value, the measurement of the deviation amount is executed. In addition, when print data is received during the measurement of the deviation amount, the print data is stored, and after the measurement of the deviation amount is finished, the print data which has been stored is expanded based on the result of the measurement of the deviation amount.
[0005] Generally, a related-art printing apparatus expands the print data per page and prints the expanded data successively. Therefore, the correction execution condition may be satisfied during expanding process of the print data per page. However, in the related-art printing apparatus, the way of executing the expanding process when the correction execution condition is satisfied during the expanding process of the print data per page is not considered. For example, if the deviation amount is measured after the expanding process, reflecting the measured deviation amount to the expanding process will be delayed.
SUMMARY
[0006] Accordingly, it is an aspect of the present invention to provide a printing apparatus and a storing medium for storing a printing program, which can prevent delay in reflecting the measured deviation amount to the expanding process of the print data when the correction execution condition is satisfied during the expanding process of the print data per page.
[0007] According to an exemplary embodiment of the present invention, there is provided a printing apparatus comprising: a printing unit configured to print an image based on expanded data; a measuring unit configured to measure a deviation amount of at least one of a position and a density of the image printed by the printing unit when a correction execution condition is satisfied; an expanding unit configured to expand print data based on the measurement by the measuring unit, so as to produce the expanded data; and a control unit, wherein when the correction execution condition is satisfied during the expanding of current print data which corresponds to a current page being expanded, the control unit is configured to control the expanding unit to suspend the expanding of the current print data, the measuring unit to measure the deviation amount, and the expanding unit to restart expanding an unexpanded portion of the current print data based on the measurement performed after the expanding is suspended.
[0008] According to another exemplary embodiment of the present invention, there is provided a printing apparatus comprising: a printing unit configured to print an image based on expanded data; a measuring unit configured to measure a deviation amount of at least one of a position and a density of the image printed by the printing unit when a correction execution condition is satisfied; an expanding unit configured to expand print data based on the measurement by the measuring unit, so as to produce the expanded data; a first determining unit, wherein when a print request is received, the first determining unit is configured to determine whether the correction execution condition may be satisfied during the expanding of the print data corresponding to the print request, before the print data is expanded, and a control unit, wherein when the first determining unit determines that the correction execution condition may be satisfied, the control unit is configured to control the expanding unit to delay the expanding of the print data, the measurement unit to measure the deviation amount, and the expanding unit to start expanding the print data which was delayed from expanding based on the measurement performed after the expanding is delayed.
[0009] According to another exemplary embodiment of the present invention, there is provided a computer readable storing medium storing a computer program for causing a printing apparatus, the printing apparatus comprising a printing unit configured to print an image based on expanded data, to perform a method of: measuring a deviation amount of at least one of a position and a density of the image printed by the printing unit when a correction execution condition is satisfied; expanding print data based on the measurement by the measuring unit, so as to produce the expanded data; and when the correction execution condition is satisfied during the expanding of current print data which corresponds to a current page being expanded, suspending the expanding of the current print data, measuring the deviation amount, and restarting expanding an unexpanded portion of the current print data based on the measurement performed after the expanding is suspended.
[0010] According to another exemplary embodiment of the present invention, there is provided a computer readable storing medium storing a computer program for causing a printing apparatus, the printing apparatus comprising a printing unit configured to print an image based on expanded data, to perform a method of: measuring a deviation amount of at least one of a position and a density of the image printed by the printing unit when a correction execution condition is satisfied; expanding print data based on the measurement by the measuring unit, so as to produce the expanded data; determining whether the correction execution condition may be satisfied during the expanding of the print data corresponding to the print request, before the print data is expanded, when a print request is received, and when it is determined that the correction execution condition may be satisfied, delaying the expanding of the print data, measuring the deviation amount, and starting expanding the print data which was delayed from expanding based on the measurement performed after the expanding is delayed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a sectional side view showing the schematic configuration of a printer according to a first exemplary embodiment of the present invention;
[0012] FIG. 2 is a block diagram briefly showing an electric configuration of the printer;
[0013] FIG. 3 is a flow chart showing a job execution process;
[0014] FIG. 4 is a diagram showing a density pattern;
[0015] FIG. 5 is a time chart of an expanding process and a density measurement; and
[0016] FIG. 6 is a flow chart showing a job execution process according to a second exemplary embodiment of the present invention.
DETAILED DESCRIPTION
First Exemplary Embodiment
[0017] Next, the first exemplary embodiment of the present invention will be described with reference to FIGS. 1 to 5 .
[0018] (Overall configuration of a printer)
[0019] FIG. 1 is a sectional side view showing a schematic configuration of a printer 1 (an example of the “printing apparatus” of the present invention) according to the first exemplary embodiment of the present invention. The printer 1 is an electro photographic color LED printer. Hereinafter, a left side of the figure is regarded as a front side of the printer. In addition, in FIG. 1 , some symbols of components, which are identical for respective colors, are omitted.
[0020] The printer 1 includes a body casing 2 . A feed tray 4 which can carry multiple sheets 3 (an example of a transfer medium) is attached at the bottom of the body casing 2 . The sheets 3 loaded on the feed tray 4 are delivered to a registration roller 6 provided at an upper side of the feed tray 4 by a supply roller 5 provided on the upper front edge of the feed tray 4 . The registration roller 6 conveys the sheets 3 to a belt unit 11 of a printing unit 10 .
[0021] The printing unit 10 mainly includes the belt unit 11 , exposure units 17 ( 17 K, 17 Y, 17 M, and 17 C), process units 19 ( 19 K, 19 Y, 19 M and 19 C) and a fixing unit 31 .
[0022] The belt unit 11 has an annular belt 13 stretched between front and rear paired belt support rollers 12 A and 12 B. The sheets 3 , which are adsorbed onto the belt 13 by static electricity, are conveyed backward by driving the belt 13 . In addition, transfer rollers 14 are provided inside the belt 13 at positions facing photoconductive drums 28 of the process units 19 with the belt 13 therebetween.
[0023] The exposure units 17 K, 17 Y, 17 M and 17 C correspond to black, yellow, magenta and cyan respectively. Each exposure unit includes a LED head 18 at a lower end portion. The LED head 18 has multiple LEDs arranged in a row. The exposure units 17 let each LED of the LED head 18 emit light according to the print data supplied to each exposure unit 17 . The light is scanned on the corresponding photoconductive drum 28 one line at a time.
[0024] A pattern sensor 15 (an example of the “measuring unit” of the invention), which is used, for example, detecting patterns formed on the surface of the belt 13 , is provided below the belt 13 . The pattern sensor 15 irradiates to the surface of the belt 13 , receives the reflected light by a phototransistor, and outputs a signal depending on an amount of the received light. Furthermore, a cleaner 16 , which recycles toner and paper dust adhered to the belt 13 , is provided below the belt unit 11 .
[0025] The process units 19 K, 19 Y, 19 M and 19 C correspond to black, yellow, magenta and cyan respectively. Each process unit includes a frame 21 and a developing cartridge 22 . Each developing cartridge 22 includes a toner storage chamber 23 , a supply roller 24 and a developing roller 25 . The toner storage chamber 23 stores a toner of a corresponding color. The toner removed from the toner storage chamber 23 is supplied to the developing roller 25 by rotating the supply roller 24 . The toner is positively charged by friction between the supply roller 24 and the developing roller 25 .
[0026] In addition, the photoconductive drum 28 and a scorotron charger 29 are provided at a lower portion of the frame 21 . The photoconductive drum 28 is formed by providing a positively charged photoconductive layer on a surface of a cylindrical drum body connected to the ground. The surface of the photoconductive drum 28 is uniformly positively charged (for example, +900V) by discharging from the charger 29 as the drum 28 rotates. By being exposed by scanning from the exposure units 17 , the surface voltage becomes partially low (for example +100 V), corresponding to the intensity of the irradiated light. An electrostatic latent image corresponding to the image to be formed on the sheet 3 is formed thereby.
[0027] The toner which is positively charged and carried by the developing roller 25 is supplied to the electrostatic latent image on the photoconductive drum 28 by applying a developing bias voltage (for example +450V) to the developing roller 25 . In this way, the electrostatic latent image on the photoconductive drum 28 is made visible as a toner image.
[0028] When the sheet 3 on the belt 13 passes through each transfer position between each photoconductive drum 28 and each transfer roller 14 , the toner images carried on the photoconductive drum 28 are sequentially transferred to the sheet 3 by applying a transfer bias voltage (for example −700 V) to the transfer roller 14 , so as to be superposed. The sheets 3 to which the toner images are transferred enter into the fixing unit 31 , which is provided at the back of the body casing 2 . Then the toner images are thermally fixed to the sheet 3 . The sheet 3 is then conveyed upward, and discharged from the top of the body casing 2 by a discharging roller 32 .
(Electrical Configuration of the Printing Apparatus)
[0029] FIG. 2 is a block diagram briefly showing an electric configuration of the printer 1 .
[0030] As shown in FIG. 2 , the printer 1 includes a central processing unit (CPU) 40 , a read-only memory (ROM) 41 , a random access memory (RAM) 42 , a non-volatile read only memory (NVRAM) 43 , and a network interface 44 . A program for executing various operations of the printer 1 , such as a job execution process which will be described later, is stored in the ROM 41 . The CPU 40 (an example of the “receiving unit, first judging unit, measuring unit, expanding unit and control unit” of the present invention) controls each units and causes the processing results to be stored in the RAM 42 or the NVRAM 43 , according to the program read from the ROM 41 . The network interface 44 is connected to an external computer (not shown in Figures), etc., via communication lines such as LAN, etc., enabling the data to be mutually communicated.
[0031] In addition to the printing unit 10 and the pattern sensor 15 , the printer 1 also includes a display unit 47 and an operating unit 48 . The display unit 47 includes a display and a lamp, which can display the operation conditions of various setting screens and devices. The operating unit 48 includes several buttons, through which a user can input various instructions.
[0032] Furthermore, the printer 1 includes a high-voltage application circuit 49 that applies voltage to the transfer roller 14 , the developing roller 25 and the charger 29 . The CPU 40 can adjust the magnitude of the voltage applied to the portions by controlling the high-voltage application circuit 49 .
(Job Execution Process)
[0033] FIG. 3 is a flowchart showing a job execution process. When the CPU 40 receives a print job (an example of the “print request” of the present invention), which is sent from the external computer via the network interface 44 , the CPU 40 registers the print job in a printer queue. Several print jobs can be registered in the printer queue. The CPU 40 executes the job execution process shown in FIG. 3 sequentially for each print job registered in the printer queue.
[0034] The print jobs received include a so-called secure job, that is, the print starts on condition that the user inputs a print starting instruction into the operating unit 48 . When the secure job is received by the CPU 40 , the CPU 40 , for example, forbids a printing process (including an expanding process) by not registering the printing process in the printer queue but storing the printing process in the NVRAM 43 . The CPU 40 registers the secure job in the printer queue when the print starting instruction is received by the operating unit 48 , so as to become an object of the job execution process. In this way, the expanding process can be executed according to the measurement data (the density correction data described later) most recent to not the timing when the printing is requested but the timing when the printing is executed. In this case, the CPU 40 servers as the “receiving unit” of the present invention.
[0035] In the job execution process, the CPU 40 first determines whether the expanding process of the whole pages of the print job currently being processed (hereinafter called “current job”) has finished (S 101 ). The CPU 40 delivers expanded data per page to the printing unit 10 and causes the printing unit to print the image based on the expanded data on the sheet 3 , each time the expanded data per page is generated.
[0036] If there is an unexpanded page (S 101 is NO), the unexpanded print data (such as PDL data) per page starts to be expanded (S 103 ). In the expanding process, the print data of a page currently being processed (hereinafter called “current page”) is analyzed, and the intermediate data for each color is generated. The expanded data (bitmap data) is generated by adjusting a tone based on the density correction data stored in the current NVRAM 43 (hereinafter called “current correction data”), while the intermediate data is expanded. In this case, the CPU 40 serves as the “expanding unit” of the invention.
[0037] Next, the CPU 40 judges whether the predetermined correction execution condition is satisfied during the expanding process of the current page (S 105 ). The correction execution condition is for determining whether it is necessary to execute density measurement (or the execution is desirable) to ensure image quality. Specifically, example of the conditions are, when time elapsed, rotation number of the photoconductive drum 28 , total print number or temperature change, since the previous density measurement, exceeds a reference value, and when the correction instruction is input into the operating unit 48 by the user, etc.
(1) The Correction Execution Condition is Satisfied, and the Current Page Needs to be Corrected
[0038] When the correction execution condition is satisfied (S 105 is YES), the CPU 40 determines whether the current page is a page that needs to be corrected according to header information or an analysis result of the print data (S 107 ). In this case, the CPU 40 serves as a “second determination unit” of the present invention. The page that needs to be corrected is a page requiring high quality print, for example, a color page, or a high-resolution page with a resolution above a predetermined level. A color page refers to a page that is printed by using more than one of black, yellow, magenta and cyan toners, and a monochrome page refers to a page that is printed by using one of the black, yellow, magenta and cyan toners. Meanwhile, a page formed by a single color toner other than black may be referred to as a color page instead of a monochrome page.
[0039] When the current page needs to be corrected (S 107 is YES), the CPU 40 interrupts the expanding process of the current page, determines the current page as a “re-expanding required page” (S 109 ), and stores an expanded data of an expanded portion of the re-expanding required page and a print data of an unexpanded portion of the re-expanding required page in, for example, the NVRAM 43 . Thereafter, the density measurement as described below is performed, and the current correction data is updated according to a most recent density measurement data produced according to the measurement (S 111 ).
[0040] In the density measurement, first, a density pattern P shown in FIG. 4 is formed on the belt 13 by the printing unit 10 . The density pattern P is composed of several patches along the moving direction of the belt 13 . In more detail, the density pattern P includes 5 patches with different densities for each color of black, yellow, magenta and cyan (black patches K 1 -K 5 , cyan patches C 1 -C 5 , magenta patches M 1 -M 5 , and yellow patches Y 1 -Y 5 , some of which are omitted from the drawings).
[0041] Next, the density of each patch is measured by the pattern sensor 15 . According to the measurement, the density correction data for each color is generated respectively so that the density of the image formed on the sheets 3 by the printing unit 10 becomes an ideal density, for each of the tones formed by dividing the density range from 0% to 100% into 256 equal portions. The density correction data thus obtained contains adjusting values for adjusting the emission intensity of the LEDs of the LED heads 18 for each tone and adjusting values for adjusting the developing bias voltage (that is, adjusting the density of all tones). The CPU 40 stores the generated density correction data in the NVRAM 43 and updates the current correction data.
[0042] Next, with regard to the re-expanding required page stored in the NVRAM 43 , the CPU 40 executes the expanding process while adjusting the tones by using the current correction data that has been updated (S 113 ). Therefore, the printing unit 10 can print the image, the density of which is corrected by the most recent density correction data, on the sheet 3 . In this case, the CPU 40 serves as the “control unit” of the invention.
[0043] The CPU 40 not only expands the unexpanded portion of the re-expanding required page that has been suspended of the expanding process, but also re-expands the expanded portion using the updated current correction data. Therefore, compared to the situation which only the unexpanded portion is expanded according to the updated current correction data, the print quality of the whole page can be improved.
[0044] Furthermore, although the print data of the unexpanded portion is expanded, the expanded data of the expanded portion, which had been expanded before the expanding process was suspended in S 109 , is stored in the NVRAM 43 , and after the current correction data is updated, the stored expanded data is re-expanded by using the updated current correction data. The print data of the expanded portion before the expanding process may be expanded by using the updated current correction data. However, according to this configuration, the print data before the expanding process needs to be stored in the NVRAM 43 until the expanding process of the whole current page is completed, and the print data needs to be obtained from the external computer again. According to the first exemplary embodiment, the expanded data before the suspension of the expanding process, which was expanded by a previous current correction data, can be re-expanded by using the updated current correction data (that is, correction data generated after the suspension). Thus, it is unnecessary to store the print data before the expanding process in the NVRAM 43 , etc.
[0045] After the CPU 40 completes the expanding process of all of the re-expanding required pages, the process returns to S 101 .
(2) The Correction Execution Condition is not Satisfied, or the Current Page does not Need to be Corrected
[0046] When the correction execution condition is not satisfied (S 105 is No), for the print data of the current page, the CPU 40 directly executes the expanding process without executing the density measurement (S 115 ). Next, whether the current page was expanded before the expanding process is suspended during the current job (refer to S 109 ), and whether the current page needs to be corrected is determined (S 117 ).
[0047] If the current page is a page that is expanded before the suspension and needs to be corrected (S 117 is YES), the current page is determined as the re-expanding required page (S 119 ), and the printing process is suspended by storing the expanded data in the NVRAM 43 without delivering it to the printing unit 10 . Then the process returns to S 101 . Accordingly, the page which was corrected before the suspension of the expanding process as well as the page whose process has been suspended in S 109 is re-expanded by using the updated density correction data in S 113 . That is, for not only the page whose expanding process has been suspended but for also the previous pages that need to be corrected, the image whose density is corrected by the current density correction data can be printed on the sheet 3 .
[0048] Thus, in the same printing job, the decrease in the print quality, such as difference in tones, can be prevented by using old and new density correction data which differs from each other. In addition, with regard to the current job, even if all of the pages are expanded (S 101 is YES), there is possibility that the expanded pages that need to be corrected before interruption or the re-expanding required pages still remain unprinted. Therefore, whether the re-expanding required pages still remain unprinted should be determined (S 121 ), and if it is determined that the re-expanding required pages still remain unprinted (S 121 is YES), expanded data of the re-expanding required page is provided to the printing unit 10 (S 123 ). If there is no re-expanding required page (S 121 is NO) or if the expanded data of the re-expanding required pages is provided to the printing unit 10 , the execution of the current job is terminated and the next printing job that has been registered in the printing queue will be started.
[0049] If the current page is not the page that is expanded before the suspension and needs to be corrected (S 117 is NO), the current page is not determined as the re-expanding required page, and the expanded data is provided to the printing unit 10 . Then, the process returns to S 101 . In addition, if the correction execution condition is satisfied but the current page is not the page that needs to be corrected (S 105 is YES and S 107 is NO), the process directly proceeds without executing the density measurement (S 115 ), and then, it is determined NO in S 117 , and the process returns to S 101 . Accordingly, when the current page is not the data that needs to be corrected, such as monochrome image data, low resolution data, etc., the printing process can be executed promptly by executing the expanding process prior to the deviation amount measurement.
(3) Specific Examples
[0050] FIG. 5 is a time chart of the expanding process and density measurement. FIG. 5 shows a process corresponding to a 4 page print job, in which page 1 is a monochrome image and pages 2 to 4 are color images. As shown in FIG. 5 , the expanding processes of the pages 1 and 2 are not suspended. However, because page 2 is a color page (S 105 is NO, and S 117 is YES), page 2 is determined as the re-expanding required page and the printing is suspended.
[0051] Next, if the correction execution condition is satisfied during the expanding of page 3 (S 105 is YES), the expanding process is suspended at that time (S 109 ). After the density measurement is performed (S 111 ), the expanding process of pages 2 and 3 is restarted by using the current density correction data. Then, page 4 is also expanded by using the current density correction data.
Effects of the Embodiment
[0052] According to the above-described embodiment, if the correction execution condition is satisfied during the expanding of the current page (which is a single page), the expanding process of the current page is suspended, the density measurement is performed, and then, according to the measurement after the suspension, expanding of at least the unexpanded portion of the current page is started. Therefore, compared to the situation when the density measurement is performed after the expanding process of the current page or the current job is terminated, the delay in reflection of the measurement of the deviation amount in the expanding process of the print data can be prevented.
Second Exemplary Embodiment
[0053] FIG. 6 corresponds to the second exemplary embodiment of the present invention. The difference between the first exemplary embodiment and the second exemplary embodiment is the content of the job process, while others in the second exemplary embodiment are similar to those of the first exemplary embodiment. Thus, the symbols that are the same as those of the first exemplary embodiment may be omitted, and the following description is based on features that differ from the first exemplary embodiment.
[0054] FIG. 6 is a flowchart showing a job process of the present embodiment. The CPU 40 executes the job execution process shown in FIG. 6 sequentially for each print job registered in the printer queue. First, determining factor, for predictively determining whether the correction execution condition may be satisfied during expanding processes of the current job, is obtained (S 201 ).
[0055] Examples of the determining factors are listed in the following.
[0056] (a) When the correction execution condition is that the total print number since the previous density measurement is higher than a predetermined amount, accumulated total printed pages P 1 which shows the accumulated total number of pages printed before the expanding process is executed to the current page and current job printed pages P 2 which shows the total number of pages printed during executing the current job are the determining factors. When the sum of the accumulated total printed pages P 1 and the current job printed pages P 2 (P 1 +P 2 ) is larger than the predetermined amount, it is determined that the correction execution condition may be satisfied during the expanding processes of the current job. Meanwhile, when the sum is smaller than the predetermined amount, it is determined that the correction execution condition will not be satisfied during the expanding processes of the current job.
[0057] (b) When the correction execution condition is that the elapsed time since the previous density measurement is larger than a predetermined amount, elapsed time T 1 until the printing is requested (or before the expanding process of the current job) and printing time T 2 of the current job are the determining factors. When the sum of the elapsed time T 1 and the printing time T 2 of the current job is larger than the predetermined amount, it is determined that the correction execution condition may be satisfied during the expanding processes of the current job. Meanwhile, when the sum is smaller than the predetermined amount, it is determined that the correction execution condition will not be satisfied during the expanding processes of the current job. The printing time 2 can be predicted from the print data amount and the printed pages of the current job.
[0058] If the CPU 40 determines that the correction execution condition will not be satisfied during the expanding processes of the current job (S 203 is NO), the CPU 40 will adjust the tone by using the current correction data while executing the expanding process, for all of the pages of the current job, without performing the density measurement (S 213 ). Then, the execution of this job is terminated.
[0059] If the CPU 40 determines that the correction execution condition will be satisfied during the expanding processes of the print job (S 203 is YES), the CPU 40 will adjust the tone by using the current correction data while executing the expanding process (S 205 ), until a previous page of a page at which the correction execution condition may be satisfied at a high possibility during the expanding process (hereinafter called “the page at which the condition may be satisfied”), without performing the density measurement. However, with regard to the pages subsequent to the page at which the condition may be satisfied, the expanding process will be delayed until the correction execution condition is satisfied (S 207 is NO). Similarly to S 111 of FIG. 3 , when the correction execution condition is satisfied (S 207 is YES), the density measurement is performed. The current correction data is updated based on the current density measurement data produced according to the measurement (S 209 ).
[0060] Next, with regard to the page at which the condition may be satisfied and pages subsequent to the page at which the condition may be satisfied, the tone is adjusted by using the updated current correction data while executing the expanding process (S 211 ). Then, this job is terminated. Therefore, the printing unit 10 can print the image, whose density has been corrected by the most recent current density correction data, on the sheets 3 .
[0061] As described above, according to the second exemplary embodiment of the present invention, when a print request is received, whether the correction execution condition may be satisfied during the expanding process of the print data corresponding to the print request can be predictively determined before the expanding process of the print data. When it is determined that the correction execution condition may be satisfied, based on the prediction, the expanding process of the print data is delayed, and then the deviation amount is measured. Subsequently, the print data which was stored is started to be expanded based on the measured deviation amount. According to this configuration, compared to that the density measurement is performed after the expanding process of the current page or the current job is terminated, the delay in reflection of the current density correction data to the expanding process of the print data can be prevented. Further, for the page in which the condition may be satisfied, because it can be previously avoided that the correction condition is satisfied during the expanding process, the decrease in the print quality such as deviation in tones, which occurs by using both the old and new density correction data, can be prevented.
Other Embodiments
[0062] While the present invention has been showed and described with reference to certain exemplary embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. Specifically, among the components described in each exemplary embodiment, components other than the components belonging to the broadest concept of the invention are additive, and can be omitted.
[0063] (1) A printer that forms an image by electrophotographic method is described in the above-described exemplary embodiments. However, for example, the present invention can also be applied to image forming apparatuses using other methods such as inkjet method. Further, the invention can also be applied when data received by facsimile is printed, data captured by a scanner (copy) is printed and data obtained from external storage media (direct printing) is printed as an example of the image forming.
[0064] (2) According to the above-described exemplary embodiments, when the correction execution condition is satisfied, the density measurement is performed, and the density of the image is corrected according to the density measurement. However, the scope of the invention is not limited by the above configuration. For example, it may be configured that a heretofore known correction pattern for correcting the deviation amount of the position is formed on the belt 13 , and the deviation amount of the position (color deviation amount) between images of different colors is measured by the pattern sensor 15 , and the deviation amount of the position is corrected according to the measurement.
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A printing apparatus comprising: a printing unit configured to print an image based on expanded data; a measuring unit configured to measure a deviation amount of at least one of a position and a density of the image printed by the printing unit when a correction execution condition is satisfied; an expanding unit configured to expand print data based on the measurement by the measuring unit, so as to produce the expanded data; and a control unit, wherein when the correction execution condition is satisfied during the expanding of current print data which corresponds to a current page being expanded, the control unit is configured to control the expanding unit to suspend the expanding of the current print data, the measuring unit to measure the deviation amount, and the expanding unit to restart expanding an unexpanded portion of the current print data based on the measurement.
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RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 62/033,387, filed Aug. 5, 2014, the entirety of which is herein incorporated by reference.
BACKGROUND
[0002] Modern vehicles include heating, ventilation, and air conditioning (HVAC) systems for improving passenger comfort.
[0003] In general, vehicle air conditioning systems include an evaporator heat exchanger in communication with a compressor and a condenser. A compressor receives heated refrigerant from the evaporator and compresses it into a high pressure gas for communication to the condenser. The condenser then cools the gaseous refrigerant into a cool liquid refrigerant for communication back to the evaporator. A blower forces air across the evaporator, providing cooled air into the passenger compartment.
[0004] A vehicle heating system includes a heater core that receives hot engine coolant from the engine. A blower forces air across the heater core, providing heated air to the passenger compartment. The system may also include one or more conduits, which are retained in place by a conduit retainer (or, pipe retainer), such as a bracket. The conduit retainer is typically fastened to the vehicle by way of a fastener (e.g., a screw or bolt).
SUMMARY
[0005] A pipe retainer assembly according to an exemplary aspect of the present disclosure includes, among other things, a mount including one of a slot and a projection, and a pipe retainer including a latch and the other of a slot and a projection. The slot is received in the projection and the latch is engaged with the mount. The assembly further includes a fluid conduit held in place by the mount and the pipe retainer.
[0006] A pipe retainer according to an exemplary aspect of the present disclosure includes, among other things, a first projection for engagement with a first slot in a mount, a second projection for engagement with a second slot in the mount, and a latch for engagement with a wall of the mount.
[0007] A method according to an exemplary aspect of the present disclosure includes, among other things, positioning a conduit relative to a mount such that an upset bead of the conduit is received within a groove of the mount, and sliding a pipe retainer relative to the mount to connect the pipe retainer to the mount.
[0008] The embodiments, examples and alternatives of the preceding paragraphs, the claims, or the following description and drawings, including any of their various aspects or respective individual features, may be taken independently or in any combination. Features described in connection with one embodiment are applicable to all embodiments, unless such features are incompatible.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The drawings can be briefly described as follows:
[0010] FIG. 1 schematically illustrates a vehicle system.
[0011] FIG. 2 is a perspective view of an example pipe retainer according to this disclosure.
[0012] FIG. 3 is a rear perspective view of the pipe retainer of FIG. 2 .
[0013] FIG. 4 illustrates the pipe retainer in an assembled condition.
[0014] FIG. 5 illustrates an example pipe according to this disclosure.
DETAILED DESCRIPTION
[0015] FIG. 1 illustrates a vehicle system 10 for thermally managing a heat source 12 of a vehicle 14 . The heat source 12 could be an engine, a transmission, or any other heat generating component of the vehicle 14 . The heat source 12 generates heat during operation of the vehicle 14 and therefore may need to be cooled during some conditions.
[0016] In one embodiment, the vehicle system 10 includes a heat exchanger 16 and a thermal bypass valve (TBV) 18 . A TBV 18 need not be present in all examples. A supply conduit 20 and a return conduit 22 connect the components of the vehicle system 10 in a closed circuit.
[0017] In one non-limiting embodiment, the heat exchanger 16 is a transmission oil cooler configured as an air/oil heat exchanger. Other types of heat exchangers are also contemplated within the scope of this disclosure, including but not limited to, engine oil coolers or hydraulic fluid oil coolers. In addition, the heat exchanger 16 may exchange heat between any two different fluid exchange medium.
[0018] The TBV 18 can be actuated to bypass the heat exchanger 16 under certain temperature conditions if the heat transfer function of the heat exchanger 16 is not required. In one embodiment, the TBV 18 is a multi-port bypass valve. The vehicle system 10 may employ any suitable bypass valve for selectively bypassing the functionality of the heat exchanger 16 .
[0019] The vehicle system 10 may communicate a fluid F 1 in the closed circuit. For example, the fluid F 1 , which is relatively hot, is communicated from the heat source 12 to the heat exchanger 16 via the supply conduit 20 . The fluid F 1 may circulate through the heat exchanger 16 to exchange heat with another fluid F 2 , such as airflow, to provide a cooled fluid F 3 . The fluid F 2 may be communicated across the heat exchanger 16 with or without the use of a fan to exchange heat with the fluid F 1 . After exchanging heat with the fluid F 2 , the fluid F 1 is returned to the heat source 12 as cooled fluid F 3 via a return conduit 22 to thermally manage (i.e., heat or cool) the heat source 12 .
[0020] FIG. 2 illustrates an example pipe retainer assembly 24 . In this example, the pipe retainer assembly 24 includes a pipe retainer 26 configured to retain the supply and return conduits 20 , 22 of an example system, such as the system 10 of FIG. 1 , relative to an HVAC (heating, ventilation, and air conditioning) module 28 . The pipe retainer 26 may be integrally formed as one plastic piece. This disclosure is not limited to plastic, however, and extends to other types of materials.
[0021] In this example, the HVAC module 28 may be an HVAC package to be mounted on a particular vehicle. The illustrated portion of the HVAC module 28 is, in one example, mounted adjacent the front of dash (FOD) of a vehicle. This disclosure is not limited to any particular HVAC module 28 , however. Further, the pipe retainer assembly 24 could be used to connect conduits to other engine components, such as the heat source 12 .
[0022] The HVAC module 28 includes a mount 30 , which in this example is integral to the HVAC module 28 , having a first platform 32 and a second platform 34 (perhaps best seen in FIG. 3 ). The first and second platforms 32 , 34 are spaced-apart from one another in a first direction D 1 (e.g., the side-to-side direction) and a second direction D 2 (e.g., the up-and-down, or vertical, direction) perpendicular to the first direction D 1 .
[0023] The first platform 32 includes an upper surface 36 having a pipe locating feature 38 ( FIG. 3 ) and a dovetail slot 40 formed therein. The pipe locating feature 38 , in this example, is a groove corresponding to an upset bead 42 formed in the supply conduit 20 ( FIG. 5 ). In this example, the upset bead 42 projects from the outer surface of the supply conduit 20 , and extends around the entire perimeter (e.g., circumference) of the supply conduit 20 .
[0024] The second platform 34 has an upper surface 43 that similarly includes a pipe locating feature 44 , in this example a groove, and a dovetail slot 46 . The pipe locating feature 44 corresponds to an upset bead 48 of the return conduit 22 .
[0025] The pipe retainer 26 includes first and second dovetail projections 50 , 52 configured to slide into the first and second dovetail slots 40 , 46 of the platforms 32 , 34 . The first and second dovetail projections 50 , 52 are also spaced-apart from one another in the first and second directions D 1 , D 2 , to correspond to the locations of the dovetail slots 40 , 46 . As is known of dovetail joints, the dovetail projections 50 , 52 and the slots 40 , 46 may be tapered to vertically maintain the position of the retainer 26 relative to the HVAC module 28 . While in this example the pipe retainer 26 includes the dovetail projections 50 , 52 and the platforms 32 , 34 include the dovetail slots 40 , 46 , the pipe retainer 26 could include slots and the platforms 32 , 34 could include projections. Further, this disclosure is not limited to dovetail joints, and extends to other types of joints, including joints that allow for sliding of the pipe retainer 26 relative to the mount 30 and resistance to separation in the direction perpendicular to sliding (e.g., D 2 ).
[0026] As illustrated in FIG. 4 , in order to axially (e.g., see the axial direction A) maintain the retainer 26 relative to the HVAC module 28 , the retainer 26 includes a latch 54 is configured to engage a latch surface 55 of a vertical wall 56 of the mount 30 between the first and second platforms 32 , 34 . The vertical wall 56 connects the first and second platforms 32 , 34 by spanning the distance between the two platforms 32 , 34 . The latch 54 is configured to snap into place relative to the vertical wall 56 .
[0027] In one example, the conduits 20 , 22 include the upset beads 42 , 48 and tapered ends 58 , 60 (respectively). At the tapered ends 58 , 60 , the diameter of the conduits 20 , 22 gradually reduce in dimension approaching the end. For installation, the retainer 26 is provided axially between the upset beads 42 , 48 and the tapered ends 58 , 60 , and is then axially slid, along the length of the supply and return conduits 20 , 22 , in the axial direction A, such that the dovetail projections 50 , 52 are fully received in the dovetail slots 40 , 46 and such that the latch 54 engages the wall 56 , as generally illustrated in FIG. 4 .
[0028] The conduits 20 , 22 may include an additional upset bead for retaining additional plumbing relative to the conduits 20 , 22 , such as under-hood plumbing. One such upset bead 57 is illustrated in FIG. 5 . In that example, upset bead 57 is spaced-apart from upset bead 42 along the length of the conduit 20 .
[0029] This disclosure allows for a secure retention between the conduits 20 , 22 and an HVAC module 28 prior to the assembly of the HVAC module 28 relative to an vehicle instrument panel or front of dash (FOD). Further, no fasteners are required, which reduces assembly time.
[0030] Although the different examples have the specific components shown in the illustrations, embodiments of this disclosure are not limited to those particular combinations. It is possible to use some of the components or features from one of the examples in combination with features or components from another one of the examples.
[0031] One of ordinary skill in this art would understand that the above-described embodiments are exemplary and non-limiting. That is, modifications of this disclosure would come within the scope of the claims. Accordingly, the following claims should be studied to determine their true scope and content.
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A pipe retainer assembly according to an exemplary aspect of the present disclosure includes, among other things, a mount including one of a slot and a projection, and a pipe retainer including a latch and the other of a slot and a projection. The slot is received in the projection and the latch is engaged with the mount. The assembly further includes a fluid conduit held in place by the mount and the pipe retainer. A method is also disclosed.
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FIELD OF THE INVENTION
The present invention relates to universal joint assemblies and more particularly to a tunable rubber isolated bipod universal joint assembly.
BACKGROUND OF THE INVENTION
The use of universal joints in automotive systems is common within the industry. Universal joints transmit constant torque through an angle between two shafts. However, it is important to reduce any noise or vibrations through the joint that may cause damage or annoyance during operation. Accordingly, isolators have been used to encase the universal joint. The isolators have typically been made from elastomeric materials that elastically deform as the universal joint moves relative to a housing surrounding the joint. In this way, the isolator absorbs a portion of the vibrations transmitted through the universal joint. While these isolators have been successful for their intended purpose, there is room in the art for improvements.
SUMMARY OF THE INVENTION
A universal joint assembly is provided. The assembly includes a universal joint and a housing encasing the universal joint. An isolator encases the housing. The isolator includes at least one chamber formed therein for defining a stiffness of the isolator. The housing is moveable relative to the isolator by compression of the isolator. The stiffness of the isolator is tunable by modifying the characteristics of the chamber.
Further areas of applicability of the present invention will become apparent from the detailed description provided hereinafter. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will become more fully understood from the detailed description and the accompanying drawings, wherein:
FIG. 1A is a front sectional view of a universal joint assembly constructed according to the principles of the present invention;
FIG. 1B is a side sectional view of universal joint assembly of the present invention;
FIG. 2 is a front view of a tunable isolation member constructed according to the principles of the present invention; and
FIG. 3 is a front view of a housing member constructed according to the principles of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to FIGS. 1A and 1B , a bipod universal joint assembly constructed according to the principles of the present invention is generally indicated by reference numeral 10 . The assembly 10 includes a bipod universal joint 12 , a bipod housing 14 , a tunable isolator 16 , and a housing 18 . In the particular example provided, the assembly 10 is used in operative association with an automotive driveshaft. However, it should be appreciated that the assembly 10 may be used in various other environments requiring torque to be transmitted through an angle.
The bipod universal joint 12 includes a spider 20 having a central hub 22 and a pair of trunnions 24 extending from opposite sides thereof. The hub 22 is coupled to a stub shaft 26 which defines a horizontal axis 23 . The stub shaft 26 is in turn coupled to a conventional driveshaft tube (not shown). The trunnions 24 are generally cylindrical in shape and include spherical ends 28 . The trunnions 24 define a vertical axis 25 .
The bipod universal joint 12 further includes a pair of rollers 30 . The rollers 30 are coupled to the trunnions 24 of the spider 20 . In the example provided, the rollers 30 have a truncated spherical outer shape and a cylindrical inner bore 32 . The cylindrical inner bore 32 includes a plurality of needles (not shown) along its inner circumference. Each roller 30 is fitted overtop a trunnion 24 such that the trunnion 24 fits within the cylindrical inner bore 32 . The rollers 30 are able to move up and down relative to the trunnions 24 along the axis 25 and are able to rotate relative to the spider 20 .
The bipod housing 14 encases the bipod universal joint 12 . In the example provided, the bipod housing 14 includes a body 34 having an inner cavity 36 sized to receive the bipod universal joint 12 therein. The inner cavity 36 includes top and bottom cylindrical tracks 38 formed therein. The top and bottom cylindrical tracks 38 are sized to constrain the spherical ends 28 of the trunnions of the spider 20 therein. The inner cavity 36 further includes roller tracks 40 formed therein. The roller tracks 40 are generally cylindrical in shape and are sized to receive the rollers 30 therein. The roller tracks 40 prevent the rollers 30 from rotating relative to the bipod housing 14 while simultaneously allowing the rollers 30 (and therefore the entire universal joint 12 ) to move along the axis 23 . The bipod universal joint 12 in conjunction with the bipod housing 14 allow torque to be transmitted through the universal joint 12 at an angle and on to a driveshaft (not shown) of the motor vehicle (not shown).
The tunable isolator 16 encases the bipod housing 14 . In the particular example provided, the tunable isolator 16 is made from rubber. However, it is to be appreciated that any elastomeric material may be employed with the present invention. Turning to FIG. 2 , the tunable isolator 16 includes an inner socket 42 that is shaped to match the outer contour of the bipod housing 14 ( FIG. 1 ). In the particular example provided, the tunable isolator 16 includes vertical wings 44 and horizontal wings 46 . The vertical wings 44 extend generally vertically and the horizontal wings 46 extend generally horizontally. The wings 44 , 46 are adapted to engage the housing 18 .
Each vertical wing 44 may include a first chamber 48 and a second chamber 50 . The first and second chambers 48 , 50 may extend throughout the length of the tunable isolator 16 along the axis 23 and may be formed within an interior portion of the tunable isolator 16 . In the particular example provided, the first and second chambers 48 , 50 have an oval cross sectional shape. Moreover, the first chambers 48 are larger than the second chambers 50 and may be formed in the tunable isolator 16 at a location that is relatively closer to the inner socket 42 . The horizontal wings 46 may each include a third chamber 52 . The third chambers 52 may extend throughout the length of the tunable isolator 16 along the axis 23 . The third chambers 52 can include a chevron, as shown in FIG. 2 . The third chambers 52 are preferably larger than the first and second chambers 48 , 50 . The first, second, and third chambers 48 , 50 , 52 allow the elastomeric material of the tunable isolator 16 to compress and deflect to a greater extent (thereby partially defining the stiffness of the tunable isolator 16 ). It is to be appreciated that the shape, size, and location of the chambers 48 , 50 , and 52 within the tunable isolator 16 may be varied without departing from the scope of the present invention. Moreover, the tunable isolator 16 may include a number of chambers greater than or fewer than those illustrated and may include none of the chambers without departing from the scope of the present invention. By adjusting the properties of the chambers 48 , 50 , 52 , the tunable isolator 16 is easily “tunable” to provide any desired stiffness.
Turning back to FIG. 1 , 1 A and 1 B. the housing 18 receives the tunable isolator 16 and is coupled to a source of torque, such as, for example, an engine (not shown). More specifically, the housing 18 includes a control bore 53 , which is sized to receive the tunable isolator 16 , the bipod housing 14 and the bipod universal joint 12 , and a plurality of drive tabs 55 that extend inwardly into the control bore 53 and drivingly engage the tunable isolator 16 . The control bore 53 is generally cylindrical, as shown in FIG. 14 . The drive tabs 55 are disposed on opposite sides of each of the horizon and vertical wings 46 , 48 . Accordingly, drive torque that is transmitted between the housing 18 and the stub shaft 26 (or vice versa) is transmitted through the tunable isolater 16 . The tunable isolator 16 allows the bipod universal joint 12 and bipod housing 14 to move relative to the housing 18 by compression and elastic deformation of the tunable isolator 16 . The stiffness of the tunable isolator 16 is determined by its geometry and material characteristics and may be designed to affect the torsional compliance of the assembly 10 in any manner desired. In the example provided, this designing or “tuning” is accomplished by adjusting the properties of the chambers 48 , 50 , 52 .
With reference to FIG. 3 , an alternate embodiment of the bipod housing 14 is generally indicated by reference numeral 14 ′. The bipod housing 14 ′ includes a plurality of plates 54 integrated with a plastic body 56 . The plates 54 may be formed of sheet steel in an appropriate process, such as stamping, though various other materials and forming processes may be employed. Additionally, the plates 50 may be heat treated and/or coated with an appropriate coating (e.g., for lubricity, corrosion, resistance and/or wear resistance). The plates 54 form the contact surfaces for the rollers 30 and the spherical ends 28 of the trunnions 24 of the spider 20 (see FIGS. 1A , 1 B). In the example provided, there are six plates 54 , each corresponding to a point of contact with the universal joint 12 . The plates 54 contact the universal joint 12 for securing the universal joint 12 the trunnions 24 and rollers 30 of the universal joint 12 , within the bipod housing 14 ′. The plastic body 56 is preferably a high strength thermosetting plastic which may be injected into a hold (not shown) that carries the plates 54 , though various other materials may be employed. Torque transmission through the bipod housing 14 ′ puts the plastic body 56 primarily under compression between the tunable isolator 16 ( FIGS. 1A , 1 B) and the rollers 30 of the universal joint 12 .
Preferably, the plates 54 are positioned during or prior to molding of the plastic body 56 . This allows the plates 54 to be precisely positioned relative to the rollers 30 and trunnions 24 . The plates 54 are positioned such that a first pair of plates 54 contact the trunnions 24 and a second pair of plates 54 contact the rollers 30 . Moreover, the plastic body 56 is relatively less expensive to manufacture and is of lighter weight than a full steel body, while the plates 54 assure that the bipod housing 14 ′ has suitable strength and durability.
The description of the invention is merely exemplary in nature and, thus, variations that do not depart from the gist of the invention are intended to be within the scope of the invention. Such variations are not to be regarded as a departure from the spirit and scope of the invention.
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A universal joint assembly includes a universal joint and a housing encasing the universal joint. An isolator encases the housing. The isolator includes at least one chamber formed therein. The housing is moveable relative to the isolator by compression of the isolator.
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CONTINUING APPLICATION DATA
This application is a National Stage of International application No. PCT/US07/70857, filed on Jun. 11, 2007, incorporated herein by reference; which claims priority to U.S. provisional application Ser. No. 60/812,078, filed on Jun. 9, 2006, and incorporated herein by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to sodium channel blockers possessing beta-adrenergic receptor agonist activity. The present invention also includes a variety of methods of treatment using these inventive sodium channel blockers/beta-adrenergic receptor agonists.
2. Description of the Background
The mucosal surfaces at the interface between the environment and the body have evolved a number of “innate defenses”, i.e., protective mechanisms. A principal form of such an innate defense is to cleanse these surfaces with liquid. Typically, the quantity of the liquid layer on a mucosal surface reflects the balance between epithelial liquid secretion, often reflecting anion (Cl − and/or HCO 3 − ) secretion coupled with water (and a cation counter-ion), and epithelial liquid absorption, often reflecting Na + absorption, coupled with water and counter anion (Cl − and/or HCO 3 − ). Many diseases of mucosal surfaces are caused by too little protective liquid on those mucosal surfaces created by an imbalance between secretion (too little) and absorption (relatively too much). The defective salt transport processes that characterize these mucosal dysfunctions reside in the epithelial layer of the mucosal surface.
One approach to replenish the protective liquid layer on mucosal surfaces is to “re-balance” the system by blocking Na + channel and liquid absorption and simultaneously activating beta-adrenergic receptors thereby causing liquid secretion. The epithelial protein that mediates the rate-limiting step of Na + and liquid absorption is the epithelial Na + channel (ENaC). ENaC and beta-adrenergic receptors are positioned on the apical surface of the epithelium, i.e. the mucosal surface-extermal environment interface. Therefore, to inhibit ENaC mediated Na + and liquid absorption, an ENaC blocker of the amiloride class (which blocks from the extracellular domain of ENaC) must be delivered to the mucosal surface and, importantly, be maintained at this site, to achieve therapeutic utility. The present invention describes diseases characterized by too little liquid on mucosal surfaces and “topical” sodium channel blockers containing beta-adrenergic receptor agonist activity designed to exhibit the increased potency, reduced mucosal absorption, and slow dissociation (“unbinding” or detachment) from ENaC and the beta-adrenergic receptor required for therapy of these diseases.
Chronic bronchitis (CB), including the most common lethal genetic form of chronic bronchitis, cystic fibrosis (CF), are diseases that reflect the body's failure to clear mucus normally from the lungs, which ultimately produces chronic airways infection. In the normal lung, the primary defense against chronic intrapulmonary airways infection (chronic bronchitis) is mediated by the continuous clearance of mucus from bronchial airway surfaces. This function in health subjects effectively removes from the lung potentially noxious toxins and pathogens. Recent data indicate that the initiating problem, i.e., the “basic defect,” in both CB and CF is the failure to clear mucus from airway surfaces. The failure to clear mucus reflects an imbalance between the amount of liquid and mucin on airway surfaces. This “airway surface liquid” (ASL) is primarily composed of salt and water in proportions similar to plasma (i.e., isotonic). Mucin macromolecules are organized into a well defined “mucus layer” which normally traps inhaled bacteria and are transported out of the lung via the actions of cilia which beat in a watery, low viscosity solution termed the “periciliary liquid” (PCL). In the disease state, there is an imbalance in the quantities of mucus and ASL on airway surfaces. This imbalance results in a relative reduction in ASL which leads to mucus concentration, a reduction in the lubricant activity of the PCL, and a failure to clear mucus via ciliary activity to the mouth. The reduction in mechanical clearance of mucus from the lung leads to chronic bacterial colonization of mucus adherent to airway surfaces. It is the chronic retention of bacteria, the failure of local antimicrobial substances to kill mucus-entrapped bacteria on a chronic basis, and the consequent chronic inflammatory responses of the body to this type of surface infection, that lead to the syndromes of CB and CF.
The current afflicted population in the U.S. is 12,000,000 patients with the acquired (primarily from cigarette smoke exposure) form of chronic bronchitis and approximately 30,000 patients with the genetic form, cystic fibrosis. Approximately equal numbers of both populations are present in Europe. In Asia, there is little CF but the incidence of CB is high and, like the rest of the world, is increasing.
There is currently a large, unmet medical need for products that specifically treat CB and CF at the level of the basic defect that cause these diseases. The current therapies for chronic bronchitis and cystic fibrosis focus on treating the symptoms and/or the late effects of these diseases. Thus, for chronic bronchitis, inhaled β-agonists, steroids, anti-cholinergic agents, and oral theophyllines and phosphodiesterase inhibitors are all in current use. However, none of these drugs alone effectively treat the fundamental problem of the failure to clear mucus from the lung. Similarly, in cystic fibrosis, the same spectrum of pharmacologic agents are used. These strategies have been complemented by more recent strategies designed to clear the CF lung of the DNA (“Pulmozyme”; Genentech) that has been deposited in the lung by neutrophils that have futilely attempted to kill the bacteria that grow in adherent mucus masses and through the use of inhaled antibiotics (e.g. “TOBI”) designed to augment the lungs' own killing mechanisms to rid the adherent mucus plaques of bacteria. A general principle of the body is that if the initiating lesion is not treated, in this case mucus retention/obstruction, bacterial infections become chronic and increasingly refractory to antimicrobial therapy. Thus, a major unmet therapeutic need for both CB and CF lung diseases is an effective means of re-hydrating airway mucus (i.e., restoring/expanding the volume of the ASL) and promoting its clearance, with bacteria, from the lung.
R. C. Boucher, in U.S. Pat. No. 6,264,975, describes the use of pyrazinoylguanidine sodium channel blockers for hydrating mucosal surfaces. These compounds, typified by the well-known diuretics amiloride, benzamil, and phenamil, are effective. However, these compounds suffer from the significant disadvantage that they are (1) relatively impotent, which is important because the mass of drug that can be inhaled by the lung is limited; (2) rapidly absorbed, which limits the half-life of the drug on the mucosal surface; and (3) are freely dissociable from ENaC. The sum of these disadvantages embodied in these well known diuretics produces compounds with insufficient potency and/or effective half-life on mucosal surfaces to have therapeutic benefit for hydrating mucosal surfaces.
Clearly, what is needed are drugs that are more effective at restoring the clearance of mucus from the lungs of patients with CB/CF. The value of these new therapies will be reflected in improvements in the quality and duration of life for both the CF and the CB populations.
Other mucosal surfaces in and on the body exhibit subtle differences in the normal physiology of the protective surface liquids on their surfaces but the pathophysiology of disease reflects a common theme, i.e., too little protective surface liquid. For example, in xerostomia (dry mouth) the oral cavity is depleted of liquid due to a failure of the parotid sublingual and submandibular glands to secrete liquid despite continued Na + (ENaC) transport mediated liquid absorption from the oral cavity. Similarly, keratoconjunctivitis sira (dry eye) is caused by failure of lacrimal glands to secrete liquid in the face of continued Na + dependent liquid absorption on conjunctional surfaces. In rhinosinusitis, there is an imbalance, as in CB, between mucin secretion and relative ASL depletion. Finally, in the gastrointestinal tract, failure to secrete Cl— (and liquid) in the proximal small intestine, combined with increased Na + (and liquid) absorption in the terminal ileum leads to the distal intestinal obstruction syndrome (DIOS). In older patients, excessive Na + (and volume) absorption in the descending colon produces chronic constipation and diverticulitis.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide compounds that have both sodium channel blocking activity and beta-adrenergic receptor agonist activity in the same molecule.
It is an object of the present invention to provide compounds that are more potent and/or absorbed less rapidly from mucosal surfaces, and/or are less reversible as compared to known compounds.
It is another aspect of the present invention to provide compounds that are more potent and/or absorbed less rapidly and/or exhibit less reversibility, as compared to compounds such as amiloride, benzamil, and phenamil. Therefore, the compounds will give a prolonged pharmacodynamic half-life on mucosal surfaces as compared to known compounds.
It is another object of the present invention to provide compounds which are (1) absorbed less rapidly from mucosal surfaces, especially airway surfaces, as compared to known compounds and; (2) when absorbed from mucosal surfaces after administration to the mucosal surfaces, are converted in vivo into metabolic derivatives thereof which have reduced efficacy in blocking sodium channels and beta-adrenergic receptor agonist activity as compared to the administered parent compound.
It is another object of the present invention to provide compounds that are more potent and/or absorbed less rapidly and/or exhibit less reversibility, as compared to compounds such as amiloride, benzamil, and phenamil. Therefore, such compounds will give a prolonged pharmacodynamic half-life on mucosal surfaces as compared to previous compounds.
It is another object of the present invention to provide methods of treatment that take advantage of the pharmacological properties of the compounds described above.
In particular, it is an object of the present invention to provide methods of treatment which rely on rehydration of mucosal surfaces.
Any of the compounds described herein can be a pharmaceutically acceptable salt thereof, and wherein the above compounds are inclusive of all racemates, enantiomers, diastereomers, tautomers, polymorphs and pseudopolymorphs thereof. Polymorphs are different physical forms—different crystal forms that have differing melting ranges, show differing differential scanning calorimetry (DSC) tracings and exhibit different X-Ray powder diffraction (XRPD) spectra. Pseudopolymorphs are different solvated physical forms—different crystal forms that have differing melting ranges as solvates, show differing differential scanning calorimetry (DSC) tracings as solvates and exhibit different X-Ray powder diffraction (XRPD) spectra as solvates.
The present invention also provides pharmaceutical compositions which contain a compound described above.
The present invention also provides a method of promoting hydration of mucosal surfaces, comprising:
administering an effective amount of a compound represented by formula (I) to a mucosal surface of a subject.
The present invention also provides a method of restoring mucosal defense, comprising:
topically administering an effective amount of compound represented by formula (I) to a mucosal surface of a subject in need thereof.
The present invention also provides a method of blocking ENaC and exerting beta-adrenergic receptor agonism comprising:
contacting sodium channels and at the same time activating beta-adrenergic receptors (beta agonists) with an effective amount of a compound represented by formula (I).
The objects of the resent invention may be accomplished with a class of pyrazinoylguanidine compounds representing a compound represented by formula (I):
wherein
X is hydrogen, halogen, trifluoromethyl, lower alkyl, unsubstituted or substituted phenyl, lower alkyl-thio, phenyl-lower alkyl-thio, lower alkyl-sulfonyl, or phenyl-lower alkyl-sulfonyl;
Y is hydrogen, hydroxyl, mercapto, lower alkoxy, lower alkyl-thio, halogen, lower alkyl, unsubstituted or substituted mononuclear aryl, or —N(R 2 ) 2 ;
R 1 is hydrogen or lower alkyl;
each R 2 is, independently, —R 7 , —(CH 2 ) m —OR 8 , —(CH 2 ) m —NR 7 R 10 , —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 CH 2 O) m —R 8 , —(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —(CH 2 ) n —C(═O)NR 7 R 10 , —(CH 2 ) n —Z g —R 7 , —(CH 2 ) m —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 ) n —CO 2 R 7 , or
R 3 and R 4 are each, independently, hydrogen, a group represented by formula (A), lower alkyl, hydroxy lower alkyl, phenyl, phenyl-lower alkyl, (halophenyl)-lower alkyl, lower-(alkylphenylalkyl), lower (alkoxyphenyl)-lower alkyl; naphthyl-lower alkyl, or pyridyl-lower alkyl, with the proviso that at least one of R 3 and R 4 is a group represented by formula (A):
—(C(R L ) 2 ) O - x -(C(R L ) 2 ) P —CR 5 R 6 R 6 (A)
wherein each R L is, independently, —R 7 , —(CH 2 ) n —OR 8 , —O—(CH 2 ) m —OR 8 , —(CH 2 ) n —NR 7 R 10 , —O—(CH 2 ) m —NR 7 R 10 , —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 CH 2 O) m —R 8 , —O—(CH 2 CH 2 O) m —R 8 , —(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —O—(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —(CH 2 ) n —C(═O)NR 7 R 10 , —O—(CH 2 ) m —C(═O)NR 7 R 10 , —(CH 2 ) n —(Z) g —R 7 , —O—(CH 2 ) m —(Z) g —R 7 , —(CH 2 ) n —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 ) n —CO 2 R 7 , —O—(CH 2 ) m —CO 2 R 7 , —OSO 3 H, —O-glucuronide, —O-glucose,
each o is, independently, an integer from 0 to 10;
each p is an integer from 0 to 10;
with the proviso that the sum of o and p in each contiguous chain is from 1 to 10;
each x is, independently, O, NR 10 , C(═O), CHOH, C(═N—R 10 ), CHNR 7 R 10 , or represents a single bond;
wherein each R 5 is, independently; Link —(CH 2 ) n —CR 11 R 11 —CAP, Link —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CR 11 R 11 —CAP, Link —(CH 2 CH 2 O) m —CH 2 —CR 11 R 11 —CAP, Link —(CH 2 CH 2 O) m —CH 2 CH 2 —CR 11 R 11 —CAP, Link —(CH 2 ) n (Z) g —CR 11 R 11 —CAP, Link —(CH 2 ) n (Z) g —(CH 2 ) m —CR 11 R 11 —CAP, Link —(CH 2 ) n —NR 13 —CH 2 (CHOR 8 )(CHOR 8 ) n —CR 11 R 11 —CAP, Link —(CH 2 ) n —(CHOR 8 ) m CH 2 —NR 13 —(Z) g —CR 11 R 11 —CAP, Link —(CH 2 ) n NR 13 —(CH 2 ) m (CHOR 8 ) n CH 2 NR 13 —(Z) g —CR 11 R 11 —CAP, Link —(CH 2 ) m —(Z) g —(CH 2 ) m —CR 11 R 11 —CAP, Link NH—C(═O)—NH—(CH 2 ) m —CR 11 R 11 —CAP, Link —(CH 2 ) m —C(═O)NR 13 —(CH 2 ) m —CR 11 R 11 —CAP, Link —(CH 2 ) n —(Z) g —(CH 2 ) m —(Z) g —CR 11 R 11 —CAP, Link —Z g —(CH 2 ) m -Het-(CH 2 ) m —CR 11 R 11 —CAP, wherein Link is, independently, —O—, (CH 2 ) n —, —O(CH 2 ) m —, —NR 13 —C(═O)—NR 13 , —NR 13 —C(═O)—(CH 2 ) m —, —C(═O)NR 13 —(CH 2 ) m , —(CH 2 ) n —Z g —(CH 2 ) n , —S—, —SO—, —SO 2 —, SO 2 NR 7 —, SO 2 NR 10 —, -Het-. wherein each CAP is, independently,
each R 6 is, independently, —R 7 , —OR 7 , —OR 11 , —N(R 7 ) 2 , —(CH 2 ) m —OR 8 , —O—(CH 2 ) m —OR 8 , —(CH 2 ) n —NR 7 R 10 , —O—(CH 2 ) m —NR 7 R 10 , —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 CH 2 O) m —R 8 , —O—(CH 2 CH 2 O) m —R 8 , —(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —O—(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —(CH 2 ) n —C(═O)NR 7 R 10 , —O—(CH 2 ) m —C(═O)NR 7 R 10 , —(CH 2 ) n —(Z) g —R 7 , —O—(CH 2 ) m —(Z) g —R 7 , —(CH 2 ) n —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 ) n —CO 2 R 7 , —O—(CH 2 ) m —CO 2 R 7 , —OSO 3 H, —O-glucuronide, —O-glucose,
where when two R 6 are —OR 11 and are located adjacent to each other on a phenyl ring, the alkyl moieties of the two R 6 may be bonded together to form a methylenedioxy group; with the proviso that when at least two —CH 2 OR 8 are located adjacent to each other, the R 8 groups may be joined to form a cyclic mono- or di-substituted 1,3-dioxane or 1,3-dioxolane,
each R 7 is, independently, hydrogen lower alkyl, phenyl, or substituted phenyl;
each R 8 is, independently, hydrogen, lower alkyl, —C(═O)—R 11 , glucuronide, 2-tetrahydropyranyl, or
each R 9 is, independently, —CO 2 R 13 , —CON(R 13 ) 2 , —SO 2 CH 2 R 13 , or —C(═O)R 13 ;
each R 10 is, independently, —H, —SO 2 CH 3 , —CO 2 R 7 , —C(═O)NR 7 R 9 , —C(═O)R 7 , or —(CH 2 ) m —(CHOH) n —CH 2 OH,
each Z is, independently, CHOH, C(═O), —(CH 2 ) n —, CHNR 13 R 13 , C═NR 13 , or NR 13 ;
each R 11 is, independently, hydrogen, lower alkyl, phenyl lower alkyl or substituted phenyl lower alkyl;
each R 12 is independently, —(CH 2 ) n —SO 2 CH 3 , —(CH 2 ) n —CO 2 R 13 , —(CH 2 ) n , —C(═O)NR 13 R 13 , —(CH 2 ) n —C(═O)R 13 , —(CH 2 ) n —(CHOH) n —CH 2 OH, —NH—(CH 2 ) n —SO 2 CH 3 , NH—(CH 2 ) n —C(═O)R 11 , —NH—C(═O)—NH—C(═O)R 11 , —C(═O)NR 13 R 13 , —OR 11 , —NH—(CH 2 ) n —R 10 , —Br, —Cl, —F, —I, SO 2 NHR 11 , —NHR 13 , —NH—C(═O)—NR 13 R 13 , NH—(CH 2 ) n —SO 2 CH 3 , NH—(CH 2 ) n —C(═O)R 11 , —NH—C(═O)—NH—C(═O)R 11 , —C(═O)NR 13 R 13 , —OR 11 , —(CH 2 ) n —NHR 13 , —NH—C(═O)—NR 13 R 13 , or —NH—(CH 2 ) n —C(═O)—R 13 ;
each R 13 is, independently, hydrogen, lower alkyl, phenyl, substituted phenyl, —SO 2 CH 3 , —CO 2 R 7 , —C(═O)NR 7 R 7 , —C(═O)NR 7 SO 2 CH 3 , —C(═O)NR 7 —CO 2 R 7 , —C(═O)NR 7 —C(═O)NR 7 R 7 , —C(═O)NR 7 —C(═O)R 7 , —C(═O)NR 7 —(CH 2 ) m —(CHOH) n —CH 2 OH, —C(═O)R 7 , —(CH 2 ) m —(CHOH) n —CH 2 OH, —(CH 2 ) m —NR 7 R 10 , —(CH 2 ) m —NR 7 R 7 R 7 , —(CH 2 ) m —(CHOR 8 ) m —(CH 2 ) m NR 7 R 7 , —(CH 2 ) M —NR 10 R 10 , —(CH 2 ) m —(CHOR 8 ) m —(CH 2 ) m NR 7 R 7 R 7 ,
with the proviso that NR 13 R 13 can be joined on itself to form a group represented by one of the following:
each Het is independently, —NR 13 , —S—, —SO—, —SO 2 —; —O—, —SO 2 NR 13 —, —NHSO 2 —, —NR 13 CO—, or —CONR 13 —;
each g is, independently, an integer from 1 to 6;
each m is, independently, an integer from 1 to 7;
each n is, independently, an integer from 0 to 7;
each V is, independently, —(CH 2 ) m —NR 7 R 10 , —(CH 2 ) m —NR 7 R 7 , —(CH 2 ) m —+NR 11 R 11 R 11 , —(CH 2 ) n —(CHOR 8 ) m —(CH 2 ) m NR 7 R 10 , —(CH 2 ) n —NR 10 R 10 +—(CH 2 ) n —(CHOR 8 ) m —(CH 2 ) m NR 7 R 7 , —(CH 2 ) n —(CHOR 8 ) m —(CH 2 ) m NR 11 R 11 R 11 with the proviso that when V is attached directly to a nitrogen atom, then V can also be, independently, R 7 , R 10 , or (R 11 ) 2 ;
wherein for of the above compounds when two —CH 2 OR 8 groups are located 1,2- or 1,3- with respect to each other the R 8 groups may be joined to form a cyclic mono- or di-substituted 1,3-dioxane or 1,3-dioxolane;
wherein any of the above compounds can be a pharmaceutically acceptable salt thereof, and wherein the above compounds are inclusive of all racemates, enantiomers, diastereomers, tautomers, polymorphs and pseudopolymorphs thereof.
The present invention also provides pharmaceutical compositions which contain a compound described above.
The present invention also provides a method of promoting hydration of mucosal surfaces, comprising:
administering an effective amount of a compound represented by formula (I) to a mucosal surface of a subject.
The present invention also provides a method of restoring mucosal defense, comprising:
topically administering an effective amount of compound represented by formula (I) to a mucosal surface of a subject in need thereof.
The present invention also provides a method of blocking ENaC, comprising:
contacting sodium channels with an effective amount of a compound represented by formula (I).
The present invention also provides a method of promoting mucus clearance in mucosal surfaces, comprising:
administering an effective amount of a compound represented by formula (I) to a mucosal surface of a subject.
The present invention also provides a method of treating chronic bronchitis, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating cystic fibrosis, comprising:
administering an effective amount of compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating rhinosinusitis, comprising:
administering an effective amount of a compound represented by a formula (I) to a subject in need thereof.
The present invention also provides a method of treating nasal dehydration, comprising:
administering an effective amount of a compound represented by formula (I) to the nasal passages of a subject in need thereof.
In a specific embodiment, the nasal dehydration is brought on by administering dry oxygen to the subject.
The present invention also provides a method of treating sinusitis, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating pneumonia, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of preventing ventilator-induced pneumonia, comprising:
administering an effective compound represented by formula (I) to a subject by means of a ventilator.
The present invention also provides a method of treating asthma, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating primary ciliary dyskinesia, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating otitis media, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of inducing sputum for diagnostic purposes, comprising:
administering an effective amount of compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating chronic obstructive pulmonary disease, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating emphysema, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating dry eye, comprising:
administering an effective amount of a compound represented by formula (I) to the eye of the subject in need thereof.
The present invention also provides a method of promoting ocular hydration, comprising:
administering an effective amount of a compound represented by formula (I) to the eye of the subject.
The present invention also provides a method of promoting corneal hydration, comprising:
administering an effective amount of a compound represented by formula (I) to the eye of the subject.
The present invention also provides a method of treating Sjögren's disease, comprising:
administering an effective amount of compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating vaginal dryness, comprising:
administering an effective amount of a compound represented by formula (I) to the vaginal tract of a subject in need thereof.
The present invention also provides a method of treating dry skin, comprising:
administering an effective amount of a compound represented by formula (I) to the skin of a subject in need thereof.
The present invention also provides a method of treating dry mouth (xerostomia), comprising:
administering an effective amount of compound represented by formula (I) to the mouth of the subject in need thereof.
The present invention also provides a method of treating distal intestinal obstruction syndrome, comprising:
administering an effective amount of compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating esophagitis, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
The present invention also provides a method of treating constipation, comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof. In one embodiment of this method, the compound is administered either orally or via a suppository or enema.
The present invention also provides a method of treating chronic diverticulitis comprising:
administering an effective amount of a compound represented by formula (I) to a subject in need thereof.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 shows the baseline activity of sodium channels before and after blockade with amiloride.
FIG. 2 shows the activity of sodium channels before and after the addition of a beta-agonist.
FIG. 3 shows the mechanism underlying the additivity of a Na channel blocker and a beta-agonist.
FIG. 4 shows the tautomers of the compounds of formula I.
DETAILED DESCRIPTION OF THE INVENTION
The present invention is based on the discovery that the compounds of formula (I) also possess both sodium channel blocking activity and beta agonist activity in the same molecule.
The present invention is also based on the discovery that the compounds of formula (I) are more potent and/or, absorbed less rapidly from mucosal surfaces, especially airway surfaces, and/or less reversible from interactions with ENaC as compared to compounds such as amiloride, benzamil, and phenamil. Therefore, the compounds of formula (I) have a longer half-life on mucosal surfaces as compared to these compounds.
The present invention is also based on the discovery that certain compounds embraced by formula (I) are converted in vivo into metabolic derivatives thereof that have reduced efficacy in blocking sodium channels and acting as beta-adrenergic receptor agonists as compared to the parent administered compound, after they are absorbed from mucosal surfaces after administration. This important property means that the compounds will have a lower tendency to cause undesired side-effects by blocking sodium channels and activating beta-receptors located at other untargeted locations in the body of the recipient, e.g., in the kidneys and heart.
Mono drug therapy leaves most major diseases such as chronic bronchitis and cystic fibrosis inadequately treated. It is therefore often necessary to discover and develop novel drugs or combination of drugs which treat and modulate multiple targets simultaneously (polypharmacology) with the goal of enhancing efficacy or improving safety relative to single target drugs. There are three possible ways to achieve this, 1) Combining therapeutic “cocktails” of two or more individual drugs; the benefits of this approach are often lessened by poor patient compliance. 2). A multiple component drug (“fixed combination” or multiple component drug) that contains two or more agents in a single tablet, liquid formulation, inhaler or dry powder device. This can sometimes improve patient compliance versus multiple component drugs but adds the complexity of carefully dosing so as to minimize multiple metabolic pathways. 3). A single molecular entity which can simultaneously modulate multiple drug targets (designed multiple ligands). The advantage of a multiple ligand over the first two approaches is that it improves compliance, enhances efficacy, it targets a known set of deficiencies in multiple systems with a single new chemical entity, it often lacks the unpredictable differences in the pharmacokinetic and pharmacodynamic variability between patients, it is often easier to formulate and potentially lowers the risk of drug-drug interactions compared to drug cocktails and multiple component drugs. It was therefore our goal to discover multiple ligands that have both sodium channel blocking activity as well as beta agonist activity.
The addition of beta-adrenergic receptor agonist activity to a sodium channel blocker will significantly increase the capacity to hydrate airway surfaces in subjects in need of hydration for therapeutic purposes. The mechanism by which beta-agonist activity adds to the hydration capacity of Na channel blockers alone, or beta-agonists alone, is described in the following diagrams that describe the electrochemical gradients for ion flows and the net secretion that results from these forces in airway epithelia.
As shown in FIG. 1 , under baseline conditions human airway epithelia absorb NaCl and H 2 O. Active Na + absorption drives this process. Cl − is absorbed passively with Na + to preserve electroneutrality. As there is no net driving force for Cl − to move across the apical cell membrane, Cl − is absorbed paracellularly in response to the transepithelial electric potential. Water moves cellularly and paracellularly in response to the osmotic gradients generated by NaCl absorbtion.
Application of a Na + channel blocker (as an example amiloride is shown) inhibits the entry of Na + into the cell which: (1) abolishes Na + absorption and (2) hyperpolarizes the apical cell membrane (Va). The hyperpolarization of Va generates an electrochemical driving force favoring Cl − secretion (Na + now follows in the secretory direction via the paracellularpath). The rate of Cl − secretion is proportional to the activity of the apicalmembrane Cl − channels which are typically 30-50% maximally active under basal conditions. In summary, application of a Na + channel blocker inhibits Na + absorption and triggers a modest amount of Cl − secretion. Note again that water will follow transcellularly in response to the secreted NaCl.
In contrast, as depicted in FIG. 2 , addition of a beta-agonist (as an example isoproterenol is shown) alone to human airway epithelia produces no changes in Na + absorption or Cl − secretion. The reason for this absence of effect is that there is no electrochemical driving force for Cl − to move across the cell (See the following references: Intracellular Cl— activity and cellular Cl— pathways in cultured human airway epithelium. Am J Physiol. 1989 May; 256(5 Pt 1):C1033-44. Willumsen N J, Davis C W, Boucher R C Cellular Cl— transport in cultured cystic fibrosis airway epithelium. Am J Physiol. 1989 May; 256(5 Pt 1):C1045-53. Willumsen N J, Davis C W, Boucher R C Activation of an apical Cl— conductance by Ca2+ ionophores in cystic fibrosis airway epithelia. Am J Physiol. 1989 February; 256(2 Pt 1):C226-33. Willumsen N J, Boucher R C). Thus, a beta-agonist mediated activation of an apical membrane Cl − channel, usually CFTR via changes in cAMP, produces no change in the rate of movement of Cl − across the barrier and, hence, no change in transepithelial sodium chloride or water secretion.
However, when a Na channel blocker is administered with a beta-agonist, additivity between these two classes of compounds is achieved with the result being accelerated Cl − (and Na + , H 2 O) secretion. The mechanism underlying the additivity is shown in FIG. 3 . In the presence of a Na channel blocker, an electrochemical gradient for Cl − secretion is generated (also see FIG. 1 ). Now when a beta-agonist is present, it converts the apical membrane CFTR from ˜30% basal activity to ˜100% activity via beta-agonist induced increase in cAMP that ultimately activates CFTR via PKA (protein kinase A). Because there is an electrochemical driving force favoring Cl − secretion as a result of ENaC blockade, the increase in Cl − channel activity translates into increasing Cl − (and Na + , H 2 O) secretion. Thus, the hydration capacity of the epithelia is greatly enhanced by the presence of both Na + channel blocker and beta-adrenergic receptor agonist activities in the environment bathing the human airway epithelia as compared to just Na + channel blocker or beta-adrenergic receptor agonist by themselves. A discovery of this invention is that administration of both activities contained within the same molecule to the epithelium is at least as effective as sequential administration of a Na channel blocker followed by a beta-agonist and therefore has the advantages cited earlier.
The compounds of formula I exist primarily as a combination of the three tautomers shown in FIG. 4 . The compounds of formula I exist primarily as a combination of the three tautomers shown in FIG. 4 . FIG. 4 shows the three tautomers represented in formula I that exist in solution. Previous studies (R L Smith et. Al. Journal of the American Chemical Society, 1979, 101, 191-201) have shown that the free base exists primarily as the acylimino tautomer, whereas the physiologically active species exists as the protonated form of the acylamino. These structural representations have been used to represent amiloride and its analogs in both the patent and scientific literature. We use both the acylamino and acylimino representations for convenience throughout this patent with the understanding that the structures are in reality a hybrid of the three forms with the actual amount of each dependent on the pH, the one of action and the nature of the substituents.
In the compounds represented by formula (I), X may be hydrogen, halogen, trifluoromethyl, lower alkyl, lower cycloalkyl, unsubstituted or substituted phenyl, lower alkyl-thio, phenyl-lower alkyl-thio, lower alkyl-sulfonyl, or phenyl-lower alkyl-sulfonyl. Halogen is preferred.
Examples of halogen include fluorine, chlorine, bromine, and iodine. Chlorine and bromine are the preferred halogens. Chlorine is particularly preferred. This description is applicable to the term “halogen” as used throughout the present disclosure.
As used herein, the term “lower alkyl” means an alkyl group having less than 8 carbon atoms. This range includes all specific values of carbon atoms and subranges there between, such as 1, 2, 3, 4, 5, 6, and 7 carbon atoms. The term “alkyl” embraces all types of such groups, e.g., linear, branched, and cyclic alkyl groups. This description is applicable to the term “lower alkyl” as used throughout the present disclosure. Examples of suitable lower alkyl groups include methyl, ethyl, propyl, cyclopropyl, butyl, isobutyl, etc.
Substituents for the phenyl group include halogens. Particularly preferred halogen substituents are chlorine and bromine.
Y may be hydrogen, hydroxyl, mercapto, lower alkoxy, lower alkyl-thio, halogen, lower alkyl, lower cycloalkyl, mononuclear aryl, or —N(R 2 ) 2 . The alkyl moiety of the lower alkoxy groups is the same as described above. Examples of mononuclear aryl include phenyl groups. The phenyl group may be unsubstituted or substituted as described above. The preferred identity of Y is —N(R 2 ) 2 . Particularly preferred are such compounds where each R 2 is hydrogen.
R 1 may be hydrogen or lower alkyl. Hydrogen is preferred for R 1 .
Each R 2 may be, independently, —R 7 , —(CH 2 ) m —OR 8 , —(CH 2 ) m —NR 7 R 10 , —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 CH 2 O) m —R 8 , —(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —(CH 2 ) n —C(═O)NR 7 R 10 , —(CH 2 ) n —Z g —R 7 , —(CH 2 ) m —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 ) n —CO 2 R 7 , or
Hydrogen and lower alkyl, particularly C 1 -C 3 alkyl are preferred for R 2 . Hydrogen is particularly preferred.
R 3 and R 4 may be, independently, hydrogen, a group represented by formula (A), lower alkyl, hydroxy lower alkyl, phenyl, phenyl-lower alkyl, (halophenyl)-lower alkyl, lower-(alkylphenylalkyl), lower (alkoxyphenyl)-lower alkyl, naphthyl-lower alkyl, or pyridyl-lower alkyl, provided that at least one of R 3 and R 4 is a group represented by formula (A).
Preferred compounds are those where one of R 3 and R 4 is hydrogen and the other is represented by formula (A).
In formula (A), the moiety —(C(R L ) 2 ) o -x-(C(R L ) 2 ) p — defines an alkylene group. The variables o and p may each be an integer from 0 to 10, subject to the proviso that the sum of o and p in the chain is from 1 to 10. Thus, o and p may each be 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10. Preferably, the sum of o and p is from 2 to 6. In a particularly preferred embodiment, the sum of o and p is 4.
The linking group in the alkylene chain, x, may be, independently, O, NR 10 , C(═O), CHOH, C(═N—R 10 ), CHNR 7 R 10 , or represents a single bond;
Therefore, when x represents a single bond, the alkylene chain bonded to the ring is represented by the formula —(C(R L ) 2 ) o+p —, in which the sum o+p is from 1 to 10.
Each R L may be, independently, —R 7 , —(CH 2 ) n —OR 8 , —O—(CH 2 ) m —OR 8 , —(CH 2 ) n —NR 7 R 10 , —O—(CH 2 ) m —NR 7 R 10 , —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 CH 2 O) m —R 8 , —O—(CH 2 CH 2 O) m —R 8 , —(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —O—(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —(CH 2 ) n —C(═O)NR 7 R 10 , —O—(CH 2 ) m —C(═O)NR 7 R 10 , —(CH 2 ) n —(Z) g —R 7 , —O—(CH 2 ) m —(Z) g —R 7 , —(CH 2 ) n —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 ) n —CO 2 R 7 , —O—(CH 2 ) m —CO 2 R 7 , —OSO 3 H, —O-glucuronide, —O-glucose,
The preferred R L groups include —H, —OH, —N(R 7 ) 2 , especially where each R 7 is hydrogen.
In the alkylene chain in formula (A), it is preferred that when one R L group bonded to a carbon atoms is other than hydrogen, then the other R L bonded to that carbon atom is hydrogen, i.e., the formula —CHR L —. It is also preferred that at most two R L groups in an alkylene chain are other than hydrogen, where in the other R L groups in the chain are hydrogens. Even more preferably, only one R L group in an alkylene chain is other than hydrogen, where in the other R L groups in the chain are hydrogens. In these embodiments, it is preferable that x represents a single bond.
In another particular embodiment of the invention, all of the R L groups in the alkylene chain are hydrogen. In these embodiments, the alkylene chain is represented by the formula —(CH 2 ) o -x-(CH 2 ) p —.
Each R 5 is, independently,
Link —(CH 2 ) n —CR 11 R 11 —CAP, Link —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CR 11 R 11 —CAP, Link —(CH 2 CH 2 O) m —CH 2 —CR 11 R 11 —CAP, Link —(CH 2 CH 2 O) m —CH 2 CH 2 —CR 11 R 11 —CAP, Link —(CH 2 ) n —(Z) g —CR 11 R 11 —CAP, Link —(CH 2 ) n (Z) g —(CH 2 ) m —CR 11 R 11 —CAP, Link —(CH 2 ) n —NR 13 —CH 2 (CHOR 8 )(CHOR 8 ) n —CR 11 R 11 —CAP, Link —(CH 2 ) n —(CHOR 8 ) m CH 2 —NR 13 —(Z) g —CR 11 R 11 —CAP, Link —(CH 2 ) n NR 13 —(CH 2 ) m (CHOR 8 ) n CH 2 NR 13 —(Z) g —CR 11 R 11 —CAP, Link —(CH 2 ) m —(Z) g —(CH 2 ) m —CR 11 R 11 —CAP, Link NH—C(═O)—NH—(CH 2 ) m —CR 11 R 11 —CAP, Link —(CH 2 ) m —C(═O)NR 13 —(CH 2 ) m —CR 11 R 11 —CAP, Link —(CH 2 ) n —(Z) g —(CH 2 ) m —(Z) g —CR 11 R 11 —CAP, or Link —Z g —(CH 2 ) m -Het-(CH 2 ) m —CR 11 R 11 —CAP.
Each Link is, independently,
—O—, (CH 2 ) n —, —O(CH 2 ) m —, —NR 13 —C(═O)—NR 13 , —NR 13 —C(═O)—(CH 2 ) m —, —C(═O)NR 13 —(CH 2 ) m , —(CH 2 ) n —Z g —(CH 2 ) n , —S—, —SO—, —SO 2 —, SO 2 NR 7 —, SO 7 NR 10 —, -Het-.
Each CAP is, independently,
Each R 6 is, independently, —R 7 , —OR 7 , —OR 11 , —N(R 7 ) 2 , —(CH 2 ) m —OR 8 , —O—(CH 2 ) m —OR 8 , —(CH 2 ) n —NR 7 R 10 , —O—(CH 2 ) m —NR 7 R 10 , —(CH 2 ) n (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 CH 2 O) m —R 8 , —O—(CH 2 CH 2 O) m —R 8 , —(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —O—(CH 2 CH 2 O) m —CH 2 CH 2 NR 7 R 10 , —(CH 2 ) n —C(═O)NR 7 R 10 , —O—(CH 2 ) m —C(═O)NR 7 R 10 , —(CH 2 ) n —(Z) g —R 7 , —O—(CH 2 ) m —(Z) g —R 7 , —(CH 2 ) n —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —O—(CH 2 ) m —NR 10 —CH 2 (CHOR 8 )(CHOR 8 ) n —CH 2 OR 8 , —(CH 2 ) n —CO 2 R 7 , —O—(CH 2 ) m —CO 2 R 7 , —OSO 3 H, —O-glucuronide, —O-glucose,
Each R 7 is, independently, hydrogen lower alkyl, phenyl, or substituted phenyl.
Each R 8 is, independently, hydrogen, lower alkyl, —C(═O)—R 11 , glucuronide, 2-tetrahydropyranyl, or
Each R 9 is, independently, —CO 2 R 13 , —CON(R 13 ) 2 , —SO 2 CH 2 R 13 , or —C(═O)R 13 ,
Each R 10 is, independently, —H, —SO 2 CH 3 , —CO 2 R 7 , —C(═O)NR 7 R 9 , —C(═O)R 7 , or —(CH 2 ) m —(CHOH) n —CH 2 OH.
Each Z is, independently, CHOH, C(═O), —(CH 2 ) n —, CHNR 13 R 13 , C═NR 13 , or NR 13 .
Each R 11 is, independently, hydrogen, lower alkyl, phenyl lower alkyl or substituted phenyl lower alkyl.
Each R 12 is independently, —(CH 2 ) n —SO 2 CH 3 , —(CH 2 ) n —CO 2 R 13 , —(CH 2 ) n —C(═O)NR 13 R 13 , —(CH 2 ) n —C(═O)R 13 , —(CH 2 ) n —(CHOH) n —CH 2 OH, —NH—(CH 2 ) n —SO 2 CH 3 , NH—(CH 2 ) n —C(═O)R 11 , NH—C(═O)—NH—C(═O)R 11 , —C(═O)NR 13 R 13 , —OR 11 , —NH—(CH 2 ) n R 10 , —Br, —Cl, —F, —I, SO 2 NHR 11 , —NHR 13 , —NH—C(═O)—NR 13 R 13 , NH—(CH 2 ) n —SO 2 CH 3 , NH—(CH 2 ) n —C(═O)R 11 , —NH—C(═O)—NH—C(═O)R 11 , —C(═O)NR 13 R 13 , —OR 11 , —(CH 2 ) n —NHR 13 , —NH—C(═O)—NR 13 R 13 , or —NH—(CH 2 ) n —C(═O)—R 13 ;
Each R 13 is, independently, hydrogen, lower alkyl, phenyl, substituted phenyl, —SO 2 CH 3 , —CO 2 R 7 , —C(═O)NR 7 R 7 , —C(═O)NR 7 SO 2 CH 3 , —C(═O)NR 7 —CO 2 R 7 , —C(═O)NR 7 —C(═O)NR 7 R 7 , —C(═O)NR 7 —C(═O)R 7 , —C(═O)NR 7 —(CH 2 ) m —(CHOH) n —CH 2 OH, —C(═O)R 7 , —(CH 2 ) m —(CHOH) n —CH 2 OH, —(CH 2 ) m —NR 7 R 10 , +—(CH 2 ) m —NR 7 R 7 R 7 , —(CH 2 ) m —(CHOR 8 ) m —(CH 2 ) m NR 7 R 7 , —(CH 2 ) m —NR 10 R 10 , +—(CH 2 ) m —(CHOR 8 ) m —(CH 2 ) m NR 7 R 7 R 7 ,
with the proviso that NR 13 R 13 can be joined on itself to form a group represented by one of the following:
Each Het is independently, —NR 13 , —S—, —SO—, —SO 2 —; —O—, —SO 2 NR 13 —, —NHSO 2 —, —NR 13 CO—, —CONR 13 —.
Each g is, independently, an integer from 1 to 6.
Each m is, independently, an integer from 1 to 7.
Each n is, independently, an integer from 0 to 7.
Each V is, independently, —(CH 2 ) m —NR 7 R 10 , —(CH 2 ) m —NR 7 R 7 , —(CH 2 ) m —+NR 11 R 11 R 11 , —(CH 2 ) n —(CHOR 8 ) m —(CH 2 ) m NR 7 R 10 , —(CH 2 ) n —NR 10 R 10 +—(CH 2 ) n —(CHOR 8 ) m —(CH 2 ) m NR 7 R 7 , —(CH 2 ) n —(CHOR 8 ) m —(CH 2 ) m NR 11 R 11 R 11 with the proviso that when V is attached directly to a nitrogen atom, then V can also be, independently, R 7 , R 10 , or (R 11 ) 2 .
In any of the compounds of the present invention, when two —CH 2 OR 8 groups are located 1,2- or 1,3- with respect to each other the R 8 groups may be joined to form a cyclic mono- or di-substituted 1,3-dioxane or 1,3-dioxolane.
In another embodiment, when two R 6 are —OR 11 and are located adjacent to each other on a phenyl ring, the alkyl moieties of the two R 6 may be bonded together to form a methylenedioxy group.
In still another embodiment of the invention, when at least two —CH 2 OR 8 are located adjacent to each other, the R 8 groups may be joined to form a cyclic mono- or di-substituted 1,3-dioxane or 1,3-dioxolane.
In addition, one of more of the R 6 groups can be one of the R 5 groups which fall within the broad definition of R 6 set forth above.
As discussed above, R 6 may be hydrogen. Therefore, 1, 2, 3, or 4 R 6 groups may be other than hydrogen. Preferably at most 3 of the R 6 groups are other than hydrogen.
Each g is, independently, an integer from 1 to 6. Therefore, each g may be 1, 2, 3, 4, 5, or 6.
Each m is an integer from 1 to 7. Therefore, each m may be 1, 2, 3, 4, 5, 6, or 7.
Each n is an integer from 0 to 7. Therefore, each n may be 0, 1, 2, 3, 4, 5, 6, or 7.
More specific examples of suitable groups represented by formula (A) are shown in formula below:
—(C(R L ) 2 ) O - x -(C(R L ) 2 ) P —CR 5 R 6 R 6 (A)
in which each RL is hydrogen and where o, x, p, R 5 , and R 6 , are as defined above.
In a preferred embodiment of the invention, Y is —NH 2 .
In another preferred embodiment, R 2 is hydrogen.
In another preferred embodiment, R 1 is hydrogen.
In another preferred embodiment, X is chlorine.
In another preferred embodiment, R 3 is hydrogen.
In another preferred embodiment, R L is hydrogen.
In another preferred embodiment, o is 4.
In another preferred embodiment, p is 0.
In another preferred embodiment, the sum of o and p is 4.
In another preferred embodiment, x represents a single bond.
In another preferred embodiment, R 6 is hydrogen.
In another preferred embodiment, at most one Q is a nitrogen atom.
In another preferred embodiment, no Q is a nitrogen atom.
In a preferred embodiment of the present invention:
X is halogen;
Y is —N(R 7 ) 2 ;
R 1 is hydrogen or C 1 -C 3 alkyl;
R 2 is —R 7 , —OR 7 , CH 2 OR 7 , or —CO 2 R 7 ;
R 3 is a group represented by formula (A); and
R 4 is hydrogen, a group represented by formula (A), or lower alkyl;
In another preferred embodiment of the present invention:
X is chloro or bromo;
Y is —N(R 7 ) 2 ;
R 2 is hydrogen or C 1 -C 3 alkyl;
at most three R 6 are other than hydrogen as described above;
at most three R L are other than hydrogen as described above
In another preferred embodiment of the present invention:
Y is —NH 2 ;
In another preferred embodiment of the present invention:
R 4 is hydrogen;
at most one R L is other than hydrogen as described above; and
at most two R 6 are other than hydrogen as described above.
In addition, one of more of the R 6 groups can be one of the R 5 groups which fall within the broad definition of R 6 set forth above.
As discussed above, R 6 may be hydrogen. Therefore, 1 or 2 R 6 groups may be other than hydrogen. Preferably at most 3 of the R 6 groups are other than hydrogen.
Each g is, independently, an integer from 1 to 6. Therefore, each g may be 1, 2, 3, 4, 5, or 6.
Each m is an integer from 1 to 7. Therefore, each m may be 1, 2, 3, 4, 5, 6, or 7.
Each n is an integer from 0 to 7. Therefore, each n maybe 0, 1, 2, 3, 4, 5, 6, or 7.
In a preferred embodiment of the invention, Y is —NH 2 .
In another preferred embodiment, R 2 is hydrogen.
In another preferred embodiment, R 1 is hydrogen.
In another preferred embodiment, X is chlorine.
In another preferred embodiment, R 3 is hydrogen.
In another preferred embodiment, R L is hydrogen.
In another preferred embodiment, o is 4.
In another preferred embodiment, p is 2.
In another preferred embodiment, the sum of o and p is 6.
In another preferred embodiment, x represents a single bond.
In another preferred embodiment, R 6 is hydrogen.
In a preferred embodiment of the present invention:
X is halogen;
Y is —N(R 7 ) 2 ;
R 1 is hydrogen or C 1 -C 3 alkyl;
R 2 is —R 7 , —OR 7 , CH 2 O 7 , or —CO 2 R 7 ;
R 3 is a group represented by formula (A); and
R 4 is hydrogen, a group represented by formula (A), or lower alkyl;
In another preferred embodiment of the present invention:
X is chloro or bromo;
Y is —N(R 7 ) 2 ,
R 2 is hydrogen or C 1 -C 3 alkyl;
at most three R 6 are other than hydrogen as described above; and
at most three R L are other than hydrogen as described above;
In another preferred embodiment of the present invention:
Y is —NH 2 ;
In another preferred embodiment of the present invention:
R 4 is hydrogen;
at most one R L is other than hydrogen as described above; and
at most two R 6 are other than hydrogen as described above;
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
In another preferred embodiment of the present invention the compound of formula (1) is represented by the formula:
The compounds of formula (I) may be prepared and used as the free base. Alternatively, the compounds may be prepared and used as a pharmaceutically acceptable salt. Pharmaceutically acceptable salts are salts that retain or enhance the desired biological activity of the parent compound and do not impart undesired toxicological effects. Examples of such salts are (a) acid addition salts formed with inorganic acids, for example, hydrochloric acid, hydrobromic acid, sulfuric acid, phosphoric acid, nitric acid and the like; (b) salts formed with organic acids such as, for example, acetic acid, oxalic acid, tartaric acid, succinic acid, maleic acid, fumaric acid, gluconic acid, citric acid, malic acid, ascorbic acid, benzoic acid, tannic acid, palmitic acid, alginic acid, polyglutamic acid, naphthalenesulfonic acid, methanesulfonic acid, p-toluenesulfonic acid, naphthalenedisulfonic acid, polygalacturonic acid, malonic acid, sulfosalicylic acid, glycolic acid, 2-hydroxy-3-naphthoate, pamoate, salicylic acid, stearic acid, phthalic acid, mandelic acid, lactic acid and the like; and (c) salts formed from elemental anions for example, chlorine, bromine, and iodine.
It is to be noted that any of the above compounds can be a pharmaceutically acceptable salt thereof, and wherein the above compounds are inclusive of all racemates, enantiomers, diastereomers, tautomers, polymorphs and pseudopolymorphs thereof. Polymorphs are different physical forms—different crystal forms that have differing melting ranges, show differing differential scanning calorimetry (DSC) tracings and exhibit different X-Ray powder diffraction (XRPD) spectra. Pseudopolymorphs are different solvated physical forms—different crystal forms that have differing melting ranges as solvates, show differing differential scanning calorimetry (DSC) tracings as solvates and exhibit different X-Ray powder diffraction (XRPD) spectra as solvates.
Without being limited to any particular theory, it is believed that the compounds of formula (I) function in vivo as sodium channel blockers and beta receptor agonists. By blocking epithelial sodium channels by activating beta adrenergic receptors present in mucosal surfaces, the compounds of formula (I) reduce the absorption of water by the mucosal surfaces. This effect increases the volume of protective liquids on mucosal surfaces, rebalances the system, and thus treats disease.
The present invention also provides methods of treatment that take advantage of the properties of the compounds of formula (I) discussed above. Thus, subjects that may be treated by the methods of the present invention include, but are not limited to, patients afflicted with cystic fibrosis, primary ciliary dyskinesia, chronic bronchitis, chronic obstructive airway disease, artificially ventilated patients, patients with acute pneumonia, etc. The present invention may be used to obtain a sputum sample from a patient by administering the active compounds to at least one lung of a patient, and then inducing or collecting a sputum sample from that patient. Typically, the invention will be administered to respiratory mucosal surfaces via aerosol (liquid or dry powders or lavage.
Subjects that may be treated by the method of the present invention also include patients being administered supplemental oxygen nasally (a regimen that tends to dry the airway surfaces); patients afflicted with an allergic disease or response (e.g., an allergic response to pollen, dust, animal hair or particles, insects or insect particles, etc.) that affects nasal airway surfaces; patients afflicted with a bacterial infection e.g., staphylococcus infections such as Staphylococcus aureus infections, Hemophilus influenza infections, Streptococcus pneumoniae infections, Pseudomonas aeuriginosa infections, etc.) of the nasal airway surfaces; patients afflicted with an inflammatory disease that affects nasal airway surfaces; or patients afflicted with sinusitis (wherein the active agent or agents are administered to promote drainage of congested mucous secretions in the sinuses by administering an amount effective to promote drainage of congested fluid in the sinuses), or combined, Rhinosinusitis. The invention may be administered to rhino-sinal surfaces by topical delivery, including aerosols and drops.
The present invention may be used to hydrate mucosal surfaces other than airway surfaces. Such other mucosal surfaces include gastrointestinal surfaces, oral surfaces, genito-urethral surfaces, ocular surfaces or surfaces of the eye, the inner ear and the middle ear. For example, the active compounds of the present invention may be administered by any suitable means, including locally/topically, orally, or rectally, in an effective amount.
The compounds of the present invention are also useful for treating a variety of functions relating to the cardiovascular system. Thus, the compounds of the present invention are useful for use as antihypertensive agents. The compounds may also be used to reduce blood pressure and to treat edema. In addition, the compounds of the present invention are also useful for promoting diuresis, natriuresis, and saluresis. The compounds may be used alone or in combination with beta blockers, ACE inhibitors, HMGCoA, reductase inhibitors, calcium channel blockers and other cardiovascular agents to treat hypertension, congestive heart failure and reduce cardiovascular mortality.
The compounds of the present invention are also useful for treating airborne infections. Examples of airborne infections include, for example, RSV. The compounds of the present invention are also useful for treating an anthrax infection.
The present invention is concerned primarily with the treatment of human subjects, but may also be employed for the treatment of other mammalian subjects, such as dogs and cats, for veterinary purposes.
As discussed above, the compounds used to prepare the compositions of the present invention may be in the form of a pharmaceutically acceptable free base. Because the free base of the compound is generally less soluble in aqueous solutions than the salt, free base compositions are employed to provide more sustained release of active agent to the lungs. An active agent present in the lungs in particulate form which has not dissolved into solution is not available to induce a physiological response, but serves as a depot of bioavailable drug which gradually dissolves into solution.
Another aspect of the present invention is a pharmaceutical composition, comprising a compound of formula (I) in a pharmaceutically acceptable carrier (e.g., an aqueous carrier solution). In general, the compound of formula (I) is included in the composition in an amount effective to inhibit the reabsorption of water by mucosal surfaces.
The compounds of the present invention may also be used in conjunction with a P2Y2 receptor agonist or a pharmaceutically acceptable salt thereof (also sometimes referred to as an “active agent” herein). The composition may further comprise a P2Y2 receptor agonist or a pharmaceutically acceptable salt thereof (also sometimes referred to as an “active agent” herein). The P2Y2 receptor agonist is typically included in an amount effective to stimulate chloride and water secretion by airway surfaces, particularly nasal airway surfaces. Suitable P2Y2 receptor agonists are described in columns 9-10 of U.S. Pat. No. 6,264,975, U.S. Pat. No. 5,656,256, and U.S. Pat. No. 5,292,498, each of which is incorporated herein by reference.
Bronchodilators can also be used in combination with compounds of the present invention. These bronchodilators include, but are not limited to, anticholinergic agents including but not limited to ipratropium bromide, as well as compounds such as theophylline and aminophylline. These compounds may be administered in accordance with known techniques, either prior to or concurrently with the active compounds described herein.
Another aspect of the present invention is a pharmaceutical formulation, comprising an active compound as described above in a pharmaceutically acceptable carrier (e.g., an aqueous carrier solution). In general, the active compound is included in the composition in an amount effective to treat mucosal surfaces, such as inhibiting the reabsorption of water by mucosal surfaces, including airway and other surfaces.
Ionic and organic osmolytes can also be used in combination with compounds of the present invention. Ionic osmolytes useful include any salt consisting of a pharmaceutically acceptable anion and a pharmaceutical cation. Organic osmolytes include, but are not limited to, sugars, sugar alcohols and organic osmolytes. Detailed examples of ionic and non-ionic osmolytes are given in U.S. Pat. No. 6,926,911 incorporated herein by reference. A particularly useful ionic osmolyte is hypertonic sodium chloride or sodium nitrite. A particularly useful organic osmolyte is the reduced sugar mannitol.
The active compounds disclosed herein may be administered to mucosal surfaces by any suitable means, including topically, orally, rectally, vaginally, ocularly and dermally, etc. For example, for the treatment of constipation, the active compounds may be administered orally or rectally to the gastrointestinal mucosal surface. The active compound may be combined with a pharmaceutically acceptable carrier in any suitable form, such as sterile physiological or dilute saline or topical solution, as a droplet, tablet or the like for oral administration, as a suppository for rectal or genito-urethral administration, etc. Excipients may be included in the formulation to enhance the solubility of the active compounds, as desired.
The active compounds disclosed herein may be administered to the airway surfaces of a patient by any suitable means, including as a spray, mist, or droplets of the active compounds in a pharmaceutically acceptable carrier such as physiological or dilute saline solutions or distilled water. For example, the active compounds may be prepared as formulations and administered as described in U.S. Pat. No. 5,789,391 to Jacobus, the disclosure of which is incorporated by reference herein in its entirety.
Solid or liquid particulate active agents prepared for practicing the present invention could, as noted above, include particles of respirable or non-respirable size; that is, for respirable particles, particles of a size sufficiently small to pass through the mouth and larynx upon inhalation and into the bronchi and alveoli of the lungs, and for non-respirable particles, particles sufficiently large to be retained in the nasal airway passages rather than pass through the larynx and into the bronchi and alveoli of the lungs. In general, particles ranging from about 1 to 5 microns in size (more particularly, less than about 4.7 microns in size) are respirable. Particles of non-respirable size are greater than about 5 microns in size, up to the size of visible droplets. Thus, for nasal administration, a particle size in the range of 10-500 μm may be used to ensure retention in the nasal cavity.
In the manufacture of a formulation according to the invention, active agents or the physiologically acceptable salts or free bases thereof are typically admixed with, inter alia, an acceptable carrier. Of course, the carrier must be compatible with any other ingredients in the formulation and must not be deleterious to the patient. The carrier must be solid or liquid, or both, and is preferably formulated with the compound as a unit-dose formulation, for example, a capsule, that may contain 0.5% to 99% by weight of the active compound. One or more active compounds may be incorporated in the formulations of the invention, which formulations may be prepared by any of the well-known techniques of pharmacy consisting essentially of admixing the components.
Compositions containing respirable or non-respirable dry particles of micronized active agent may be prepared by grinding the dry active agent with a mortar and pestle, and then passing the micronized composition through a 400 mesh screen to break up or separate out large agglomerates.
The particulate active agent composition may optionally contain a dispersant which serves to facilitate the formulation of an aerosol. A suitable dispersant is lactose, which may be blended with the active agent in any suitable ratio (e.g., a 1 to 1 ratio by weight).
Active compounds disclosed herein may be administered to airway surfaces including the nasal passages, sinuses and lungs of a subject by an suitable means know in the art, such as by nose drops, mists, etc. In one embodiment of the invention, the active compounds of the present invention and administered by transbronchoscopic lavage. In a preferred embodiment of the invention, the active compounds of the present invention are deposited on lung airway surfaces by administering an aerosol suspension of respirable particles comprised of the active compound, which the subject inhales. The respirable particles may be liquid or solid. Numerous inhalers for administering aerosol particles to the lungs of a subject are known.
Inhalers such as those developed by Inhale Therapeutic Systems, Palo Alto, Calif., USA, may be employed, including but not limited to those disclosed in U.S. Pat. Nos. 5,740,794; 5,654,007; 5,458,135; 5,775,320; and 5,785,049, each of which is incorporated herein by reference. The Applicant specifically intends that the disclosures of all patent references cited herein be incorporated by reference herein in their entirety. Inhalers such as those developed by Dura Pharmaceuticals, Inc., San Diego, Calif., USA, may also be employed, including but not limited to those disclosed in U.S. Pat. Nos. 5,622,166; 5,577,497; 5,645,051; and 5,492,112, each of which is incorporated herein by reference. Additionally, inhalers such as those developed by Aradigm Corp., Hayward, Calif., USA, may be employed, including but not limited to those disclosed in U.S. Pat. Nos. 5,826,570; 5,813,397; 5,819,726; and 5,655,516, each of which is incorporated herein by reference. These apparatuses are particularly suitable as dry particle inhalers.
Aerosols of liquid particles comprising the active compound may be produced by any suitable means, such as with a pressure-driven aerosol nebulizer or an ultrasonic nebulizer. See, e.g., U.S. Pat. No. 4,501,729, which is incorporated herein by reference. Nebulizers are commercially available devices which transform solutions or suspensions of the active ingredient into a therapeutic aerosol mist either by means of acceleration of compressed gas, typically air or oxygen, through a narrow venturi orifice or by means of ultrasonic agitation. Suitable formulations for use in nebulizers consist of the active ingredient in a liquid carrier, the active ingredient comprising up to 40% w/w of the formulation, but preferably less than 20% w/w. The carrier is typically water (and most preferably sterile, pyrogen-free water) or dilute aqueous alcoholic solution. Perfluorocarbon carriers may also be used. Optional additives include preservatives if the formulation is not made sterile, for example, methyl hydroxybenzoate, antioxidants, flavoring agents, volatile oils, buffering agents and surfactants.
Aerosols of solid particles comprising the active compound may likewise be produced with any solid particulate medicament aerosol generator. Aerosol generators for administering solid particulate medicaments to a subject produce particles which are respirable, as explained above, and generate a volume of aerosol containing predetermined metered dose of medicament at a rate suitable for human administration. One illustrative type of solid particulate aerosol generator is an insufflator. Suitable formulations for administration by insufflation include finely comminuted powders which may be delivered by means of an insufflator or taken into the nasal cavity in the manner of a snuff. In the insufflator, the powder (e.g., a metered dose thereof effective to carry out the treatments described herein) is contained in capsules or cartridges, typically made of gelatin or plastic, which are either pierced or opened in situ and the powder delivered by air drawn through the device upon inhalation or by means of a manually-operated pump. The powder employed in the insufflator consists either solely of the active ingredient or of powder blend comprising the active ingredient, a suitable powder diluent, such as lactose, and an optional surfactant. The active ingredient typically comprises of 0.1 to 100% w/w of the formulation. A second type of illustrative aerosol generator comprises a metered dose inhaler. Metered dose inhalers are pressurized aerosol dispensers, typically containing a suspension or solution formulation of active ingredient in a liquified propellant. During use, these devices discharge the formulation through a valve adapted to deliver a metered volume, typically from 10 to 150 μl, to produce a fine particle spray containing the active ingredient. Suitable propellants include certain chlorofluorocarbon compounds, for example, dichlorodifluoromethane, trichlorofluoromethane, dichlorotetrafluoroethane and mixtures thereof. The formulation may additionally contain one of more co-solvents, for example, ethanol, surfactants, such as oleic acid or sorbitan trioleate, antioxidants and suitable flavoring agents.
The aerosol, whether formed from solid or liquid particles, may be produced by the aerosol generator at a rate of from about 10 to 150 liters per minute, more preferable from 30 to 150 liters per minute, and most preferably about 60 liters per minute. Aerosols containing greater amounts of medicament may be administered more rapidly.
The dosage of the active compounds disclosed herein will vary depending on the condition being treated and the state of the subject, but generally may be from about 0.01, 0.03, 0.05, 0.1 to 1, 5, 10 or 20 mg of the pharmaceutic agent, deposited on the airway surfaces. The daily dose may be divided among one or multiple unit dose administrations. The goal is to achieve a concentration of the pharmaceutic agents on lung airway surfaces of between 10 −9 -10 4 M.
In another embodiment, they are administered by administering an aerosol suspension respirable or non-respirable particles (preferably non-respirable particles) comprised of active compound, which the subject inhales through the nose. The respirable or non-respirable particles may be liquid or solid. The quantity of active agent included may be an amount of sufficient to achieve dissolved concentrations of active agent on the airway surfaces of the subject of from about 10 −9 , 10 −8 , or 10 −7 to about 10 −3 , 10 −2 , 10 −1 moles/liter, and more preferably from about 10 −9 to about 10 −4 moles/liter.
The dosage of active compound will vary depending on the condition being treated and the state of the subject, but generally may be an amount sufficient to achieve dissolved concentrations of active compound on the nasal airway surfaces of the subject from about 10 −9 , 10 −8 , 10 −7 to about 10 −3 , 10 −2 , or 10 −1 moles/liter, and more preferably from about 10 −7 to about 10 −4 moles/liter. Depending upon the solubility of the particular formulation of active compound administered, the daily dose may be divided among one or several unit dose administrations. The daily dose by weight may range from about 0.01, 0.03, 0.1, 0.5 or 1.0 to 10 or 20 milligrams of active agent particles for a human subject, depending upon the age and condition of the subject. A currently preferred unit dose is about 0.5 milligrams of active agent given at a regimen of 2-10 administrations per day. The dosage may be provided as a prepackaged unit by any suitable means (e.g., encapsulating a gelatin capsule).
In one embodiment of the invention, the particulate active agent composition may contain both a free base of active agent and a pharmaceutically acceptable salt to provide both early release and sustained release of active agent for dissolution into the mucus secretions of the nose. Such a composition serves to provide both early relief to the patient, and sustained relief over time. Sustained relief, by decreasing the number of daily administrations required, is expected to increase patient compliance with the course of active agent treatments.
Pharmaceutical formulations suitable for airway administration include formulations of solutions, emulsions, suspensions and extracts. See generally, J. Nairn, Solutions, Emulsions, Suspensions and Extracts, in Remington: The Science and Practice of Pharmacy, chap. 86 (19 th ed. 1995), incorporated herein by reference. Pharmaceutical formulations suitable for nasal administration may be prepared as described in U.S. Pat. Nos. 4,389,393 to Schor; 5,707,644 to Illum; 4,294,829 to Suzuki; and 4,835,142 to Suzuki, the disclosures of which are incorporated by reference herein in their entirety.
Mists or aerosols of liquid particles comprising the active compound may be produced by any suitable means, such as by a simple nasal spray with the active agent in an aqueous pharmaceutically acceptable carrier, such as a sterile saline solution or sterile water. Administration may be with a pressure-driven aerosol nebulizer or an ultrasonic nebulizer. See e.g. U.S. Pat. Nos. 4,501,729 and 5,656,256, both of which are incorporated herein by reference. Suitable formulations for use in a nasal droplet or spray bottle or in nebulizers consist of the active ingredient in a liquid carrier, the active ingredient comprising up to 40% w/w of the formulation, but preferably less than 20% w/w. Typically the carrier is water (and most preferably sterile, pyrogen-free water) or dilute aqueous alcoholic solution, preferably made in a 0.12% to 0.8% solution of sodium chloride. Optional additives include preservatives if the formulation is not made sterile, for example, methyl hydroxybenzoate, antioxidants, flavoring agents, volatile oils, buffering agents, osmotically active agents (e.g. mannitol, xylitol, erythritol) and surfactants.
Compositions containing respirable or non-respirable dry particles of micronized active agent may be prepared by grinding the dry active agent with a mortar and pestle, and then passing the micronized composition through a 400 mesh screen to break up or separate out large agglomerates.
The particulate composition may optionally contain a dispersant which serves to facilitate the formation of an aerosol. A suitable dispersant is lactose, which may be blended with the active agent in any suitable ratio (e.g., a 1 to 1 ratio by weight).
The compounds of formula (I) may be synthesized according to procedures known in the art. A representative synthetic procedure is shown in the scheme below (scheme 1):
These procedures are described in, for example, E. J. Cragoe, “The Synthesis of Amiloride and Its Analogs” (Chapter 3) in Amiloride and Its Analogs , pp. 25-36, incorporated herein by reference. Other methods of preparing the compounds are described in, for example, U.S. Pat. No. 3,313,813, incorporated herein by reference. See in particular Methods A, B, C, and D described in U.S. Pat. No. 3,313,813. Other methods useful for the preparation of these compounds, especially for the preparation of the novel HNR 3 R 4 fragment are described in, for example, U.S. Pat. No. 6,858,614, U.S. Pat. No. 6,858,615, and U.S. Pat. No. 6,903,105, incorporated herein by reference.
Scheme 1-2 are representative of but not limited to, procedures used to prepare the Sodium Channel Blockers/Beta Adrenergic Agonists described herein.
Several assays may be used to characterize the compounds of the sent invention. Representative assays are described below.
1. In Vitro Measure of Epithelial Sodium Channel Block and Beta Agonist Activity
To assess the potency of epithelial sodium channel block and beta agonist activity each compound was tested using two separate experimental procedures with similar methodology.
To assess epithelial sodium channel blocker potency the compounds of the present invention involves the determination of lumenal drug inhibition of airway epithelial sodium currents measured under short circuit current (I SC ) using airway epithelial monolayers mounted in Ussing chambers. Cells obtained from freshly excised human, or dog airways are seeded onto porous 0.4 micrometer Transwell® Permeable Supports (Corning Inc. Acton, Mass.), cultured at air-liquid interface (ALI) conditions in hormonally defined media, and assayed for sodium transport activity (I SC ) while bathed in Krebs Bicarbonate Ringer (KBR) in Ussing chambers. All test drug additions are to the lumenal bath with approximately half-log dose additions (from 1×10 −11 M to 6×10 −5 M), and the cumulative change in I SC (decreases) recorded. All drugs are prepared in dimethyl sulfoxide as stock solutions at a concentration of approximately 1×10 −2 and stored at −20° C. Six preparations are typically run in parallel; one preparation per run incorporates 552-02 as a positive control. Before the start of the concentration-effect relationship propranolol, a non-selective beta agonist blocker, was applied to the lumenal bath (10 μM) to inhibit the beta agonist component of the designer multiple ligand (DML). All data from the voltage clamps are collected via a computer interface and analyzed off-line.
Concentration-effect relationships for all compounds are considered and analyzed Using GraphPad Prism version 3.00 for Windows, GraphPad Software, San Diego Calif. USA. IC 50 values, maximal effective concentrations, are calculated and compared to the 552-02 potency as a positive control.
To assess beta agonist activity the compounds of the present invention involves the determination of lumenal drug addition to promote airway epithelial anion currents measured under short circuit current (I SC ) using airway epithelial monolayers mounted in Ussing chambers. Cells obtained from freshly excised human, dog, or sheep airways are seeded onto porous 0.4 micron Transwell® Permeable Supports (Corning), cultured at air-liquid interface (ALI) conditions in hormonally defined media, and assayed for anion secretion (I SC ) while bathed in Krebs Bicarbonate Ringer (KBR) in Ussing chambers. All test drug additions are to the lumenal bath with approximately half-log dose additions (from 8×10 −10 M to 6.5×10 −5 M), and the cumulative change in I SC (excitation) recorded. All drugs are prepared in dimethyl sulfoxide as stock solutions at a concentration from 1×10 −1 to 1×10 −2 M and stored at −20° C. Six preparations are typically run in parallel; one preparation per run incorporates either formoterol, salmeterol, or another well recognized beta agonists as a positive control depending on the analog incorporated in the compound being tested. Before the start of the concentration-effect relationship 552-02 a potent sodium channel blocker was applied to the apical surface (1 μM) to eliminate changes in Isc caused by sodium absorption. All data from the voltage clamps are collected via a computer interface and analyzed off-line.
Concentration-effect relationships for all compounds are considered and analyzed Using GraphPad Prism version 3.00 for Windows, GraphPad Software, San Diego Calif. USA. EC 50 values, maximal effective concentrations, are calculated and compared to either formoterol or salbutamol as the positive control.
2. In Vitro Assay of Compound Absorption and Biotransformation by Airway Epithelia
Airway epithelial cells have the capacity to metabolize drugs during the process of transepithelial absorption. Further, although less likely, it is possible that drugs can be metabolized on airway epithelial surfaces by specific ectoenzyme activities. Perhaps more likely as an ecto-surface event, compounds may be metabolized by the infected secretions that occupy the airway lumens of patients with lung disease, e.g. cystic fibrosis. Thus, a series of assays are performed to characterize any compound biotransformation (metabolism or conjugation) that results from the interaction of test compounds with human airway epithelia and/or human airway epithelial lumenal products.
In the first series of assays, the interaction of test compounds in KBR as an “ASL” stimulant are applied to the apical surface of human airway epithelial cells grown in the Transwell® Permeable Supports (Corning), insert system. For most compounds, metabolism or conjugation (generation of new species) is tested for using high performance liquid chromatography (HPLC) to resolve chemical species and the endogenous fluorescence properties of these compounds to estimate the relative quantities of test compound and novel metabolites. For a typical assay, a test solution (1 mL KBR, containing 100 μM n test compound) is placed on the epithelial lumenal surface. Sequential 5 to 600 μl samples are obtained from the lumenal and serosal compartments respectively for HPLC analysis of (1) the mass of test compound permeating from the lumenal to serosal bath and (2) the potential formation of metabolites from the parent compound. From the HPLC data, the rate of and/or formation of novel metabolite compounds on the lumenal surface and the appearance of test compound and/or novel metabolite in the basolateral solution is quantitated based on internal standards. The data relating the chromatographic mobility of potential novel metabolites with reference to the parent compound are also quantitated.
To analyze the potential metabolism of test compounds by CF sputum, a “representative” mixture of expectorated CF sputum obtained from 10 CF patients (under IRB approval) has been collected. The sputum has been be solubilized in a 1:5 mixture of KBR solution with vigorous vortexing, following which the mixture was split into a “neat” sputum aliquot and an aliquot subjected to ultracentrifugation so that a “supernatant” aliquot was obtained (neat=cellular; supernatant=liquid phase). Typical studies of compound metabolism by CF sputum involve the addition of known masses of test compound to “neat” CF sputum and aliquots of CF sputum “supernatant” incubated at 37° C., followed by sequential sampling of aliquots from each sputum type for characterization of compound stability/metabolism by HPLC analysis as described above. As above, analysis of compound disappearance, rates of formation of novel metabolities, and HPLC mobilities of novel metabolites are then performed.
EXAMPLES
Having generally described this invention, a further understanding can be obtained by reference to certain specific examples which are provided herein for purposes of illustration only and are not intended to be limiting unless otherwise specified.
Preparation of Sodium Channel Blockers with Beta Agonist Activity
Materials and methods. All reagents and solvents were purchased from Aldrich Chemical Corp. and used without further purification. NMR spectra were obtained on either a Bruker WM 360 ( 1 H NMR at 360 MHz and 13 C NMR at 90 MHz) or a Bruker AC 300 ( 1 H NMR at 300 MHz and 13 C NMR at 75 MHz). Flash chromatography was performed on a Flash Eluteθ system from Elution Solution (PO Box 5147, Charlottesville, Va. 22905) charged with a 90 g silica gel cartridge (40M FSO-0110-040155, 32-63 μm) at 20 psi (N 2 ).
GC-analysis was performed on a Shimadzu GC-17 equipped with a Heliflex Capillary Column (Alltech); Phase: AT-1, Length: 10 meters, ID: 0.53 mm, Film: 0.25 micrometers. GC Parameters: Injector at 320° C., Detector at 320° C., FID gas flow: H 2 at 40 ml/min., Air at 400 ml/min. Carrier gas: Split Ratio 16:1, N 2 flow at 15 N 2 velocity at 18 cm/sec. The temperature program is 70° C. for 0-3 min, 70-300° C. from 3-10 min, 300° C. from 10-15 min.
HPLC analysis was performed on a Gilson 322 Pump, detector UV/Vis-156 at 360 nm, equipped with a Microsorb MV C8 column, 100 A, 25 cm. Mobile phase: A=acetonitrile with 0.1% TFA, B=water with 0.1% TFA. Gradient program: 95:5 B:A for 1 min, then to 20:80 B:A over 7 min, then to 100% A over 1 min, followed by washout with 100% A for 11 min, flow rate: 1 ml/min.
Example 1
Synthesis of (R)-3,5-diamino-6-chloro-N—(N-{11-[2-(3-formamido-4-hydroxyphenyl)-2-hydroxyethylamino]undecyl}carbamimidoyl)pyrazine-2-carboxamide (15) (Scheme 1)
1-(4-Benzyloxy-3-nitrophenyl)ethanone (2)
A mixture of 1-(4-hydroxy-3-nitrophenyl)ethanone (50.00 g, 276 mmol), sodium iodide (20.00 g, 133.4 mmol), potassium carbonate (115.00 g, 832.00 mmol), and benzyl bromide (43.00 mL, 362.00 mmol) in acetone (120 mL) was stirred under reflux for 16 h. The solids were removed by filtration and the filtrate concentrated by rotary evaporation. After this time the resulting residue was diluted with dichloromethane and insoluble inorganics were removed by filtration. The filtrate was concentrated in vacuo and the resulting residue was dissolved in hot chloroform. Hexanes were added to form a precipitate. The solids were collected by filtration to give benzyl ether 2 as a white solid (65.60 g, 87%): 1 H NMR (500 MHz, CDCl 3 ) δ 2.60 (s, 3H), 5.32 (s, 2H), 7.18 (d, 1H), 7.41 (m, 5H), 8.12 (dd, 1H), 8.44 (d, 1H).
1-(4-Benzyloxy-3-nitrophenyl)-2-bromoethanone (3)
Phenyltrimethylammonium tribromide (109.00 g, 290.00 mmol) was added to a solution of 1-(4-benzyloxy-3-nitrophenyl)ethanone (2) (65.60 g, 242.00 mmol) in anhydrous THF (600 mL) in three portions, and the reaction mixture was stirred at rt for 12 h. The solids were then collected by filtration and the filtrate concentrated. The product was precipitated from chloroform upon the addition of hexanes, then collected by filtration and dried under vacuum to give bromo ketone 3 as a light yellow solid (63.33 g, 75% yield): 1 H NMR (500 MHz, CDCl 3 ) δ 4.37 (s, 3H), 5.35 (s, 2H), 7.21 (d, 1H), 7.40 (m, 5H), 8.15 (dd, 1H), 8.49 (d, 1H).
1-(4-Benzyloxy-3-nitrophenyl)-2-bromo-1-(R)-ethanol (4)
A solution of BH 3 .THF in THF (1 M, 108.00 mL, 108.00 mmol) was added to a solution of 1-(4-benzyloxy-3-nitrophenyl)-2-bromoethanone (3) (63.30 g, 180.00 mmol) and R-methyl-CBS-oxazoborolidine (1 M in toluene, 36.00 mL, 36.00 mmol) in anhydrous THF (500 mL). The resulting reaction mixture was stirred at rt for 16 h. Methanol (250 mL) was then slowly added to quench the reaction. After removal of solvent by rotary evaporation, the resulting residue was purified by column chromatography (silica gel, a gradient of 70:30 to 100:0 dichloromethane/hexanes) to give the desired bromo alcohol 4 as a yellow, viscous oil (36.80 g, 75% yield): 1 H NMR (500 MHz, CDCl 3 ) δ 2.72 (d, 1H), 3.48 (dd, 1H), 3.59 (dd, 1H), 4.89 (m, 1H), 5.21 (s, 2H), 7.11 (d, 1H), 7.39 (m, 5H), 7.50 (dd, 1H), 7.87 (d, 1H).
N-[2-Benzyloxy-5-(2-bromo-1-(R)-hydroxyethyl)phenyl]formamide (5)
A Parr hydrogenator was charged with PtO 2 and 1-(4-benzyloxy-3-nitro-phenyl)-2-bromo-1-(R)-ethanol (4) (3.60 g, 10.22 mmol) dissolved in a mixed solvent of THF (25 mL) and toluene (25 mL); and the mixture shaken under an atmosphere of hydrogen at 55 psi at rt for 14 h. The hydrogen pressure was then released. To the mixture was added directly a mixture of formic acid (0.65 mL, 17.23 mmol) and acetic anhydride (1.10 mL, 11.65 mmol). The newly resulting mixture was stirred at rt for an additional 16 h. The catalyst was removed by filtration through a Celite pad and the filtrate was concentrated by rotary evaporation. The resulting residue was purified by column chromatography (silica gel, a gradient of 30:70 to 50:50 ethyl acetate/hexanes) to give the desired formamide 5 as a white solid (3.62 g, >99% yield): 1 H NMR (300 MHz, CDCl 3 ) δ 2.95 (s, 1H), 3.52 (m, 1H), 3.60 (m, 1H), 4.85 (m, 1H), 5.08 (s, 2H), 6.96 (d, 1H), 7.13 (dd, 1H), 7.39 (m, 5H), 7.88 (br s, 1H), 8.37 (dd, 1H).
tert-Butyl 11-aminoundecylcarbamate (7)
Using a syringe pump, a solution of di-tert-butyl dicarbonate (2.50 g, 11.45 mmol) in methanol (50 mL) was added to a stirred solution of undecane 1,11-diamine (6) (3.00 g, 16.10 mmol) and diisopropylethylamine (2.90 mL, 16.60 mmol) in methanol (200 mL) over 10 h, and the resulting reaction mixture was stirred at rt for 12 h. The reaction was then concentrated to a white solid. Purification by column chromatography (silica gel, 10:90 methanol/dichloromethane, then 20:80 (10% concentrated ammonium hydroxide in methanol)/dichloromethane) afforded the protected amine 7 (2.19 g, 67% yield) as a white solid: 1 H NMR (300 MHz, CD 3 OD) δ 1.30 (br s, 14H), 1.43 (br s, 13H), 2.61 (t, 2H), 3.00 (t, 2H).
Benzyl 11-(1-tert-butylamino)undecyl carbamate (8)
Benzylchloroformate (1.30 mL, 9.14 mmol) was added to a mixture of tert-butyl 11-aminoundecylcarbamate (7) (2.19 g, 7.65 mmol) in dichloromethane (40 mL) and 25% sodium carbonate in water (20 mL), and the resulting reaction mixture was stirred at ambient temperature for 3 h. After this time the reaction was extracted with dichloromethane (2×50 mL). The organic extracts combined, concentrated and placed under vacuum. Purification by column chromatography (silica gel, 10:90 methanol/dichloromethane, followed by a gradient of 5:95 to 10:90 (10% concentrated ammonium hydroxide in methanol)/dichloromethane) gave the desired diamine 8 (2.88 g, 92% yield) as a white solid: 1 H NMR (500 MHz, CDCl 3 ) δ 1.25-1.28 (m, 14H), 1.43-1.55 (m, 13H), 3.09-3.18 (m, 4H), 4.51 (br s, 1H), 4.70 (br s, 1H), 5.09 (s, 2H), 7.22-7.34 (m, 5H); m/z (ESI) 411 [C 26 H 38 N 2 O 2 +H] + .
Benzyl 11-aminoundecylcarbamate (9)
Diamine 8 (1.00 g, 2.45 mmol) was dissolved in methanolic hydrogen chloride (10 M, mL) and stirred at ambient temperature for 2 h. After removal of solvent by rotary evaporation, the residue was dissolved in dichloromethane/methanol (2:1, v/v) and triethylamine (0.40 mL, 2.84 mmol) was added. The solution was stirred for 30 min, and then the solvent was removed under vacuum. The residue was carried into the next reaction without purification or characterization.
Benzyl 11-(benzylamino)undecylcarbamate (11)
Benzaldehyde 10 (0.25 mL, 2.47 mmol) was added to a mixture of carbamate 23 (0.76 g, 2.36 mmol), sodium sulfate (100 mg) and ethereal hydrogen chloride (1 M, 2 drops) in dichloroethane (25 mL). The reaction was stirred at ambient temperature for 14 h, then sodium triacetoxyborohydride (0.75 g, 3.54 mmol) was added and stirring continued for an additional 1 h. The reaction was quenched by the addition of saturated aqueous sodium bicarbonate and extracted with dichloromethane (3×25 mL). The combine organics were concentrated under vacuum, then purified by column chromatography (silica, 10:90 (10% concentrated ammonium hydroxide in methanol)/dichloromethane) to give benzylamine 11 (0.44 mg, 59% yield) as a white solid: 1 H NMR (500 MHz, CD 3 OD) δ 1.29 (m, 14H), 1.46-1.55 (m, 2H), 2.61 (t, 2H), 3.09 (t, 2H), 3.78 (s, 2H), 4.59 (s, 1H), 5.05 (s, 2H), 7.22-7.34 (m, 10H); m/z (ESI) 411 [C 26 H 38 N 2 O 2 +H] + .
(R)-Benzyl 11-(benzyl{2-[4-(benzyloxy)-3-formamidophenyl]-2-hydroxyethyl}-amino)undecylcarbamate (12)
Benzylamine 11 (0.32 g, 0.79 mmol) was added to a suspension of bromoalcohol 19 (0.33 g, 0.95 mmol) and potassium carbonate (0.27 g, 1.98 mmol) in isopropanol (7 mL). The suspension was heated to 83° C. for 40 h. After this time the mixture was cooled, the solid was removed by vacuum filtration and the filtrate was concentrated under vacuum. The resulting yellow solid was subjected to column chromatography (silica, a gradient of 20:80 to 50:50 ethyl acetate/hexanes) to afford the desired product 12 (0.28 g, 52% yield) as a clear oil: 1 H NMR (300 MHz, CD 3 OD) δ 1.19-1.72 (m, 18H), 2.48-2.73 (m, 2H), 3.04-3.08 (m, 2H), 3.61-3.84 (m, 2H), 4.66 (t, 1H), 5.04 (br s, 2H), 5.18 (br s, 2H), 6.99-7.67 (m, 18H), 8.22-8.32 (m, 1H);
(R)—N-{5-[2-(11-Aminoundecylamino)-1-hydroxyethyl]-2-hydroxyphenyl}formamide (13)
Aminoalcohol 12 (028 g, 0.41 mmol) was dissolved in ethanol (10 mL). Following the standard hydrogenation procedure, palladium dihydroxide (20% on carbon, 50% wet) was added. The reaction mixture was stirred for 48 h at ambient temperature under atmospheric hydrogen pressure. The catalyst was removed by filtration through diatomaceous earth and the filtrate was concentrated. Drying under vacuum gave 27 (0.12 g, 77% yield) as an orange oil: 1 H NMR (300 MHz, CD 3 OD) δ 1.19-1.72 (m, 18H), 2.58-2.89 (m, 4H), 3.51-3.72 (m, 1H), 4.74 (m, 1H), 6.72-6.81 (m, 1H), 6.91-7.06 (m, 1H), 8.02-8.08 (m, 1H), 8.29 (br, 1H).
(R)-3,5-Diamino-6-chloro-N—(N-{11-[2-(3-formamido-4-hydroxyphenyl)-2-hydroxyethylamino]undecyl}carbamimidoyl)pyrazinecarboxamide (15)
Diisopropylethylamine (0.07 mL, 0.40 mmol) and 1-(3,5-diamino-6-chloropyrazine-2-carbonyl)-2-methylisothiourea hydriodide (125 mg, 0.32 mmol) were sequentially added to a solution of amine 14 (116 mg, 0.32 mmol) in ethanol (5 mL). The reaction mixture was heated to 75° C. for 3.5 h. After this time it was cooled and concentrated under vacuum. The resulting residue was purified by column chromatography (silica, a gradient of 10:90 to 80:20 (10% concentrated ammonium hydroxide/methanol)/dichloromethane) affording the crude product. Further purification by prep HPLC [10 to 90% acetonitrile in water (both with 0.01% TFA added) over 40 minutes] and then prep TLC (silica, 10:90 to 30:70 (10% concentrated ammonium hydroxide/methanol)/dichloromethane gave product 15 (26 mg, 14%) as a brown solid: mp 112-116° C.; 1 H NMR (500 MHz, CD 3 OD) δ 1.27-1.49 (m, 15H), 1.61-1.74 (m, 4H), 2.91-3.08 (m, 4H), 6.85-6.87 (m, 1H), 7.02-7.05 (m, 1H), 8.01-8.02 (m, 1H), 8.31 (br s, 1H); m/z (ESI) 578 [C 26 H 40 ClN 9 O 4 +H] + .
Example 2
Compound 15, ENaC Blocking Activity, IC50 (nM)=27.8 (39× Amiloride)
Beta Agonist Activity, EC50 (nM)=206 (fomoterol=5.3)
Example 3
Compound 16 ENaC Blocking Activity, IC50 (nM)=6.5 (158× Amiloride)
Synthesis of 3,5-diamino-6-chloro-N—(N—((S)-11-(R)-2-(3-formamido-4-hydroxyphenyl)-2-hydroxyethylamino)dodecyl)carbamimidoyl)pyrazine-2-carboxamide di-L-lactate [26a and 26b] (Scheme 2)
11-(Benzyloxycarbonylamino)undecanoic acid (18)
To a suspension of 11-aminoundecanoic acid (17) in 1:1 water/dioxane (160 mL total) was added K 2 CO 3 (10.28 g, 74.51 mmol) followed by the slow addition over 30 min of benzylchloroformate (CbzCl, 4.55 mL, 32.29 mmol), and the mixture was stirred at room temperature for 2 h. The solid was then removed by filtration, washed with water (3×30 mL) and dried in a vacuum oven at 40° C. for 72 h to afford a white solid 18 (2.91 g, 35% yield): 1 H NMR (500 MHz, CD 3 OD) δ 1.36 (m, 12H), 1.50 (m, 2H), 1.62 (m, 2H), 2.18 (m, 2H), 3.08 (m, 2H), 5.14 (s, 2H), 7.38 (m, 5H); m/z (ESI) 336 [M+H] + .
Methyl 11-(benzyloxycarbonylamino)undecanoate (19)
A suspension of 18 (2.91 g, 8.68 mmol), Cs 2 CO 3 (4.25 g, 13.02 mmol) and DMF (anhydrous, 40 mL) was stirred at room temperature for 1.5 h. To the mixture was then added methyl iodide (0.83 mL, 13.02 mmol), and stifling was continued for an additional 3 h at the ambient temperature. The mixture was then partitioned between water (150 mL) and dichloromethane (150 mL), aqueous layer was separated and washed with dichloromethane (3×300 mL). Organics were combined, dried over anhydrous Na 2 SO 4 , concentrated and further dried under high vacuum overnight to afford the desired methyl ester 19 (3.41 g, quant yield): 1 H NMR (500 MHz, CDCl 3 ) δ 1.26 (m, 12H), 1.47 (m, 2H), 1.52 (m, 2H), 2.28 (m, 2H), 3.16 (m, 2H), 3.66 (s, 3H), 5.10 (s, 2H), 7.32 (m, 5H); m/z (ESI) 350 [M+H] + .
Benzyl 11-(methoxy(methyl)amino)-11-oxoundecylcarbamate (20)
A solution of 19 (2.25 g, 6.44 mmol), methyl methoxyamine hydrochloride (1.26 g, 12.88 mmol) and THF (anhydrous, 30 mL) was cooled to −15 to −20° C. with an ice/methanol bath containing a few pieces of dry ice. To this cold solution was added dropwise i-PrMgCl (3M solution in pentane, 11.27 mL, 22.54 mmol) over 15 min and temperature was then raised to −10° C. and stirring continued at the temperature for additional 2 h. After this time the reaction was quenched by the slow addition of saturated aqueous NH 4 Cl (50 mL). The aqueous layer was separated and washed with dichloromethane (2×50 mL). Organics were combined, dried over anhydrous Na 2 SO 4 , concentrated and further dried under high vacuum overnight to afford the desired product 20 (2.04 g, 84% yield) as a colorless, viscous oil: 1 H NMR (300 MHz, CDCl 3 ) δ 1.27 (m, 12H), 1.48 (m, 2H), 1.60 (m, 2H), 2.40 (m, 2H), 3.18 (m, 5H), 3.68 (s, 3H), 5.09 (s, 2H), 7.34 (m, 5H); m/z (ESI) 379 [M+H] + .
Benzyl 11-oxododecylcarbamate (21)
To a solution of 20 (1.11 g, 2.94 mmol) in THF (anhydrous, 10 mL) and cooled in an ice bath was added dropwise MeMgCl (3 M solution in diethyl ether, 3.92 mL, 11.75 mmol) over 10 min, and stirring continued at 0° C. for 6 h. The reaction was quenched by the slow addition of methanol (10 mL), and then concentrated under vacuum. The residue was chromatographed (silica gel, a gradient of 0:100 to 18:82 ethyl acetate/hexanes) to afford the desired product 21 (0.78 g, 80% yield) as a white solid: 1 H NMR (300 MHz, CDCl 3 ) δ 1.26 (m, 12H), 1.49-1.57 (m, 4H), 2.13 (s, 3H), 2.41 (m, 2H), 3.19 (m, 5H), 5.09 (s, 2H), 7.34 (m, 5H); m/z (ESI) 334 [M+H] + .
(R)-Benzyl 11-(2-(3-formamido-4-hydroxyphenyl)-2-hydroxyethylamino)dodecyl-carbamate (23)
A solution containing compound 19 (0.43 g, 1.29 mmol) and (R)—N-(5-(2-amino-1-hydroxyethyl)-2-benzyloxy)phenyl)formamide 22 (0.27 g, 1.35 mmol) in methanol (anhydrous, 6 mL) was stirred at room temperature for 4 h. To this solution was then added NaCNBH 3 (0.24 g, 3.87 mmol) in one portion, and the mixture was continuously stirred at room temperature overnight. After this time, the mixture was concentrated and the residue was subjected to chromatography (a gradient of 0:100 to 10:90 methanol/dichloromethane) to afford the desired product 23 (0.54 g, 82% yield): 1 H NMR (300 MHz, CD 3 OD) δ 1.31 (m, 15H), 1.48-1.58 (m, 4H), 1.75 (m, 2H), 3.10 (m, 5H), 4.83 (m, 1H), 5.09 (s, 2H), 6.89 (d, 1H), 7.04 (d, 1H), 7.34 (m, 6H), 8.12 (s, 1H), 8.32 (s, 1H); m/z (ESI) 514 [M+H] + .
(R)—N-(5-(2-(12-Aminododecan-2-ylamino)-1-hydroxyethyl)-2-hydroxyphenyl)-formamide (24)
A mixture of compound 23 (0.54 g, 1.05 mmol) dissolved in methanol (30 mL) and palladium catalyst (0.15 g, 10% Pd on carbon, 50% we) was stirred overnight at room temperature under one atmospheric hydrogen pressure. The catalyst was removed by filtration and washed with methanol (3×10 mL). The filtrate and washings were combined and concentrated under vacuum to complete dryness, affording the desired product 24 (0.40 g, 91% yield) as an off-white solid: 1 H NMR (300 MHz, CD 3 OD) δ 1.31 (m, 15H), 1.48-1.58 (m, 4H), 1.75 (m, 2H), 260-2.80 (m, 5H), 4.66 (m, 1H), 5.09 (s, 2H), 6.82 (d, 1H), 7.00 (d, 1H), 8.02 (s, 1H), 8.30 (s, 1H); m/z (ESI) 380 [M+H] + .
3,5-Diamino-6-chloro-N—(N—((R)-11-((R)-2-(3-formamide-4-hydroxyphenyl)-2-hydroxyethylamino)dodecyl)carbamimidoyl)pyrazine-2-carboxamide (25a) and 3,5-Diamino-6-chloro-N—(N—((S)-11-(R)-2-(3-formamide-4-hydroxyphenyl)-2-hydroxyethylamine)dodecyl)carbamimidoyl)pyrazine-2-carboxamide (25b)
A suspension of compound 24 (0.40 g, 1.05 mmol), Hunig's base (0.89 mL, 5.27 mmol) and ethanol (14 mL) was heated at 70° C. for 30 min, and then 1-(3,5-diamino-6-chloropyrazine-2-carbonyl)-2-methylisothiourea hydriodide (0.43, 1.17 mmol) was added. The resulting solution was continuously stirred at that temperature for an additional 3 h before it was cooled to room temperature. The un-dissolved solid was removed by filtration, and the filtrate was concentrated. The resulting residue was subjected to column chromatography eluting with a mixture of methanol (0-16%), concentrated ammonium hydroxide (0-1.6%) and dichloromethane (100-83.4%) to afford a mixture of 25a and 25b (0.12 g total, 20% overall yield): 1 H NMR (500 MHz, CD 3 OD) δ 1.12 (m, 6H), 1.38-1.50 (m, 30H), 1.57 (m, 4H), 1.73 (m, 4H), 2.72-2.90 (m, 6H), 3.33 (m, 4H), 4.60-4.70 (m, 2H), 6.84 (d, 2H), 7.04 (d, 2H), 8.10 (s, 2H), 8.30 (s, 2H); m/z (ESI) 592 [M+H] + . This material was subjected to further chromatography by prep TLC plates eluting several times with a mixture of methanol (0-22%), concentrated ammonium hydroxide (0-2.2%) and dichloromethane (100-75.8%) to afford 25a (42 mg) and 256 (56 mg), respectively, both as yellow solids. The stereochemistry of the chiral methyl groups in 68a and 69a were arbitrarily assigned.
3,5-Diamino-6-chloro-N—(N—((R)-11-(R)-2-((3-formamido-4-hydroxyphenyl)-2-hydroxyethylamino)dodecyl)carbamimidoyl)pyrazine-2-carboxamide di-L-lactate [26a]
L-lactic acid (13.7 mg, 0.14 mmol) was added to a suspension of compound 25a (42 mg, 0.15 mmol) in absolute ethanol (3 mL). The mixture was stirred at room temperature for 1 h and turned to a clear solution. The solution was then concentrated under vacuum and completely dried to afford 26a (46 mg, quant yield) as a brown, viscous oil: 1 H NMR (500 MHz, DMSO-d 6 ) δ 1.18-1.24 (m, 21H), 1.40-1.75 (m, 6H), 2.96 (m, 2H), 3.07 (m, 1H), 3.28 (m, 2H), 4.10 (m, 2H), 4.82 (m, 1H), 6.08 (br s, 1H), 6.84 (d, 1H), 7.04 (d, 1H), 7.48 (br s, 2H), 8.16 (s, 1H), 8.30 (s, 1H), 8.88-9.10 (br s, 2H), 9.66 (s, 1H), 9.96 (br s, 1H); m/z (ESI) 592 [M+H] + .
3,5-Diamino-6-chloro-N—(—((S)-11-(R)-2-((3-formamide-4-hydroxyphenyl)-2-hydroxyethylamino)dodecyl)carbamimidoyl)pyrazine-2-carboxamide di-L-lactate [26b]
Compound 26b (44 mg, quant yield), a brown solid, was prepared from 25b in a similar method to 68a: mp 86-88° C. (decomposed); 1 H NMR (500 MHz, DMSO-d 6 ) δ 1.11 (d, 3H), 1.20 (s, 6H), 1.28-1.36 (m, 12H), 1.48-1.70 (m, 6H), 2.78-3.26 (m, 5H), 3.92 (m, 2H), 4.64 (m, 1H), 6.72-6.82 (br s, 2H), 6.84 (d, 1H), 6.92 (d, 1H), 8.09 (s, 1H), 8.28 (s, 1H), 9.59 (br s, 1H); m/z (ESI) 592 [M+H] + .
Methods
Pharmacological Effects and Mechanism of Action of the Drug in Animals
The effect of compounds for enhancing mucociliary clearance (MCC) can be measured using an in vivo model described by Sabater et al., Journal of Applied Physiology, 1999, 87(6) pp. 2191-2196, incorporated herein by reference.
Animal Preparation: Adult ewes up to 75 Kg were placed in a restrain and positioned upright using a specialized body harness. The heads of the animals were immobilized, and local anesthesia of the nasal passage was provided (2% lidocaine) prior to nasal intubation (7.5 mm-I.D. endotracheal tube (ETT) (Mallinckrodt Medical, St. Louis, Mo.). The cuff of the ETT was placed just below the vocal cords. After intubation, the animals were allowed to equilibrate for approximately 20 min before MCC measurements began.
Sheep MCC in vivo Measurement: Aerosols of sulfur colloid radiolabled with technetium ( 99m Tc—SC 3.1 mg/mL, ˜10-15 mCi) were generated by a Raindrop Nebulizer (Nellcor Puritan Bennett, Pleasanton, Calif.) which produces a median aerodynamic droplet diameter of 3.6 μm. The nebulizer was connected to a dosimeter system consisting of a solenoid valve and a source of compressed air (20 psi). The output of the nebulizer was directed into a T piece, with one end attached to a respirator (Harvard apparatus, South Natick, Mass.). The system was activated for 1 second at the onset of the respirator's inspiratory cycle. The tidal volume was set at 300 mL, with an inspiratory-to-expiratory ratio of 1:1, and a rate of 20 breaths/min, to maximize central airway deposition. The sheep breathed the 99m Tc—SC aerosol for up to 5 min. Following tracer deposition, a gamma camera was used to measure the clearance of 99m Tc—SC from the airways. The camera was positioned above the animal's back with the sheep in its natural upright position in the harness. The field of the image was perpendicular to the animal's spinal cord. External radiolabled markers were placed on the sheep to facilitate proper alignment of the gamma camera. A region of interest was traced over the image corresponding to the right lung of the sheep and counts were recorded. The counts were corrected for decay and expressed as a percentage of radioactivity present in the baseline image. The left lung was excluded from the analysis because the outline of the lung was superimposed over the stomach and counts could be affected by swallowed 99m Tc—SC-labeled mucus. All deposition images were stored on a computer interfaced to the gamma camera. The protocol included a baseline deposition image obtained immediately post radio-aerosol administration. After acquisition of baseline images, either 4 mL of H 2 O (vehicle), formoterol (3 mM), or novel chemical entity (3 mM) were aerosolized using the Pari LC JetPlus nebulizer to free-breathing sheep using two separate protocols. Protocol 1, acquired data immediately after dosing (time 0 to 1 hour), and indicated the immediate physiological response ‘short-term efficacy’ protocol 2, acquired data 4 hours post dosing indicated compound durability and ‘long-term efficacy’. The nebulizer had a flow rate of 8 L/min and the time to deliver the solution was 10-12 min. On the completion of compound administration, the animal was immediately extubated to prevent false elevations in counts due to aspiration of excess 99m Tc—SC-labeled mucus from the ETT. Serial measurements of 99m Tc—SC retained in the lung were obtained over a 1 hour period at 5 min intervals. A washout period of at least 7 days (half life of 99m TC=6 h) separated studies with the different agents.
Statistical Analysis: Data from the in vivo sheep MCC assays were analyzed using a two way ANOVA with repeated measures, followed by slope analysis of the linear regression of the retention vs time plot using an ANOCOVA to compare slopes, and if needed a multiple comparison test (Newman-Keuls). The percent activity retained (post 4 hours) was calculated by dividing the slope value from protocol 2 by the slope value obtained in protocol 1 and multiplying by 100%.
Animal Preparation: Adult ewes (ranging in weight from 25 to 35 kg) were restrained in an upright position in a specialized body harness adapted to a modified shopping cart. The animals' heads were immobilized and local anesthesia of the nasal passage was induced with 2% lidocaine. The animals were then nasally intubated with a 7.5 mm internal diameter endotracheal tube (ETT). The cuff of the ETT was placed just below the vocal cords and its position was verified with a flexible bronchoscope. After intubation the animals were allowed to equilibrate for approximately 20 minutes prior to initiating measurements of mucociliary clearance.
Administration of Radio-aerosol: Aerosols of 99m Tc-Human serum albumin (3.1 mg/ml; containing approximately 20 mCi) were generated using a Raindrop Nebulizer which produces a droplet with a median aerodynamic diameter of 3.6 p.m. The nebulizer was connected to a dosimetry system consisting of a solenoid valve and a source of compressed air (20 psi). The output of the nebulizer was directed into a plastic T connector; one end of which was connected to the endotracheal tube, the other was connected to a piston respirator. The system was activated for one second at the onset of the respirator's inspiratory cycle. The respirator was set at a tidal volume of 500 mL, an inspiratory to expiratory ratio of 1:1, and at a rate of 20 breaths per minute to maximize the central airway deposition. The sheep breathed the radio-labeled aerosol for 5 minutes. A gamma camera was used to measure the clearance of 99m Tc-Human serum albumin from the airways. The camera was positioned above the animal=s back with the sheep in a natural up ht position supported in a cart so that the field of image was perpendicular to the animal=s spinal cord. External radio-labeled markers were placed on the sheep to ensure proper alignment under the gamma camera. All images were stored in a computer integrated with the gamma camera. A region of interest was traced over the image corresponding to the right lung of the sheep and the counts were recorded. The counts were corrected for decay and expressed as percentage of radioactivity present in the initial baseline image. The left lung was excluded from the analysis because its outlines are superimposed over the stomach and counts can be swallowed and enter the stomach as radio-labeled mucus.
Treatment Protocol (Assessment of activity at t-zero): A baseline deposition image was obtained immediately after radio-aerosol administration. At time zero, after acquisition of the baseline image, vehicle control (distilled water), positive control (amiloride), or experimental compounds were aerosolized from a 4 ml volume using a Pari LC JetPlus nebulizer to free-breathing animals. The nebulizer was driven by compressed air with a flow of 8 liters per minute. The time to deliver the solution was 10 to 12 minutes. Animals were extubated immediately following delivery of the total dose in order to prevent false elevations in counts caused by aspiration of excess radio-tracer from the ETT. Serial images of the lung were obtained at 15-minute intervals during the first 2 hours after dosing and hourly for the next 6 hours after dosing for a total observation period of 8 hours. A washout period of at least 7 days separated dosing sessions with different experimental agents.
Treatment Protocol (Assessment of Activity at t-4 hours): The following variation of the standard protocol was used to assess the durability of response following a single exposure to vehicle control (distilled water), positive control compounds (amiloride or benzamil), or investigational agents. At time zero, vehicle control (distilled water), positive control (amiloride), or investigational compounds were aerosolized from a 4 ml volume using a Pari LC JetPlus nebulizer to free-breathing animals. The nebulizer was driven by compressed air with a flow of 8 liters per minute. The time to deliver the solution was 10 to 12 minutes. Animals were restrained in an upright position in a specialized body harness for 4 hours. At the end of the 4-hour period animals received a single dose of aerosolized 99m Tc-Human serum albumin (3.1 mg/ml; containing approximately 20 mCi) from a Raindrop Nebulizer. Animals were extubated immediately following delivery of the total dose of radio-tracer. A baseline deposition image was obtained immediately after radio-aerosol administration. Serial images of the lung were obtained at 15-minute intervals during the first 2 hours after administration of the radio-tracer (representing hours 4 through 6 after drug administration) and hourly for the next 2 hours after dosing for a total observation period of 4 hours. A washout period of at least 7 days separated dosing sessions with different experimental agents.
Statistics: Data were analyzed using SYSTAT for Windows, version 5. Data were analyzed using a two-way repeated ANOVA (to assess overall effects), followed by a paired t-test to identify differences between specific pairs. Significance was accepted when P was less than or equal to 0.05. Slope values (calculated from data collected during the initial 45 minutes after dosing in the t-zero assessment) for mean MCC curves were calculated using linear least square regression to assess differences in the initial rates during the rapid clearance phase.
Obviously, numerous 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 herein.
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The present application provides sodium channel blockers exemplified by the following structure:
The compounds of the invention useful for treating chronic bronchitis, cystic fibrosis, sinusitis, vaginal dryness, dry eye, Sjogren's disease, distal intestinal obstruction syndrome, dry skin, esophagitis, dry mouth (xerostomia), nasal dehydration, ventilator-induced pneumonia, asthma, primary ciliary dyskinesia, otitis media, chronic obstructive pulmonary disease, emphysema, pneumonia, constipation, and chronic diverticulitis, for example.
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BACKGROUND OF THE INVENTION
The following invention relates to a thin-film electroluminescent (TFEL) device for providing an improved optical display. More particularly, the invention relates to a thin-film absorption layer within the device for absorbing incident light.
TFEL displays are constructed of a laminar stack comprising a set of transparent front electrodes which are typically made of indium tin oxide formed on a transparent substrate (glass), and a transparent electroluminescent phosphor layer sandwiched between transparent dielectric layers situated behind the front electrodes. Disposed behind the rear dielectric layer are rear electrodes which are usually constructed of aluminum because it provides both good electrical conductivity and a self-healing failure characteristic. Aluminum rear electrodes also enhance the luminescence of the display by reflecting back towards the viewer most of the light that would otherwise be lost to the rear of the display. This reflected light nearly doubles the light of the displayed image because the phosphor layer emits light that is directed in equal amounts in both the forward and rearward directions. However, the aluminum rear electrodes also reflect forward ambient light entering from outside of the display which is superimposed with the display information thus reducing its contrast.
To increase the contrast of the display, an antireflection coating is sometimes used on the front transparent substrate of the display to reduce the amount of ambient light reflected from the front of the display. The TFEL laminar stack may further include an enclosure seal against the substrate, with the rear wall of the enclosure blackened to block light entering from extraneous light sources behind the display. The black coating absorbs ambient light passing through the display from the front that was not reflected by the rear electrodes.
The reflection off the rear electrodes, which are typically aluminum, has a diffuse reflectance due to the surface roughness of the reflective rear electrodes, which in turn adds to the diffuse scattering from other thin-film layers of the display. The diffuse reflectance is typically measured with a photometer placed in the viewing position and perpendicular to the display. With ambient light directed at the display from a 45 degree angle to the perpendicular viewing direction, a typical TFEL display has approximately 15% diffuse reflectance. A circular polarizer filter reduces the diffuse reflectance from about 15% to about 1%, but transmits only about 37 to 42 percent of the emitted light from the display and adds substantially to the cost of the display.
Another approach that has been tried for improving the display contrast is to use indium tin oxide transparent rear electrodes. This reduces the reflectance of light off the rear electrodes and permits light to pass on through to the back of the display where it may be absorbed. However, indium tin oxide is of higher resistivity than metallic electrodes, such as those made of aluminum, and therefore must be made much thicker to achieve adequate electric conductivity. Further, thick layers of indium tin oxide do not exhibit the self-healing characteristics of aluminum rear electrodes. This can lead to an unacceptable loss in device reliability due to dielectric breakdown.
In yet another approach, shown in Steel et al., U.S. Pat. No. 3,560,784, a light-absorbing layer is incorporated into the thin-film laminate structure. This reference suggests that if a conventional metallic rear electrode is used, then a light absorbing layer may be added as an insulating layer or as a conductive layer. Insertion of a dark layer immediately behind the phosphor layer, however, can interfere with the phosphor/insulator interface leading to inferior display performance. The light pulse for one polarity may be reduced which can give rise to a flicker effect as well as to a loss in overall brightness.
Shimizu, U.S. Pat. No. 5,003,221 discloses the use of a thin-film layer that is formed between a transparent substrate and a layer formed adjacent to the transparent substrate in a TFEL laminar stack. The refractive index of the thin-film layer is made to change to approximate that of layers toward the interfaces between the thin-film layer and the corresponding layers, so that a difference in the refractive index at these interfaces is minimized. Shimizu is directed to solving the problem of maximizing the transmission of light between layers by using different real indexes of refraction. To this end, Shimizu teaches the use of multiple graded layers or a single continuous gradation, of the thin-film layer between two adjacent layers of the laminar stack to maximize the transmission of light between those respective layers.
Upon the application of an electric field between the transparent electrode layer and the rear electrode layer, light-emitting pixels are formed in the phosphor layer. Due to the physical structure of the phosphor layer, the pixels emit light mostly directed within the plane of the phosphor layer. As the emitted light travels in the phosphor layer, it is scattered by defects in the phosphor layer causing a substantial portion of the emitted light to be directed in the forward and rearward directions. Light that is directed or scattered rearwardly will be reflected forward off the rear electrodes adding to the forwardly directed light. This causes a fuzzy-looking region to appear around the addressed pixel. A circular polarizer cannot selectively reduce this effect without decreasing the overall amount of emitted light.
Emitted light striking the phosphor-dielectric boundaries at small angles to the boundaries is totally internally reflected. Light striking the phosphor-dielectric boundaries at a greater angle of incidence, refracts into the respective dielectric. The difference between the indexes of refraction of the front glass and exterior air are substantial, so the required angle of incidence for light to refract into the air is greater than all other internal interfaces. In other words, light that cannot escape the front glass-air boundary may freely refract between other layers of the TFEL laminar stack. The rearwardly directed light reflected off the glass-air boundary, and other rearwardly directed light, will impact the rear electrodes causing the light to reflect forward. Such light is either diffusely scattered or strikes a defect, thereby, will travel within the display until it possibly increases its angle with respect to the glass-air boundary permitting its escape from the display generally at a location distant from the pixel.
The apparent color of a TFEL display appears to depend upon the wavelengths of light emitted by the phosphor layer and the thicknesses of the individual thin-film layers. Amber displays typically vary in color from yellow at a perpendicular viewing angle to red/orange when viewing off the perpendicular viewing angle. Alternatively, the color of the perpendicular viewing angle may be red/orange and when viewing off the perpendicular viewing angle the color may be yellow. With current processing techniques for depositing the thin-film layers, it is hard to control the process sufficiently to produce consistent colors from screen to screen.
What is desired, therefore, is a way to enhance the contrast of the display, reduce the fuzzy looking region around the addressed pixel, reduce color variations between displays, and nearly eliminate the diffuse reflectance.
SUMMARY OF THE INVENTION
The present invention overcomes the foregoing drawbacks of the prior art by providing an electroluminescent display comprising a plurality of layers including at least a transparent electrode layer, a rear electrode layer, and at least three layers including an electroluminescent layer sandwiched between front and rear dielectric layers. All three layers are disposed between the rear electrode layer and the transparent electrode layer, so as to emit light upon the application of an electric field between the transparent electrode layer and the rear electrode layer. A thin-film absorption layer that absorbs a substantial percentage of light incident thereon is disposed between the rear electrode layer and the rear dielectric layer.
In a preferred embodiment of the invention the thin-film absorption layer has a first complex refractive index at a first side thereof that substantially match the rear dielectric thin-film layer's complex refractive index. The thin-film absorption layer also has a second complex refractive index at a second side thereof that substantially match the rear electrode layer's complex refractive index.
By locating the thin-film absorption layer in front of the rear electrode layer, ambient light and rearwardly-directed light originating from the electroluminescent element, is mostly absorbed prior to incidence with the rear electrode thereby increasing the contrast of the display. Further, by substantially matching the complex refractive indexes at both interfaces of the thin-film absorption layer with the rear electrode layer and the next adjacent layer, usually a dielectric layer, the reflections at the respective interfaces are minimized.
The absorption layer reduces the diffuse reflectance from about 15% to about 0.6% by absorbing the ambient light that would have been incident on the rear electrodes and thereby reflected forward. Further, the absorption layer reduces the color variation between displays by 80%.
Additionally, the absorption layer reduces the fuzzy looking region around the addressed pixel by absorbing rearwardly-directed light emitted from the phosphor layer and emitted light that is internally reflected rearwardly from thin-film layers.
The foregoing and other objectives, features, and advantages of the invention will be more readily understood upon consideration of the following detailed description of the invention, taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partial cutaway view of a TFEL device constructed according to the present invention and including a single-graded continuous thin-film absorption layer.
FIG. 2 is a partial cutaway view of a TFEL device constructed according to the present invention and including a multiple graded thin-film absorption layer.
FIG. 3 is a partial cutaway view of an alternative embodiment of a TFEL device constructed according to the present invention and including a multiple graded thin-film absorption layer.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, a TFEL device includes a transparent substrate 10 typically made of glass, supporting a laminar stack comprising the TFEL display elements. The laminar stack includes a set of transparent front electrodes 12 and a sandwich structure including an electroluminescent layer 16 sandwiched between front and rear dielectric layers 14 and 18, respectively. Rear electrodes 20, typically made of aluminum, are disposed behind the rear dielectric 18 and extend in a direction perpendicular to the transparent front electrodes 12 so that pixel points of light are created when electrodes in both sets are energized simultaneously. The TFEL components are sealed against the substrate 10 by an enclosure 22 which may be affixed to the substrate 10 by any suitable adhesive 24. An optically absorbent material may be injected into the cavity defined by the enclosure 22 to further absorb light. This may take the form of a silicone oil 24 which is conveniently used as a filler material or a solid filler of the type disclosed in U.S. Pat. No. 5,194,027. The silicone oil 24 may include a black-die to make it optically absorbent. The optical absorption is also enhanced by providing a black coating 26 on the rear inside cavity wall of the enclosure 22.
By providing a thin-film absorption layer 28 between the rear electrodes 20 and the rear dielectric 18 a substantial percentage of light incident thereon can be absorbed. The absorption layer 28 should substantially eliminate any reflection of light at the interface between the absorption layer 28 and the rear dielectric 18.
Each material has a complex refractive index, commonly referred to as n-ik, where n is the index of refraction relating to the speed of light in the medium and k is the extinction coefficient relating to the absorption of light in the medium. By substantially matching the index of refraction and the extinction coefficient of both the absorption layer 28 and rear dielectric 18 at the interface between them, a significant amount of light will not be reflected forward at the interface. The complex refractive indexes at the interface between the absorption layer 28 and rear electrodes 20 should also be substantially matched to minimize reflection. In other words, the complex refractive indexes of the absorption layer 28 should match the complex refractive indexes of the respective materials at both interfaces.
To match the complex refractive indexes at both the surfaces of the absorption layer 28, the index of refraction and the extinction coefficient should be varied in some manner from one interface to the other interface so as to minimize the reflection of light within the absorption layer 28. To minimize reflection, the absorption layer 28 can be designed as a transparent material at the rear dielectric interface which gradually changes to an opaque material that absorbs a substantial amount of light at the rear electrode interface. Preferably, the absorption layer is only disposed between the individual rear electrodes 20 and the rear dielectric layer 18. The construction of the absorption layer 28 can be made either as a continuous graded thin film or as a multiple graded thin film such as absorption layers 28', as shown in FIG. 2 (The primed reference numbers of FIG. 2 refer to the same respective structure as shown in FIG. 1 except for the construction of the absorption layer 28 and 28'.) It should be noted that the absorption layer 28 may be a metal, and if this is the case, it must be patterned as shown in FIG. 2 so as not to form short circuits between the rear electrodes. Thus, the layers 28' are patterned strips with gaps therebetween that extend coextensively with the electrodes.
It has been found that an absorption layer that follows three simple design constraints provides the desired absorption properties, while minimizing unwanted reflection. The three constraints are as follows and are subsequently discussed in order:
(1) any discrete step gradations in the indexes of refraction must be extremely thin relative to the wavelength of light used in the display;
(2) the optical constants change monotonically from one material to the other; and
(3) the average optical thickness of the absorption layer overall is at least large enough to be on the order of the wavelength of the display light.
First, the requirement that any steps or gradations be extremely thin relative to the wavelength of light refers to changes in the index of refraction and the extinction coefficient within the absorption layer, respectively, n and k. These are made small to avoid any significant interference. For an absorption layer 28' constructed of multiple graded layers, the changes between the index of refraction and the extinction coefficient (n-ik) of each adjacent layer are kept sufficiently small. To maintain sufficiently small changes in the complex refractive index, many thin-film layers must be employed. For a continuous absorption layer 28, the index of refraction and the extinction coefficient should change with a gradual gradient from the rear dielectric layer interface to the rear electrodes interface. By changing the complex refractive index gradually the refraction of light is reduced.
Second, the optical constants should monotonically change from one material to the other. The index of refraction and the extinction coefficient, n and k, should change in value, either respectively increasing or decreasing, without swinging back and forth within the absorption layer. If the value of either the index of refraction or the extinction coefficient, n or k, were to increase then decrease, or, alternatively, decrease then increase, within the absorption layer then reflections may result.
Third, the average optical thickness of the absorption layer must be at least large enough to be on the order of the wavelength of light. The optical thickness is the product of the index of refraction and the physical thickness of the absorption layer. The optical thickness should be at least 1/2 of the wavelength of light used in the display.
An absorption layer, as described, has many desirable properties when located in front of the rear electrodes 20. First, it may be optically modeled as an infinitely thick layer of transparent material because there is no substantial reflection of light within the graded layer or at the interfaces with the rear dielectric layer or rear electrodes, and it internally absorbs the incident light without substantial reflection. In other words, the absorption layer absorbs incident light directed to the rear of the display without substantial reflection of the incident light forward.
The contrast of a display is a measurement of the ambient light reflecting from a display compared to the light emitted by the display without the ambient light. By absorbing the ambient light in the absorption layer, it does not reflect forward off the rear electrodes, and the contrast of the display is increased. However, there is a brightness penalty associated with using such an absorption layer. A display with an absorption layer was found to have approximately 28% of the luminescence of an unfiltered standard reflective electrode display. This reduction is due to the loss of light initially emitted by the phosphor in other directions such as to the side and to the rear that would have been reflected forward to the viewer by standard rear electrodes. Nevertheless, even with the reduction in luminescence, a display with an absorption layer has superior contrast to the standard reflective electrode display and in some applications higher contrast is needed more than high luminescence.
Diffuse reflectance is primarily caused by light striking the rear electrodes which are typically made of shiny aluminum with a rough surface. Eliminating light from reaching the rear electrodes by the absorption layer eliminates the major component causing diffuse reflectance. A minor amount of diffuse reflectance will still occur because of the interfaces between the various laminar stack elements and the imperfections in the elements themselves. It was found that a display with an absorption layer reduces the diffuse reflectance from about 15% to about 0.6%, which greatly enhances the contrast of the display.
Also, the absorption layer is highly angle-independent in its absorption of light. Therefore, light that is scattered in a rearwardly direction that strikes the absorption layer at most angles of incidence is absorbed, thereby reducing the fuzzy looking region around the addressed pixel.
Further, light that is refracting between different thin-film layers that lacks the requisite incident angle to escape the air-dielectric boundary will also be absorbed by the absorption layer. The effect of the absorption of such refracting light is random light leaving the display.
Additionally, the absorption layer reduces the color variations between "identical" displays. It is thought that part of the color variations between different displays is caused by the interference from light being reflected forward by the rear electrodes 20. Color variations may be caused by a change in the viewing angle as well as by the small differences in the thickness of the thin-film layers between different displays. By eliminating the interference of light caused by reflections off the rear electrodes, the color variations between "identical" displays may be reduced by 80%.
A typical rear dielectric layer has an index of refraction and an extinction coefficient at a wavelength of 550 nm that are, n=1.75 and k˜0, relating to a transparent material. Aluminum rear electrodes have an index of refraction and an extinction coefficient that are, n=0.82 and k=6.0, relating to an opaque material. With these values the absorption layer is designed to change from n=1.75 to n=0.82 and from k˜0 to k=6.0, preferably within about 300-600 angstroms. The absorption layer can also be substantially thicker if desired. Other dielectric materials such as quartz (n=146, k˜0) and Ta 2 O 5 (n=2.3, k˜0) may be used. Rear electrodes can be constructed of other materials such as chrome (n=2.48, k=2.3) if desired.
Aluminum is a preferred metal for the rear electrodes because of its conductivity and self healing characteristics, and aluminum oxide is a fusing dielectric that has some self healing characteristics. In inverted structures molybdenum is the preferred metal. The ideal method for forming an anti-reflection absorption layer then, would be by grading an aluminum oxide to aluminum electrodes. The preferred method to perform a deposition of such a material is DC reactive sputtering. This allows the use of a single target such as aluminum that is deposited at high rates. The transition from oxide at the interface with the rear dielectric layer to metal at the interface with the rear electrodes is accomplished by controlling the amount of oxygen gas in the chamber. Starting at a level sufficient to assure a pure aluminum oxide film that closely matches the complex index of refraction at the dielectric, the user slowly reduces the oxidant pressure until a pure aluminum metal is deposited, thereby matching the dielectric qualities n and k at the rear electrodes. The same outcome may also be achieved by using an RF cathode to deposit aluminum oxide and mixing this material with sputter material from an aluminum target.
Alternatively, silicon nitride could be mixed in a graded fashion with molybdenum to form an absorption layer having a gradient that goes from pure Si 3 N 4 to pure molybdenum metal. If desired, any metal could be then added to the molybdenum to provide the necessary conductivity. Although several methods could be used for depositing such a material, the preferred method is a vacuum deposition. The oxide in metal could be co-deposited from separate sources, with a relatively slow change from high oxide/low metal rates to low oxide/high metal rates, and finally to pure metal. Other deposition techniques such as depositing metals and transparent materials such as oxides, fluorides and nitrides could also successfully be used.
Although many system configurations could work, the preferred geometry is a "carousel" type configuration such as those manufactured by Kurdex Corporation or Leybold, with the substrates on the side of a polygon which forms a rough cylinder. The cylinder is then spun with the substrates passing in front of one or more cathodes. The process is then slowly changed from a metal oxide process to a metal process as the carousel turns. Because of the conductivity of the absorption layer the absorption layer is preferably located only between each rear electrode and the rear dielectric by using a standard lift-off or etching process well known to one skilled in the art. Regardless of the deposition technique, however, gaps 29' must be left between the electrodes if the change in material takes the absorption layer to pure metal at the end adjacent the electrodes.
FIG. 3 shows an "inverted" structure electroluminescent device 40 that is similar to FIGS. 1 and 2. The device 40 is constructed with a substrate 44 that preferably has a black coating 46 on the lower side if the substrate 44 is transparent. On the substrate 44 are deposited rear electrodes 48. Between the rear electrodes 48 and the rear dielectric layer 50 is a thin-film absorption layer 42. The absorption layer is either constructed of multiple graded thin-film layers or as a continuous graded thin-film layer using any appropriate method previously described. An electroluminescent layer 52 is sandwiched between the rear dielectric layer 50 and a front dielectric layer 54. A transparent electrode layer 56 is formed on the front dielectric layer 54 and is enclosed by a transparent substrate 58 that is either bonded directly to the transparent electrode layer 56 or separated by a gap. The graded absorption layer 42 is designed, as previously described, such that it absorbs a substantial percentage of incident light thereon.
Several alternative design changes are within the scope of the invention. In the case of using a grading from an oxide mixture to a metal, the index of refraction and the extinction coefficient could switch back toward the oxide without detracting from the overall performance of the absorption layer if the switch occurs after enough thickness of material has been deposited so as to absorb a majority of the incident light. Further, a portion of the reflected light at the switch will further be absorbed by the absorption layer as it passes forward. It is possible to add additional thin-film layers to the laminar stack, including between the rear dielectric layer and the rear electrode layer.
A little bit of leeway exists on the metal side of the absorption layer since most of the light has been absorbed by the time it reaches that point. As a result one can reduce the reflection off the rear electrodes to less than 2 percent (from 90 percent without the absorption layer) with about 400 angstroms total thickness in the absorption layer.
The terms and expressions which have been employed in the foregoing specification are used therein as terms of description and not of limitation, and there is no intention, in the use of such terms and expressions, of excluding equivalents of the features shown and described or portions thereof, it being recognized that the scope of the invention is defined and limited only by the claims which follow.
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An electroluminescent display having a plurality of layers including at least a transparent electrode layer, a rear electrode layer, and at least three layers including an electroluminescent layer sandwiched between front and rear dielectric layers. All three layers thereof are disposed between the rear electrode layer and the transparent electrode layer wherein the transparent electrode layer is formed on a transparent substrate, so as to emit light upon the application of an electric field between the transparent electrode layer and the rear electrode layer. A thin-film absorption layer that absorbs a substantial percentage of light incident thereon is disposed between the rear electrode layer and the rear dielectric layer. The thin-film light absorption layer includes a first absorption portion having a complex refractive index that substantially matches the complex refractive index of the rear dielectric layer where they are adjacent and a second absorption portion having a complex refractive index that substantially matches the complex refractive index of the rear electrode layer where they are adjacent. In one embodiment the thin-film light absorption layer is a single layer having a complex refractive index which gradually changes. In an alternate embodiment the thin-film light absorption layer is composed of a plurality of discrete layers.
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DESCRIPTION OF PRIOR ART
Spread spectrum communication is characterized by modulation schemes which greatly expand the bandwidth occupied by a voice or data information signal. The two most frequently used schemes are direct sequence spreading and frequency hopping. In direct sequence frequency spreading, which is employed in this invention, a digitized information signal typically modulates a pseudo-random (also referred to as pseudo-noise or PN) digital signal. If the bit rate of the PN signal is, say 32 times as large as that of the information signal, the bandwidth of the resulting modulated signal becomes 32 times that of the original information.
The key to receiving spread spectrum signals is a receiver capable of generating a second PN signal identical to that used to spread the transmitted signal's bandwidth. This is possible because both transmitter and receiver use identical random digital sequence (PN) generator circuits. The PN signal is used by the receiver to synchronously demodulate the received signal. To do this successfully, the time-variations of the PN signal must be in synchronism with those in the received (modulated) signal. If they are not in time synchronism, the detected signal will be minuscule. Traditionally the time-phase of the PN signal generator at the receiver is varied slowly in time until signal output is found to be a maximum, and kept locked to the phase of the transmitter's PN generator by a phase-locked loop circuit.
An important capability of spread-spectrum communication, also used in this invention, is code-division multiple access. This involves carrying on a multiplicity of communications simultaneously, in the same bandwidth and geographic area, by using different time-varying PN codes which define each independent communication "channel".
Diversity reception is a well-known technique wherein several receiving antennas are used in connection with one or more receivers and some form of manual or automated antenna switching. The object of such schemes is to overcome fading in propagation paths between transmitter and receiver, by selecting the signal from that antenna (or combination) whose received signal is strongest at any given instant.
SUMMARY OF THE INVENTION
The wireless telephone system of this invention provides for a combination of a base station unit and multiple handsets to provide, in the embodiment described herein, sixty-two concurrent communication channels.
Two operating environments are envisioned: indoor (within buildings) and outdoor. The operating range in each case will be limited to about 500 meters by (U.S.) Federal Communication Commission limits on transmitter power. Typically the indoor operating range will be on the order of 200 meters or less depending on the environment in which the system operates. The reduction of operating range is a result of additional path loss, which can be experienced due to multi-path fading and/or intervening walls, partitions, or other structures between the handset and the base station.
One object of the invention is to achieve a wireless telephone system which is both reliable and economically producible. This is accomplished by the choice of communication techniques and waveform structure, and by the use of modern application specific integrated circuits (ASICs).
Another objective is to simplify manufacturing procedures and reduce costs through extensive use of digital signal processing techniques throughout the system. The use of digital circuits minimizes need for circuit adjustments, alignment or tuning often required by prior art wireless telephony equipment. In the preferred embodiments, a minimal part of the circuits are implemented using analog technology.
Still another object is to minimize, in a real-time sense, the effects of transmission impairments imposed by the operating environment. This is implemented through the combination of four specific techniques:
1) Mutual interference between the multiple user signals is minimized by use of pseudo-noise modulation signals which are orthogonal to one another, i.e. which can be independently demodulated.
2) Direct sequence spread spectrum modulation is used to provide protection against unintentional jamming by ambient narrow-band signals such as those from personal computer oscillators. It further protects against other interfering users sharing a common area, and provides users with a high degree of privacy.
3) Antenna polarization diversity reception is combined with a real-time means of selecting the antenna with the best signal-to-noise ratio (SNR).
4) Automatic power control is implemented so that all signals will be maintained at appropriate levels, thereby controlling mutual interference due to one communication signal overpowering others, where user handsets are located a widely varying distances from the base station.
Yet another object of this invention is to significantly increase the number of user channels in a given area in the allocated bandwidth. In the preferred embodiment, each 62-user group channel occupies approximately 1.33 MHz. This permits up to 19 base stations to operate within communication range of one another without interfering. The system embodiment described provides means to permit a handset user to move from the area served by one base station to that served by another, with automatic handoff from one to the other.
A further object of the invention is to provide means for interconnecting users for communication, and for connecting users to stations on remote telephone systems. In the embodiment described, this is done by connecting each base station to telephone switching equipment, providing each handset user with separate access to a local dial network, and through that to common carrier networks.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a single base station embodiment of the invention in schematic form,
FIG. 2 shows a single handset, along with its removable cradle, a representative means to ensure that batteries powering it are maintained at full charge,
FIG. 3 shows in block diagram form a configuration including a multiplicity of base stations, each supporting in this case 128 handsets of which 62 may be in use at any given instant,
FIG. 4A illustrates the assignment of (group) channels in a portion of the electromagnetic spectrum allocated for use by this type of communication service,
FIG. 4B illustrates the use of alternate channels in a given physical area to minimize interference between groups of handsets,
FIG. 5 shows a representative configuration for the handset, with a vertically polarized whip antenna mounted at top and a horizontally polarized loop antenna embedded in its base,
FIG. 6 Portrays one 10 millisecond frame of a preferred overall (order wire and voice channel) signal structure,
FIG. 7 shows the combination of sub-frames into a 640 millisecond signal,
FIG. 8 illustrates the detailed signal structure of an order wire channel,
FIG. 9 is a generic representation of information layout of order wire commands and the associated response,
FIG. 10 illustrates the location and utilization of control data embedded in voice transmissions, for system control during communication between a handset and base station,
FIG. 11 is a voice channel control command format and extraction from voice channel signals,
FIG. 12 is a general block diagram of the sub-frame synchronization incorporated in the invention,
FIG. 13 is a block diagram of signal power measurement for antenna selection and transmit power control,
FIG. 14 is a diagram of the frequency discriminator and AFC carrier tracking loop incorporated in the invention,
FIG. 15 illustrates a PN code phase discriminator and tracking loop at handset incorporated in the invention,
FIG. 16 illustrates a PN code phase discriminator and tracking loop at a base station,
FIG. 17 is an exemplary block phase estimation and differential data decoding circuits incorporated in the invention,
FIG. 18 is a diagrammatic illustration of differential data encoding incorporated in the invention, and
FIG. 19 is a block diagram of automatic gain control (AGC) in the handsets.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 illustrates the hardware configuration for one 62 user system hardware set, e.g., basic single base station system configuration. Each hardware set is comprised of one base station 10 and up to 62 handsets 11-1, 11-2 . . . 11-N with cradle. The system defines a star network configuration with the base station as the center of the star. The base station 10 contains one transceiver 12 for each individual user handset in the operating system. Polarization diversity is provided in the system by using dual cross polarized antennas 11A1 and 11A2 in each handset.
A single antenna 13 is used in the base station 10. Only one antenna is required because the communication channel is symmetrical with respect to direction, to and from the base station, so that dual cross-polarized antennas at the handset are sufficient to provide diversity in the system. Transceivers 12 are coupled by up/down converter and distribution amplifiers 14 to antenna 13 and served by a common reference oscillator 15 clock, logic 16 and telephone system (TELCO) interface 17.
The handset hardware configuration is shown in FIG. 2. The handset cradle 18 serves two purposes. It provides a place to physically store the handset 19 when not in use, and it provides a charging capability to replenish the charge on the handset batteries as required. Red and green alarm lights 20 are provided on the handset 19. These lights 20 serve to indicate the adequacy of the physical location of the cradle. If the received signal strength is adequate, a green light will illuminate. If the received signal strength is not adequate a red light will illuminate and the handset 19 can be moved a few inches. Since the handset contains polarization diversity, the need to relocate the cradle location will almost never occur.
The primary purpose of the system in this embodiment is to provide voice traffic capability to the potentially mobile user community. In order to provide this capability, a telephone system (TELCO) support and interface capability is provided. This TELCO support functions consists of 1) call establishment operations support, 2) user information data base support and update, 3) multicall programming operations capability, and 4) peripheral support functions.
The present invention provides a practical system for achieving in effect orthogonal CDMA operation thereby significantly increasing the number of user channels in a given area in a given bandwidth as compared to conventional CDMA operation. This is done by two means: 1) having the base station measure the time base error of each handset and transmitting the correction information to the handset, and 2) using "instantaneous" power control of the return or inbound (handset to base station) link based on the time-division duplex operation, measuring the power of the pilot or sounding signal, and performing the appropriate compensation of the handset transmit power, e.g., if the pilot signal is received 10 dB too low as compared to the desired reference level then the handset transmit power is increased by 10 dB with respect to nominal. If true orthogonality were achievable in practice power control would not be a crucial issue. However, truly orthogonal signals, i.e., those which cannot interfere with each other no matter what the power level difference, do not exist in the practical world with finite bandwidth, filtering effects, and minor time base errors. Thus, there is some cross-talk or interference between our "orthogonal" signals and it is important to control the power of each return signal precisely and quickly so that significant interference does not occur. Thus, the innovative power control system described herein is a crucial feature of the invention.
Another feature of the invention is that the handset locks its frequencies to the base station reference frequency by phase-locking to the powerful pilot or sounding signal. This permits the return link signal from the handset to have a very precise frequency without requiring the handset to have a costly, high stability oscillator. It is necessary to control the frequency of the handset signals reasonably closely if the signal orthogonality is to be maintained. The system described herein does this in a very cost-effective manner.
CALL ESTABLISHMENT OPERATIONS
This comprises interfacing with the TELCO, providing and interpreting all signaling operations required to establish both incoming and outgoing calls. This includes such things as dialing, a busy signal, and a phone ringing operation. All these functions are handled by the order wire (OW) channel and described in later herein.
BASE STATION CONFIGURATION
A typical multiple base station system configuration is illustrated in FIG. 3. A system of N base stations BS-#1 . . . BS#N each with 62 voice traffic channel capability is shown. Also shown is that each base station may be required to support up to 128 (not all in use at once) users (HS#1 . . . HS#128) part time. For these assumed conditions the TELCO (this TELCO unit is sometimes referred to as a Mobile Telecommunications Switching Office (MTSO) base station system must have the capability to recognize and properly route calls to 128n different phone numbers (different users).
MULTIPLE CELL OPERATION
So long as users are confined to operate through only one particular base station, operations are well defined and the equipment need concern itself only with maintaining signal timing and appropriate transmitter power level. If the system is defined to consist of many base stations over an extended geographical area, or covering multiple floors in a multi-floor building, the user must be able to roam, or execute a handover operation from one base station to another. Thus, in a multiple base station system it is assumed that any user can roam from the cell area serviced by his original base station to the cell area covered by any other compatible base station.
The importance of a cell pattern is threefold: 1) it defines a minimum range between two cells sharing the same frequency thereby defining co-channel interference effects, 2) it can define the exclusive neighbors of any given cell thereby reducing the search time for a new cell when attempting a roaming/handover operation, and 3) it defines whether a multifloor building can be serviced without suffering significant interference between like cells on adjacent floors.
A twelve pattern is very desirable for all these reasons. A hexagonal 12 cell pattern has six uniquely defined neighbors per cell and provides a 6 cell radii separation between like cells. For multifloor operation, this provides 3 cell radii separation plus the attenuation between floors. For indoor operation it is likely that a square pattern may be used since a square, or rectangular, pattern may lend itself better for use within a building.
As a user roams about his cell, he will at times reach the boundary of good coverage. As the handset realizes it is reaching the limits of its operating range, it will identify the cell area he is about to enter. The handset will constantly search for signals from other adjacent user groups which are members of the total system but outside his present cell. This will be done by searching for other OW signals than the OW of his own cell group. In order to minimize the search time and minimize the likelihood of losing the presently in use voice channel before he can establish a new one with the next base station, a handset maintains a data base defining relative timing between all adjacent base stations. The details of this operation are presented later.
Once the OW of the "next" cell is contacted, the handset must now require admission to the cell as a new user. If admitted, the handset is assigned an identification number as an authorized user of the group. At this time all pertinent data on the handset, i.e., handset serial number, identification number, and telephone number must be relayed to and stored in the base station database. The local TELCO data base must also be updated so that it knows where, i.e., to which base station, to direct calls intended for that particular telephone number. If a call is in progress, handover now involves the local TELCO intimately. The local TELCO must now not only have its data base updated, it must re-route a call in progress from one base station to another in real time.
The system is limited by FCC rule to operating with no more than 1 watt (30 dBm) transmitted power from either the handout or the base station. Based on this, the base station is clearly the limiting factor. However, according to the invention, a very viable system can be set up while satisfying the 1 watt total maximum power limitation. In general when servicing a densely populated user community high capacity base stations capable of servicing a large number of users can be employed and will operate over a relatively short range. Alternately, when servicing a sparsely populated user community, lower capacity base stations capable of servicing a smaller number of users can be utilized operating over a greater communication range.
AUTOMATIC GAIN CONTROL
USER TO BASE STATION
Each base station transmits a reference signal at a fixed level against which all estimates of received handset signal levels are compared. On the basis of these comparisons, the transmit power of each handset is adjusted as described later. The power control system can maintain the power received at the base station from each handset to within an accuracy of about 1 dB even in presence of severe multipath fading.
BASE STATION TO USER
The base station transmit power level is held fixed at the maximum power setting. As a handset is transported throughout the cell, its received signal level will vary over a maximum dynamic range of about 90 dB. In order to maintain the input voltage to the main signal path analog-to-digital converter in the user unit at nominally half of full scale, and thereby avoid clipping and loss-of-resolution problems, an AGC function is implemented prior to the analog-to-digital.
FREQUENCY PLAN
The system RF frequency plan for the disclosed embodiment is illustrated in FIG. 4. The FCC rule 15.247 band intended for this type of application extends from 902 MHz to 928 MHz, providing a 26 MHz total system bandwidth. Each subgroup signal is allocated a 1.33 MHz bandwidth. The frequency spacing between adjacent subgroup carrier frequencies is set to 0.663 MHz. This is possible since precise chip timing is maintained such that orthogonal operation is possible even with substantial spectral overlap. Thus, a total of 38 subgroups can be accommodated.
The system provides the feature that different PN sequences may be used in different cells. The use of different PN sequences in neighbor cells minimizes co-channel interference. Different PN sequences would be used in neighbor cells when a given cell configuration forces neighbor cells to be placed closer to each other than desired.
POLARIZATION DIVERSITY
Antenna polarization diversity at the user handset is selected, in the preferred embodiment, as the most effective method to reduce multipath fading. Implementation of polarization diversity at the handset requires two antennas at the handset and a single switch to select between them. Channel sounding is performed in order to select the best antenna, in each 10 ms time subframe.
Studies conducted indicate that polarization diversity provides an improvement in signal reception capability as good as or better than any other diversity technique. The use of polarization diversity does not impact system capacity as some techniques do and, the additional hardware complexity required to add polarization diversity is minimal. The system implements the use of dual cross polarized antennas at the handset. A typical handset antenna configuration is illustrated in FIG. 5. The antenna configurations shown in FIG. 5 makes use of a whip 11A1 and an Alford loop 11A2. Separation of whip 11A1 and loop 11A2 may compromise polarization diversity performance but will then provide spatial diversity. In the preferred embodiment, the loop should be approximately 3 inches square to have the same sensitivity as whip antenna 11A1.
The base station antenna pattern should be appropriate to the area to be served. If the Base Station is located in the center of the service area its pattern should be omnidirectional in the horizontal plane. In most cases, the user will be distributed over a narrow vertical span and the Base Station antenna can have a narrow vertical pattern. Such patterns are ordinarily obtained by the use of vertical linear arrays. A convenient element for such an array is the Lindenblad radiator invented in 1936 for use at 120 MHz. It is an assembly of four dipoles spaced around a center support post; tilted at 45 degrees, and fed in phase.
This antenna provides a circular polarized wave. An array of these elements can easily be assembled to narrow the vertical pattern, with a practical limit imposed by the space available for mounting. This assembly has been used commercially. The advantage of the Lindenblad design is that it is simple and very tolerant of implementation variations.
In the event the user distribution is wide in the vertical direction--as for several floors in a tall building, a less directive antenna would be desired. Then a single element or short array would be preferred.
MULTIPLE BASE STATIONS: SYNCHRONIZATION
When two handsets operating in two mutually adjacent cells (served by different base stations) find themselves near each other and at the cell boundary, an adjacent channel interference (ACI) ratio of I/S=80 dB or more can result. If the two cell systems are not synchronized, and if one handset is transmitting while the other is receiving, operations at both handsets will be disrupted. This can be avoided by making adjacent base stations mutually synchronous to an accuracy of ±8 μs. This is so because there is a 16.6 μs minimum gap time between successive receive/transmit time intervals in each subframe.
The preferred timing approach in this disclosed embodiment is to provide input from a precision timing source to a central site (one of the base stations (FIG. 3) is designated to be Master base station). This timing signal can then be distributed to a constellation of base stations along with the other TELCO interface lines. This approach applies to both indoor and outdoor base station systems. In an indoor system there would be one Master base station or central site. In an outdoor system there could be many depending on the extent of the system and its configuration.
Synchronization for a limited system, for example, a system intended to service one building, is not a problem. One base station can be designated as the Master station and it would distribute timing to all other base stations. The timing signal can be distributed along with the TELCO interface wiring. Alternatively, the GPS, local telephone company central office time source, etc. can be used.
SIGNAL STRUCTURE, DATA CONTENT, PROTOCOLS, AND SIGNAL PROCESSING
In this embodiment of the invention, the signal structure for the system is predicated on two underlying objectives:
(1) to operate synchronously with 20-msec frames of a 16 Kbps voice encoder/decoder, and
(2) to keep added signal path delays to under 10 msec.
Accordingly, the preferred signal structure is a sequence of 10-msec subframes, as shown in FIG. 6, each consisting of four distinct periods, two for inbound and two for outbound signalling, and each being one of 64 subframes composing a 640-msec frame as shown in FIG. 7. The inbound signals are spread with a different PN code than the outbound signals but with the same code length and chipping rate.
The voice channel data consists of 16 Kbps bidirectional digital voice, plus a 400 bps bidirectional control link. The data modulation is differentially encoded QPSK, transmitted at a burst rate of 20.72 Kps. The data signal is bi-phase modulated with a spreading code at 32 times the burst symbol rate (663 KHz). The spreading code is the modulo-2 sum of a length-255 PN sequence and a length-32 Rademacher-Walsh (R-W) function. The all-ones R-W function is used as an order-wire channel within each 32-channel subgroup; the remaining 31 functions are each associated with a different voice channel in that subgroup.
From the perspective of a handset already associated with a particular base station, the four time periods within each subframe may be viewed as follows:
Throughout this discussion, the term "symbol" is used to mean "voice channel symbol duration", i.e., 32 chip times, even when the activity is on the order wire channel. The term "voice channel" means one frequency channel and non-unity Rademacher-Walsh code combination.
(1) (SOUND) The base station transmits a 121/4 symbol all-ones sounding pattern (i.e., no data transitions) on each order wire channel, at a level 15 dB higher than for individual BS→HS voice channels; each handset receives the first six symbols on one antenna A1, switches to the other antenna A2 during the next 1/8 symbol, receives the next six symbols on A2, compares the power between A1 and A2, chooses the antenna with the higher power, and switches to that antenna during the next 1/8 symbol.
The power level from the chosen antenna is used by the handset to determine transmit power during the following HS SYNC and HS→BS portions of the signal, and also as a code sync error measure to be input to its delay-lock code tracking loop.
(2) (BS→HS) On each active voice channel, the base station transmits a voice data burst of 91 QPSK symbols, followed by a guard time of 11 chips. The handset receives this data on the antenna selected during the sounding period. The voice channel data is constructed as follows:
1 phase reference symbol
2 channel control symbols
80 encoded voice data symbols
8 spare symbols (reserved for future use)
(3) (HS SYNC) On an automatic cyclic time division multiple access (TDMA) basis, one member handset in each 64 member subcommunity (i.e., one per order wire channel) transmits a continuous all-ones ranging signal (i.e., no data transitions but PN chip transitions) to the base station on its associated order wire channel for a duration of 121/8 symbols, followed by a 1/8-symbol guard time. The base station order wire channel performs a delay lock loop error measurement on this signal, and prepares and queues a timing correction command, if required, to be sent to that handset at the next opportunity. Each transmitting handset transmits using the antenna it selected during the sounding period, at a power level determined from the power received by that antenna during that period.
(4) (HS→BS) On each active voice channel, the handset transmits a voice data burst of 91 symbols, followed by a guard time of 11 chips, on the antenna selected
during the sounding period. This inbound burst is of the same format as the BS→HS burst of period (2).
Thus the time-division duplex signal is symmetrical, with respect to format and content, its inbound and outbound portions being essentially identical to each other, of the total time available, 77.2% is used for voice data, 10.6% for related overhead and spare capacity, 5.8% for channel sounding, 5.8% for handset timing synchronization, and 0.6% for various switching and guard times.
Advantages of selected signal structure include:
1) One dedicated bidirectional order wire channel (for link control) for each 31 voice channels.
2) No voice channel activity during sounding burst (at 15 dB higher than individual voice channels, allows very accurate measurements of received power, time offset, and frequency offset.
3) Dedicated handset sync per channel allows accurate measurement of handset power and time offset with no interference due to timing errors in other channels.
4) Bidirectional 400 bps control link incorporated into each voice channel (for handset power and timing control, as well as link control).
ORDER WIRE CHANNEL SIGNAL STRUCTURE
The order wire channel signal structure is shown in FIG. 8. Four periods of the overall time-division duplex structure are superimposed on an order wire signal structure consisting of (in each direction) two OW symbol periods followed by ten actual OW symbols plus a 7 voice channel symbol frame sync/parity check signal and a 31-chip guard time. Each half subframe is exactly 13 OW symbol periods in duration.
The order wire signal structure has been designed so as to maximize signal search effectiveness, i.e., to minimize expected search times. Each OW symbol period=255 PN chips=one PN code sequence length, thus by taking energy measurements over one OW symbol period, we are integrating over one PN code sequence length and taking full advantage of the PN code's autocorrelation properties.
Also, the choice of an exact integer number of PN sequence lengths per half subframe both 1) greatly simplifies the PN coder design and the search algorithm, and 2) is critical to avoiding code phase ambiguities which would increase typical and worst-case initial search times by more than ten fold.
During the two sounding periods, the switching times allotted at the end of each, and the reference phase period (i.e. for a total of (192+4)*2+118=510 chips=2 OW symbol periods), the base station is transmitting a continuous (spread) tone corresponding to an all-ones data modulation (i.e. no data transitions). The next 10 OW symbols contain order wire data, as described below.
The outbound order wire channel frame sync field contains 7 voice channel symbols (14 bits) organized as 6 bits parity check on the 20 OW bits, 6 bits subframe number within frame (0-63), and 2 bits parity check on the subframe number. Thus 12/13=92.3% of the base station order wire channel transmit time (i.e., 46.1% of the total time) is available to handsets for signal acquisition purposes.
The inbound order wire signal format consists of two segments. During the first, on a cyclic basis, one handset out of each community of 64 transmits a continuous (spread) tone corresponding to an all-ones data modulation (i.e. no data transitions), for a duration of 388 chips, for the purpose of allowing the base station to measure that handset's transmit code synchronization, power, and quality during a period wherein there is guaranteed to be no interference from other handsets on the same channel.
Four chips guard time later, if the current order wire time slot is assigned, the handset assigned to this slot transmits first a 118-chip phase reference symbol, then 10 OW symbols, and finally a 7-voice-channel-symbol (14-bit) field containing a parity check of the 20 order wire bits; the last 31 chips of the inbound order wire signal segment are merely guard time.
If the current order wire time slot is not assigned, it may be accessed by roaming handsets seeking membership in a new base station community, or by handsets which have just been switched from STANDBY to ACTIVE mode and are seeking a voice channel assignment. The signal structure for such accesses is identical to that for assigned accesses.
ORDER WIRE CHANNEL DATA STRUCTURE AND PROTOCOL
Each outbound order wire burst contains a 10-symbol (20-bit) order wire command, formatted as shown in FIG. 9. The 5-bit function field specifies which of the various command or broadcast functions is being invoked. For most command functions, a 7-bit landset ID field is also included to specify to which of up to 128 handsets in the local base station community the command is directed. The remaining 8 bits (or in some cases, all remaining 15 bits) are defined as required by the specific command or broadcast function.
The response to any outbound (i.e., to a handset) command or inbound request which requires a response will be provided in the third half subframe following that command or request. Failure to receive a valid response at that time shall be considered an error and shall cause recovery measures to be taken. Thus, each third half sub-frame following a base station command requiring a response is defined as being assigned, and is not available for use by handsets attempting to initiate communication.
A handset's response to a base station command requiring one is to echo the received command's function and handset ID fields, and follow with whatever additional meaningful information is required for that command. Thus a handset response generally constitutes a specific acknowledgement of the received command, plus an implied request for the next step in the dialog leading to the end objective. Similarly, a base station's response to a handset request both acknowledges the request and provides the next step in the dialog toward the desired objective.
The example diagrammed in FIG. 10 and described below serves to illustrate this:
(1) A base station detects that an incoming call from the TELCO interface is directed to a handset with the corresponding telephone number. It then schedules a Ring Alert command to be sent to the handset, addressed to it via its 7-bit Handset ID.
(2) On recognizing its ID, the handset responds by echoing tile Ring Alert Command and enabling a local "ring" function.
(3) When the user picks up the handset and switches it from STANDBY to ACTIVE mode, the handset disables the local ring function and attempts to reestablish the dialog by issuing an Allocate Channel request in the next available CSMA slot.
(4) Assuming for the moment that the CSMA Allocate Channel request is received properly at the base station (recovery from collisions and other errors is discussed in sections later herein), the base station echoes the Allocate Channel request to the requesting handset,
(5) which then resubmits it in the now implicitly assigned (i.e., "guaranteed" collision-free TDMA slot 15 msec later.
(6) Having thus confirmed the Allocate Channel request, the base station then allocates a voice channel and issues a channel Assignment command to the handset,
(7) which echoes the Channel Assignment command in acknowledgement.
(8) Having thus confirmed that the handset has correctly received the channel assignment information, the base station connects the corresponding TELCO line to the allocated voice channel and issues a Make Link command to the handset,
(9) which then begins transceiving on the assigned voice channel.
For calls originating at the handset, essentially the same procedure would be followed, except for steps (1) and (2), which of course would be eliminated.
At the end of any call, the user would switch the handset from ACTIVE back to STANDBY mode, and the handset would signal a Deallocate Channel request to the base station via its in-band order wire (or channel control) path (see Section 3.6). This request would be acknowledge by the base station, via the same path, prior to releasing the channel on either end.
ORDER WIRE CHANNEL DATA STRUCTURE
Approximately 15 specific order wire channel commands are necessary or very useful. Some are "broadcast" by the base station on the order wire channel to indicate network status. Others are involved in initiating communication with a handset, terminating communication, and adjusting timing. These include:
1) Ring Alert command.
2) Allocate Channel request.
3) channel Assignment command.
4) Make Link command.
5) Deallocate Channel request.
6) Base Station Memberships Available broadcast. The 8-bit data field of the broadcast contains the number of memberships currently available in this base station community. This broadcast will occur at least once every 200 msec on each order wire channel.
7) Membership Enrollment request. Submitted on a CSMA basis by roaming handsets seeking membership in a new community.
8) Enrollment Interview commands. Eight different commands, actually: three to get the 24-bit handset serial number, three to get the 24-bit handset telephone number, one to identify the previous membership cell, if any, and one to assign a 7-bit ID number to the handset, thereby completing its acceptance into the new cell community.
9) Adjacent Cell Map broadcast. The 12 lease significant bits of this broadcast indicate, for each of 12 possible frequency cells, whether that cell is (1) adjacent to the current cell or (0) not adjacent to the current cell.
10) Adjacent Cell Time Offset report. Three different reports, actually: one to indicate PN code phase offset, one to indicate symbol offset within a subframe, and one to indicate subframe offset within a frame. The 8-bit data field of these reports indicates the particular offset, relative to the current cell, of the adjacent cell base station identified in the Handset ID field. These reports are submitted, initially on a CSMA basis, by any scouting or roaming handset, and are then confirmed on an assigned TDMA basis.
11) Adjacent cell Time Offset broadcast. Three different broadcasts, actually: one to indicate PN code phase offset, one to indicate symbol offset within a subframe, and one to indicate subframe offset within a frame. The 8-bit data field of these broadcasts indicates the particular offset, relative to the current cell, of the adjacent cell base station identified in the Handset ID field.
12) Voice channels Available broadcast. The 8-bit data field of this broadcast contains the number of currently unassigned voice channels within this base station. This broadcast will occur nominally once each second.
13) CSMA Statistics broadcast. The 15 least significant bits of this broadcast contain CSMA slot capacity, loading, and collision statistics for the previous 1-second period.
14) Adjust Transmit Code Phase command. The 8-bit data field of this command is a two's complement number indicating the handset transmit code phase adjustment, in sixteenths of a chip to be advanced; thus a value of -3 would indicate to retard the transmit phase of the handset identified in the Handset ID field by 3/16 of a chip. Data values outside the range of -4 to +4 are ignored.
15) Adjust Transmit Power Level command. The 8-bit data field of this command is a two's complement number indicating the handset transmit power adjustment, in units of db gain; this value is essentially added to the transmit power control bias term (see Section 4.3) of the handset identified in the handset ID field. Data values outside the range of -4 to +4 are ignored.
CARRIER SENSE MULTIPLE ACCESS (CSMA) ISSUES
Handsets seeking entry to a cell (i.e., a base station) are unknown entities to the base station, thus the invention provides for the handset to access the base station. Also, in order to accommodate other asynchronous events (e.g., handset transition from STANDBY to ACTIVE mode and requesting allocation of a voice channel) and avoid the delays inherent in a purely cyclical or polling approach, again, some other means is desirable.
A carrier sense multiple access (CSMA) approach seems well suited to supporting these relatively infrequent demands, but it brings with it the requirement to manage the CSMA resources intelligently. Several design features have been incorporated in this regard.
First, the fraction of slots available for CSMA use will be arranged to provide a suitable probability of no collision on the first access attempt.
Second, the base station will maintain statistics of the use of available CSMA slots and will broadcast these statistics to the handsets for use in making intelligent choices of initial access and backoff strategies.
Third, the powerful parity check code included in inbound order wire transmissions minimizes the possibility that when collisions do occur they would not be recognized as such, thus the likelihood of the base station erroneously interpreting the demodulated results of collided transmissions is extremely low.
Any CSMA access attempt which is not acknowledge within 35 msec will be considered to have failed, the appropriate backoff strategy will be selected, and a retry will be scheduled accordingly.
VOICE CHANNEL CONTROL DATA STRUCTURE AND PROTOCOL
Each voice channel burst contains a 2-symbol field allocated for channel control, i.e., inband order wire functions such as handset transmit power control, handset transmit code phase control, and other functions to be identified. This provides a capacity of:
200 symbols/sec=128 symbols/frame
400 bits/sec=256 bits/frame
in each direction, inbound and outbound, for these purposes, so that handsets with calls in progress still have access to full order wire functionality as described earlier.
Outbound channel control data is organized into 16-bit commands and acknowledgements formatted as shown in FIG. 11 and frame synchronized to provide 16 such commands per frame (25 per second) per voice channel.
Each command is composed of a 6-bit function field and a 10-bit data field. Unlike the order wire channel, no handset ID field is required since the handset being addressed is implicit in he voice channel assignment.
Inbound channel control data is organized into 16-bit requests and acknowledgements formatted identically to outbound commands and synchronized with them but offset by half a subframe. Inbound responses to outbound commands commence three half-subframes after the command transmission is complete, and outbound responses to inbound requests commence in the burst following completion of the request.
DETAILED SIGNAL PROCESSING OPERATIONS
The following describes the signal processing operations and sequences utilized by the system to acquire and track the signal, maximize its quality, demodulate data from it, determine when to transfer to an adjacent cell, and accomplish such transfers.
INITIAL SIGNAL ACQUISITION (HANDSETS ONLY)
When a handset is first powered on, it is assumed to have a priori knowledge of its "home" base station PN code and frequency channel, but to have no knowledge of its time offset from that base station, and to know to within only 9 KHz its frequency offset from nominal for that channel. (The frequency offset from nominal at the base station is assumed to be less than 100 hertz.)
The initial search resolves these time and frequency uncertainties by seeking to acquire the base station order wire signal at each of 255*2=510 PN code phase uncertainty states and 19 frequency bins spaced 1 KHz apart. Each of the resulting 19*510=9690 composite uncertainty states is examined for 398.44 μsec (=one 255-chip PN sequence length), and since there are 3 correlators per receiver, a total of 9690*398.44 μsec/3=1.29 sec would be required to complete the search if the signal were constantly present.
Since the base station order wire signal is present only half the time, however, (the inbound signal being spread with a different PN code), each uncertainty state must be searched at least twice, once at time t and again t+(2n+1)*5 msec, so the total time required to acquire PN chip sync (to within 0.25 chip or so) and resolve frequency offset (to within 500 Hz or so) is at least twice this, or 2.6 seconds.
If the peak power measure of all the uncertainty states is not at least TBD db greater than the average of all the non-peak states, then it is assumed that the first attempt failed due to an antenna null, and the search process is repeated on the other antenna, for a worst case total of 5.2 seconds.
Note again that subsequent acquisitions will in general be essentially instantaneous, because the initial acquisition and carrier pull-in will have removed all frequency uncertainty, and Adjacent cell Time Offset broadcasts will have eliminated most code phase and other time uncertainties.
Note too that acquiring PN code phase sync automatically also achieves OW symbol sync, but an additional several frames will be required to achieve frame sync and carrier pull-in prior to being able to demodulate data. These processes are described in the sections following:
SUBFRAME SYNCHRONIZATION (HANDSETS ONLY)
Subframe synchronization is achieved as follows (see FIG. 12):
1) Return the coder and the carrier frequency to the code phase and frequency corresponding to the initial acquisition energy peak (with the order wire signal still selected).
2) Observe 3 subframes of (I,Q) measures from the correlator, each integrated over one OW symbol; in particular, observe the power profile of the data (modulo 26 OW symbol times per subframe), determine the peak power measure, and verify that it is at least 9 db above the average of the others. This corresponds to the onset of the outbound sounding burst at the start of each subframe.
This observation is accomplished by constructing a 26-element histogram, clearing all elements to zero, then adding to each the power measure of the corresponding (I,Q) sample (that is, sample number i mod 26, for i=0 to 77), where the measure of power is defined as I 2+Q A2.
3) The histogram index j such that
h(j)>h(i), all i/=j
and
h(j)>Pavg+9 db
where:
Pavg=(Ptot-h(j)-h(j+1 mod 26))/24
and
Ptot=Sum(h(i),i=0, 77)
represents the delay, in OW-symbol increments, of the actual frame start relative to the postulated frame start (i=0). If no such index j exists, then repeat steps (2) and (3) using the other antenna.
4) Set OW symbol count=(26j) mod 26. (OW symbol count will be incremented by 1 (modulo 26) on each subsequent OW symbol). This completes the frame sync process, so it may be disabled and the carrier and code tracking functions enabled.
ANTENNA SELECTION AND TRANSMIT POWER CONTROL (HANDSETS ONLY)
During each of the two sounding bursts at the start of each subframe (one burst received on each antenna), a power measurement is made and projected to the midpoint of the inbound signalling period. The antenna corresponding to the larger projected power measure is selected to be used during the remainder of the subframe (both outbound and inbound portions). The larger projected power measure itself, plus a bias correction term determined by the base station over a longer time frame, is used to set the power level for the inbound transmission (if any). Reference is made to the elements shown in FIG. 13.
The power is measured for each sounding burst as follows: (I, Q) samples are input from the correlator and integrated in integrators coherently over 6 voice symbols; total power is then computed from these burst-coherent (Ij, Qj) measures as
______________________________________P1 = I1 2 + Q1 2 ; antenna 1P2 = I2 2 + Q2 2 ; antenna 2______________________________________
and projected to the midpoint of the inbound signalling period:
______________________________________PWR1 = P1 + 0.75 * (P1 - P1') ; proj = current +0.75*PWR2 = P2 + 0.75 * (P2 - P2') ; (current - previous)P1' = P1; P2' = P2 ; set previous = current______________________________________
Antenna Selection is then simply
If PWR1>PWR2
then select antenna 1 (k=2)
else select antenna 2 (k=2)
The antenna selected algorithm is the same independent of whether a call is in progress on the handset.
The transmit power Pxmit for this subframe is then computed as
Pxmit=Kp+Pref-log (PWRk)-Atten+Bias
where
Kp=nominal transmit power for log (PWRk)=Pref-Atten+Bias
Pref=reference receive power level.
Attn=attenuator setting set by AGC (see Section 4.9)
This bias correction term for each handset is determined at the base station once each 64 frames as follows:
Bias=Bias+K1d*log (Prcv/Pref)
where
______________________________________Prcv = Pp from base station code phase tracking function (seeSection 4.5.2).= Ip 2 + Qp 2, Ip and Qp integrated coherently over a12-1/8 symbol handset sync periodPref = reference receive power level______________________________________
and K1d is chosen to provide a loop bandwidth of 0.10 Hz. The transmit power control algorithm is the same independent of whether a call is in progress on the handset.
CARRIER PULL-IN AND TRACKING (HANDSETS ONLY)
Carrier pull-in and tracking are achieved using the AFC function described in the following, which is enabled on the first OW symbol count of 0 following subframe sync. FIG. 14 exemplifies the frequency discriminator and AFC carrier tracking loop subsystem used in the invention.
Base on the power measurements taken during the sounding bursts, if PWR1>PWR2, then let k=1 (else k=2) and compute the discriminator Dafc as
Dafc=adjust (phi2-phi1)
where
phi1=a tan (Qk1, Ik1)
phi2=a tan (Qk2, Ik2)
adjust (×)=if abs(×)<pi then×else×-2*pi*sign (x×).
and the subscripts 1 and 2 denote samples taken during the first and second halves of each sounding burst, respectively.
Next, input Dafc to a first-order AFC loop
df=df+K1a*Dafc±3450/pi
and output df+nominal, scaled appropriately, to the carrier NCO. The loop is iterated at the subframe rate, i.e. 100 Hz and K1a is chosen to provide a loop bandwidth of 6 Hz. The discriminator operates only on outbound order wire sounding bursts and has a range of ±3450 Hz.
Carrier pull-in will be essentially complete within three loop time constants, or about 0.15 sec, so at that time the data demodulation function is enabled.
The carrier tracking function is the same, independent of whether a call is in progress on the handset.
CODE PHASE TRACKING
Code phase tracking is performed both at the handsets and at the base stations, but it is done differently in either place. This following describes the code phase tracking algorithms both for handsets and for base stations.
Code phase tracking is accomplished at the handsets using the delay lock loop function described following, which is enabled on the first OW symbol count of 0 following subframe sync.
Base on the power measurements taken during the sounding bursts, if PWR1>PWR2 then let k=1 (else k=2), and compute the discriminator Dco as
Dco=(Pe-P1)/Pp
where
Pe=(Iek1+Iek2) 2+(Qek1+Qek2) 2
P1=(Ilk1+Ilk2) 2+(Qlk1+Qlk2) 2
Pp=(Ipk1+Ipk2) 2+(Qpk1+Qpk2) 2
and the subscripts e, l, and p denote measures taken with the reference code displaced 1/2 chip early and 1/2 chip late relative to nominal, and at nominal, respectively, and the subscripts 1 and 2 denote samples taken during the first and second halves of each sounding burst, respectively.
Dco is then input to a first order delay lock loop
dp=K1b*Dco/4
and the loop output dp is used to adjust the code phase in units of 1/16 of a chip. The loop is iterated at the subframe rate, i.e. at 100 Hz, and K1b is chosen to provide a loop bandwidth of 6 Hz.
Note that the code phase tracking function is the same at each handset, independent of whether a call is in progress on that handset.
CODE PHASE TRACKING AT BASE STATIONS
In order to maximize the synchronicity of the inbound signals at each base station, the code phase at arrival is measured for each handset in each community at the base station associated with that community. This process, illustrated in FIG. 16, is implement as follows:
Each handset has an associated 7-bit ID number which it receives from the base station at the time it joins that base station community. Handsets with ID numbers from 0 to 63 are implicitly associated with order wire subgroup 0 of that base station; those with ID numbers from 64 to 127 are implicitly associated with order wire subgroup 1. Each order wire channel must thus support up to 64 handsets.
During the Handset Sync portion of each inbound half subframe, the handset whose ID number modulo 64 equals the number of the current subframe within the frame transmits a 121/8 symbol all-ones sync burst. The base station receives this burst and computes the discriminator Dco2 as
Dco2=(Pe-Pl)/Pp
where
Pe=Ie 2+Qe 2
Pl=Il 2+Ql 2
pp=Ip 2+Qp 2
and the subscripts e, l, and p denote measures taken with the reference code displaced 1/2 chip early and 1/2 chip late relative to nominal, and at nominal, respectively, and each of the I and Q inputs have been coherently integrated over the full 121/8 symbol (388-chip) measurement period.
Dco2 is then input to a first order delay lock loop
dp=K1c*Dco2/4
and the loop output dp is used to adjust the handset transmit code phase in units of 1/16 of a chip. This function is iterated at the subframe rate, i.e. at 100 Hz, so for each handset, it's at the frame rate (640 msec, or 1.56 Hz), and K1c is chosen to provide a loop bandwidth of 0.02 Hz.
The loops are actually closed via communication with each handset, using the order wire channel for handsets with no call in progress or using the voice channel control field for handsets with calls in progress. Other than this difference, the code phase tracking function at the base station is the same for each handset, independent of whether a call is in progress on the handset.
DATA DEMODULATION
Once its AFC loop has settled, a handset may begin to demodulate order wire data and engage in order wire dialogs with the base station in order to subscribe to and participate in the cell community as described earlier. Once it has subscribed to a particular community or cell, it may then receive and originate calls, initially via the order wire channel but predominantly via a voice channel, which of course requires voice channel data demodulation as well.
The algorithm used to demodulate this data is a combination of block phase estimation, which adjusts the phase of the received symbols for optimum detection in the presence of phase and frequency offsets, and differential data decoding of the received symbols. This algorithm is applied straightforwardly to the voice channel and with minor modifications to the order wire channel. For the voice channel, the algorithm operates as shown in FIG. 4.6.1 and described as follows:
For each of the 91 symbols (Ij, Qj) following the sounding bursts (in the handset) or the handset sync burst (in the base station), compute the equivalent symbols (14j, Q4j) (with the date removed) as
(I2, Q2)=(Ij, Qj) 2
(14j, Q4j)=(I2, Q2) 2.
Then initialize the block integrators and phase estimate as
______________________________________SumI4 = Sum (14j, j=0,15) ;block lengthSumQ4 = Sum (Q4j, j=0,15) ;= 16 symbolsPhi4 = atan (SumQ4, SumI4)Phi = -Phi4/4 + pi/4PhiO = Phi______________________________________
and rotate the first 8 symbols (Ij,Qj), j=0,7, by Phi:
(Ij,Qj)=(Ij, Qj)*(cos (Phi), sin (Phi)).
For the next 75 symbols (Ij, Qj), j=8,82, update the block integrators and phase estimate and rotate the symbol accordingly:
______________________________________SumI4 = SumI4+14(j+8)-14(j-8)SumQ4 = SumQ4+Q4(j+8)-Q4(j-8)Phi4 = atan (SumQ4,SumI4)Phi = -Phi4/4+pi/4+Ntrack*pi/2(Ij,Qj) = (Ij,Qj)* (cos(Phi), sin(Phi))PhiO = Phi______________________________________
where Ntrack=0, 1, 2 or 3 such that ABS (Phi-PhiO) is a minimum, i.e., so as to produce minimum rotation relative to the previous rotation.
Next, rotate the final 8 symbols (Ij,Qj),j=83,90, by the final value of Phi:
(Ij,Qj)=(Ij,Qj)*(cos (Phi), sin (Phi)).
Finally, quantize the rotated symbols to 00, 01, 10, or 11 according to the sign of Ij and Qj
(Ij,Qj)=(sign(Ij),sign(Qj)), j=0,90,
and input the result to the differential decoder as shown in FIG. 17. Symbols 1 through 90 of the decoder output are the demodulated data for this burst. (Date to be transmitted are first differentially encoded as shown in FIG. 18.
For the order wire channel, the algorithm is essentially the same except that the block length is 2 OW symbols rather than 16 voice channel symbols, and the phase reference symbol is shorter than the other OW symbols. Also, the frame sync portion of each order wire burst is handled differently, namely as 7 voice channel symbols. Thus the algorithm becomes:
For each of the 11 symbols (Ij,Qj) following the sounding bursts (in the handset) or the handset sync burst (in the base station), compute the equivalent symbols (I4j,Q4j) with the data removed, as
(I2,Q2)=(Ij,Qj) 2
(14j,Q4j)=(12,Q2) 2.
Then initialize the block integrators and phase estimate as
______________________________________SumI4 = Sum (14j,j=0,1) ;block length =SumQ4 = Sum (Q4j,j=0,1) ; 2 OW symbolsPhi4 = atan (SumQ4,SumI4)Phi = -Phi4/4 + pi/4Phi0 = Phi______________________________________
and rotate the first symbol (I0,Q0) by Phi:
(I0,Q0)=(I0,Q0)*(cos (Phi), sin (Phi)).
For the next 10 symbols (Ij,Qj), j-1,10, update the block integrators and phase estimate and rotate the symbol accordingly:
______________________________________SumI4 = SumI4+I4(j+1)-I4(j-1)SumQ4 = SumQ4+Q4(j+1)-Q4(j-1)Phi4 = atan (SumQ4,SumI4)Phi = -Phi4/4+pi/4 +Ntrack *pi/2(Ij,Qj) = (Ij,Qj)* (cos(Phi), sin(Phi))Phi0 = Phi______________________________________
where
Ntrack=0, 1, 2, or 3 such that ABS (Phi-Phi0) is a minimum, i.e. so as to produce minimum rotation relative to the previous rotation.
Next, rotate the 7 frame sync symbols (Ij,Qj),j=11,17, by the final value of Phi:
(Ij,Qj)=(Ij,Qj)*(cos (Phi), sin (Phi)).
Finally, quantize the rotated symbols to 00, 01, 10, or 11 according to the sign of Ij and Qj
(Ij,Qj)=(sign(Ij),sign(Qj)),j=0,17,
and input the result to the differential decoder. Symbols 1 through 10 of the decoder output are the demodulated OW data for this burst. Symbols 11 through 17 of the decoder output are the demodulated frame sync data for this burst. (OW data to be transmitted are also first differentially encoded.)
SCOUTING, ROAMING, AND CELL TRANSFER
The system implements certain features to support rapid cell transfer. One of these is the maintenance and broadcast of a database of the relative time offsets of adjacent cell base stations. The information in the database is supplied by handsets which acquire adjacent cell order wire signals on a scouting or roaming basis.
Again, scouting activity is essentially roaming activity, but with the intent of gathering data about the surrounding environment, rather than of actually transferring cell membership. Scouting handsets relay time offset information regarding adjacent cells back to the base station of their currently assigned cell; roaming handsets which transfer to an adjacent cell impart this information regarding previous cell timing to the base station of the new cell.
The information so gathered is verified and broadcast by each base station via the order wire channel and via the channel control portion of each active voice channel.
Scouting and roaming searches differ from initial searches primarily in that they are more focussed, that is, they search at only a single frequency, namely the handset's current carrier tracking frequency within the current cell, and, at least initially, they search only a few chips of PN code phase uncertainty (proportional to data staleness). The other main difference is that carrier frequency, PN code phase, and power level tracking operations are maintained on the original signal during scouting and roaming searches.
SCOUTING
For scouting, if the more focussed search fails on both antennas, it is then broadened to include all 255 PN chips code phase uncertainty. If even this broader search fails on both antennas, the current scouting effort is terminated and normal operation within the current cell is resumed, without a scouting report (Adjacent cell Time Offset report) being submitted to the base station.
If any of the searches succeed, however, subframe and frame synchronization are also performed and a scouting report is submitted.
ROAMING AND CELL TRANSFER
Received power is measured once each subframe. A filtered average of this measure is also maintained so as to provide a 2-second time constant. Whenever this filtered average falls below a threshold defined by the signal level at which transfer to another cell becomes desirable, a roaming search is initiated, which searches first for the adjacent cell order wire signal most recently acquired.
If this focussed search fails on both antennas, a similar search is conducted on both antennas for the next most likely adjacent signal to be acquired, and so on, until all adjacent signals have been searched. For each adjacent signal acquired, if the measured power level on that signal is greater than on the current signal, then the handset listens for a Base Station Memberships Available broadcast.
If memberships are available (and, if a call is in progress on the handset, if voice channels are also available), then the handset issues a Membership Enrollment request. On verification of the enrollment request, the base station conducts an enrollment interview with the handset, and the transfer of the handset membership, to the adjacent cell base station is completed, along with any call in progress on the handset.
SIGNAL PRESENCE MONITORING AT BASE STATIONS
In order to detect those situations in which a handset signal can reasonably be assumed to be lost, especially if it is currently assigned a voice channel and voice channels are currently in high demand, a filtered average of the received power from each of the handset sync periods is maintained as:
Fp(j)=(I-K1f)*Fp(j)+K1f*Prcv(j)
where
Prcv(j)=Ip 2+Qp 2, Ip and Qp integrated coherently over 121/8 symbols,
and where K1f is chosen to provide a time constant of 2 seconds. Whenever the Fp value for any handset j falls below a specified lower threshold, the handset is noted as being off-line; whenever its Fp value returns above an upper threshold, it is noted as being on-line.
Any call in progress on a handset determined to be off-line is terminated. Incoming calls whose destination handset is off-line are given a busy signal.
AUTOMATIC GAIN CONTROL (AGC) IN HANDSETS
In order to minimize the dynamic range requirements (and thus the power and cost) of the signal-path A-to-D converter used in handsets, some form of automatic gain control (AGC) of the A-to-D input signal is required. FIG. 19 depicts the AGC approach selected for this system. The concept is as follows:
During each sounding burst, the analog input signal is correlated with the reference PN waveform and coherently integrated over 6 symbols, then dumped to square-law devices SLD whose outputs are summed and log-amplified, then converted to digital. This digital log-domain power measure is read by software at the end of each sounding burst. At the end of the second burst, the larger of the two power measures (Pmax) is selected by software to set the signal-path attenuation for the remainder of the current subframe and the sounding period of the following subframe. The attenuation is determined as:
Atten=Atten+Kpow*(Pmax-Plimit+6 dB)
where Kpow is a function of the log amplifier gain and attenuator gain. The attenuator setting is also used in the determination of the handset transmit power setting for the current subframe.
For signal acquisition, the attenuator is set (separately for each antenna and for each new code phase and carrier frequency uncertainty range scan) so that the rms noise level P0 is 18 db below the maximum A-to-D converter input level, thus:
Attn=Attn+Kpow*(P0-Plim+18 db).
An embedded microcontroller or microprocessor can be used to control not only the operational sequences involved in command handling, but there are decided advantages to incorporating not only the sequence control functions but much of the signal processing as well into a programmable device such as a digital signal processor. These advantages include:
reduced hardware design time, due to:
having fewer parts to incorporate no ASIC design time or fab lead time greatly reduced FPGA complexity and design time;
increased flexibility to modify or fine-tune algorithms once the system is already built and in test.
While a preferred embodiment of the invention has been shown and described, it will be appreciated that various modifications and adaptations of the invention will be obvious to those skilled in the art and still be within the spirit and scope of the invention as set forth in the claims appended hereto.
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The present invention is based on novel implementation techniques which makes orthogonal CDMA practical in a short range mobile telephone environment where significant multipath fading exists. Specifically, this invention provides novel techniques for establishing the time base, frequency, and power control necessary to achieve orthogonality. Use of a high power sounding burst on the outbound link permits: 1) antenna diversity selection to minimize the probability of a faded condition, 2) local frequency locking at the subscriber terminal which avoids the requirement for a costly precision frequency standard, and 3) essentially instantaneous inbound power control based on the outbound receive signal level. This is effective since time division duplexing is used and both transmission and reception take place on the same frequency. With the short frame structure and unique placement of the sounding burst the correlation between the outbound and inbound path losses is very high. Thus, according to the invention, the signal structure and control algorithms result in a greatly reduced signal level range at the base station/PBX to achieve high efficiency in a orthogonal CDMA system. Real world effects such as filtering, multipath time spread, and time base error destroy orthogonality and introduce a degree of cross coupling between supposedly orthogonal channels. Thus, the invention provides accurately controlled power levels in this highly dynamic environment.
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This application is a national stage completion of PCT/EP2006/010981 filed Nov. 16, 2006, which claims priority from German Application Serial No. 10 2005 059 356.9 filed Dec. 13, 2005.
FIELD OF THE INVENTION
The invention concerns a hydraulic system in motor vehicles with at least one hydraulically actuated clutch, which is activated by an oil pressure supplied by an oil pump.
BACKGROUND OF THE INVENTION
From DE 43 42 233 A1 an oil pump drive device is known, which is combined with a transmission coupled to a drive machine in order to deliver working oil to the transmission for lubrication and to enable shift processes in the transmission. In this, the transmission comprises a first force transfer path to connect the output shaft of an electric motor to the drive input shaft of the oil pump, and a second force transfer path to connect the output shaft of the drive machine to the drive input shaft of the oil pump. A control device selects the first force transfer path to drive the oil pump by way of the electric motor when the speed of the drive machine's output shaft is below a predetermined speed, and selects the second force transfer path when the speed of the drive machine exceeds the predetermined speed.
Further, from DE 101 43 929 A1, an electro-hydraulic transmission control device for generating and emitting hydraulic pressure input signals to the clutches, brakes and shift mechanisms of an automatic transmission is known, such that a module body accommodates and carries the components of the transmission control device and generates flow messages. Several control valves are fixed on the module body and control hydraulic fluid in the lines. In addition, several magnetic control valves are arranged on the module body. A regulator is also connected to the electromagnets of the magnetic control valves and controls them by actuating the electromagnets as a function of input signals supplied by sensors for detecting various parameters of the operating status of the vehicle. A mechanically or electrically driven oil pump, integrated in the transmission control device, delivers the pressurized oil to the control valves.
Furthermore, DE 101 62 973 A1 proposes an automatic transmission with a main oil pump driven by a combustion engine, an auxiliary oil pump driven by an electric motor and with a drive control device for the auxiliary oil pump driven by the electric motor, such that the operating voltage supplied to the latter is adapted on the basis of the measured oil temperature corresponding to the operating status of the automatic transmission in each case. In essence, the intention is to maintain the hydraulic pressure required and, in addition, to prevent a hydraulic pressure greater than required from being delivered. Regardless of this, here too a hydraulic control device is provided which, for its part, entails greater expenditure.
To keep the expenditure for an electric auxiliary oil pump low, in EP 1 223 365 A2, it is proposed in certain operating situations to maintain the necessary clutch pressure, a mechanical and an electric motor driven oil pump are operated together and then, when the measured clutch pressure reaches a value that the mechanical main oil pump can deliver on its own, the electric auxiliary oil pump is immediately switched off. Accordingly, the auxiliary oil pump is controlled in such a way that a necessary and measured system pressure and clutch pressure is maintained in the transmission.
From U.S. Pat. No. 6,390,947 B1, a hydraulic circuit is known for controlling the oil pressure delivered to an automatic transmission of a vehicle with a mechanical oil pump driven by the drive engine and with an automatic engine start/stop system. In the hydraulic circuit a bypass line is arranged with an electrically driven oil pump. The mechanically and electrically driven oil pumps are connected in parallel. This measure is designed to adapt the oil pressure in the system to the current operating conditions.
Finally from U.S. Pat. No. 4,531,485 B, a switching logic system is known for a mechanically driven oil pump and an electrically driven auxiliary oil pump associated with a combustion engine.
In summary and supplementarily, it can be said that hydraulically actuated clutches are controlled by clutch valves, electric pressure regulators, timed magnetic valves, actuators and/or other components. The pressure is supplied predominantly by a mechanical oil pump driven by the drive mechanism of the main drive (internal combustion engine) of a vehicle. Further, electric oil pumps are also known, which supplement the mechanical oil pump in drive technological terms (auxiliary oil pumps).
Conventionally, downstream from such electric oil pumps is connected a hydraulic control unit that consists of at least one hydraulically actuated valve (clutch valve) and an electric actuator, such as an electronic pressure control valve or a hydraulic actuator. In addition, such hydraulic control units often comprise a system-pressure control system as well, which limits the hydraulic power output of the oil pump (in most cases an oversupply to ensure that the maximum demand is covered) in that too much oil is delivered into the intake line of the oil pump or to the oil sump.
For example, if individually controlled clutches are arranged in structural groups of a vehicle, for example in a transfer gearbox which can also be combined with manual shift transmissions and can then not make use of a pressure supply from an automatic transmission, the cost and complexity entailed by the oil pumps, system controls, clutch valves and electric actuators for the pressure actuation of the clutches are considerable. The fewer clutches there are in such a structural group, the greater are the costs for this complexity, in relation to the clutch to be actuated.
It should also be pointed out that although in the prior art the cooling of known wet-operating clutches is often designed to be controllable as a function of need, this entails additional control cost and complexity and also influences the size of the oil pumps. To that extent, the efficiency of the oil pumps is reduced because the delivery volume demand for the wet clutch is too large.
Against this background, the purpose of the present invention is to provide a hydraulic system in motor vehicles with at least one hydraulically actuated clutch and an oil pump which, as a further improvement of known generic devices, entails minimized control cost and complexity in terms of components and software for supplying the clutch with hydraulic oil and, if necessary, cooling oil and which also requires less structural space for the controls concerned.
SUMMARY OF THE INVENTION
The objective set is achieved by a hydraulic system in a motor vehicle, having at least one hydraulically actuated clutch, for the actuation of which an oil pressure is supplied by an oil pump and in which oil pressure control of the clutch takes place directly and exclusively by way of an oil pump which can be driven electrically and controlled by electronic means. In this way, at least most of the additional control valves used in the prior art can advantageously be omitted.
According to a first embodiment of the invention, to regulate the oil pressure, the electrically driven and electronically controlled oil pump is associated with an oil pressure sensor that provides measurement values to an electronic pump control unit which, for its part, generates control signals for controlling the electric motor of the oil pump as a function of clutch pressure and/or clutch torque specifications.
According to a second embodiment of the invention to regulate the oil pressure, the electrically driven and electronically controlled oil pump can be associated with at least one pump current sensor, i.e., a sensor for determining the electric current for the oil pump, or a pump torque sensor or a pump speed sensor. The measurement values obtained are made available to the pump control unit which, for its part, generates control signals for controlling the electric motor of the oil pump as a function of predetermined clutch pressure and/or clutch torque specifications.
For the determination of the control signals, the measured current temperature and/or viscosity of the hydraulic oil can also be taken into consideration.
Moreover, the pump control unit can either be made as a separate control unit or implemented in other control devices of the drive train of the motor vehicle known in themselves, such as a transmission control system, an engine control system or the like.
If the clutch in question is a wet-operating clutch, the oil pump can also be used to supply cooling oil to it and, in that case, to ensure long-term operation of the oil pump and a dynamic response thereof to varying pressure specifications, a bypass with a bypass valve or bypass throttle is provided in the hydraulic oil or the cooling oil circuit. The bypass formed can be made in such manner that the “internal leakage” of the oil pump is fed back to its intake side and/or to the clutch, at least as a basic supply for cooling.
When the clutch concerned is the wet-operating clutch, to cover the eventuality of a somewhat elevated cooling oil volume flow in it a mechanically driven second oil pump can be associated therewith. The mechanically driven second oil pump can be in active connection with the wet-operating clutch in such manner that with the aid of suitable drive means, the oil pump can be actuated by a speed difference between the primary side and the secondary side of the clutch.
On the other hand, it can also be that the mechanically driven oil pump is actively connected with the wet-operating clutch, via an upstream drive output gear, in such a manner that in every case a minimum pump speed that delivers the oil is maintained.
Likewise, the mechanically driven second oil pump can be driven by any component rotating at an appropriate speed in the driving direction, while the pump is supported on a non-rotating component. The component rotation speed can be derived from any rotating component of the motor vehicle's drive train and the non-rotating component can be a housing element such as a transmission housing or the like.
The above-mentioned particular design embodiments of the mechanical drive of the second oil pump provide a cooling oil supply according to need without complex control measures. In addition, the provisions also improve efficiency substantially since the drag torques of the clutch and the reactive power of the pump are reduced.
As the invention also provides, to enable the cooling to be switched on at least one hydraulically actuated switching valve or an electrically operated actuator such as a magnetic valve or the like is associated with the suction side or the pressure side of the mechanically driven second oil pump. The at least one hydraulically actuated switching valve can be actuated, as necessary, by virtue of the control pressure of the electrically driven and electronically controlled oil pump specified by the electronic pump control unit.
With regard to the at least one electrically operated actuator, this can be activated or de-activated, as necessary, by the electronic pump control unit or any other suitable control unit.
Further, it is proposed that both when the clutch is actively actuated and also when the wet-operating clutch has to be operated in a partially disengaged condition with a speed difference when, having regard to the desired low drag torques already mentioned above, it is desirable to have only slight cooling. The cooling is switched on by opening the at least one hydraulically actuated switching valve or electrically activated actuator and is otherwise interrupted.
Furthermore, it is regarded as expedient for a buffer reservoir, designed to temporarily hold any surplus cooling oil that results from elevated delivery amounts during short speed surges of the mechanically driven second oil pump, to be associated with the wet-operated clutch. The stored oil surplus can then be used for after-cooling once the speed surge and accordingly the volume flow maximum have ended.
Finally, it can be provided that the cooling oil supply to the wet-operated clutch can take place radially from the inside outward or in the reverse direction.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described, by way of example, with reference to the accompanying drawings in which:
FIG. 1 is a schematic illustration of the principle of the pressure control system of a hydraulically actuated clutch;
FIG. 2 is a schematic illustration of a principle relating to the arrangement of a mechanically driven oil pump for cooling a hydraulically operated, wet clutch, considering the sample of a transfer gearbox, according to a first embodiment, and
FIG. 3 is a schematic illustration of a principle as in FIG. 2 , but relating to another design embodiment.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is a schematic illustration showing a hydraulically actuated clutch 1 , in this case a lamellar or disk clutch of a transmission known in itself (not shown in greater detail), for example a transfer gearbox of a motor vehicle.
As already explained earlier, the pressure control of the clutch 1 is, in this case, effected directly and exclusively by way of an electrically driven and electronically controlled oil pump 2 . The necessary hydraulic oil is drawn from a tank or oil sump 3 and delivered to the clutch 1 as a clutch actuation pressure p_kpl, via a suction filter 4 , by the electrically driven oil pump 2 through a pressure line 5 .
The oil pump 2 is associated with an electronic pump control unit 6 which, as a function of clutch pressure specifications and/or clutch torque specifications provided and after evaluating measurement values supplied continuously by an oil pressure sensor (not shown in more detail), generates control signals for controlling an electric motor 2 a of the oil pump 2 or to regulate a control current 7 thereof. Accordingly, the oil pump 2 and the pump control unit 6 are expediently connected to an on-board electrical network 8 of the motor vehicle.
Alternatively to the oil pressure sensor, a pump flow detection sensor, a pump torque sensor or a pump speed sensor can also be used, whose measurement values are sent to the pump control unit 6 for evaluation (not illustrated further). If, as an alternative to the pressure sensor, the pump pressure currently applied is not measured but calculated, then the calculation algorithm can be refined by determining the temperature of the hydraulic oil and taking its viscosity into consideration.
In the present case, the pump control unit 6 is made as a separate control unit. It is certainly also possible and accordingly covered by the scope of the present invention, to implement it in other control devices of the motor vehicle's drive train, known in themselves (not illustrated in more detail here), such as a transmission control device, an engine control device or the like, or to arrange it as an on-the-spot electronic unit directly in the area of the pump or even to integrate it in a hydraulic control system supplied with pressure by the pump.
If the clutch 1 is a wet-operating clutch 1 , the oil pump 2 can be associated with a bypass in the hydraulic circuit comprising a bypass valve or a bypass throttle (not shown). This meets the requirement for long-term operation of the oil pump 2 without providing an essential working pressure for clutch actuation, whereby a dynamic response of the oil pump 2 to varying pressure conditions is achieved when the oil pump 2 is already operating and does not first have to be started as necessary from rest. The “internal leakage” of the oil pump 2 then produced can expediently be injected back into the suction side thereof in order to maintain or increase the efficiency of the oil pump 2 .
In the case of a wet-operating clutch 1 , the “internal leakage” can in addition be used as a basic supply for cooling the clutch 1 . Furthermore, this “leakage” can be designed to be sufficient for cooling the clutch 1 , this being particularly appropriate for clutches 1 , which are not so highly loaded so that there is no need for a costly clutch cooling system with the corresponding structural complexity.
In contrast, if the clutch is a highly loaded wet-operating clutch 1 , such as a wet-operating clutch 1 of a transfer gearbox 9 , then to cover a rather higher cooling volume flow thereof, a mechanically driven, second oil pump 10 is provided.
FIG. 2 schematically shows a drive train of a motor vehicle that comprises the distributor gearbox 9 , with a drive engine 11 , a transmission 12 , a rear axle 13 and a front axle 14 , on which in each case there are differential transmissions. The differential transmissions of the two vehicle axles 13 and 14 are driven by drive shafts (not shown in more detail) which are drivingly connected with the output shaft of the transmission 12 by way of the transfer gearbox 9 . The differential transmission of the front axle 14 can be actively connected with the transfer gearbox 9 by the wet-operating clutch 1 and can, in that way, be driven by a drive torque, as necessary.
In the present case, the second oil pump 10 can be mechanically actively connected with the clutch 1 in such a manner that the oil pump 10 is speed-controlled as a function of the clutch speed differences n_secondary−n_primary or n_primary−n_secondary between the primary side and the secondary side of the clutch 1 , whereby a slip-controlled oil delivery by the oil pump 10 can also be used to provide a supply of cooling oil to the clutch 1 in a simple way and as necessary. In the example illustrated in FIG. 2 , the housing of the oil pump 10 is connected to the secondary side and the delivery means of the oil pump 10 to the primary side of the wet-operating clutch 1 , to the latter of which the drive shaft leading to the front axle 14 , is also connected so that the oil pump 10 draws oil from a tank or oil sump and can also supply components other than the clutch 1 with cooling oil, as needed.
If there is no speed difference between the primary and secondary sides of the clutch 1 , then as is known, only a small amount of cooling oil is sufficient for the after-cooling or constant cooling thereof and can be dealt with by the above-mentioned “internal leakage” of the electrically driven and electronically controlled oil pump 2 .
Only when there is a speed difference between the primary and secondary sides of the clutch 1 is there a steep rise in the demand for cooling oil as clutch torque increases, which is then provided for by the forced coupling of delivery power from the mechanically driven, second oil pump 10 .
For those with knowledge of the subject, it is easy to deduce from an understanding of the invention that the mechanically driven, second oil pump 10 can also be connected with the wet-operating clutch 1 by additional drive gearing upstream from the latter (not shown), in such a manner that in any case, i.e., even if there is no or only a very small speed difference between the primary and secondary sides of the clutch 1 , a pump speed is maintained which produces a certain minimum oil delivery to cover the basic cooling oil demand.
Likewise, the mechanically driven oil pump 10 can also be driven by any rotating component in the drive train and can itself be supported on a non-rotating component 15 , such as a transmission housing.
According to the example embodiment shown in FIG. 3 , the mechanically driven oil pump 10 with its delivery means is in active connection with the secondary portion of the clutch 1 and, with its pump housing, is supported on the housing of the transfer gearbox 9 , which can also be made as an automatic transmission known as such.
Particularly in the case of conventional automatic transmissions, it has been found expedient to design the oil circuit for cooling the clutch 1 so that it can be blocked so that the flow of cooling oil is switched on only when the clutch is actively actuated or when the clutch 1 has to be operated in an at least partially disengaged condition with a speed difference, but is otherwise interrupted.
Accordingly, to switch on or interrupt the flow of cooling oil at least one hydraulically actuated switching valve or an electrically operated actuator, such as a magnetic valve (not shown), is associated with the suction side or the pressure side of the mechanically driven oil pump 10 . The at least one hydraulically actuated switching valve can advantageously be actuated, as necessary, by the control pressure for the electrically driven oil pump 2 determined by the electronic pump control unit 6 ( FIG. 1 ).
On the other hand, if an electrically operated actuator is used, this can be activated or de-activated, as necessary, directly by the electronic pump control unit 6 or any other suitable control unit incorporated in the drive train of the motor vehicle.
Furthermore, it has been found expedient for the wet-operated clutch 1 to comprise a buffer reservoir for temporarily holding surplus cooling oil, i.e., cooling oil produced as a result of increased delivery power of the mechanically driven, second oil pump 10 caused by any speed surges. Such speed surges or even speed difference peaks under load can give rise to a certain brief delivery power boost of the oil pump 10 and thus to a higher cooling oil volume flow which, however, cannot pass through the clutch 1 in a short time. When any such speed surge and consequent volume flow maximum have abated, the stored oil surplus can be used for after-cooling the clutch.
Such a buffer reservoir can be made as an oil reservoir which is arranged directly on or in the clutch and is filled or charged if peaks in volume flow occur.
As can also been seen from FIGS. 1 to 3 in the present case, the cooling oil supply to the wet-operating clutch 1 takes place radially from the inside, i.e., from the center of rotation radially outward. Of course, the invention is not limited to this design form rather the cooling oil supply can also take place radially from the outside inward.
REFERENCE NUMERALS
1 clutch
2 oil pump (electrically driven)
2 a electric motor (of oil pump 2 )
3 oil sump
4 suction filter
5 pressure duct
6 pump control unit
7 control current
8 on-board electrical system
9 transfer gearbox
10 oil pump (mechanically driven)
11 drive engine
12 transmission
13 rear axle
14 front axle
15 non-rotating component, housing
p_kpl clutch actuation
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A hydraulic system in motor vehicles with at least one hydraulically actuated clutch, which entails minimized control complexity for supplying the clutch with hydraulic oil and which takes up less structural space. These characteristics are achieved essentially in that the pressure control of the hydraulically actuated clutch is effected directly and exclusively by an electrically driven and electronically controlled oil pump.
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BACKGROUND OF THE INVENTION
1. Field of The Invention
The present invention relates to a dispersion compensation technique for an optical fiber as a transmission path in an optical communication system.
2. Related Background Art
In an optical communication system, an optical fiber is used as a transmission path. A signal light output from an optical transmitter is propagated in the optical fiber to conduct the optical communication. In the past, a laser diode, which emits a laser beam having a center wavelength of 1.3 μm, was used as the optical transmitter and an optical fiber for a 1.3 μm band was installed as the transmission path to conduct the digital transmission (optical communication). Thereafter, it has been found that the wavelength of 1.55 μm exhibits a minimum transmission loss in the glass used as the material of the optical fiber, and it is known to propagate a laser beam having a center wavelength of 1.55 μm through the existing optical fiber in order to attain the communication over a longer distance. However, the laser diode has a specific spectrum width (Δω) in its oscillation wavelength. The propagation speeds in the optical fiber are different between a short wavelength component and a long wavelength component contained in the signal light (dispersion characteristic of the optical fiber). Thus, when the laser beam having the center wavelength of 1.55 μm is propagated through the optical fiber optimized for the 1.3 μm band, the optical signal is distorted so that the transmission distance, the transmission band, and the bit rate are limited.
In order to compensate for the dispersion characteristic of the optical fiber, dispersion compensation techniques disclosed in Japanese Laid-Open Patent Application 62-65529 and Conf. on Optical Fiber Comm. 1992. PD-14, PD-15 have been proposed. An optical fiber having a dispersion characteristic opposite to that of the optical fiber used as the transmission path is inserted to compensate the dispersion characteristic.
On the other hand, the inventors of the present invention have proved that the longer the optical fiber, the more the dispersion compensating fiber and a carrier to noise ratio (CNR) is deteriorated, which impedes good optical communication.
SUMMARY OF THE INVENTION
In the present invention, it is intended to construct an optical CATV network as an optical communication system. More specifically, when an optical signal having a center wavelength of 1.55 μm is to be used while using a fiber optical amplifier (doped with erbium Er 3+ ), an optical fiber for the 1.3 μm (single-mode fiber) may have to be used, or an optical signal having the center wavelength of 1.3 μm may be propagated through the single mode fiber at a 1.55 μm wavelength.
It is an object of the present invention to construct an optical communication system which compensates a dispersion of an optical fiber and overcomes the problem in the above-mentioned environment.
In accordance with a first aspect of the present invention, a dispersion compensating fiber which sufficiently compensates the dispersion of the optical fiber used as the transmission path is divided into at least two fibers, and the first and second divided dispersion compensating fibers are connected in series to the opposite ends of the optical fiber.
The dispersion compensating fiber has an opposite dispersion characteristic to a dispersion characteristic of the optical fiber and the length thereof is limited to a range in which a relative intensity noise (RIN) of the dispersion compensating fiber can retain a proportional relationship to the length. Accordingly, the dispersion compensating fiber is divided into a plurality of dispersion compensating fibers within that length, or the above-mentioned first and second dispersion compensating fibers are further divided.
Because each of the dispersion compensating fibers includes a large amount of element (for example, germanium which may be doped with Er 3+ ) added to a core, it has a large RIN due to multi-reflection by Rayleigh scattered light, and it increases at a larger rate than a rate to be proportional to the length.
Accordingly, by connecting the dispersion compensating fibers, which meet the proportional condition in series to the optical fiber at a plurality of points on the transmission path, the RIN may be suppressed low in compensating the dispersion of the optical fiber.
In accordance with a second aspect of the present invention, a plurality of divided dispersion compensating fibers are connected in series to an optical transmitter side end of the optical fiber used as the transmission path.
In accordance with a third aspect of the present invention, a plurality of divided dispersion compensating fibers are connected in series to an optical receiver side end of the optical fiber used as the transmission path.
In the first to third aspects, it should be noted that the divided dispersion compensating fibers are optically spaced from each other to assure that rear scattered light generated therein is sufficiently attenuated, because the rear scattered light is one cause of the transmission loss.
In a first aspect to optically space the dispersion compensating fibers, an optical fiber having a length to sufficiently attenuate the rear scattered light is used as a connecting member to serially connect the dispersion compensating fibers.
In a second aspect, an optical isolator is used as the connecting member to serially connect the dispersion compensating fibers.
In a third aspect, an optical coupler having a loss to sufficiently attenuate the rear scattered light is used as the connecting member to serially connect the dispersion compensating fibers.
Where the optical fiber is used as the connecting member, the optical fiber may be used as the transmission path. In the first to third aspects, it is assumed that the already installed optical fiber cable is used. If the optical fiber which is the connecting member is used as the transmission path, the configuration having the dispersion compensating fibers connected in series between one transmission path and another transmission path is provided.
When a fiber optical amplifier doped with Er 3+ is used as the optical fiber which is the connecting member, the increase of a transmission loss can be prevented.
When the lengths of the dispersion compensating fibers are equal to each other, normalization in system design such as providing a dispersion compensating fiber at as predetermined pitch for a given optical fiber is attained. As a result, a design efficiency is improved and a labor productivity is improved.
The present invention 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 to be considered as limiting the present invention.
Further 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. Various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art form this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a first configuration of an optical communication system of the present invention;
FIG. 2 shows a refractive index distribution of a dispersion compensating fiber;
FIG. 3 shows a configuration of an optical communication system which is a first comparative example;
FIG. 4 shows a configuration of an optical communication system which is a second comparative example;
FIG. 5 shows a relation between a length of the dispersion compensating fiber and a RIN;
FIGS. 6 to 8 show applications of the optical communication system shown in FIG. 1;
FIGS. 9 to 12 show applications of a second configuration of the optical communication system of the present invention; and
FIGS. 13 to 16 show applications of a third configuration of the optical communication system of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiments of the optical communication system of the present invention are explained below with reference to FIGS. 1 to 16.
FIG. 1 shows a simplest one of a first configuration of the optical communication system of the present invention.
In the present communication system, simple one-to-one communication is performed. A first optical fiber 100a is used as a transmission path from an optical transmitter 300 to an optical receiver 400. The optical receiver 400 receives an optical signal from the optical transmitter 300 which converts an electrical signal S in to the optical signal, and outputs an electrical signal S out . Two dispersion compensating fibers of the same length are used to compensate the dispersion of the first optical fiber 100a, and the first and second dispersion compensating fibers 200a and 200b are connected in series at the opposite ends of the first optical fiber 100a.
The total length of the first and second dispersion compensating fibers 200a and 200b is long enough to compensate the dispersion of the first optical fiber 100a and the length of each of the first and second dispersion compensating fibers 200a and 200b is respectively limited to a range in which the RIN of the dispersion compensating fiber can retain a proportional relationship to the length.
A specific configuration in which the optical communication system shown in FIG. 1 (first configuration) is configured as a system for 40-channel amplitude modulated vestigial sideband (AM-VSB) transmission is explained.
An optical transmitter 300 converts an input electrical signal S in to an optical signal and it uses a distributed feed-back laser diode (DBF-LD) having an oscillation wavelength of 1.552 μm and an optical output of +7 dBm. A distortion characteristic or composite second-order distortion (CSO) thereof is -62.3 dB and a modulation index per channel is 4%. The input signal S in is 40 channels of AM-VSB and frequency division multiplexing (FDM) video signals. The range of carrier frequencies thereof is from 91.25 MHz to 337.25 MHz.
A single mode fiber of a 10 km length for a 1.3 μm band is used as the optical fiber 100 which is a transmission path. A dispersion value of the first optical fiber 100a is approximately 17 ps/nm/km at a wavelength of 1.552 μm and a transmission loss is 0.2 dB/km. The first and second dispersion compensating fibers 200a and 200b have a germanium doped silica core of 1.7 μm in diameter and a fluorine doped silica cladding. A refractive index distribution thereof is shown in FIG. 2. A refractive index difference A of the first dispersion compensating fiber 200a is 2.8%, a transmission loss at a wavelength of 1.552 μm is 0.87 dB/km, a mode field diameter (MFD) is 3.7 μm, and a dispersion value is -95 ps/nm/km. These parameters of the second dispersion compensating fiber 200b are same values. The lengths thereof are 1 km, respectively. An optical receiver 400 converts an optical signal propagated through the first optical fiber 100a to an electrical signal S out .
FIGS. 3 and 4 show comparative examples for proving the improvement in a CNR and a CSO in the optical communication system of the present invention (first configuration). The components thereof are identical to those of the optical communication system of the present invention shown in FIG. 1.
FIG. 3 shows a first comparative example of a configuration without a dispersion compensating fiber, and FIG. 4 shows a second comparative example of a configuration in which one dispersion compensating fiber 250 is used. In FIG. 4, the dispersion compensating fiber 250 has the same composition as those of the first and second dispersion compensating fibers 200a and 200b of the optical communication system shown in FIG. 1. The length thereof is 2 km to compensate the dispersion of the first optical fiber 100a.
The CNRs and the CSOs were measured for the optical communication system shown in FIG. 1, the first comparative example shown in FIG. 3 and the second comparative example of FIG. 4. The received power at the optical receiver 400 was adjusted to -1.5 dBm by inserting a variable attenuator.
The results of the measurement are shown below.
(1) The optical communication system shown in FIG. 1 (The first configuration in the present invention)
CNR=50.8 dB
CSO=-62.3 dB
(2) The first comparative example shown in FIG. 3
CNR=51.2 dB
CSO=-53.7 dB
(3) The second comparative example shown in FIG. 4
CNR=49.9 dB
CSO=-62.1 dB
By compensating the dispersion of the first optical fiber 100a, the degrated CSO in the first comparative example shown in FIG. 3 is improved in the systems shown in FIGS. 1 and 4. The improved CSO is substantially equal to the intrinsic CSO of the optical transmitter itself. On the other hand, the CNR dropped by 1.3 dB in the second comparative example shown in FIG. 4 owing to the connection of the dispersion compensating fiber 250, while the deterioration of the CNR in the system shown in FIG. 1 is small. Namely, by serially connecting the dispersion compensating fibers divided into a predetermined length to the first optical fiber 100a at a plurality of points on the transmission path, the RIN can be suppressed and the CSO is improved at the same time.
As for the reason therefor, the inventors observes as follows. In general, a large amount of elements are added to the core of the dispersion compensating fiber in order to attain a desired characteristic. For example, in the dispersion compensating fiber of the present embodiment, germanium is added. When an optical amplification function is desired, Er 3+ may be further added. As a result, the relative intensity noise (RIN) by the multi-reflection due to the Rayleigh scattered light is large and it significantly increases relative to the length. FIG. 5 shows a relation between the RIN and the fiber length for different Rayleigh scatter coefficients A. It increases with a larger factor than a proportional factor. As a result, as seen in the second comparative example shown in FIG. 4, the RIN is deteriorated by simply serially connecting the dispersion compensating fiber of a sufficient length to compensate the dispersion of the first optical fiber 100a, and it leads to the deterioration of the CNR. Where the first optical fiber 100a is long, the dispersion compensating fiber of a correspondingly long length is required. Thus, the length of the first optical fiber 100a is limited in order to attain a high CNR.
In the optical communication system of the present invention (first configuration), the first and second dispersion compensating fibers 200a and 200b are connected serially to the ends of the first optical fiber 100a so that a total length of the first and second dispersion compensating fibers 200a and 200b attains the desired dispersion compensating.
In the present configuration, it may be considered that the first optical fiber 100a is used as a connecting member to serially connect the first and second dispersion compensating fibers 200a and 200b. Thus, a rear scattered light of the Rayleigh scattered light is attenuated by the first optical fiber 100. Since the first and second dispersion compensating fibers 200a and 200b are optically spaced from each other to an extent for the rear scattered light to be sufficiently attenuated, the multi-reflection is reduced. Therefore the RIN is suppressed and the CSO is improved. A transmission loss between the first dispersion compensating fiber 200a and the second dispersion compensating fibers 200b may be 3 dB or higher judging from the above result.
The CNR is restricted by a larger one of the RINs of the first and second dispersion compensating fibers 200a and 200b. The dispersion compensating fibers 200a and 200b are further divided to prevent a large RIN from appearing so that the CNR is improved and a long distance optical communication is attained.
When the first and second dispersion compensating fibers 200a and 200b are to be divided, the divided dispersion compensating fibers 201a and 201b are serially connected through the connecting member.
A second optical fiber (a third optical fiber) 500a shown in FIG. 6 may be used as the connecting member when the first dispersion compensating fiber 200a or the second dispersion compensating fiber 200b is to be divided. The second optical fiber 500a has a length to sufficiently attenuate the rear scattered light generated in the dispersion compensating fiber 200a or 200b. In the present configuration, a total length of the dispersion compensating fibers 200a and 200b is long enough to compensate the dispersions of the first optical fibers 100a and the second optical fiber 500a.
Where Er 3+ is doped to the second optical fiber 500a to construct the optical fiber amplifier, the increase of a transmission loss can be prevented.
An optical isolator 500b shown in FIG. 7 may be used as the connecting member.
Where an optical coupler 500c having a loss of 3 dB as shown in FIG. 8 is used as the connecting member, a configuration equivalent to that in which the dispersion compensating fiber 201a is connected in series with the dispersion compensating fibers 201b 1 -201b n is attained, and a configuration which is applicable to one-to-multi, multi-to-one or multi-to-multi optical communication network is attained.
As shown in the application of FIG. 6, the system design may be normalized by providing a dispersion compensating fiber at a predetermined pitch by using the second optical fiber (the third optical fiber) 500a as the transmission path. As a result, the design efficiency is improved and a labor productivity of the system designer is improved. While the dispersion compensating fiber is divided into two fibers in the present embodiment, the dispersion compensating fiber may be divided into three or more fibers depending on the RIN and CNR required, and the connecting member for the dispersion compensating fibers may be those shown in FIGS. 6-8.
A second configuration of the optical communication system of the present invention is explained with reference to FIGS. 9-12.
In the second configuration, third and fourth dispersion compensating fibers 210a and 210b are serially connected to the fourth optical fiber 100b at an end facing the optical transmitter 300 through a connecting member. A total length of the third and fourth dispersion compensating fibers 210a and 210b is long enough to compensate the dispersion of the fourth optical fiber 100b.
The connecting member may be an optical fiber 510a shown in FIG. 9. The fifth optical fiber (sixth optical fiber, seventh optical fiber) 510a may be used as a transmission path or it may be doped with Er 3+ for use as an optical fiber amplifier.
As another connecting member, an optical isolator 510b shown in FIG. 10 may be used. It has been known that the optical isolator 510b is usually fabricated by using a YAG crystal containing Bi.
As a further connecting member, as shown in FIG. 11 (1-to-2 optical communication), an optical coupler 510c may be used and the rear scattered lights of the third and fourth dispersion compensating fibers 210a and 210b may be attenuated by an insertion loss of the optical coupler 510c.
FIG. 12 shows a configuration of a one-to-multi optical communication by using the system shown in FIG. 11. An optical coupler 511c is used as the connecting member for 1-n (n=2 m )optical communication. In the present configuration, there is an attenuation by the insertion loss (3×m dB) between the third and fourth dispersion compensating fibers 210a and 210b 1 -210b n so that they are optically separated.
The third dispersion compensating fiber 210a and the fourth dispersion compensating fiber 210b 1 -210b n are serially connected.
In the second configuration, when the third and fourth dispersion compensating fibers 210a and 210b are to be further divided, the connecting schemes shown in FIGS. 6-8 may be adopted as they are in the first configuration.
A third configuration of the optical communication system of the present invention is now explained with reference to FIGS. 13 to 16.
In the third configuration, fifth and sixth dispersion compensating fibers 220a and 220b are serially connected to the eighth optical fiber 100c at an end facing the optical receiver 400 through a connecting member. A total length of the fifth and sixth dispersion compensating fibers 220a and 220b is long enough to compensate the dispersion of the eighth optical fiber 100c.
As the connecting member, a ninth optical fiber (tenth optical fiber, eleventh optical fiber) 520a shown in FIG. 13 may be used. The optical fiber 520a may be used as a transmission path or it may be doped with Er 3+ for use as an optical fiber amplifier.
As another connecting member, an optical isolator shown in FIG. 14 may be used. It has been known that the optical isolator 520b is usually fabricated by using a YAG crystal containing Bi.
As a further connecting member, as shown in FIG. 15 (1-2 optical communication), an optical coupler 520c may be used and the rear scattered lights of the fifth and sixth dispersion compensating fibers 220a and 220b 1 and 220b 2 may be attenuated by an insertion loss of the optical coupler 520c.
FIG. 16 shows a configuration for one-to-multi optical communication using the system shown in FIG. 15. The optical coupler 521c is used as the connecting member to attain the 1-n (n=2 m ) optical communication. In the present configuration, there is an attenuation by the insertion loss (3×m dB) between the fifth and sixth dispersion compensating fibers 220a and 220b 1 -220b n so that they are optically separated.
The fifth dispersion compensating fiber 220a and the sixth dispersion compensating fiber 220b 1 -220b n are serially connected.
In the third configuration, when the fifth and sixth dispersion compensating fibers 220a and 220b (220b 1 -220b n ) are to be further divided, the connecting schemes shown in FIGS. 6-8 may be adopted as they are in the first configuration.
In the first to third embodiments, the single-mode fiber for the 1.3 μm band is used as the optical fiber (100a, 100b, 100c) although a single mode fiber for a 1.55 μm band may be used to propagate a laser beam having a center wavelength of 1.3 μm. While the input signal Sin is for 40 channel AM-VSB signal, other analog signal (for example, FM, PM, FSK or PSK modulated signal) or digital signal may be used. A communication network (including an optical fiber network) such as a CATV network and a telephone path network may be connected to the optical transmitter 400.
As described above, the dispersion compensating fiber may be doped with Er 3+ and a pumping light may be injected to achieve the optical amplification.
By combining the optical communication systems of the present invention, a communication network having a various network topologies such as star, tree, loop or their combination thereof may be attained.
In accordance with the present invention, a plurality of divided dispersion compensating fibers of a predetermined length are serially inserted in the path of the optical fiber which is the transmission path and they are connected in series. Accordingly, in compensating the dispersion, the relative intensity noise is reduced, the CNR is improved and the improved optical communication with a longer communication distance is attained.
From the invention thus described, it will be obvious that the invention 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.
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An optical communication system that compensate for the dispersion of an optical fiber serving as a transmission path is provided. In its simplest form a dispersion compensating fiber having a sufficient length to compensate for the chromatic dispersion of the optical fiber is divided into portions, each portion having a length selected so as to maintain a linear characteristic of a relative intensity noise of the dispersion compensating fiber, and the divided portions of the dispersion compensating fiber are inserted in the path of the optical fiber while they are optically separated.
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PRIORITY TO RELATED APPLICATION(S)
[0001] This application claims the benefit of European Patent Application No. 08157952.6, filed Jun. 10, 2008, which is hereby incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] The three main mammalian tachykinins, substance P (SP), neurokinin A (NKA) and neurokinin B (NKB) belong to the family of neuropeptides sharing the common COOH-terminal pentapeptide sequence of Phe-X-Gly-Leu-Met-NH 2 . As neurotransmitters, these peptides exert their biological activity via three distinct neurokinin (NK) receptors termed as NK-1, NK-2 and NK-3. SP binds preferentially to the NK-1 receptor, NKA to the NK-2 and NKB to the NK-3 receptor.
[0003] The NK-3 receptor is characterized by a predominant expression in CNS and its involvement in the modulation of the central monoaminergic system has been shown. These properties make the NK-3 receptor a potential target for central nervous system disorders such as anxiety, depression, bipolar disorders, Parkinson's disease, schizophrenia and pain ( Neurosci. Letters, 2000, 283, 185-188 ; Exp. Opin. Ther. Patents 2000, 10, 939-960 ; Neuroscience, 1996, 74, 403-414 ; Neuropeptides, 1998, 32, 481-488).
[0004] Schizophrenia is one of the major neuropsychiatric disorders, characterized by severe and chronic mental impairment. This devastating disease affects about 1% of the world's population. Symptoms begin in early adulthood and are followed by a period of interpersonal and social dysfunction. Schizophrenia manifests as auditory and visual hallucinations, paranoia, delusions (positive symptoms), blunted affect, depression, anhedonia, poverty of speech, memory and attention deficits as well as social withdrawal (negative symptoms).
[0005] For decades scientists and clinicians have made efforts with the aim of discovering an ideal agent for the pharmacological treatment of schizophrenia. However, the complexity of the disorders, due to a wide array of symptoms, has hampered those efforts. There are no specific focal characteristics for the diagnosis of schizophrenia and no single symptom is consistently present in all patients. Consequently, the diagnosis of schizophrenia as a single disorder or as a variety of different disorders has been discussed but not yet resolved. The major difficulty in the development of a new drug for schizophrenia is the lack of knowledge about the cause and nature of this disease. Some neurochemical hypotheses have been proposed on the basis of pharmacological studies to rationalize the development of a corresponding therapy: the dopamine, the serotonin and the glutamate hypotheses. But taking into account the complexity of schizophrenia, an appropriate multireceptor affinity profile might be required for efficacy against positive and negative signs and symptoms. Furthermore, an ideal drug against schizophrenia would preferably have a low dosage allowing once-per-day dosage, due to the low adherence of schizophrenic patients.
[0006] In recent years clinical studies with selective NK1 and NK2 receptor antagonists appeared in the literature showing results for the treatment of emesis, depression, anxiety, pain and migraine (NK1) and asthma (NK2 and NK1). The most exciting data were produced in the treatment of chemotherapy-induced emesis, nausea and depression with NK1 and in asthma with NK2-receptor antagonists. In contrast, no clinical data on NK3 receptor antagonists have appeared in the literature until 2000. Osanetant (SR 142,801) from Sanofi-Synthelabo was the first identified potent and selective non-peptide antagonist described for the NK3 tachykinin receptor for the potential treatment of schizophrenia, which was reported in the literature ( Current Opinion in Investigational Drugs, 2001, 2(7), 950-956 and Psychiatric Disorders Study 4 , Schizophrenia , June 2003, Decision Recources, Inc., Waltham, Mass.). The proposed drug SR 142,801 has been shown in a phase II trial as active on positive symptoms of schizophrenia, such as altered behaviour, delusion, hallucinations, extreme emotions, excited motor activity and incoherent speech, but inactive in the treatment of negative symptoms, which are depression, anhedonia, social isolation or memory and attention deficits.
[0007] The neurokinin-3 receptor antagonists have been described as useful in pain or inflammation, as well as in schizophrenia, Exp. Opinion. Ther. Patents (2000), 10(6), 939-960 and Current Opinion in Investigational Drugs, 2001, 2(7), 950-956 956 and Psychiatric Disorders Study 4 , Schizophrenia , June 2003, Decision Recources, Inc., Waltham, Mass.).
SUMMARY OF THE INVENTION
[0008] The present invention provides compounds of formula I
[0000]
[0000] wherein
R 1 is hydrogen or lower alkyl; each R 2 is independently halogen, CN, lower alkyl, or lower alkyl substituted by halogen; Ar is aryl or heteroaryl; R′ is hydrogen, lower alkyl, halogen, cyano or lower alkyl substituted by halogen; R 3 is hydrogen, lower alkyl or hydroxy; X is —CH(R 4 )—, —N(R 4′ )— or —O—; R 4 is hydrogen, hydroxy, ═O, lower alkyl, lower alkynyl, —S(O) 2 -lower alkyl, —C(O)-lower alkyl, —C(O)CH 2 O-lower alkyl, —CH 2 CN, —C(O)CH 2 CN, —C(O)-cycloalkyl wherein the cycloalkyl group is optionally substituted by cyano, lower alkyl, one or two halogen atoms, ═O or amino, or is
—C(O)O-lower alkyl, —NH-lower alkyl, —NRC(O)O-lower alkyl, —NRC(O)-lower alkyl or —CH 2 O-lower alkyl;
R 4′ is hydrogen, lower alkyl, —S(O) 2 -lower alkyl, —C(O)-lower alkyl, —C(O)CH 2 —O-lower alkyl, —CH 2 CN, —C(O)CN, —C(O)CH 2 CN,
—C(O)-cycloalkyl wherein the cycloalkyl group is optionally substituted by cyano, lower alkyl, one or two halogen atoms, ═O or amino, or is —C(O)O-lower alkyl or —CH 2 O-lower alkyl;
R is hydrogen or lower alkyl; or R 3 and R 4 together with the carbon atoms to which they are attached form a five or six-membered non aromatic ring or R 3 and R 4′ together with the nitrogen and carbon atoms to which they are attached form a five or six-membered non aromatic ring; n is 0 or 1; m is 0, 1, or 2 when n is 0; or m is 0 or 1 when n is 1; and o is 0, 1, 2 or 3;
or pharmaceutically active salts, racemic mixtures, enantiomers, optical isomers or tautomeric forms thereof.
[0026] The invention includes all sterioisomeric forms, including individual diastereoisomers and enantiomers of the compound of formula I as well as racemic and non-racemic mixtures thereof. The invention also includes pharmaceutical compositions containing compounds of formula and methods for the manufacture of the compounds and compositions of the invention.
[0027] The present compounds are high potential NK-3 receptor antagonists for the treatment of depression, pain, psychosis, Parkinson's disease, schizophrenia, anxiety and attention deficit hyperactivity disorder (ADHD).
[0028] The preferred indications using the compounds of the present invention are depression, psychosis, Parkinson's disease, schizophrenia, anxiety and attention deficit hyperactivity disorder (ADHD).
DETAILED DESCRIPTION OF THE INVENTION
[0029] The following definitions of the general terms used in the present description apply irrespective of whether the terms in question appear alone or in combination.
[0030] As used herein, the term “lower alkyl” denotes a straight- or branched-chain hydrocarbon group containing from 1-8 carbon atoms, for example, methyl, ethyl, propyl, isopropyl, n-butyl, i-butyl, t-butyl and the like. Preferred lower alkyl groups are groups with 1-4 carbon atoms.
[0031] The term “lower alkyl substituted by halogen” denotes an alkyl group as defined above, wherein at least one hydrogen atom is replaced by halogen, for example —CF 3 , —CHF 2 , —CH 2 F, —CH 2 CF 3 , —CH 2 CH 2 CF 3 , —CH 2 CF 2 CF 3 and the like. Preferred lower alkyl substituted by halogen groups are groups having 1-4 carbon atoms.
[0032] The term “lower alkynyl” denotes a straight- or branched-chain hydrocarbon group containing from 2-8 carbon atoms and at least one triple bond, for example, ethynyl, propynyl, n-butynyl, i-butynyl, and the like. Preferred lower alkynyl groups are groups with 2-4 carbon atoms.
[0033] The term “halogen” denotes chlorine, iodine, fluorine and bromine.
[0034] The term “cycloalkyl” denotes a saturated carbon ring containing from 3-7 carbon atoms, for example, cyclopropyl, cyclobutyl, cyclpentyl, cyclohexyl, cycloheptyl, and the like.
[0035] The term “aryl” denotes a cyclic aromatic hydrocarbon radical consisting of one or more fused rings containing 6-14 carbon atoms in which at least one ring is aromatic in nature, for example phenyl, benzyl, naphthyl or indanyl. Preferred is the phenyl group.
[0036] The term “heteroaryl” denotes a cyclic aromatic radical consisting of one or more fused rings containing 5-14 ring atoms, preferably containing 5-10 ring atoms, in which at least one ring is aromatic in nature, and which contains at least one heteroatom selected from N, O and S, for example quinoxalinyl, dihydroisoquinolinyl, pyrazinyl, pyrazolyl, pyridinyl, pyridyl, pyrimidinyl, oxadiazolyl, triazolyl, tetrazolyl, thiazolyl, thiadiazolyl, thienyl, furyl, imidazolyl, or benzofuranyl. Preferred heteroaryl group is pyridinyl.
[0037] “Pharmaceutically acceptable,” such as pharmaceutically acceptable carrier, excipient, etc., means pharmacologically acceptable and substantially non-toxic to the subject to which the particular compound is administered.
[0038] The term “pharmaceutically acceptable acid addition salts” embraces salts with inorganic and organic acids, such as hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, citric acid, formic acid, fumaric acid, maleic acid, acetic acid, succinic acid, tartaric acid, methanesulfonic acid, p-toluenesulfonic acid and the like.
[0039] “Therapeutically effective amount” means an amount that is effective to prevent, alleviate or ameliorate symptoms of disease or prolong the survival of the subject being treated.
[0040] Preferred compounds of the present invention are compounds of formula I
[0000]
[0000] wherein
R 1 is lower alkyl; each R 2 is independently halogen or CN; Ar is heteroaryl; R′ is halogen, cyano or lower alkyl substituted by halogen; R 3 is hydrogen or hydroxy; x is —CH(R 4 )—, —N(R 4′ )— or —O—; R 4 is hydrogen, hydroxy, ═O, lower alkynyl, —S(O) 2 -lower alkyl, —NH-lower alkyl, —NRC(O)O-lower alkyl, —NRC(O)-lower alkyl or —CH 2 O-lower alkyl; R 4′ is hydrogen, lower alkyl, —S(O) 2 -lower alkyl, —C(O)-lower alkyl, —C(O)CH 2 —O-lower alkyl, —CH 2 CN, —C(O)CH 2 CN, —C(O)-cycloalkyl wherein the cycloalkyl group is optionally substituted by cyano, lower alkyl, one or two halogen atoms, ═O or amino, or is —C(O)O-lower alkyl; R is hydrogen or lower alkyl; n is 0 or 1; m is 0, 1, or 2 when n is 0; or m is 0 or 1 when n is 1; and o is 1 or 2;
or pharmaceutically active salts, racemic mixtures, enantiomers, optical isomers or tautomeric forms thereof.
[0054] Compounds of formula I, wherein Ar is heteroaryl, are preferred. Especially preferred are compounds of formula I, wherein Ar is pyridinyl.
[0055] Compounds of formula I, wherein X is —CH(R 4 )—, are preferred. For example the following compounds:
{4-[(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cycloheyl}-carbamic acid methyl ester; [(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(4-methoxymethyl-cyclohexyl)-methanone; [(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(4-ethynyl-cyclohexyl)-methanone; 4-[(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexanone; {4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-methyl-carbamic acid tert-butyl ester; {4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-carbamic acid tert-butyl ester; and N-{4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-N-methyl-acetamide.
[0063] Compounds of formula I, wherein X is —N(R 4′ )—, are preferred. For example the following compounds:
1-{4-[(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidin-1-yl}-ethanone; 6-{(SR)-1-[(3RS,4SR)-1-(1-acetyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(1-cyclobutanecarbonyl-piperidin-4-yl)-methanone; [(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile; [(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(1-isobutyl-piperidin-4-yl)-methanone; 4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester; 6-{(SR)-1-[(3RS,4SR)-1-(1-cyclopropanecarbonyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile; 6-((SR)-1-{(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-[1-(1-methyl-cyclopropanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile; 6-{(SR)-1-[(3RS,4SR)-1-[1-(1-amino-cyclopropanecarbonyl)-piperidine-4-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile; 6-{(SR)-1-[(3RS,4SR)-1-(1-cyclobutanecarbonyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile; 6-((SR)-1-{(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-[1-(3-oxo-cyclobutanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile; 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-(1-propionyl-piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile; 6-{(SR)-1-[(3RS,4SR)-1-[1-(2-cyano-acetyl)-piperidine-4-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile; 6-((SR)-1-{(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-[1-(2-methoxy-acetyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile; 1-(4-{(3SR,4RS)-3-(3,4-dichloro-phenyl)-4-[(SR)-1-(5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidine-1-carbonyl}-piperidin-1-yl)-ethanone; 6-((SR)-1-{(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-[1-(1-methyl-cyclopropanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile; [(3RS,4SR)-3-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-4-(2,4-difluoro-phenyl)-pyrrolidin-1-yl]-[1-(1-methyl-cyclopropanecarbonyl)-piperidin-4-yl]-methanone; {(3S,4R)-3-(4-chloro-phenyl)-4-[(S)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-[1-(1-methyl-cyclopropanecarbonyl)-piperidin-4-yl]-methanone; and {(3S,4R)-3-(4-chloro-3-fluoro-phenyl)-4-[(S)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-[1-(1-methyl-cyclopropanecarbonyl)-piperidin-4-yl]-methanone.
[0082] Compounds of formula I, wherein X is —O—, are also preferred, for example the following compound:
{(3SR,4RS)-3-(3,4-Dichloro-phenyl)-4-[(SR)-1-(5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-(tetrahydro-pyran-4-yl)-methanone.
[0084] The preparation of compounds of formula I of the present invention can be carried out in sequential or convergent synthetic routes. Syntheses of the compounds of the invention are shown in the following schemes. The skills required for carrying out the reaction and purification of the resulting products are known to those skilled in the art. The substituents and indices used in the following description of the processes have the significance given herein before unless indicated to the contrary.
[0085] The compounds of formula I can be manufactured by the methods given below, by the methods given in the examples or by analogous methods. Appropriate reaction conditions for the individual reaction steps are known to a person skilled in the art. The reaction sequence is not limited to the one displayed in scheme 1, however, depending on the starting materials and their respective reactivity the sequence of reaction steps can be freely altered. Starting materials are either commercially available or can be prepared by methods analogous to the methods given below, by methods described in references cited in the description or in the examples, or by methods known in the art.
[0086] The present compounds of formula I and their pharmaceutically acceptable salts can be prepared by methods, known in the art, for example by the process described below, which process comprises
[0000] a) coupling a compound of formula VII
[0000]
[0000] with a suitable acid chloride or carboxylic acid of formula
[0000]
[0000] wherein Y is halogen or hydroxy,
to obtain a compound of formula I
[0000]
[0000] wherein the substituents R 1 , R 2 , R 1 , R 3 , X and Ar and the definitions o, n and m are described above, or
b) reacting a compound of formula VIII
[0000]
[0000] with a compound of formula
[0000] R 4 ′-Z
[0000] wherein Z is halogen,
to obtain a compound of formula
[0000]
[0000] wherein the substituents R 1 , R 2 , R 3 , R 4′ , R′, Ar and the definitions o, n and m are described above, or,
if desired, converting the compounds obtained into pharmaceutically acceptable acid addition salts.
[0087] The preparation of compounds of formula I is further described in more detail in schemes I-V and in examples 1-53.
Abbreviations:
[0088] CH 2 Cl 2 : dichloromethane;
DMAP: dimethylaminopyridine;
HOBt: 1-hydroxy-benzotriazol hydrat;
EDC: 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride;
Et 3 N: triethylamine;
EtOAc: ethyl acetate;
H: hexane;
RT: room temperature;
PPh 3 : triphenylphosphine;
DBAD: di-tert-butyl azodicarboxylate
[0000]
[0000] wherein Y is halogen or hydroxy, R 1 a lower alkyl and the other definitions are as above.
[0089] The 3,4-disubstituted pyrrolidines IV are prepared via a stereo specific 1,3-dipolar cycloaddition between substituted (E)-4-phenyl-but-3-en-2-one derivative II and the azomethine ylide generated in situ from the N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine III in the presence of a catalytic amount of acid, such as TFA. Reduction of the acetyl moiety using standard conditions for example LiAlH 4 yields the two diasteroisomers V-A and V-B which are subsequently separated by column chromatography. Each of the diastereoisomers is then separately converted to the final derivatives I-A and I-B in the same manner. For instance V-B is subjected to a standard Mitsunobu reaction with for example a phenol, pyridin-ol, pyrimidin-ol to give the aryl-ether VI-B. Selective N-debenzylation is then carried out using several known procedures which are compatible with the substitution patterns of the aromatic rings to afford VII-B. Final derivatives I-B are prepared via a coupling with a suitable acid chloride or carboxylic acid using known methods, wherein Y is hydroxy or halogen, R 1 a methyl moiety and the other definitions are as described above.
[0000]
[0000] wherein Y is hydroxy or halogen, Z is halogen and the other definitions are as described above.
[0090] Alternatively the pyrrolidine VII-B can undergo a coupling with a carboxylic acid derivative which after selective Boc deprotection generated the intermediate VIII-B. Final derivatives 1-B-1 are prepared via a coupling with R 4′ -Y using well known reactions and procedures.
[0091] In the same manner, the diastereomer VII-A can be converted to final derivatives I-A.
[0000]
[0092] Alternatively to the Mitsunobu reaction shown scheme I, derivatives V-A and V-B can used in a nucleophilic aromatic substitution reaction when the Ar moiety is a o-pyridinyl or a o-pyrimidinyl to yield respectively VI-B and VI-A.
[0000]
[0093] An alternative method for the preparation of intermediates IV (with R 1 is Me) is highlighted scheme 4. A 1,3-dipolar cycloaddition between the commercially available but-3-yn-2-one IX and the azomethine ylide generated in situ from the N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine III in the presence of a catalytic amount of acid, such as TFA afforded the dihydropyrrole derivative X. A 1,4-addition of a boronic acid catalysed by a Rh(I) catalyst such as the Rhacetylacetonatbis(ethylene) in a presence of a chiral phosphine ligand such as the (R) or (S)-BINAP afforded the optically enriched disubstituted pyrrolidine IV. Similar Rh-catalysed asymmetric 1,4-arylation have been reported earlier ( Tet. Lett., 2004, 45(16), 3265)
[0000]
[0094] The derivatives of the type I-C with R 1 equal H where prepared via the following route (scheme 5). The 3,4-disubstituted pyrrolidines XII were prepared via a stereo specific 1,3-dipolar cycloaddition between the (E)-3-substituted phenyl-acrylic acid ethyl ester derivatives XI and the azomethine ylide generated in situ from the N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine III in the presence of a catalytic amount of acid, such as TFA. Reduction of the ester moiety using standard conditions for example LiAlH 4 yielded the primary alcohol V-C. Standard Mitsunobu reaction with for example a phenol, pyridin-ol, pyrimidin-ol gave the aryl-ether VI-C. Selective N-debenzylation was then carried out using several known procedures which are compatible with the substitution patterns of the aromatic rings to afford VII-C. Final derivatives I-C were obtained via a coupling with a suitable acid chloride or carboxylic acid using known methods.
EXPERIMENTAL PROCEDURES
[0095] As mentioned earlier, the compounds of formula I and their pharmaceutically usable addition salts possess valuable pharmacological properties. Compounds of the present invention are antagonists of neurokinin 3 (NK-3) receptors.
Experimental Procedure
[0096] The compounds were investigated in accordance with the tests given hereinafter.
[0000] [ 3 H]SR142801 competition binding assay
[0097] hNK3 receptor binding experiment were performed using [ 3 H]SR142801 (Catalog No. TRK1035, specific activity: 74.0 Ci/mmol, Amersham, GE Healthcare UK limited, Buckinghamshire, UK) and membrane isolated from HEK293 cells transiently expressing recombinant human NK3 receptor. After thawing, the membrane homogenates were centrifuged at 48,000×g for 10 min at 4° C., the pellets were resuspended in the 50 mM Tris-HCl, 4 mM MnCl 2 , 1 μM phosphoramidon, 0.1% BSA binding buffer at pH 7.4 to a final assay concentration of 5 μg protein/well. For inhibition experiments, membranes were incubated with [ 3 H]SR142801 at a concentration equal to K D value of radioligand and 10 concentrations of the inhibitory compound (0.0003-10 μM) (in a total reaction volume of 500 μl) for 75 min at room temperature (RT). At the end of the incubation, membranes were filtered onto unitfilter (96-well white microplate with bonded GF/C filter preincubated 1 h in 0.3% PEI+0.3% BSA, Packard BioScience, Meriden, Conn.) with a Filtermate 196 harvester (Packard BioScience) and washed 4 times with ice-cold 50 mM Tris-HCl, pH 7.4 buffer. Nonspecific binding was measured in the presence of 10 μM SB222200 for both radioligands. The radioactivity on the filter was counted (5 min) on a Packard Top-count microplate scintillation counter with quenching correction after addition of 45 μl of microscint 40 (Can berra Packard S. A., Zürich, Switzerland) and shaking for 1 h. Inhibition curves were fitted according to the Hill equation: y=100/(1+(x/IC 50 ) nH ), where n H =slope factor using Excel-fit 4 software (Microsoft). IC 50 values were derived from the inhibition curve and the affinity constant (K i ) values were calculated using the Cheng-Prussoff equation K i =IC 50 /(1+[L]/K D ) where [L] is the concentration of radioligand and K D is its dissociation constant at the receptor, derived from the saturation isotherm. All experiments were performed in duplicate and the mean±standard error (SEM) of the individual K i values was calculated.
[0098] Results of some compounds of the invention are shown in the following Table 1.
[0000]
TABLE 1
Example
Data [μM]
1
0.0047
2
0.0076
3
0.0012
5
0.0095
6
0.0058
10
0.009
11
0.0061
12
0.0092
13
0.0044
14
0.0049
17
0.0046
19
0.0077
20
0.0026
21
0.0021
22
0.0036
23
0.0075
24
0.0036
42
0.0028
43
0.007
45
0.004
46
0.0018
47
0.0019
48
0.0074
52
0.001
53
0.0008
[0099] The present invention also provides pharmaceutical compositions containing compounds of the invention, for example, compounds of formula I or pharmaceutically acceptable salts thereof and a pharmaceutically acceptable carrier. Such pharmaceutical compositions can be in the form of tablets, coated tablets, dragées, hard and soft gelatin capsules, solutions, emulsions or suspensions. The pharmaceutical compositions also can be in the form of suppositories or injectable solutions.
[0100] The pharmaceutical compositions of the invention, in addition to one or more compounds of the invention, contain a pharmaceutically acceptable carrier. Suitable pharmaceutically acceptable carriers include pharmaceutically inert, inorganic or organic carriers.
[0101] Lactose, corn starch or derivatives thereof, talc, stearic acid or its salts etc can be used as such excipients e.g. for tablets, dragées and hard gelatine capsules. Suitable excipients for soft gelatine capsules are e.g. vegetable oils, waxes, fats, semi-solid and liquid polyols etc. Suitable excipients for the manufacture of solutions and syrups are e.g. water, polyols, saccharose, invert sugar, glucose etc. Suitable excipients for injection solutions are e.g. water, alcohols, polyols, glycerol, vegetable oils etc. Suitable excipients for suppositories are e.g. natural or hardened oils, waxes, fats, semi-liquid or liquid polyols etc.
[0102] Moreover, the pharmaceutical compositions can contain preservatives, solubilizers, stabilizers, wetting agents, emulsifiers, sweeteners, colorants, flavorants, salts for varying the osmotic pressure, buffers, masking agents or antioxidants. They can also contain still other therapeutically valuable substances.
[0103] The dosage at which compounds of the invention can be administered can vary within wide limits and will, of course, be fitted to the individual requirements in each particular case. In general, in the case of oral administration a daily dosage of about 10 to 1000 mg per person of a compound of general formula I should be appropriate, although the above upper limit can also be exceeded when necessary.
Example A
[0104] Tablets of the following composition are manufactured in the usual manner:
[0000]
mg/tablet
Active substance
5
Lactose
45
Corn starch
15
Microcrystalline cellulose
34
Magnesium stearate
1
Tablet weight
100
Example B
[0105] Capsules of the following composition are manufactured:
[0000]
mg/capsule
Active substance
10
Lactose
155
Corn starch
30
Talc
5
Capsule fill weight
200
[0106] The active substance, lactose and corn starch are firstly mixed in a mixer and then in a comminuting machine. The mixture is returned to the mixer, the talc is added thereto and mixed thoroughly. The mixture is filled by machine into hard gelatin capsules.
Example C
[0107] Suppositories of the following composition are manufactured:
[0000]
mg/supp.
Active substance
15
Suppository mass
1285
Total
1300
[0108] The suppository mass is melted in a glass or steel vessel, mixed thoroughly and cooled to 45° C. Thereupon, the finely powdered active substance is added thereto and stirred until it has dispersed completely. The mixture is poured into suppository moulds of suitable size, left to cool, the suppositories are then removed from the moulds and packed individually in wax paper or metal foil.
[0109] The following Examples illustrate the present invention without limiting it. All temperatures are given in degrees Celsius.
General Procedure I: Amid Coupling (Pyrrolidine VII and Carboxylic Acid)
[0110] To a stirred solution of a carboxylic acid derivative (commercially available or known in the literature) (1 mmol) in 10 mL of CH 2 Cl 2 was added (1.3 mmol) of EDC, (1.3 mmol) of HOBt and Et 3 N (1.3 mmol). After one hour at RT, was added a pyrrolidine intermediate of general formula (VII). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Flash chromatography or preparative HPLC afforded the title compound.
[0000] General Procedure II: Coupling Between a Compound of Formula VII or VIII with an Acid Chloride, Chloroformate or Sulfonyl Chloride
[0111] A solution of the pyrrolidine (1 mmol) of formula (VII) in CH 2 Cl 2 (10 mL) was treated with Et 3 N (1.2 mmol) and an acid chloride, chloroformate or sulfonylchlorid (1.2 mmol) and stirred at RT overnight. Purification by preparative HPLC yielded the title compound.
Pyrrolidine Intermediates of Formula VII-B
Pyrrolidine VII-B-1
5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine
[0112]
a) 1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanone (IV-1)
[0113] A solution of N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine (32.78 g, 0.138 mol) in CH 2 Cl 2 (50 mL) was added dropwise, over a 30 minutes period, to a stirred solution of (E)-4-(3,4-dichloro-phenyl)-but-3-en-2-one (19.80 g, 0.092 mol) and trifluoroacetic acid (1.05 mL, 0.009 mol) in CH 2 Cl 2 (100 mL) at 0° C. The ice bath was removed, and the solution was stirred at 25° C. for an additional 48 h. It was then concentrated and purification by flash chromatography (SiO 2 , CH 2 Cl 2 /MeOH 98:2) afforded 28.3 g (88%) of the title compound as a yellow oil. ES-MS m/e: 348.2 (M+H + ).
b) (SR)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-A-1) and (RS)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-1)
[0114] To a solution of 1-[(3SR,4RS)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanone (IV-1) (14.90 g, 0.043 mol) in THF (300 mL) at 0° C. were added portion wise LiAlH 4 (2.05 g, 0.051 mol). Stirring was continued for one hour, and the reaction mixture was carefully quenched by addition of aq. NH 4 Cl, concentrated under vacuo and the product extracted with EtOAC. The combined organic phases were dried on Na 2 SO 4 and concentrated under vacuo. The two diastereoisomeres were separated by column chromatography (SiO 2 , EtOAc/H, 1:1) to yield (RS)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-1) 4.69 g (31%) as a white solid ES-MS m/e: 350.2 (M+H + ) and (SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-A-1) 5.30 g (35%) as a white solid ES-MS m/e: 350.2 (M+H + ).
c) 2-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy-}-5-chloro-pyridine
[0115] To a suspension of PPh 3 (PPh 3 polymer bound, 3 mmol PPh 3 /g resin) (3.14 g, 9.4 mmol) in THF (70 mL) at 0° C. were added 5-chloro-pyridin-2-ol (0.832 g, 6.42 mmol) and then DBAD (1.578 g, 6.85 mmol). After 5 minutes was added (RS)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-1) (1.50 g, 4.28 mmol). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO 2 , EtOAc/H, 1:6) yielded 1.71 g (87%) of the title compound as a colorless oil. ES-MS m/e: 461.2 (M+H + ).
d) 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0116] To a solution of 2-{(SR)-1-[(3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine (1.71 g (3.71 mmol) dissolved in CH 3 CN (50 mL) was added 0.75 mL (5.57 mmol) of 2,2,2-trichloroethyl chloroformate and stirring was continued for 4 hours at RT. Volatiles were removed under vacuo, and the crude was dissolved in AcOH (30 mL) before a total of 1.0 g of Zn dust was added portion wise. After three hours at RT, the reaction mixture was filtered on celite, the solvent removed under vacuo, followed by an extraction with EtOAc/aq. NaHCO 3 (basic pH). The organic phases were dried on Na 2 SO 4 and column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 0.74 g (54%) of the title compound as a colorless oil. ES-MS m/e: 373.1 (M+H + ).
Pyrrolidine VII-B-2
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0117]
a) 6-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0118] To a suspension of PPh 3 (PPh 3 polymer bound, 3 mmol PPh 3 /g resin) (1.97 g) in THF (300 mL) at 0° C. were added 6-hydroxy-nicotinonitrile (0.61 g, 5.1 mmol) and then DBAD (1.10 g). After 5 minutes was added (RS)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-1) (1.20 g, 3.4 mmol, described herein above). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO 2 , EtOAc/H, 1:4) yielded 1.02 g (66%) of the title compound as a colorless oil. ES-MS m/e: 452.0 (M+H + ).
b) 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0119] To a solution of 6-{(SR)-1-[(3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile 0.75 g (1.70 mmol) dissolved in CH 3 CN (50 mL) was added 0.56 mL (4.14 mmol) of 2,2,2-trichloroethyl chloroformate and stirring was continued for 4 hours at RT. Volatiles were removed under vacuo, and the crude was dissolved in AcOH (30 mL) before a total of 0.45 g of Zn dust was added portion wise. After three hours at RT, the reaction mixture was filtered on celite, the solvent removed under vacuo, followed by an extraction with EtOAc/aq. NaHCO 3 (basic pH). The organic phases were dried on Na 2 SO 4 and column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 0.36 g (60%) of the title compound as a colorless oil. ES-MS m/e: 362.3 (M+H + ).
Pyrrolidine VII-B-3
2-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine
[0120]
a) 2-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine
[0121] To a suspension of PPh 3 (PPh 3 polymer bound, 3 mmol PPh 3 /g resin) (0.77 g) in THF (25 mL) at 0° C. were added 5-trifluoromethyl-pyridin-2-ol (0.28 g, 1.75 mmol) and then DBAD (0.43 g). After 5 minutes was added (RS)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-1) (0.41 g, 1.17 mmol, described herein above). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO 2 , EtOAc/H, 1:4) yielded 0.45 g (78%) of the title compound as a colorless oil. ES-MS m/e: 495.8 (M+H + ).
b) 2-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine (VII-B-3)
[0122] To a solution of 2-{(SR)-1-[(3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine 0.45 g (0.91 mmol) dissolved in toluene (5 mL) were added 0.30 mL (2.7 mmol) of 1-chloroethyl chloroformate and 0.46 mL of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (5 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 0.32 g (87%) of the title compound as a light yellow oil. ES-MS m/e: 405.9 (M+H + ).
Pyrrolidine VII-B-4
5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine
[0123]
a) (E)-4-(2,4-Difluoro-phenyl)-but-3-en-2-one
[0124] A two necked flask was charged with 2,4-difluorobenzaldehyde (4.0 g, 28.1 mmol) and (2-oxo-propyl)-phosphonic acid dimethyl ester (5.78 g, 33.0 mmol) and cooled down at 0° C. K 2 CO 3 (7.62 g, 55.1 mmol) in H 2 O (14 mL) was added dropwise. Stirring was continued over night at RT. The product was extracted with EtOAc, and the organic phase was dried over Na 2 SO 4 . Flash chromatography (SiO 2 , Heptane/EtOAc 1:3) afforded 4.0 g (79%) of the title compound as alight yellow oil.
b) 1-[(3RS,4SR)-1-Benzyl-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethanone (IV-4)
[0125] A solution of N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine (7.82 g, 32.9 mmol) in CH 2 Cl 2 (40 mL) was added dropwise, over a 30 minutes period, to a stirred solution of (E)-4-(2,4-difluoro-phenyl)-but-3-en-2-one (4.0 g, 21.9 mmol) and trifluoroacetic acid (0.17 mL, 0.21 mmol) in CH 2 Cl 2 (10 mL) at 0° C. The ice bath was removed, and the solution was stirred at 25° C. for an additional 48 h. It was then concentrated and purification by flash chromatography (SiO 2 , CH 2 Cl 2 /MeOH 98:2) afforded 6.2 g (89%) of the title compound as a yellow oil. ES-MS m/e: 316.1 (M+H + ).
c) (RS)-1-[(3SR,4RS)-4-(2,4-Difluoro-phenyl)-pyrrolidin-3-yl]-ethanol (V-A-4) and (SR)-1-[(3SR,4RS)-4-(2,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-4)
[0126] To a solution of 1-[(3RS,4SR)-1-benzyl-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethanone (IV-4) (1.87 g, 5.92 mmol) in THF (30 mL) at 0° C. were added portion wise LiAlH 4 (0.19 g, 5.21 mol). Stirring was continued for one hour, and the reaction mixture was carefully quenched by addition of aq. NH 4 Cl, concentrated under vacuo and the product extracted with EtOAC. The combined organic phases were dried on Na 2 SO 4 and concentrated under vacuo. The two diastereoisomeres were separated by column chromatography (SiO 2 , EtOAc/H, 1:1) to yield (RS)-1-[(3RS,4SR)-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-4) 0.72 g (38%) as a white solid ES-MS m/e: 318.1 (M+H + ) and (SR)-1-[(3RS,4SR)-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethanol (V-A-4) 0.374 g (19%) as a white solid ES-MS m/e: 318.1 (M+H + ).
d) 2-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine (VI-B-4)
[0127] To a suspension of PPh 3 (PPh 3 polymer bound, 3 mmol PPh 3 /g resin) (1.27 g, 4.85 mmol) in THF (25 mL) at 0° C. were added 5-chloro-pyridin-2-ol (0.429 g, 3.31 mmol) and then DBAD (0.81 g, 3.51 mmol). After 5 minutes was added (RS)-1-[(3RS,4SR)-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-4) (0.70 g, 2.20 mmol). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO 2 , EtOAc/H, 1:6) yielded 0.69 g (73%) of the title compound as a colorless oil. ES-MS m/e: 429.2 (M+H + ).
e) 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-4)
[0128] To a solution of 2-{(SR)-1-[(3RS,4SR)-1-benzyl-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine 570 mg (1.32 mmol) dissolved in toluene (12 mL) were added 0.43 mL (3.96 mmol) of 1-chloroethyl chloroformate and 0.68 mL (3.96 mmol) of Hunig's base.
[0129] The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (10 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 350 mg (78%) of the title compound as a light yellow oil. ES-MS m/e: 339.1 (M+H + ).
Pyrrolidine VII-B-5
6-{(SR)-1-[(3RS,4SR)-4-(4-Cyano-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0130]
a) 4-((E)-3-Oxo-but-1-enyl)-benzonitrile
[0131] A two necked flask was charged with 4-formyl-benzonitrile (20.0 g, 0.152 mol) and (2-oxo-propyl)-phosphonic acid dimethyl ester (30.4 g, 0.18 mol) and cooled down at 0° C. K 2 CO 3 (42.16 g, 0.305 mol) in H 2 O (45 mL) was added dropwise. Stirring was continued over night at RT. The product was extracted with EtOAc, and the organic phase was dried over Na 2 SO 4 . Flash chromatography (SiO 2 , Heptane/EtOAc 1:1) afforded 18.7 g (72%) of the title compound as alight yellow solid.
b) 4-((3SR,4RS)-4-Acetyl-1-benzyl-pyrrolidin-3-yl)-benzonitrile (IV-5)
[0132] A solution of N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine (22.46 g, 94.6 mmol) in CH 2 Cl 2 (100 mL) was added dropwise, over a 30 minutes period, to a stirred solution of 4-((E)-3-oxo-but-1-enyl)-benzonitrile (10.8 g, 63.1 mmol) and trifluoroacetic acid (0.48 mL, 6.30 mmol) in CH 2 Cl 2 (40 mL) at 0° C. The ice bath was removed, and the solution was stirred at 25° C. for an additional 48 h. It was then concentrated and purification by flash chromatography (SiO 2 , EtOac/Heptane 1:1) afforded 6.3 g (33%) of the title compound as a yellow oil. ES-MS m/e: 305.1 (M+H + ).
c) 4-[(3 SR,4RS)-1-Benzyl-4-((SR)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-A-5) and 4-[(3 SR,4RS)-1-Benzyl-4-((RS)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-B-5)
[0133] To a solution of 4-((3SR,4RS)-4-acetyl-1-benzyl-pyrrolidin-3-yl)-benzonitrile (IV-5) (IV-5) (6.30 g, 20.7 mmol) in MeOH (300 mL) at RT were added portion wise LiBH 4 (9.49 g, 0.43 mol). Stirring was continued for overnight, and the reaction mixture was carefully quenched by addition of aq. NH 4 Cl, concentrated under vacuo and the product extracted with EtOAC. The combined organic phases were dried on Na 2 SO 4 and concentrated under vacuo. The two diastereoisomeres were separated by column chromatography (SiO 2 , EtOAc/H, 1:1) to yield 4-[(3SR,4RS)-1-benzyl-4-((RS)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-B-5) 1.35 g (21%) as a colorless oil ES-MS m/e: 307.2 (M+H + ) and 4-[(3SR,4RS)-1-benzyl-4-((SR)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-A-5) 1.30 g (20%) as a colorless oil ES-MS m/e: 307.2 (M+H + ).
d) 6-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(4-cyano-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VI-B-5)
[0134] To a stirred solution of 4-[(3SR,4RS)-1-benzyl-4-((SR)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-A-5) (0.65 g, 2.12 mmol) in DMF (40 mL) at RT was added NaH (55% purity, 0.10 g, 4.1 mmol). After 10 minutes, 6-chloro-nicotinonitrile (0.32 g, 2.33 mmol) was added. The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NH 4 Cl sat, followed by column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.39 g (45%) of the title compound as a colorless oil. ES-MS m/e: 409.3 (M+H + ).
e) 6-{(SR)-1-[(3RS,4SR)-4-(4-Cyano-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-5)
[0135] To a solution of 6-{(SR)-1-[(3RS,4SR)-1-benzyl-4-(4-cyano-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VI-B-5) 380 mg (0.93 mmol) dissolved in toluene (10 mL) were added 0.30 mL (2.79 mmol) of 1-chloroethyl chloroformate and 0.47 mL (2.79 mmol) of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (10 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 105 mg (35%) of the title compound as a light yellow oil. ES-MS m/e: 319.2 (M+H + ).
Pyrrolidine VII-B-6
4-{(3SR,4RS)-4-[1-((SR)-5-Trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile
[0136]
a) 4-{(3 SR,4RS)-1-Benzyl-4-[1-((SR)-5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VI-B-6)
[0137] To a stirred solution of 4-[(3SR,4RS)-1-benzyl-4-((SR)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-A-5) (0.65 g, 2.12 mmol, described herein above) in DMF (40 mL) at RT was added NaH (55% purity, 0.10 g, 4.1 mmol). After 10 minutes, 2-chloro-5-trifluoromethyl-pyridine (0.42 g, 2.33 mmol) was added. The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NH 4 Cl sat, followed by column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.15 g (15%) of the title compound as a colorless oil. ES-MS m/e: 452.1 (M+H + ).
b) 4-{(3 SR,4RS)-4-[1-((SR)-5-Trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VII-B-6)
[0138] To a solution of 4-{(3SR,4RS)-1-benzyl-4-[1-((SR)-5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VI-B-6) 150 mg (0.33 mmol) dissolved in toluene (5 mL) were added 0.11 mL (1.00 mmol) of 1-chloroethyl chloroformate and 0.17 mL (1.00 mmol) of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (7.5 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 60 mg (50%) of the title compound as a colorless oil. ES-MS m/e: 362.2 (M+H + )
Pyrrolidine VII-B-7
4-{(3SR,4RS)-4-[1-((SR)-5-Chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile
[0139]
a) 4-{(3 SR,4RS)-1-Benzyl-4-[1-((SR)-5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VI-B-7)
[0140] To a stirred solution of 4-[(3SR,4RS)-1-benzyl-4-((SR)-1-hydroxy-ethyl)-pyrrolidin-3-yl]-benzonitrile (V-A-5) (0.65 g, 2.12 mmol, described herein above) in DMF (40 mL) at RT was added NaH (55% purity, 0.10 g, 4.1 mmol). After 10 minutes, 2,5-dichloro-pyridine (0.34 g, 2.33 mmol) was added. The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NH 4 Cl sat, followed by column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.75 g (78%) of the title compound as a colorless oil. ES-MS m/e: 418.3 (M+H + ).
b) 4-{(3 SR,4RS)-4-[1-((SR)-5-Chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VII-B-7)
[0141] To a solution of 4-{(3SR,4RS)-1-benzyl-4-[1-((SR)-5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VI-B-7) 700 mg (1.65 mmol) dissolved in toluene (20 mL) were added 0.54 mL (5.03 mmol) of 1-chloroethyl chloroformate and 0.85 mL (5.03 mmol) of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (30 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 260 mg (47%) of the title compound as a colorless oil. ES-MS m/e: 328.2 (M+H + ).
Pyrrolidine VII-B-8
5-Chloro-2-{(S)-1-[(3R,4S)-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine
[0142]
a) 1-(1-Benzyl-2,5-dihydro-1H-pyrrol-3-yl)-ethanone
[0143] To a solution of N-(methoxymethyl)-N-(phenylmethyl)-N-(trimethylsilyl)methylamine (9.76 g, 0.041 mol) in CH 2 Cl 2 (40 mL) at 0° C., was added dropwise over a 5 minutes period but-3-yn-2-one (2.0 g, 0.029 mol) followed by trifluoroacetic acid (0.22 mL, 0.003 mol) (very exothermic reaction). The ice bath was removed after 30 minutes, and the solution was stirred at 25° C. for an additional 2 h. It was then concentrated and purification by flash chromatography (SiO 2 , EtOAc/Heptane 1:1) afforded 2.90 g (49%) of the title compound as a yellow oil. ES-MS m/e: 202.2 (M+H + ).
b) 1-[(3R,4S)-1-Benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanone (IV-8)
[0144] A two necked flask was charged under argon with rhodium(acac)bis ethylene (45 mg, 0.05 eq.), (R)-BINAP (110 mg, 0.05 eq.) and 4-chloro-phenylboronic acid (1.20 g, 2.2 eq.). 100 mL of MeOH and 10 mL of H 2 O were added followed by 1-(1-benzyl-2,5-dihydro-1H-pyrrol-3-yl)-ethanone (0.70 g). The reaction mixture was heated at 55° C. for 8 hours, cooled down to RT and concentrated under vacuo. Purification by flash chromatography (SiO 2 , EtOAc/Heptane 2/1) afforded 0.36 g (33%) of the title product as a light yellow oil. ES-MS m/e: 314.0 (M+H + ).
c) (S)-1-[(3R,4S)-1-Benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-A-8) and (R)-1-[(3R,4S)-1-Benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-8)
[0145] To a solution of 1-[(3R,4S)-1-benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanone (0.52 g, 1.65 mmol) in THF (20 mL) at 0° C. were added portion wise LiAlH 4 (55 mg, 1.45 mmol). Stirring was continued for one hour, and the reaction mixture was carefully quenched by addition of aq. NH 4 Cl, concentrated under vacuo and the product extracted with EtOAC. The combined organic phases were dried on Na 2 SO 4 and concentrated under vacuo. The two diastereoisomeres were separated by column chromatography (SiO 2 , EtOAc/H, 1:1) to yield (R)-1-[(3R,4S)-1-benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-B-8) 0.24 g (46%) as a white solid ES-MS m/e: 316.1 (M+H + ) and (S)-1-[(3R,4S)-1-benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanol (V-A-8) 0.25 g (47%) as a white solid ES-MS m/e: 316.1 (M+H + ).
d) 2-{(S)-1-[(3R,4S)-1-Benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine (VI-B-8)
[0146] To a suspension of PPh 3 (PPh 3 polymer bound, 3 mmol PPh 3 /g resin) (0.44 g, 1.69 mmol) in THF (50 mL) at 0° C. were added 5-chloro-pyridin-2-ol (0.15 g, 1.15 mmol) and then DBAD (0.28 g, 1.23 mmol). After 5 minutes was added (R)-1-[(3R,4S)-1-benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanol (0.25 g, 0.79 mmol). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO 2 , EtOAc/H, 1:3) yielded 0.22 g (65%) of the title compound as a colorless oil. ES-MS m/e: 427.8 (M+H + ).
e) 5-Chloro-2-{(S)-1-[(3R,4S)-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-8)
[0147] To a solution of 2-{(S)-1-[(3R,4S)-1-benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine 220 mg (0.51 mmol) dissolved in toluene (5 mL) were added 0.17 mL (1.53 mmol) of 1-chloroethyl chloroformate and 0.27 mL (1.53 mmol) of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (10 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 110 mg (62%) of the title compound as a light yellow oil. ES-MS m/e: 337.1 (M+H + ).
Pyrrolidine VII-B-9
5-Chloro-2-{(S)-1-[(3R,4S)-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine
[0148]
a) 1-[(3R,4S)-1-Benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanone (IV-9)
[0149] A two necked flask was charged under argon with rhodium(acac)bis ethylene (31 mg, 0.05 eq.), (R)-BINAP (74 mg, 0.05 eq.) and 4-chloro-3-fluoro-phenylboronic acid (825 mg, 2.5 eq.). 30 mL of MeOH and 3 mL of H 2 O were added followed by 1-(1-benzyl-2,5-dihydro-1H-pyrrol-3-yl)-ethanone (480 mg, described herein above). The reaction mixture was heated at 55° C. for 3 hours, cooled down to RT and concentrated under vacuo. Purification by flash chromatography (SiO 2 , EtOAc/Heptane 2/1) afforded 261 mg (33%) of the title product as a light yellow oil. ES-MS m/e: 332.1 (M+H + ).
b) (S)-1-[(3R,4S)-1-Benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanol (IV-A-9) and (R)-1-[(3R,4S)-1-Benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanol (IV-B-9)
[0150] To a solution of 1-[(3R,4S)-1-benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanone (260 mg, 0.78 mmol) in THF (10 mL) at 0° C. were added portion wise LiAlH 4 (26 mg, 0.68 mmol). Stirring was continued for one hour, and the reaction mixture was carefully quenched by addition of aq. NH 4 Cl, concentrated under vacuo and the product extracted with EtOAC. The combined organic phases were dried on Na 2 SO 4 and concentrated under vacuo. The two diastereoisomeres were separated by column chromatography (SiO 2 , EtOAc/H, 1:1) to yield (R)-1-[(3R,4S)-1-benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanol (IV-B-9) 101 mg (38%) as a white solid ES-MS m/e: 334.2 (M+H + ) and (S)-1-[(3R,4S)-1-benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanol (IV-A-9) 80 mg (30%) as a white solid ES-MS m/e: 334.2 (M+H + ).
c) 2-{(S)-1-[(3R,4S)-1-Benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine (VI-B-9)
[0151] To a suspension of PPh 3 (PPh 3 polymer bound, 3 mmol PPh 3 /g resin) (216 mg, 0.65 mmol) in THF (10 mL) at 0° C. were added 5-chloro-pyridin-2-ol (58 mg, 0.45 mmol) and then DBAD (110 mg, 0.48 mmol). After 5 minutes was added (R)-1-[(3R,4S)-1-benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethanol (100 mg, 0.30 mmol). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO 2 , EtOAc/H, 1:3) yielded 100 mg (75%) of the title compound as a colorless oil. ES-MS m/e: 445.1 (M+H + ).
d) 5-Chloro-2-{(S)-1-[(3R,4S)-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-9)
[0152] To a solution of 2-{(S)-1-[(3R,4S)-1-benzyl-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-chloro-pyridine 98 mg (0.22 mmol) dissolved in toluene (5 mL) were added 0.072 mL (0.66 mmol) of 1-chloroethyl chloroformate and 0.11 mL (0.66 mL) of Hunig's base. The reaction mixture was heated at 100° C. for one hour. After cooling down to RT, volatiles were removed under vacuo and the crude was dissolved in MeOH (5 mL). The reaction mixture was heated at 85° C. for 30 minutes and after cooling down to RT, volatiles were removed under vacuo and the residue was directly purified on column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9:1) yielded 75 mg (95%) of the title compound as a light yellow oil. ES-MS m/e: 355.1 (M+H + ).
Pyrrolidine intermediates of formula VIII-B
Pyrrolidine VIII-B-1
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0153]
a) 4-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester
[0154] To a stirred solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (0.165 g, 0.72 mmol) in 20 mL of CH 2 Cl 2 was added (0.14 g, 0.94 mmol) of EDC, (0.10 g, 0.94 mmol) of HOBt and Et 3 N (0.11 mL, 1.1 mmol). After one hour at RT, was added 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2, 0.26 g, 0.72 mmol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.29 g (91%) of the title compound as a white foam. ES-MS m/e: 574.8 (M+H + ).
b) 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0155] To a stirred solution of 4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester (0.28 g, 0.50 mmol) in 24 mL of CH 2 Cl 2 was added 6 mL of TFA. After one hour at RT, the reaction was quenched by addition of aq. NaOH 1M (until ph=10) and the product was extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo to yield 0.237 g (99%) of the title compound as a white foam. ES-MS m/e: 473.0 (M+H + ). Pyrrolidine VIII-B-2
6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0156]
a) 3-[(3R,4S)-3-[(S)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-azetidine-1-carboxylic acid tert-butyl ester
[0157] To a stirred solution of azetidine-1,3-dicarboxylic acid mono-tert-butyl ester (0.072 g, 0.36 mmol) in 15 mL of CH 2 Cl 2 was added (0.069 g, 0.36 mmol) of EDC, (0.048 g, 0.36 mmol) of HOBt and Et 3 N (0.06 mL, 0.42 mmol). After one hour at RT, was added 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2, 0.10 g, 0.27 mmol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.14 g (98%) of the title compound as a white solid. ES-MS m/e: 545.3 (M+H + ).
b) 6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-2)
[0158] To a stirred solution of 3-[(3R,4S)-3-[(S)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-azetidine-1-carboxylic acid tert-butyl ester (0.14 g, 0.25 mmol) in 4 mL of CH 2 Cl 2 was added 1 mL of TFA. After one hour at RT, the reaction was quenched by addition of aq. NaOH 1M (until ph=10) and the product was extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo to yield 0.106 g (92%) of the title compound as a white foam. ES-MS m/e: 445.1 (M+H + ).
Example 1
1-{4-[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidin-1-yl}-ethanone
[0159]
[0000] Coupling according to general procedure I:
[0160] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0161] Carboxylic acid: 1-Acetyl-piperidine-4-carboxylic acid (commercially available), ES-MS m/e: 524.3 (M+H + ).
Example 2
6-{(SR)-1-[(3RS,4SR)-1-(1-Acetyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0162]
[0163] Coupling according to general procedure I:
[0164] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0165] Carboxylic acid: 1-Acetyl-piperidine-4-carboxylic acid (commercially available),
[0166] ES-MS m/e: 515.0 (M+H + ).
Example 3
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(1-cyclobutanecarbonyl-piperidin-4-yl)-methanone
[0167]
[0168] Coupling according to general procedure I:
[0169] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0170] Carboxylic acid: 1-Cyclobutanecarbonyl-piperidine-4-carboxylic acid (commercially available),
[0171] ES-MS m/e: 565.7 (M+H + ).
Example 4
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(1-methyl-piperidin-4-yl)-methanone
[0172]
[0173] Coupling according to general procedure I:
[0174] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0175] Carboxylic acid: 1-Methyl-piperidine-4-carboxylic acid (commercially available),
[0176] ES-MS m/e: 496.04 (M+H + ).
Example 5
{4-[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-carbamic acid methyl ester
[0177]
[0178] Coupling according to general procedure I:
[0179] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0180] Carboxylic acid: 4-Methoxycarbonylamino-cyclohexanecarboxylic acid,
[0181] ES-MS m/e: 555.72 (M+H + ).
4-Methoxycarbonylamino-cyclohexanecarboxylic acid
[0182] To a stirred solution of trans-4-amino-cyclohexanecarboxylic acid methyl ester (commercially available) in CH 2 Cl 2 was added Et 3 N (2 eq.) and methyl-chloroformate (1.05 eq.). Stirring was continued overnight at RT. The reaction was quenched by addition of H 2 O, the product was extracted with CH 2 Cl 2 and the organic phase washed with aq. HCl 1M. The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. The residue was dissolved in MeOH and a 2M KOH aq. solution was added. The reaction was stirred at RT 4 hours, aq. HCl was added until ph=6, and then the product was extracted with EtOAc. The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo to afford the title product as a white foam which was used in the next step without further purification.
Example 6
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(4-methoxymethyl-cyclohexyl)-methanone
[0183]
[0184] Coupling according to general procedure I:
[0185] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0186] Carboxylic acid: 4-Methoxymethyl-cyclohexanecarboxylic acid (described in JP60258141),
[0187] ES-MS m/e: 526.8 (M+H + ).
Example 7
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0188]
a) 4-[(3RS 4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester
[0189] To a stirred solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (0.165 g, 0.72 mmol) in 20 mL of CH 2 Cl 2 was added (0.14 g, 0.94 mmol) of EDC, (0.10 g, 0.94 mmol) of HOBt and Et 3 N (0.11 mL, 1.1 mmol). After one hour at RT, was added 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2, 0.26 g, 0.72 mmol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.29 g (91%) of the title compound as a white foam.
b) 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0190] To a stirred solution of 4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester (0.28 g, 0.50 mmol) in 24 mL of CH 2 Cl 2 was added 6 mL of TFA. After one hour at RT, the reaction was quenched by addition of aq. NaOH 1M (until ph=10) and the product was extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo to yield 0.237 g (99%) of the title compound as a white foam. ES-MS m/e: 473.0 (M+H + ).
Example 8
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-((2R,4S,5S)-3,4-dihydroxy-cyclohexyl)-methanone
[0191]
[0192] Coupling according to general procedure I:
[0193] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0194] Carboxylic acid: (1R,3S,4S)-3,4-Dihydroxy-cyclohexanecarboxylic acid (commercially available), ES-MS m/e: 513.3 (M+H + ).
Example 9
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-((2S,4S,5S)-3,4-dihydroxy-cyclohexyl)-methanone
[0195]
[0196] Coupling according to general procedure I:
[0197] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0198] Carboxylic acid: (1S,3S,4S)-3,4-Dihydroxy-cyclohexanecarboxylic acid (described in patent WO2006/016167), ES-MS m/e: 513.3 (M+H + ).
Example 10
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(4-ethynyl-cyclohexyl)-methanone
[0199]
[0200] Coupling according to general procedure I:
[0201] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0202] Carboxylic acid: 4-Ethynyl-cyclohexanecarboxylic acid (commercially available),
[0203] ES-MS m/e: 506.9 (M+H + ).
Example 11
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-1-yl]-(1-isobutyl-piperidin-4-yl)-methanone
[0204]
[0205] Coupling according to general procedure I:
[0206] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0207] Carboxylic acid: 1-Isobutyl-piperidine-4-carboxylic acid (commercially available),
[0208] ES-MS m/e: 540.3 (M+H + ).
Example 12
4-[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexanone
[0209]
[0210] Coupling according to general procedure I:
[0211] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-1)
[0212] Carboxylic acid: 4-Oxo-cyclohexanecarboxylic acid (commercially available),
[0213] ES-MS m/e: 497.0 (M+H + ).
Example 13
4-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester
[0214]
[0215] Coupling according to general procedure I:
[0216] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0217] Carboxylic acid: Piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (commercially available), ES-MS m/e: 572.7 (M+H + ).
Example 14
6-{(SR)-1-[(3RS,4SR)-1-(1-Cyclopropanecarbonyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0218]
[0219] Coupling according to general procedure I:
[0220] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0221] Carboxylic acid: Cyclopropanecarboxylic acid (commercially available), ES-MS m/e: 540.9 (M+H + ).
Example 15
{(3SR,4RS)-3-(3,4-Dichloro-phenyl)-4-[(SR)-1-(5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-(tetrahydro-pyran-4-yl)-methanone
[0222]
[0223] Coupling according to general procedure I:
[0224] Pyrrolidine intermediate: 2-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine (VII-B-3)
[0225] Carboxylic acid: Tetrahydro-pyran-4-carboxylic acid (commercially available), ES-MS m/e: 517.3 (M+H + ).
Example 16
6-{(SR)-1-[(3RS,4SR)-1-[1-(1-Cyano-cyclopropanecarbonyl)-piperidine-4-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0226]
[0227] Coupling according to general procedure I:
[0228] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0229] Carboxylic acid: 1-Cyano-cyclopropanecarboxylic acid (commercially available), ES-MS m/e: 566.4 (M+H + ).
Example 17
6-((SR)-1-{(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-[1-(1-methyl-cyclopropanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile
[0230]
[0231] Coupling according to general procedure I:
[0232] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0233] Carboxylic acid: 1-Methyl-cyclopropanecarboxylic acid (commercially available),
[0234] ES-MS m/e: 555.2 (M+H + ).
Example 18
6-((SR)-1-{(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-[1-(2,2-difluoro-cyclopropanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile
[0235]
[0236] Coupling according to general procedure I:
[0237] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0238] Carboxylic acid: 2,2-Difluoro-cyclopropanecarboxylic acid (commercially available),
[0239] ES-MS m/e: 577.3 (M+H + ).
Example 19
6-{(SR)-1-[(3RS,4SR)-1-[1-(1-Amino-cyclopropanecarbonyl)-piperidine-4-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0240]
[0241] Coupling according to general procedure I:
[0242] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0243] Carboxylic acid: 1-Amino-cyclopropanecarboxylic acid (commercially available),
[0244] ES-MS m/e: 556.2 (M+H + ).
Example 20
6-{(SR)-1-[(3RS,4SR)-1-(1-Cyclobutanecarbonyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0245]
[0246] Coupling according to general procedure I:
[0247] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0248] Carboxylic acid: Cyclobutanecarboxylic acid (commercially available),
[0249] ES-MS m/e: 555.2 (M+H + ).
Example 21
6-((SR)-1-{(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-[1-(3-oxo-cyclobutanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile
[0250]
[0251] Coupling according to general procedure I:
[0252] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0253] Carboxylic acid: 3-Oxo-cyclobutanecarboxylic acid (commercially available),
[0254] ES-MS m/e: 569.3 (M+H + ).
Example 22
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(1-propionyl-piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0255]
[0256] Coupling according to general procedure II:
[0257] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0258] Acid chlorid: Propionyl chloride (commercially available),
[0259] ES-MS m/e: 529.2 (M+H + ).
Example 23
6-{(SR)-1-[(3RS,4SR)-1-[1-(2-Cyano-acetyl)-piperidine-4-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0260]
[0261] Coupling according to general procedure I:
[0262] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0263] Carboxylic acid: Cyano-acetic acid (commercially available),
[0264] ES-MS m/e: 540.3 (M+H + ).
Example 24
6-((SR)-1-{(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-[1-(2-methoxy-acetyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile
[0265]
[0266] Coupling according to general procedure II:
[0267] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0268] Acid chlorid: Methoxy-acetyl chloride (commercially available),
[0269] ES-MS m/e: 545.2 (M+H + ).
Example 25
6-{(SR)-1-[(3RS,4SR)-1-(1-Acetyl-azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0270]
[0271] Coupling according to general procedure II:
[0272] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-2)
[0273] Acid chlorid: Acetyl chloride (commercially available),
[0274] ES-MS m/e: 487.3 (M+H + ).
Example 26
6-{(SR)-1-[(3RS,4SR)-1-(1-Cyclopropanecarbonyl-azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0275]
[0276] Coupling according to general procedure I:
[0277] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-2)
[0278] Carboxylic acid: Cyclopropanecarboxylic acid (commercially available),
[0279] ES-MS m/e: 513.4 (M+H + ).
Example 27
6-{(SR)-1-[(3RS,4SR)-1-[1-(1-Cyano-cyclopropanecarbonyl)-azetidine-3-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0280]
[0281] Coupling according to general procedure I:
[0282] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-2)
[0283] Carboxylic acid: 1-Cyano-cyclopropanecarboxylic acid (commercially available),
[0284] ES-MS m/e: 538.3 (M+H + ).
Example 28
6-{(SR)-1-[(3RS,4SR)-1-[1-(2-Cyano-acetyl)-azetidine-3-carbonyl]-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0285]
[0286] Coupling according to general procedure I:
[0287] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-2)
[0288] Carboxylic acid: Cyano-acetic acid (commercially available),
[0289] ES-MS m/e: 512.4 (M+H + ).
Example 29
3-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-azetidine-1-carboxylic acid tert-butyl ester
[0290]
[0291] Coupling according to general procedure I:
[0292] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0293] Carboxylic acid: Azetidine-1,3-dicarboxylic acid mono-tert-butyl ester (commercially available), ES-MS m/e: 545.3 (M+H + ).
Example 30
6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0294]
a) 3-[(3R,4S)-3-[(S)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-azetidine-1-carboxylic acid tert-butyl ester
[0295] To a stirred solution of azetidine-1,3-dicarboxylic acid mono-tert-butyl ester (0.072 g, 0.36 mmol) in 15 mL of CH 2 Cl 2 was added (0.069 g, 0.36 mmol) of EDC, (0.048 g, 0.36 mmol) of HOBt and Et 3 N (0.06 mL, 0.42 mmol). After one hour at RT, was added 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2, 0.10 g, 0.27 mmol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 0.14 g (98%) of the title compound as a white solid.
b) 6-{(SR)-1-[(3RS,4SR)-1-(Azetidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-2)
[0296] To a stirred solution of 3-[(3R,4S)-3-[(S)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-azetidine-1-carboxylic acid tert-butyl ester (0.14 g, 0.25 mmol) in 4 mL of CH 2 Cl 2 was added 1 mL of TFA. After one hour at RT, the reaction was quenched by addition of aq. NaOH 1M (until ph=10) and the product was extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo to yield 0.106 g (92%) of the title compound as a white foam. ES-MS m/e: 445.1 (M+H + ).
Example 31
{(3SR,4RS)-3-(3,4-Dichloro-phenyl)-4-[(SR)-1-(5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-(1-methyl-piperidin-4-yl)-methanone
[0297]
[0298] Coupling according to general procedure I:
[0299] Pyrrolidine intermediate: 2-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine (VII-B-3)
[0300] Carboxylic acid: 1-Methyl-piperidine-4-carboxylic acid (commercially available),
[0301] ES-MS m/e: 529.9 (M+H + ).
Example 32
3-[(3RS,4SR)-3-[(SR)-1-((S)-5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-pyrrolidine-1-carboxylic acid tert-butyl ester
[0302]
[0303] Coupling according to general procedure I:
[0304] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0305] Carboxylic acid: (S)-Pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester (commercially available), ES-MS m/e: 558.7 (M+H + ).
Example 33
3-[(3RS,4SR)-3-[(SR)-1-((R)-5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-pyrrolidine-1-carboxylic acid tert-butyl ester
[0306]
[0307] Coupling according to general procedure I:
[0308] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0309] Carboxylic acid: (R)-Pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester (commercially available), ES-MS m/e: 558.7 (M+H + ).
Example 34
6-{(SR)-1-[(3RS,4SR)-1-(1-Cyanomethyl-piperidine-4-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0310]
[0311] To a stirred solution of 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1) (25 mg, 0.053 mmol) in THF (2 mL) was added NaH (2.4 mg, 55% purity, 0.056 mmol). After 10 min. 2-iodo acetonitrile (13 mg, 0.079 mmol) was added and stirring was continued at RT overnight.
[0312] The reaction was quenched with H 2 O, and the product extracted with EtOAc. The combined organic phases were dried over Na 2 SO 4 , concentrated under vacuo and the residue was purified by column chromatography (SiO 2 , CH 2 Cl 2 /MeOH 9/1) to yield 20 mg (74%) of the title compound as a light brown foam. ES-MS m/e: 512.0 (M+H + ).
Example 35
4-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid methyl ester
[0313]
[0314] Coupling according to general procedure II:
[0315] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0316] Chloroformate: Methyl chloroformate (commercially available), ES-MS m/e: 531.6 (M+H + ).
Example 36
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(pyrrolidine-3-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0317]
[0318] To a stirred solution of 3-[(3RS,4SR)-3-[(SR)-1-((S)-5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-pyrrolidine-1-carboxylic acid tert-butyl ester (described herein above) (80 mg, 0.140 mmol) in CH 2 Cl 2 (4 mL) was added TFA (1 mL). Stirring was continued at RT for 1 hour, and an aqueous solution of NaHCO 3 was added (until ph=8). The product was extracted with CH 2 Cl 2 and the combined organic phase dried over Na 2 SO 4 . Concentration under vacuo afforded 64 mg (97%) of the title compound as a white solid. ES-MS m/e: 459.1 (M+H + ).
Example 37
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(pyrrolidine-3-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0319]
[0320] To a stirred solution of 3-[(3RS,4SR)-3-[(SR)-1-((R)-5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-pyrrolidine-1-carboxylic acid tert-butyl ester (described herein above) (80 mg, 0.140 mmol) in CH 2 Cl 2 (4 mL) was added TFA (1 mL). Stirring was continued at RT for 1 hour, and an aqueous solution of NaHCO 3 was added (until ph=8). The product was extracted with CH 2 Cl 2 and the combined organic phase dried over Na 2 SO 4 . Concentration under vacuo afforded 62 mg (94%) of the title compound as a white solid. ES-MS m/e: 459.1 (M+H + ).
Example 38
6-{(SR)-1-[(3RS,4SR)-1-(1-Acetyl-pyrrolidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0321]
[0322] Coupling according to general procedure II:
[0323] Intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-dichloro-phenyl)-1-(pyrrolidine-3-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (described hereinabove)
[0324] Acid chlorid: Acetyl chloride (commercially available), ES-MS m/e: 500.9 (M+H + ).
Example 39
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(1-methanesulfonyl-piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0325]
[0326] Coupling according to general procedure II:
[0327] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(piperidine-4-carbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VIII-B-1)
[0328] Sulfonyl chlorid: Methanesulfonyl chloride (commercially available),
[0329] ES-MS m/e: 551.6 (M+H + ).
Example 40
6-{(SR)-1-[(3RS,4SR)-1-(1-Acetyl-piperidine-3-carbonyl)-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0330]
[0331] Coupling according to general procedure I:
Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0333] Carboxylic acid: 1-Acetyl-piperidine-3-carboxylic acid (commercially available),
[0334] ES-MS m/e: 515.2 (M+H + ).
Example 41
3-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-piperidine-1-carboxylic acid tert-butyl ester
[0335]
[0336] Coupling according to general procedure I:
[0337] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0338] Carboxylic acid: Piperidine-1,3-dicarboxylic acid 1-tert-butyl ester (commercially available),
[0339] ES-MS m/e: 573.2 (M+H + ).
Example 42
{4-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-methyl-carbamic acid tert-butyl ester
[0340]
[0341] Coupling according to general procedure I:
[0342] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0343] Carboxylic acid: trans-4-(tert-Butoxycarbonyl-methyl-amino)-cyclohexanecarboxylic acid (described in US20050065210), ES-MS m/e: 601.3 (M+H + ).
Example 43
{4-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-carbamic acid tert-butyl ester
[0344]
[0345] Coupling according to general procedure I:
[0346] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0347] Carboxylic acid: trans-4-tert-Butoxycarbonylamino-cyclohexanecarboxylic acid (commercially available), ES-MS m/e: 587.2 (M+H + ).
Example 44
6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-(4-methylamino-cyclohexanecarbonyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0348]
[0349] To a stirred solution of {4-[(3RS,4SR)-3-[(SR)-1-(5-cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-methyl-carbamic acid tert-butyl ester described herein above (30 mg, 0.050 mmol) in CH 2 Cl 2 (4 mL) was added TFA (1 mL). After 1 hour, aqueous NaHCO 3 was added until ph=8, the product was extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 to give the title product as a colorless oil (25 mg, 98%). ES-MS m/e: 500.9 (M+H + ).
Example 45
N-{4-[(3RS,4SR)-3-[(SR)-1-(5-Cyano-pyridin-2-yloxy)-ethyl]-4-(3,4-dichloro-phenyl)-pyrrolidine-1-carbonyl]-cyclohexyl}-N-methyl-acetamide
[0350]
[0351] Coupling according to general procedure I:
[0352] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0353] Carboxylic acid: 4-(Acetyl-methyl-amino)-cyclohexane carboxylic acid (described in JP2006298909), ES-MS m/e: 542.9 (M+H + ).
Example 46
1-(4-{(3SR,4RS)-3-(3,4-Dichloro-phenyl)-4-[(SR)-1-(5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidine-1-carbonyl}-piperidin-1-yl)-ethanone
[0354]
[0355] Coupling according to general procedure I:
[0356] Pyrrolidine intermediate: 2-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-5-trifluoromethyl-pyridine (VII-B-3)
[0357] Carboxylic acid: 1-Acetyl-piperidine-4-carboxylic acid (commercially available),
[0358] ES-MS m/e: 558.1 (M+H + ).
Example 47
6-((SR)-1-{(3RS,4SR)-4-(3,4-Dichloro-phenyl)-1-[1-(1-methyl-cyclopropanecarbonyl)-piperidine-4-carbonyl]-pyrrolidin-3-yl}-ethoxy)-nicotinonitrile
[0359]
[0360] Coupling according to general procedure I:
[0361] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(3,4-Dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-2)
[0362] Carboxylic acid: 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid (described herein after), ES-MS m/e: 592.0 (M+H + ).
1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
a) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester
[0363] To a stirred solution of 1-methyl-cyclopropanecarboxylic acid (14.4 g, 0.144 mol) in 200 mL of CH 2 Cl 2 was added (27.10 g, 0.141 mol) of EDC, (19.10 g, 0.141 g) of HOBt and Et 3 N (35.93 mL, 0.259 mol). After one hour at RT, was added piperidine-4-carboxylic acid ethyl ester (18.90 g, 0.120 mol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 26.1 g (92%) of the title compound as a light yellow oil.
b) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
[0364] To a stirred solution of 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester (26.09 g, 0.109 mol) in 500 mL of a mixture of THF, EtOH and H 2 O) (1/1/1) was added LiOH.H 2 O) (6.86 g, 0.163 mol). After one hour at RT, the solvent were evaporated and the residue taken up in CH 2 Cl 2 and the organic phase was washed with aqueous HCl 1M. The organic phases were dried over Na 2 SO 4 and evaporated under vacuo to gave 19.8 g (86%) of the title compound as a white solid. ES-MS m/e: 212.1 (M+H + ).
Example 48
[(3RS,4SR)-3-[(SR)-1-(5-Chloro-pyridin-2-yloxy)-ethyl]-4-(2,4-difluoro-phenyl)-pyrrolidin-1-yl]-[1-(1-methyl-cyclopropanecarbonyl)-piperidin-4-yl]-methanone
[0365]
[0366] Coupling according to general procedure I:
[0367] Pyrrolidine intermediate: 5-Chloro-2-{(SR)-1-[(3RS,4SR)-4-(2,4-difluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-4)
[0368] Carboxylic acid: 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid (described herein after), ES-MS m/e: 532.2 (M+H + ).
1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
a) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester
[0369] To a stirred solution of 1-methyl-cyclopropanecarboxylic acid (14.4 g, 0.144 mol) in 200 mL of CH 2 Cl 2 was added (27.10 g, 0.141 mol) of EDC, (19.10 g, 0.141 g) of HOBt and Et 3 N (35.93 mL, 0.259 mol). After one hour at RT, was added piperidine-4-carboxylic acid ethyl ester (18.90 g, 0.120 mol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 26.1 g (92%) of the title compound as a light yellow oil.
b) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
[0370] To a stirred solution of 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester (26.09 g, 0.109 mol) in 500 mL of a mixture of THF, EtOH and H 2 O) (1/1/1) was added LiOH.H 2 O) (6.86 g, 0.163 mol). After one hour at RT, the solvent were evaporated and the residue taken up in CH 2 Cl 2 and the organic phase was washed with aqueous HCl 1M. The organic phases were dried over Na 2 SO 4 and evaporated under vacuo to gave 19.8 g (86%) of the title compound as a white solid. ES-MS m/e: 212.1 (M+H + ).
Example 49
6-{(SR)-1-[(3RS,4SR)-1-(1-Acetyl-piperidine-4-carbonyl)-4-(4-cyano-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
[0371]
[0372] Coupling according to general procedure I:
[0373] Pyrrolidine intermediate: 6-{(SR)-1-[(3RS,4SR)-4-(4-Cyano-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile (VII-B-5)
[0374] Carboxylic acid: 1-Acetyl-piperidine-4-carboxylic acid (commercially available),
[0375] ES-MS m/e: 472.3 (M+H + ).
Example 50
4-{(3SR,4RS)-1-(1-Acetyl-piperidine-4-carbonyl)-4-[(SR)-1-(5-trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile
[0376]
[0377] Coupling according to general procedure I:
[0378] Pyrrolidine intermediate: 4-{(3SR,4RS)-4-[1-((SR)-5-Trifluoromethyl-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VII-B-6)
[0379] Carboxylic acid: 1-Acetyl-piperidine-4-carboxylic acid (commercially available),
[0380] ES-MS m/e: 515.3 (M+H + ).
Example 51
4-{(3SR,4RS)-1-(1-Acetyl-piperidine-4-carbonyl)-4-[(SR)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile
[0381]
[0382] Coupling according to general procedure I:
[0383] Pyrrolidine intermediate: 4-{(3SR,4RS)-4-[1-((SR)-5-Chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-3-yl}-benzonitrile (VII-B-7)
[0384] Carboxylic acid: 1-Acetyl-piperidine-4-carboxylic acid (commercially available),
[0385] ES-MS m/e: 481.2 (M+H + ).
Example 52
{(3S,4R)-3-(4-Chloro-phenyl)-4-[(S)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-[1-(1-methyl-cyclopropanecarbonyl)-piperidin-4-yl]-methanone
[0386]
[0387] Coupling according to general procedure I:
[0388] Pyrrolidine intermediate: 5-Chloro-2-{(S)-1-[(3R,4S)-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-8)
[0389] Carboxylic acid: 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid (described herein after),
[0390] ES-MS m/e: 530.1 (M+H + ).
1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
a) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester
[0391] To a stirred solution of 1-methyl-cyclopropanecarboxylic acid (14.4 g, 0.144 mol) in 200 mL of CH 2 Cl 2 was added (27.10 g, 0.141 mol) of EDC, (19.10 g, 0.141 g) of HOBt and Et 3 N (35.93 mL, 0.259 mol). After one hour at RT, was added piperidine-4-carboxylic acid ethyl ester (18.90 g, 0.120 mol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 26.1 g (92%) of the title compound as a light yellow oil.
b) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
[0392] To a stirred solution of 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester (26.09 g, 0.109 mol) in 500 mL of a mixture of THF, EtOH and H 2 O) (1/1/1) was added LiOH.H 2 O) (6.86 g, 0.163 mol). After one hour at RT, the solvent were evaporated and the residue taken up in CH 2 Cl 2 and the organic phase was washed with aqueous HCl 1M. The organic phases were dried over Na 2 SO 4 and evaporated under vacuo to gave 19.8 g (86%) of the title compound as a white solid. ES-MS m/e: 212.1 (M+H + ).
Example 53
{(3S,4R)-3-(4-Chloro-3-fluoro-phenyl)-4-[(S)-1-(5-chloro-pyridin-2-yloxy)-ethyl]-pyrrolidin-1-yl}-[1-(1-methyl-cyclopropanecarbonyl)-piperidin-4-yl]-methanone
[0393]
[0394] Coupling according to general procedure I:
[0395] Pyrrolidine intermediate: 5-Chloro-2-{(S)-1-[(3R,4S)-4-(4-chloro-3-fluoro-phenyl)-pyrrolidin-3-yl]-ethoxy}-pyridine (VII-B-9)
[0396] Carboxylic acid: 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid (described herein after), ES-MS m/e: 548.2 (M+H + ).
1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
a) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester
[0397] To a stirred solution of 1-methyl-cyclopropanecarboxylic acid (14.4 g, 0.144 mol) in 200 mL of CH 2 Cl 2 was added (27.10 g, 0.141 mol) of EDC, (19.10 g, 0.141 g) of HOBt and Et 3 N (35.93 mL, 0.259 mol). After one hour at RT, was added piperidine-4-carboxylic acid ethyl ester (18.90 g, 0.120 mol). The mixture was stirred at RT over night and then poured onto water and extracted with CH 2 Cl 2 . The combined organic phases were dried over Na 2 SO 4 and concentrated under vacuo. Column chromatography (SiO 2 , EtOAc/H, 1:1) yielded 26.1 g (92%) of the title compound as a light yellow oil.
b) 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid
[0398] To a stirred solution of 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester (26.09 g, 0.109 mol) in 500 mL of a mixture of THF, EtOH and H 2 O) (1/1/1) was added LiOH.H 2 O) (6.86 g, 0.163 mol). After one hour at RT, the solvent were evaporated and the residue taken up in CH 2 Cl 2 and the organic phase was washed with aqueous HCl 1M. The organic phases were dried over Na 2 SO 4 and evaporated under vacuo to gave 19.8 g (86%) of the title compound as a white solid. ES-MS m/e: 212.1 (M+H + ).
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The present invention relates to compounds of formula I
wherein R 1 , R 2 , R 3 , R′, Ar, m, n, and o are as defined herein. The invention also relates to pharmaceutical compositions containing compounds of formula I and methods for the manufacture of such compounds and compositions. Compounds of the invention are high potential NK-3 receptor antagonists for the treatment of depression, pain, psychosis, Parkinson's disease, schizophrenia, anxiety and attention deficit hyperactivity disorder (ADHD).
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This is a division of application Ser. No. 753,481 filed July 10, 1985, now U.S. Pat. No. 4,665,468.
BACKGROUND OF THE INVENTION
This invention relates to a module having a wired substrate and a multi-layer circuit overlaid on the substrate and a method of manufacturing the same.
The technique for realizing many LSI chips mounted on a ceramic wired substrate, the so-called multi-chip technique, has developed into the mounting technique which predominates for large scale and high speed digital systems, such as large scale computers and the like. In addition, remarkable progress in the technique of fabricating the multi-layer substrate used above has been achieved.
Various structures are already known for a high density multi-layer wired substrate. In U.S. Pat. No. 4,245,273 issued to Feinberg et al., a multi-layer substrate is formed by the method of green sheets. On the surface of green sheets, the patterns of a signal wire layer, a power source layer and a connecting layer is made by a printing method. Then all the green sheets are mounted together and the multi-layer substrate is formed by a one time sintering. This manufacturing method is, however, not suitable for fine geometry processing.
To solve this problem, a multi-layer ceramic substrate supporting thin-film lines and a VLSI chip is proposed in the technical article by C. W. Ho et al. entitled "The Thin-Film Module as a High-Performance Semiconductor Package" and appearing in IBM J. RES. DEVELOP., Vol 26, No. 3, May 1982, pp. 286-296. The module in this article does not necessarily provicde fine geometry processing on the ceramic multi-layer substrate since the multi-layer wire matrix instead can be used to obtain fine and individual patterns. One problem in such a multi-layer substrate is that the rate of contraction by sintering during the manufacturing process of the ceramic multi-layer substrate varies widely. Accordingly, a gap often occurs between the pattern for connecting to the ceramic multi-layer substrate and the pattern for connecting to the multi-layer wire matrix. Thus a defective connection can easily occur.
On the other hand, in the U.S. Pat. No. 4,245,273 and the article mentioned above, a ceramic is used for the substrate. A ceramic, for example, alumina green sheet, requires a sintering temperature of more than 1400° C. thus prompting the use of high melting point metals like tungsten or molybdenum etc. as a conductive material. The inherent electric resistivity of such a metal is higher than that of metals like gold, silver, or palladium. As a result, the problem arises that it is difficult to reduce the value of the power wire resistance in the ceramic substrate. Furthermore, in the case that the multi-layer wire matrix is formed on top of the ceramic substrate, when tungsten or molybdenum is sintered in air at more than 400° C., the tungsten or molybdenum is oxidized and thus cannot be used as a conductive layer. Accordingly, the process and material for manufacturing multi-layer wire matrices are greatly limited.
Furthermore, for the multi-layer wire matrix, an insulting layer is inserted between upper and lower conductive layers. The electric connection between the upper conductive layer and the lower conductive layer is realized by forming the upper conductive layer on the side of a via hole formed in the insulating layer and the via hole directly connects the upper and lower conductive layers. However, in the multi-layer wire substrate, the thickness of the portion of upper conductive layer at the corner between the upper surface of the insulating layer and the side of the via hold is reduced and becomes so thin that a portion of the upper conductive layer is likely to be cut off from the conductive layer in the via hole.
Next is described a method for fixing a defective portion. A test of the defective signal wire line is possible either at the time of completing the printing of the green sheet or of completing the fabricating of a multi-layer substrate. The check at the completion of printing of the green sheet can be performed optically but an electrical check is impossible because the green sheet is not conductive before sintering. When the multi-layer substrate is completed it is possible to check electrically. However, fixing the defect is not possible in an interior layer of the completed substrate, and it is thus necessary to fix the defect from outside of the substrate. One example of this technique is proposed in an article contributed by Bernard T. Clark et al. to IEEE TRANSACTIONS ON COMPONENTS, HYBRIDS, AND MANUFACTURING TECHNOLOGY, Vol. CHMT-3, No. 1, March 1980, pp. 89-93, under the title of "IBM Multi-Chip Multi-layer Ceramic Modules for LSI Chips--Design for Performance and Density". In the article, fixing of this kind of substrate is done by wiring to pads of a connecting layer on the surface of the substrate. Such a method causes the problems that the reliability of connection is degraded, the number of fixing lines are increased, a great amount of labor for wiring is needed, and the area for mounting elements is reduced by preparing the area for wiring.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a multi-layer substrate which is able to avoid the defective connections caused by the variation of the rate of contraction.
It is another object of this invention to provide a multi-layer substrate which is free from the limitation of the prior manufacturing process and materials.
It is still another object of this invention to provide a multi-layer substrate which is free from the cut-off of the wire line corresponding to the via hole.
It is a further object of this invention to provide a more reliable multi-layer substrate.
According to one feature of the present invention, there is provided a multi-layer substrate comprising a ceramic multi-layer. The conductive layer covers the through hole on the surface of the substrate. A multi-layer wire matrix is formed on the conductive layer and the substrate.
According to another feature of the present invention, there is provided a multi-layer substrate with a multi-layer wire matrix comprising an upper conductive layer and a lower conductive layer. The insulating layer is located between the upper and lower conductive layers and has a via hole which is metal plated.
According to still another feature of the present invention, the steps of forming the multi-layer substrate comprise the steps of forming a ceramic multi-layer substrate by sintering the green sheet laminating substrate having through hole wiring, forming a conductive layer on the surface of the ceramic multi-layer substrate, and forming an insulating layer so that it covers the desired portion of the conductive layer and the desired portion of the surface of the ceramic multi-layer substrate.
According to yet another feature of the present invention, there are provided the steps of forming an insulating layer with the via hole corresponding to the desired portion of the lower conductive layer, filling up the via hole with the metal for electrically connection to the lower conductive layer by plating, and then forming an upper conductive layer for electrically connecting to the filled up via hole.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic vertical sectional view of a module according to a first embodiment of the present invention.
FIGS. 2A to 2E show in schematic vertical section, steps of manufacturing the module depicted in FIG. 1;
FIGS. 3 and 4 are schematic vertical sectional views of a module according to a second embodiment of the present invention;
FIGS. 5A-5F, show in schematic vertical section, the steps of manufacturing the module depicted in FIGS. 3 and 4;
FIG. 6 is a schematic vertical sectional view of a module according to a third embodiment of the present invention;
FIGS. 7A-7C show, in schematic vertical section, one example of the steps of manufacturing the module depicted in FIG. 6;
FIG. 8 shows, in schematic vertical section, another example of the steps of manufacturing the module depicted in FIG. 6;
FIGS. 9A-9C show, in schematic vertical section, one example of the steps of fixing the module; and
FIGS. 10A and 10B show, in schematic vertical section, another example of the steps of fixing the module.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, a module according to a first embodiment of the present invention comprises a ceramic multi-layer substrate 10 and a multi-layer wire line matrix 19. The ceramic multi-layer substrate 10 has three alumina substrates 11, on respective ones of which inner power and ground layers 12 are printed with a paste made of molybdenum or tungsten, and then they are fired and sintered after lamination of all the alumina substrates 11. There are several methods to form metal connecting pads 16. For example, the metal pads 16 can be formed by evaporation or sputtering, or plating the metal on top of already evaporated or sputtered metal. Also, there is the thick film method. In this embodiment, the shape of the metal connecting pad 16 is a disk of 1 mm diameter, and comprises a titanium layer of 0.1 μm thickness and a palladium layer of 3 μm thickness. Chromium, aluminum, or nickel can be used in place of titanium or palladium. Insulating layers 17 are formed on the surface of the substrate having the metal connecting pad 16. The insulating layers 17 and wire lines 18 are laminated on the other insulating layers 17 and wire lines 18, respectively, so that a multi-layer wired line matrix 19 is formed. In this embodiment, the material of the insulating layers 17 is polyimide and the principal ingredient of the material of the wire lines 18 is gold (Au). The thickness of each of the insulating layers 17 is 15 μm, and the thickness of each layer of the wire line 18 is 5 μm. The area of the via hole formed in the insulating layer 17 is square and 40 μm on a side. The minimum width of a pattern of a wire line 18 is 20 μm.
The advantage of this embodiment is as follows. First, the variability of location caused by the variation of the rate of contraction of the ceramic multi-layer substrate 10 is allowed for by use of the large metal connecting pad and this connection defect is prevented. Furthermore, it is not necessary to enlarge the diameter of the through hole 13. For example, in the case of a large substrate of 100 μm on a side, the filling up of the through hole 13 of the ceramic multi-layer substrate 10 is easily performed so that the via portion is easily formed.
Next, as the diameter of the through hole 13 can be reduced, the remaining area of the substrate 10 can be usefully and densely used for interior power and ground layers 12. Then, as the metal connecting pad 16 is formed to cover the through hole 13 of the substrate 10, the subsequent steps for manufacturing thin film do not affect the metal of the through holes 13, so that it can be protected within the interior for increased reliability.
Also, as polyimide is used as the insulating material between layers of thin film wire matrix 19 and since titanium, chromium, aluminum, nickel or palladium is used as the material of the metal pad 16, the embodiment can obtain high connection reliability and high insulation between layers.
Now, the manufacturing method of the first embodiment mentioned above will be explained with reference to FIGS. 2A-2E. Referring to FIG. 2A, the ceramic multi-layer substrate 10 is formed by the normal green sheet method, here illustrated with six green sheets 11. After the inner power and ground layers 12 and the metal of the through hole 13 are formed on the desired sheets of the six sheets of green sheet alumina substrate 11, all the sheets 11 are laminated. After that, the sheets 11 are fired and sintered in a reducing atmosphere at more than 1400° C. A thick film paste of tungsten or molybdenum is used as the material of the inner power and ground layers 12 and the metal of the through hole 13. Next, lands 14 are fixed to the reverse side of the substrate 10, and the pins 15 are fixed on each of the lands 14 by silver solder.
Next, the formation of the multi-layer wired matrix on the substrate wall be explained. There are two problems in this formation. One problem is the possible undulation of the surface of the substrate 10, and the other problem is that the pitch of the through holes is different from one another in each of the substrates.
The two problems obstruct the formation of the multi-layer wire matrix. Referring to FIG. 2B, to solve the first problem, the surface of the substrate 10 is polished to be flat and then the metal connection pad 16 is formed. In the case that the maximum distance from the edge of one through hole 13 to the edge of another through hole 13 is 100 mm (the lateral dimension of the entire module) and the variation of the rate of contraction by sintering is ±0.5%, the variation of the maximum distance between through holes 13 is ±0.5 μm. In this embodiment, to take this variation into account, the diameter of the metal connecting pad 16 is set to 1 mm. The pad 16 is formed by an etching method after titanium of 0.1 μm and palladium of 3 μm are deposited by sputtering on top of the substrate 10.
Referring to FIG. 2C, a pre-polyimide varnish 17A is coated on the substrate 10 including the pads 16. The coating can be accomplished by a spray method or a spin coating method. The thickness of varnish 17A is about 20 μm. In this embodiment, photonese sold by Toray is used as the pre-polyimide varnish 17A. As the varnish is photosensitive, it is not necessary to use photo-resist in the following step for forming a via-hole.
Referring to FIG. 2D, after the coated varnish 17A is dried at 60° C. for sixty minutes, the varnish 17A is exposed and developed, so that via holes 17B are formed. Next, the pre-polyimide varnish 17A is cured under the condition that a first thirty minutes of curing are at 200° C. and a second thirty minutes are at 400° C. As a result, a polyimide insulating layer 17 with via holes 17B is established. The thickness of the insulating layer 17 is 15 μm.
Then a conductive layer 18 is formed into the via holes 17B and on top of the insulating layer 17. For example, after chromium of 0.1 μm and palladium of 0.2 μm thickness is formed by a sputtering method, gold is selectively plated on the desired portion of the gold pattern. The thickness of the gold plating is, for example, 15 μm in the via holes, and 5 μm on the insulating layer. The minimum width of the via hole 17B is 40 μm and the minimum width of the wire line 18 is 20 μm.
Referring to FIG. 2E, after forming the conductive layer 18, another polyimide insulating layer 17C is formed. This step is repeated, so that the multi-layer wire matrix 19 is formed on the substrate 10 having the pins 15. In the described embodiment although polyimide is used as an organic resin, instead an epoxy resin, Teflon sold by Du Pont, melamine resin, or phenol resin could be used as the organic resin in this invention.
A second embodiment of the present invention will now be explained with reference to FIG. 3.
FIG. 3 shows the glass-ceramic substrate, which can be fired and sintered at less than 1400° C., and corresponds to the substrate example of the present invention. FIG. 3 illustrates a glass ceramic substrate 1, including a first power wire line layer 101, a second power wire line layer 102 and a surface layer 103. Terminals 104 are connected through first through holes 105 in the first power wire layer 101. Second through holes 106 and third through holes 107 pierce other layers. Surface exposed parts 108 of the third through holes 107 appear at the surface. The through holes 105, 106 and 107 pierce respective green sheets 109, 110 and 111, which are laminated during the manufacture of the glass ceramic substrate 1. The glass ceramic substrate 1 can be fired and sintered at less than 1400° C. in air. The green sheets 109, 110 and 111 of the substrate 1 can be made from the inorganic composition shown in Japanese Kokai No. 57-17474, published on Jan. 29, 1982.
Referring to FIG. 4, a multi-layer wire line matrix 2 uses inorganic insulating material made from photo-sensitive insulating paste and comprises a first inorganic insulating layer 201, a second inorganic insulating layer 202, a first via hole wire line 204, a second wire line 206 and a third wire line 207. The wire line matrix 2 is formed on the ceramic substrate 1 because the terminal 104 on the substrate is connected to the terminals of power on a number of IC chips, and the wire line matrix 2 interconnects this number of IC chips mounted on its surface. The first via holes 203 are provided for connecting the first wire lines 204 with selected second wire lines 206. Each of the second via holes 205 is provided for connecting each of the second wire lines 206 with selected ones the third wire lines 207. Each of the first wire lines 204 connects each of the exposed parts 108 of the through hole wire lines in the ceramic substrate 1 with a corresponding first via hole wire line 203. The wiring paste and the photo-sensitive insulating paste, which can be fired and sintered at 700° C. to 900° C. are used to form the inorganic wire line matrix 2.
The reason for manufacturing according to the above method is as follows. The ceramic substrate 1 is made by printing the conductor made of high melting point metal, for example, tungsten, on the alumina green sheet 105, 106 or 107 and firing and sintering at 1400° C. in a reducing atmosphere. Thus such a substrate is made from a material which is easily oxidized, like tungsten or molybdenum. Accordingly, it is impossible to form the wire line matrix 2 and its insulating layers 201 and 202 by sintering in oxidizing air on the already sintered substrate. On the other hand, when the glass ceramic substrate 1 according to the present invention is used for the main component, the substrate 1 itself is fired and sintered at 700° C. to 900° C. in air. After that, it is possible to attach the insulating layers 201 and 202 and the wire lines 204, 206 and 207 in air.
The signal wire lines 204, 206 and 207 in the module are made according to the present invention by a thin film technique. The reason is because the thin film technique is able to form the wire line with finer geometry than that available with a thick film, so that a higher number of wire lines can be realized with many fewer wire line layers. For example, the thin film wire line is formed by a plating technique of gold wiring incorporating photo-lithography, after titanium and palladium are formed by sputtering as a base metal thick film. For such a line, a material, such as gold, of low electrical resistance which is unoxidized in the sintering process in air, can be used. As a result, the wire line has an advantage that its time constant and signal transmission delay can be reduced. For making the best use of the advantage of such a thin film wiring technique, the via hole of the insulating layer must be also made of fine geometry.
In this invention a photo-sensitive insulating paste is used for the following reason. If this photo-sensitive material is used, photo-lithographic techniques can be used for forming the via holes. Accordingly, it is possible to form the via hole, the size of which is 20% to 25% of the size of a via hole made by normal screen printing. The step of firing and sintering in air is necessary for burning out completely the photo-sensitive element used in the photo-sensitive insulating paste. In this embodiment, because the gold, silver or palladium alloy can be used as a conductive material, it is possible to eliminate the photo-sensitive element. The main component of the glass ceramic is SiO 2 and Al 2 O 3 , while secondary components include PbO, B 2 O 3 , BaO, CaO, ZnO and MgO.
Next, the manufacturing method for the second embodiment mentioned above will be explained. Referring to FIG. 5A, the glass ceramic substrate 1 is formed. For example, the inorganic composition shown in Japanese Kokai No. 57-17474 is used as the material of the substrate 1. First the holes for through holes 105, 106 and 107 are punched into each of the green sheets 109, 110, 111. A thick film conductive paste, including gold, silver or palladium alloy as its main component, is filled into the through hole punched in each of the sheets. Next, the first power wire line layer 101 is printed on the surface of the green sheet 109 and the pad for forming the terminal 104 is printed on the reverse side of the green sheet 109. The second power wire line layer 102 is printed on the surface of the green sheet 110. Next, all the green sheets 109-111 are laminated after registering and then forced together with a press. After that, the laminated green sheets are fired and sintered at 700° C. to 900° C. in air. In this step, the ceramic substrate 1 is formed from the green sheets 109-111, and the conductive paste is fired to form wire lines in the through holes 105 to 107. The exposed parts 108 of the through hole wire lines 107 are formed on the surface and reverse side of the ceramic substrate 1. The front and back surfaces of the ceramic substrate 1 are very uneven because of the state of the wire lines in the through hole 107 that have been fired and sintered following the printing, as described above. Accordingly, it is necessary to polish the front and rear surfaces of the ceramic substrate 1 after firing and sintering. As a result, the surfaces of the substrate including the through hole wire lines are made smooth. The formation of the multi-layer wired matrix and the land on the surface of the substrate is thus facilitated.
Referring to FIG. 5B, after polishing, the first wire line layer 204 is formed on the surface of the substrate and the land 112 for the terminal pin is formed on the reverse side of the substrate. After titanium and palladium of 0.1 μm thickness is formed by sputtering as a base metal for the layer 204 and the land 112, the layer 204 is obtained on the desired parts of the substrate 1 by gold plating. The thickness of gold is 3 to 5 μm.
Referring to FIG. 5C, the photo-sensitive insulating paste 201A is uniformly coated by a printing process on the surface of the substrate 1 having the first wire line layer 204. For example, NTP sold by Tokyo Ouka Company can be used as the photo-sensitive insulating paste 201A. The thickness of the paste 201A is about 30 μm after drying and the paste 201A is applied with a stainless steel screen of 150 mesh.
Referring to FIG. 5D, the via hole 201B is obtained by the patterned exposure and development after drying at 85° C. for twenty minutes. The photo-sensitive insulating paste has a photo-sensitive character and high resolving power. It is not necessary to use photo-resist in the step of the exposure and development because of the use of the photo-sensitive paste. In the embodiment, it is relatively easy to make the via hole, the minimum diameter of which is 80 μm. Next, the paste is fired and burned at 700° C. to 900° C. in air to be the inorganic insulating layer 201. The thickness of the layer 201 after firing and sintering is about 20 μm.
Referring to FIG. 5E, the first wire lines 203 for via holes are formed by filling up the via holes with thick film paste or by plating gold. The second wire line 206, the second insulating layer 202, the second wire line for via hole 205, and third wire line 207 are formed by repeating the steps mentioned above. The minimum width of the wire line is 50 μm. Next, referring to FIG. 5F, the pin 104 is fixed to the land 112 by use of silver solder.
Now, the third embodiment of the present invention will be explained. The module shown in FIG. 6 includes a substrate 311 and a multi-layer wire line matrix 312 formed on the substrate 311. The multi-layer wire line matrix 312 comprises an under conductive layer 313 formed on the substrate 311; an insulating layer 314 with via holes 314a corresponding to the desired parts of the layer 313, formed on top of the substrate 311 including the layer 313; a conductive layer 315 formed by filling up the via holes 314a by metal plating; and an upper conductive layer 316 formed on the surface of the insulating layer 314 including the surface of the conductive layer 315. The upper conductive layer 316 is electrically connected to the under conductive layer 313 via the conductive layer 315.
By the structure mentioned above, the upper conductive layer 316 is not cut off in the part of the upper layer 316 corresponding to the corner 314b between the side wall of the via hole 314a and the surface of the insulating layer 314, thus protecting against cut off.
Now one example of the method for manufacturing the third embodiment of the present invention will be explained. Referring to FIG. 7A, the under conductive layer 313 is formed on the substrate 311. Then the insulating layer 314 with via holes 314a is formed on the parts corresponding to the desired parts of the upper conductive layer 313. Referring to FIG. 7B, the conductive layer 315 is formed by filling up the via 314a hole of the insulating layer 314 by metal plating. In the case that the plating method is a non-electrolytic plating method, the combination of the metal for the under conductive layer 313 and the plating metal is limited. Copper, nickel or gold can be practically used as a plating metal. Examples of the combination of the metal for the under conductive layer 313 and the plating metal are shown in the following table.
______________________________________metal for the conductive copper nickel palladiumlayer 313plating metal copper nickel nickel(non-electrolysis) gold______________________________________
As it is not necessary to provide electric paths for non-electrolytic plating, the operation is more efficient than that of electrolytic plating. On the other hand, although for electrolytic plating, the choice of metal to be used for plating is wider than that for electrolytic plating, electrolytic plating requires that the parts to be plated be used as electrodes in order to provide electrical connectivity as an electrode. In any case, the central feature of the embodiment is to utilize the insulating layer 314 itself as a plating resist. As the metal is filled up into only the via holes 314a of the insulating layer 314 by selective plating, it is not necessary to use a special resist.
By adopting the steps, the step for forming the conductive layer 315 (via hole parts) is reduced, and it produces perfect self alignment which plates to only the via holes. Accordingly, the occurrence of the problem of the formation of a gap between the via holes 314a and conductive layer 315 can be reduced.
Referring to FIG. 7C, the upper conductive layer 316 is formed on the insulating layer 314 to connect with the conductive layer 315 in the via hole 314a. As the plated metal fills up the via holes 314a, almost all of the surface of the conductive layer 315 is even. Accordingly, the cutting off of the upper conductive layer 315 can be eliminated.
FIG. 8 is a cross sectional view showing another example of the method for manufacturing the third embodiment according to the present invention. In this method, a through hole 318, connected between terminal 317 at the one edge of the hole 318 and the under conductive layer 313 at the other edge of the hole 18, is formed on the substrate 311. The other elements are the same of the other method for the third embodiment, and the same reference numbers are used for corresponding elements. The conductive layer 315 in such a configuration of the multi-layer wire line substrate can be formed by electrolytic plating. At that time, the through holes 318 and the terminals 317 are utilized. The conductive layer 315 is formed by filling up the via holes 314 by metal plating while the cathode is the under conductive layer 313 connected to the terminal 317 by the through hole 318. Also, in this case, the insulating layer 314 functions as a plating resist, so that only the via hole 314a is plated.
Next, one example of the method for fixing the module according to the present invention will be explained with reference to FIGS. 9A to 9D. Referring to FIG. 9A, the conductive layers 322 and the insulating layers 323 are alternatively laminated so that a multi-layer wire line matrix is formed. There are two typical methods to form the conductive layer 322. One way is a substractive method. After a metal film is formed on the entire surface, only the desired portion is covered by photo-resist and the other parts are etched away. The other way is an additive method in which metal film is put only on the desired portion by photo-resist. This described embodiment uses the subtractive method. Of course, the additive method can be used in the present invention. High molecular resin film like SiO 2 , Si x N y and polyimide, or a fired glass and alumina film can be used as the insulator 323. In the embodiment, polyamide film is used.
Referring to FIG. 9B, the signal line in the multi-layer wire line matrix is inspected by a contact method. In the embodiment, a probe 324 sequentially contacts each of the terminals of the signal wire lines. This method measures the electrical capacitance between the opposite electrode 326 and the contacted signal wire line. The feature of this method is that only one inspection probe 324 is used. A cut off or a short circuit of the signal wire line can be detected by measuring the electrical capacitance, if the electrical capacitance is proportional to the length of the signal wire line. This proportional relationship can be obtained to a good approximation by using a suitable shape and material for the opposite electrode 326. For example, FIG. 9B shows the case of cut off portion 327.
Referring to FIG. 9C, a fixing signal wire lines 328 having the same connecting function as the non-defective signal wire line, is formed on the multi-layer signal wire line matrix. For example, the method for forming the firing line 328 is as follows. A metal film is formed on the entire surface of the multi-layer signal wired line matrix. Next, photo-resist is coated thereupon. Then, based on the inspection of the previous step, the fixing wire line pattern corresponding to the signal wire line is exposed by a direct scanning exposure unit, that is, direct writing is used. The photo-resist is thus selectively exposed and polymerized. The remaining metal film under the photo-resist is not etched away. Finally, the photo-resist is peeled off or removed and the fixing signal wire line 328 made of the metal film is formed. If necessary, a defective wire line is disconnected from the fixing wire line 328 by cutting off of the defective wiring terminal. FIG. 9C shows two examples of a cut off portion 329.
Referring to FIG. 9D, another conductive layer 332 and another insulating layer 333 are formed on the fixing signal wire line 328. The conductive layer 332 provides pads for mounting LSI chips. The same functional connectivity pattern can be obtained by using the fixing signal wire line 328 in place of the defective line 322.
Next, another example of the method for fixing the module according to the present invention will be explained with reference to FIGS. 10A and 10B. FIG. 10A shows the non-defective structure while FIG. 10B shows an example of a short-circuited structure, as exemplified by a short 47. A comparison of these two structures will clarify the function of fixing wire line layer. A multi-layer signal wire line matrix 43 is formed on the surface of a multi-layer ceramic substrate 42 in both FIGS. 10A and 10B. The multi-layer signal wire line matrix 43 can be obtained by alternatively laminating conductive layers 43A and insulating layers 43B. Then, the integrity of the multi-layer signal wire line matrix 43 is checked by electrical test.
Referring to FIG. 10A, when no defects are found in the signal wire line matrix 43, the uppermost signal wire line conductive layer 43A is connected to a surface connecting layer 45 through an upper insulating layer 44 to a signal terminal pin 41A via a fixing wire line conductive layer 44A. The fixing wire line layer 44A, in this case, is merely a path for the signal wire line, and does not provide any further function.
However, in the case of a defective signal wire line layer, exemplified by two lines 43A being short-circuited in the short 47. At this time, the fixing wire line conductive layer 44A is cut off at four locations 44A1, 44A2, 44A3 and 44A4. The original surface connecting terminals 45 are connected to the signal terminals pins 41A via fixing re-wired line patterns 445A and 44A6. The re-wired line fixed patterns 44A5 and 44A6 are formed by using the fixing wire line layer 44A, even if the defects occur in some other part of the multi-layer signal wire line matrix 43. Accordingly, it is desirable that a wide selection of wired line patterns can be obtained early in the formation of the fixing signal wired line and at low cost. Photo-lithographic techniques using glass masks are utilized in the normal forming of a wiring pattern. However, forming separate masks each time in the formation of such a fixing wire line pattern necessarily requires much time and is a high cost operation. This problem is resolved in this embodiment by using the direct scanning exposure unit in the step of exposing the resist for manufacturing the fixing signal wire line. That is, only the necessary fixing wire pattern (including the normal fixing wire pattern for a non-defective chip) is directly scanned and thus exposed on the substrate, based on the defect information obtained from the inspection result of the signal wire line matrix 43 in order to produce the fixing signal wire line layer 44A. The fixing patterns 44A5 and 44A6 are directly exposed by the direct scanning exposure unit, as shown in FIG. 10B. The fixing signal wire line can thus be obtained by correcting the resist pattern in the etching and plating steps.
As explained above, in the module built according to the present invention, the metal connecting pad is formed to cover the through hole exposed at the surface, and the multi-layer line matrix is formed on the surface of the multi-layer ceramic substrate including the metal connecting pad. As a result, the connection defect caused by the variation of the rate of construction of the multi-layer ceramic substrate can be prevented. In addition, the via holes can be easily formed. Furthermore, the area of the multi-layer ceramic substrate can be densely and effectively used for an interior power and ground grid. The module of the present invention is formed by using insulating photo-sensitive paste material which is exposed by light incident on the surface of the glass ceramic and which is able to be fired and sintered at a low temperature in air. The glass ceramic has, as an inner conductive layer, the material that was not oxidized in the firing and sintering step in air. For example, gold, silver and palladium, can be used as conductive material for the inner conduction layers of the ceramic substrate, as well as for the conductive material of the multi-layer wire line matrix. As a result, a power wire line with the best impedance can be achieved, and in particular, a high density multi-layer wire line matrix can be formed without limitations on the materials and processes.
The module of the present invention is formed so that the conductive layers that electrically connect the upper and lower conductive layers are different from the upper and low conductive layers, with the result that the cutting of the upper conductive layer is prevented. Using the described manufacturing method for the module, the conductive layer is formed by plating with the result that the formation of the conductive layer is easy. The advantages of the structure arise from the fact that the fixing signal wire line is formed in the signal wire line matrix. The advantages are as follows. First, the check for defective signal wire lines need not be done at each layer of fabrication of the signal wire lines but instead is performed at the time of completing of the wire line matrix. Since the signal wiring has been finished at this stage, the electrical check is straight forward. Next, because the formation of the rewiring pattern can be done by using only a single fixing wire line layer, the fixing is easily accomplished. Then, as the fixing wired line layer is formed as a inner layer, the reliability of the fixing lines is significantly higher than that of fixing wires outside of the substrate.
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A multi-layer comprising a multi-layer glass ceramic substrate and a multi-layer wire line matrix. The multi-layer wired line matrix includes an insulating layer made from a photosensitive insulating layer, amenable to time geometry processing. The insulating layer of the multi-layer wire line matrix has a pad for accommodating variations of the locations of the through holes. The metal is plated in and fills the through holes so that the metal is not cut off at the corners. The wire line matrix is composed of a plurality of layers of a photo-lithographically formed fine conductive pattern. The glass ceramic insulating layer is also formed photo-lithographically, and is formed of the source material of the insulating layers.
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FIELD OF THE INVENTION
The present invention relates generally to medical devices, and more particularly to a system that automates the assembly of components of a fabric-covered prosthetic heart valve, and associated methodology.
BACKGROUND OF THE INVENTION
Heart valve replacement may be indicated when there is a narrowing of the native heart valve, commonly referred to as stenosis, or when the native valve leaks or regurgitates, such as when the leaflets are calcified. In one therapeutic solution, the native valve may be excised and replaced with either a biologic or a mechanical valve. Prosthetic valves attach to the patient's fibrous heart valve annulus, with or without the leaflets being present.
Two primary types of heart valve replacements or prostheses are known. One is a mechanical-type heart valve that uses a ball and cage arrangement or a pivoting mechanical closure supported by a base structure to provide unidirectional blood flow, such as shown in U.S. Pat. No. 6,645,244 to Shu, et al. The other is a tissue-type or “bioprosthetic” valve having flexible leaflets supported by a base structure and projecting into the flow stream that function much like those of a natural human heart valve and imitate their natural action to coapt against each other and ensure one-way blood flow. In tissue-type valves, a whole xenograft valve (e.g., porcine) with leaflets or a plurality of individual xenograft leaflets (e.g., bovine pericardium) provide the fluid occluding surfaces. Synthetic leaflets have been proposed, and thus the term “flexible leaflet valve” refers to both natural and artificial “tissue-type” valves. Two or more flexible leaflets are mounted within a peripheral support structure that usually includes posts or commissures extending in the outflow direction to mimic natural fibrous commissures in the native annulus. For example, the CARPENTIER-EDWARDS Porcine Heart Valve and PERIMOUNT Pericardial Heart Valve available from Edwards Lifesciences of Irvine, Calif. each include a peripheral support structure with an undulating wireform and surrounding stent.
Certain support components of prosthetic valves are assembled with one or more biocompatible fabric (e.g., Dacron, polyethylene terepthalate) coverings, and a fabric-covered sewing ring is typically provided on the inflow end of the valve. The fabric coverings provide anchoring surfaces for sutures to hold the flexible leaflets and sewing ring to the peripheral support structure. In a typical assembly procedure, a technician manually holds a tubular fabric around the support component, and the sewing occurs in two stages; first, intermittent stitches are placed to secure the fabric in its gross position around the stent, and then a closely-spaced line of stitches is applied to complete the seam, still with some manual tension on the fabric. The holding and stitching operation is entirely manual and done under a magnifier, which makes it quite labor-intensive and time-consuming. The work requires the passage of needle and thread through multiple layers of fabric and sometimes biological tissue, and requires considerable effort and precision. Needless to say, repetitive stress injuries can occur which is painful to the worker and indirectly increases the cost of making the valve. The number one factor for injury and lost time in this field is the intricacy of manual sewing.
Rigorous quality control in the manufacture of heart valves further increases the difficulty of the task because the fabric must be tightly fitted around the support component and every stitch carefully placed for consistency. Operator-to-operator variability in sewing technique, stitch tension, stitch pitch, and other variables can result in subtly different construction and end product quality. A typical tissue-based heart valve requires 6-8 hours of manual construction, and the manual sewing procedure represents a substantial portion of the cost of the entire valve fabrication process. Moreover, training of heart valve assembly operators to become proficient in sewing can take upwards of 12-14 months.
Automation is usually an option in manufacturing processes, but is not a factor in the production of prosthetic heart valves because of their odd shapes and strict quality control. Indeed, manual sewing has the advantage of the operator being able to continually check the quality and success of their sewing. Mistakes can be corrected on the spot. Although automation speeds the process up, and is quite repeatable and reliable, it is not infallible and the careful manual visual inspection of each stitch would be lost. In general, because most of the steps in assembling prosthetic heart valves are specialized tasks performed in a clean room to produce an implant that must be highly sterile and perfectly assembled, robotics and other such ubiquitous tools of automation are not easily adapted.
There is thus a need for an improved method for assembling flexible heart valves that reduces the assembly time and the instances of injury to the assembly-line workers.
SUMMARY OF THE INVENTION
In accordance with one aspect of the present invention, an automated system is provided for assembling components of a prosthetic heart valve having a fabric-covered support structure defining a central axis. The system comprises a sewing machine including a needle and bobbin for forming a seam with thread in fabric, the sewing machine having components that satisfy FDA class III device manufacturing requirements. A mount holds and rotates a support structure of the prosthetic heart valve about its axis in conjunction with movement of the sewing machine needle during formation of the seam. A sensor detects the presence of thread over the bobbin on each successful stitch, and a processor receives input from the sensor and controls the movements of the sewing machine and clamp based upon said input.
Desirably, the components of the sewing machine that satisfy FDA class III device manufacturing requirements include medical and food grade bearing lubricants materials, and/or at least one factory sealed servo- or stepper-type motor. The support structure of the prosthetic heart valve may be an annular stent and the mount has separable parts for receiving and clamping the fabric over the stent during formation of the seam. Preferably, the sensor comprises a monitoring laser. An air jet may be positioned adjacent the sewing machine needle and directed to form a loop in the thread and facilitate its capture by a bobbin hook. In one embodiment, the sewing machine has at least two speeds, and the processor includes instructions to repeat a stitch at a slower speed on condition of an unsuccessful stitch.
Another aspect of the invention is an automated method for assembling components of a prosthetic implant having a fabric-covered support structure defining a central axis. The method comprises establishing a clean room that satisfies FDA class III device manufacturing requirements, and within the clean room providing a prosthetic implant support structure and a fabric for covering the support structure. The support structure with the fabric thereover is secured on a mount that is rotated adjacent a needle of the sewing machine. A circular seam is formed by the sewing machine with a plurality of thread stitches in the fabric. The success of each thread stitch is monitored and the sewing process modified on the occurrence of an unsuccessful thread stitch.
Desirably, the support structure comprises a stent for a prosthetic heart valve, and may further include a sewing ring wherein the fabric covers both the sewing ring and stent. The mount may have separable components, wherein the method includes clamping the fabric tautly around the support structure with the separable components of the mount. Preferably, the step of monitoring comprises using a non-contact sensor. For example, the non-contact sensor is a monitoring laser, and the sewing machine comprises a bobbin, the monitoring laser being directed toward the bobbin to monitor the passage of a needle thread thereover. The step of modifying may involve repeating an unsuccessful stitch at a slower speed. A flow of air may be directed toward the needle of the sewing machine to form a loop in the thread and facilitate its capture by a bobbin hook.
In accordance with another aspect of the present invention, a method of increasing yield in the fabrication of prosthetic heart valves comprises automatically forming a thread seam in fabric surrounding a support structure of the prosthetic heart valve, the seam comprising a plurality of individual stitches, and automatically monitoring the successful completion of each stitch in the seam prior to formation of another stitch. The support structure may comprise an annular stent and sewing ring, and the fabric covers both the sewing ring and the stent. The method is preferably performed in a clean room and comprises a sewing machine component which interacts with a workpiece handling component both being built and operated to satisfy FDA class III device manufacturing requirements. The movements of the sewing machine component and workpiece handling component may be controlled by a processor which indexes the prosthetic heart valve support structure prior to every stitch. Desirably, placement of each stitch is accurate to within a tolerance of 0.002 inches (0.051 mm). In one embodiment, the step of automatically monitoring comprises directing a monitoring laser toward a bobbin of the sewing machine to monitor the passage of a needle thread thereover. The method may include repeating an unsuccessful stitch at a slower speed on the occurrence of an unsuccessful stitch.
A further understanding of the nature and advantages of the present invention are set forth in the following description and claims, particularly when considered in conjunction with the accompanying drawings in which like parts bear like reference numerals.
BRIEF DESCRIPTION OF THE DRAWINGS
Features and advantages of the present invention will become appreciated as the same become better understood with reference to the specification, claims, and appended drawings wherein:
FIG. 1A is a perspective view of an exemplary system for automatically forming a seam in fabric surrounding a prosthetic heart valve support structure, prior to an assembly procedure;
FIG. 1B is a perspective view of the system of FIG. 1A during an automated assembly procedure to form a seam in the fabric surrounding the support structure;
FIGS. 2A and 2B are enlarged perspective views of a needle and bobbin subsystem of the system of FIG. 1A illustrating one technique for monitoring the formation of successful stitches;
FIG. 3 is a partially cutaway view of an exemplary heart valve support stent and sewing ring covered by fabric and held firmly together on a mount so as to be secured by a seam formed in accordance with the present invention;
FIG. 4 is an enlarged view of the sectioned edge of the fabric-covered support structure in FIG. 3 ;
FIG. 5 is a partial top view of an edge of a fabric-covered support structure illustrating a circular seam formed therein;
FIG. 6 is a sectional view through two layers of fabric showing a typical series of stitches used to form the seam of FIG. 5 ;
FIG. 7 is an axial sectional view through a needle carrying a thread used to form a stitch;
FIG. 8 is a sectional view through the needle taken along line 8 - 8 of FIG. 7 , and an adjacent air jet subsystem; and
FIG. 9 is a flow chart illustrating several possible outcomes of a stitch monitoring process.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention provides a system for automating one or more steps of a prosthetic heart valve fabrication procedure. The steps of the procedure illustrated and described involve sewing a tubular piece of fabric around a support structure of the prosthetic heart valve, typically a support stent. It should be understood by those of skill in the art that the illustrated support stent is only exemplary, and the present invention can be used to cover various support stents or structures. Furthermore, various aspects of the present invention may be used in other steps of a heart valve fabrication process. For example, mechanisms similar to those shown and described may be used to cover other parts of a prosthetic heart valve with fabric. Up to now, prosthetic heart valve assembly has been an almost entirely manual, labor-intensive process. The present invention therefore represents a pioneering effort to automate at least some of the process of assembling heart valves.
The present invention involves automatically fastening or sewing fabric over the support stent. Desirably, the sewing step is accomplished with a means for automatically forming a seam in the fabric, such as with a sewing machine needle. The term “sewing machine” is intended to refer to any automated device for forming a seam in fabric using a plurality of thread stitches. Likewise, “thread” refers to a filament suitable for forming continuous stitches in fabric, typically polypropylene thread for surgical implant applications. In the context of the present invention, the term “automated” means that once initiated, a particular assembly procedure, in this case forming a seam, may proceed without further manual assistance. Of course, the presence of system operators who monitor the automated assembly procedure may be required, as well as their involvement during steps such as changing workpieces or thread, or attending to malfunctions. However, these manual tasks are not to be considered as part of the “automated” assembly procedure.
With reference now to FIGS. 1A and 1B , an automated system 20 for forming a seam in fabric is explained. The system 20 generally comprises a sewing machine component 22 which interacts with a workpiece handling component 24 . The workpiece in this case is a support structure for a prosthetic heart valve around which a fabric covering will be secured by forming a seam therein using the sewing machine 22 . The equipment essentially duplicates the eye-hand coordination and motion of manual sewing. The valve or valve components are held, presented, and indexed via custom designed fixtures and tools that free up the hands of the operator. The operator essentially is tasked with the loading of the parts and the control of the equipment via control panel instructions and motions. Pre-programmed sewing routines or sophisticated pixel-based vision systems replace the eyes of the operators and eliminate eye strain, the need for magnification, and the tedious job of “counting loops” to determine stitch pitch and suture placement.
As mentioned, various heart valve support structures, and other surgical implant workpieces, may be processed by the system 20 . In the exemplary embodiment, as seen better in FIG. 3 , the workpiece comprises an annular heart valve support stent 26 secured to an annular suture-permeable sewing ring 28 with a fabric covering 30 . In particular, the fabric covering 30 is initially formed as a tube which is draped or wrapped around the support stent 26 and sewing ring 28 and fastened thereover by forming a seam 32 to secure the free ends together. The cross-section indicates that the support stent 26 and sewing ring 28 are the same material, though typically the support stent is metal or rigid plastic while the sewing ring is soft, such as silicone. It will be understood that these elements represent a “support structure” of a prosthetic heart valve, and also represent other implant support structures, such as a metal stent that will be covered with fabric using a seam.
The assembly of the support stent 26 , sewing ring 28 , and fabric 30 , is held on a rotatable mount 40 while forming the seam 32 . The mount 40 generally comprises a split cylinder with top and bottom halves 41 a , 41 b ( FIG. 4 ) for clamping around the support stent 26 using a locking key or thumb screw 42 . The top and bottom cylinder halves 41 a , 41 b hold the fabric 30 tautly around the support stent 36 and sewing ring 28 , and represent any number of such mounts or clamps that perform the function of maintaining tension on the fabric during the sewing process. These semi-autonomous mounts eliminate manual stretching of cloth over wireforms, for example, and holding and squeezing of the part for registration and resistance, all of which can cause significant hand, wrist, and shoulder joint trauma. Also, manual handling, squeezing, and manipulation of valve components can result in out-of-specification dimensions and the need for re-work or rejection. An additional benefit of fixtures such as the mount 40 is that they induce minimal stress or component deflection to the sewn parts and therefore result in a more consistent post-sewn component.
With reference again to FIGS. 1A and 1B , the mount 40 rests on a pedestal 44 which, in turn, rotates about the shaft 46 via a pair of bevel gears 48 journaled at 90° to one another. The bevel gears 48 rotate on a housing 50 capable of vertical movement and horizontal movement toward and away from the sewing machine 22 , as indicated by arrows 52 . The mechanisms and systems for translating and rotating the workpiece mount 40 are conventional, such as servo motors controlled by a programmed linear controller (PLC), and will not be described further herein. Suffice it to say that the edge of the workpiece can be brought into proximity with a needle 60 of the sewing machine 22 and thereupon rotated to form the continuous circular seam 32 .
The sewing machine 22 comprises mechanisms and systems for reciprocating the needle 60 relative to a bobbin platform 62 , also seen in detail in FIGS. 2A and 2B . There are a number of different automated stitches that may be performed by the sewing machine 22 , including a basic chain stitch and a lock stitch. To ensure integrity of the heart valve, a 301 lock stitch is preferred. FIG. 6 illustrates several lock stitches joining two layers of fabric 64 a , 64 b . Namely, a thread 66 carried by the needle 60 on one side of the layers loops around a segment of another thread 68 that is carried by a bobbin (described below) on the other side. Repetitive cycles of this looping operation at evenly-spaced locations around the fabric tube 30 creates the circular lock-stitch seam 32 ( FIG. 5 ). For further explanation of a lock-stitch and other seams the reader should refer to the web site http://home.howstuffworks.com/sewing-machine2.htm.
The workpiece mount 40 may be programmed to incrementally rotate the workpiece and form stitches of different pitches. Desirably, the pitch of the stitches remains constant for different sized prosthetic heart valve support stents, even though the stents are of different diameters and fit on different sized mounts 40 . An average stent requires sixty stitches to complete a full seam 32 , less for the smallest stents and more for the largest. The software and drive mechanisms of the system 20 are desirably accurate enough to place stitches within a tolerance of 0.002 inches (0.051 mm), which is well beyond the capability of a manual operation. Additionally, stitch tension is controlled and monitored with specific ranges using tight bands (not shown), whereas there is considerable variation from operator to operator in prior manual methods.
FIGS. 2A and 2B best illustrates an exemplary system for ensuring continuity of the stitch sequence in the seam 32 . A bobbin platform 62 includes a sewing table 70 that defines a small aperture 72 for receiving the reciprocating needle 60 . The needle thread 66 passes through an eye 74 in the needle 60 and is thereby carried through the aperture 72 and below the table 70 . A bobbin assembly 80 mounts for rotation in a space under the table 70 , and in proximity with the lower end of the aperture 72 . The bobbin assembly 80 carries the bobbin thread 68 which pays out as needed.
As customary with such rotating bobbin assemblies 80 , a hook 82 ( FIG. 8 ) captures a loop 84 formed by the needle thread 66 and carries it around the bobbin assembly 80 to form the lockstitch. Passage of the needle thread loop 84 over the bobbin assembly 80 is seen in stages in FIG. 2A , and after having gone completely around the bobbin assembly in FIG. 2B . Each time the needle thread loop 84 passes over the bobbin assembly 80 , it captures a segment of the bobbin thread 68 which forms one stitch of the seam 32 .
The small diameter and material characteristics of the needle thread 66 sometimes impede the formation of an initial small loop that can be snagged by the hook 82 . FIG. 8 illustrates an exemplary technique for ensuring formation of this initial loop, and thus reducing the possibility of a missed stitch. Specifically, a manifold 90 defines an air passage 92 within that opens at a nozzle 94 . The nozzle 94 points directly toward the sewing needle 60 just below the sewing table 70 . A conduit 96 supplies compressed air which is forced out of the nozzle 94 and causes the needle thread 66 on the right side to bend to the right, much like a flag waving in the wind, ensuring that the bobbin hook 82 snags it. The needle thread 60 on the left side is maintained in greater tension and is thus not carried into the path of the hook 82 .
The automated system 20 of FIG. 1A further includes a monitoring subsystem including a sensor 100 mounted above the bobbin platform 62 that provides 100% inspection of stitch completion during the actual sewing (i.e., in “real-time”). As seen better in FIGS. 2A-2B , the sensor 100 monitors a space adjacent the bobbin assembly 80 over which the needle thread loop 84 crosses. The sensor 100 monitors for the presence or passage of the loop 84 to ensure that a proper stitch is formed. If the loop 84 is not present, the sensor 100 alerts the system 20 of the failure. Several different actions by the system 20 are then possible, as will be detailed below.
It should be noted that a missed stitch or series of stitches may be detected and corrected by post sewing visual inspection. Therefore, a “real-time” monitoring system for each stitch may not be necessary. However, there are situations where a missed stitch can result in the need to junk the entire component. Moreover, post-sewing visual inspection of stitch placement and quality is currently commonly used in industry, but is time-consuming and difficult due to the fact that the sutured cloth material and sutures themselves are the same material and identical in terms of color, contrast and texture. Attempting to visually inspect white stitches against a white cloth background is difficult. Ideally, the present system 20 can be validated such that post-sewing visual inspection can be eliminated.
In an exemplary embodiment, the sensor 100 comprises a monitoring laser that directs an optical beam downwards to the edge of the bobbin assembly 80 , and an optical receiver to detect the presence of the loop 84 . Such monitoring lasers are available from Keyence of Osaka, Japan (world.keyence.com). The receiver is programmed and instructed to look for optical changes in the reflected field of view it is monitoring. For example, the laser beam is aimed to the bobbin assembly 80 , or the space adjacent thereto, which results in a known reflected light that can be calibrated into the system. Upon passage of the typically white thread loop 84 , the expected transient reflection from the thread is sensed by the optical receiver. Through a controlling programmer, the system 20 receives a signal that a stitch is being initiated and the optical receiver watches for the reflection of the thread loop 84 . Failure to sense the presence of the light reflected from the thread loop 84 at the proper time denotes failure of the completed stitch, and the software connected to the sensor 100 is so notified.
A correctly completed stitch can, of course, be detected in several ways, for example using load cells or thread path tension switches. However, the non-contact optical system described above is believed much more robust for the present application which must satisfy the requirements of the United States Food and Drug Administration for class III devices (described below). The monitoring system ideally provides assurance of 100% stitch success which, in turn, potentially leads to the elimination of 100% post-process quality inspection and its associated cost. For example, after a validation period in which every sewn component is inspected, a level of confidence may be attained permitting a reduction of inspection to every other component, or less. Because of the critical importance of stitch perfection, random or periodic reinstitution of 100% inspection of components is advisable to justify the switch to a reduced inspection level.
There are a number of possible outcomes upon a missed stitch. For example, the system 20 may halt so that the operator can determine the cause of the error. Or, the system 20 may not index to the next stitch and attempt to correctly place a stitch again in the same spot it previously missed. The equipment can be programmed to attempt multiple tries and then stop if unsuccessful. During the retries the machine may assume a slower speed to try and optimize sewing conditions and complete the previously missed stitch.
FIG. 9 is a flow chart indicating several possible outcomes of the stitch monitoring process.
Furthermore, the system 20 can be programmed to report on the initial success rate of every sound component. Components that have reports showing increasing levels of initial failures and retry stitches may indicate to the operator that the system requires adjustment or maintenance.
Tests of the system 20 have reduced cycle time for assembling the fabric 30 over the support stent 26 and sewing ring 28 to less than one third of the time for the manual operation (e.g., 18 minutes down to 5). Once completed, the entire automated sewing initiative for conventional tissue heart valves has the potential to reduce sewing cycle time by nearly 50% (with associated direct labor savings). It is estimated that the direct annual labor savings to the present assignee could be in the area of $4 million.
It is important to understand the difference between the present implant fabrication system and existing textile manufacturing systems with which it shares some general aspects (e.g., a reciprocating needle creating a lock stitch). The Medical Device Amendments of 1976 to the Federal Food, Drug, and Cosmetic Act (the act) established three regulatory classes for medical devices. The three classes are based on the degree of control necessary to assure that the various types of devices are safe and effective. The most regulated devices are in Class III, which are defined as those that support or sustain human life or are of substantial importance in preventing impairment of human health or present a potential, unreasonable risk of illness or injury. Under Section 515 of the act, all devices placed into Class III are subject to pre-market approval requirements. Pre-market approval by FDA is the required process of scientific review to ensure the safety and effectiveness of Class III devices.
In the context of a manufacturing facility that produces Class III medical implants, the requirements are numerous and detailed. One of those is that the products be manufactured in a clean environment. Of course, there are various notions of “clean” manufacturing facilities, from those used in food processing all the way up to the ultra-clean conditions within silicone wafer handling rooms. For Class III medical devices, the standards for ensuring that the products remain sterile are relatively stringent. One of those is that any machinery utilized not generate particulate matter which might contaminate the clean room environment.
Consequently, the system 20 has been designed to operate in the absence of particulate matter and contaminants such as grease, oil, and heavy metal contact. Conventional sewing machines are quite dirty in operation due to exposed mechanisms such as cams, followers, belt drives, bearings, etc. To avoid these sources of contamination, the system 20 operates without conventional bearing surfaces by, for example, substituting traditional lubricants with medical and food grade bearing materials. Further, mechanization is limited by replacing cams and levers with factory sealed servo and stepper-type motor technology. Also, conventional machine materials such as case iron, steel, bronze, etc. are replaced with FDA grade stainless steel, anodized aluminum and medical grade plastics such as Delrin and Teflon. Furthermore, to the extent possible, shrouds and seals are provided to physically separate different areas of the system, and as much as possible mechanization is placed below product areas. The aggregate of these efforts produces a system that satisfies FDA Class III device manufacturing requirements, and is accordingly significantly more complex and expensive than conventional sewing machines.
While the invention has been described in its preferred embodiments, it is to be understood that the words which have been used are words of description and not of limitation. Therefore, changes may be made within the appended claims without departing from the true scope of the invention.
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A system and method for assembling a prosthetic heart valve, including a procedure for sewing fabric around a heart valve support stent. The system includes a support stent handling component that works in conjunction with a sewing machine component. The sewing machine has a bobbin, and the system includes a non-contact sensor to monitor the passage of a needle thread loop over the bobbin. The sensor may be a monitoring laser, and a controlling processor receives information therefrom for 100% real-time inspection of each stitch. The occurrence of an unsuccessful stitch may prompt the processor to repeat the stitch at a slower speed. The automation of the fabric sewing procedure greatly enhances manufacturing throughput and reduces ergonomic strain on workers.
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FIELD OF THE INVENTION
[0001] This invention relates generally to shock isolated systems and, more specifically, to a wall mounted display that is cantileverly supported and isolated from harmful shock and vibration forces though shear resistance of a plurality of elastomer mounts.
CROSS REFERENCE TO RELATED APPLICATIONS
[0002] None.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0003] None
REFERENCE TO A MICROFICHE APPENDIX
[0004] None
BACKGROUND OF THE INVENTION
[0005] Various elastomeric materials have been used, or suggested for use, to provide shock and/or vibration damping as stated in U.S. Pat. No. 5,766,720, which issued on Jun. 16, 1998 to Yamagisht, et al. These materials include natural rubbers and synthetic resins such as polyvinyl chlorides, polyurethane, polyamides polystyrenes, copolymerized polyvinyl chlorides, and polyolefine synthetic rubbers as well as synthetic materials such as urethane, EPDM, styrene-butadiene rubbers, nitrites, isoprene, chloroprenes, propylene, and silicones. The particular type of elastomeric material is not critical but urethane material sold under the trademark Sorbothane® is currently employed. Suitable material is also sold by Aero E.A.R. Specialty Composites, as Isoloss VL. The registrant of the mark Sorbothane® for urethane material is the Hamiltion Kent Manufacturing Company (Registration No. 1,208,333), Kent, Ohio 44240.
[0006] Generally, the shape and configuration of elastomeric isolators have a significant effect on the shock and vibration attenuation characteristics of the elastomeric isolators. The elastomeric isolators employed in the prior art are commonly formed into geometric 3D shapes, such as spheres, squares, right circular cylinders, cones, rectangles and the like as illustrated in U.S. Pat. No. 5,776,720. These elastomeric isolators are typically attached to a housing to protect equipment within the housing from the effects of shock and vibration.
[0007] In contrast to prior art devices that provide compressional support for an article, the present invention comprises a wall mountable display for cantileverly supporting articles such as display equipment or the like in a spaced condition form a support wall with a set of triad elastomers that are positioned between the wall and the equipment to cantileverly support the weight of the equipment while at the same time isolating the equipment from shock and vibration.
[0008] One of the difficulties with wall mounting sensitive equipment, such as a digital display system is to prevent the sensitive electronic equipment from receiving excessive shock and vibration from the support surface it is secured to. The shock and vibrations can come from a number of different sources. For example, excessive shock and vibrations forces can be encountered in a ship, a land vehicle or even a building which is subject to periodic earthquakes. This problem is particularly acute with costly sensitive equipment such as large screen displays which could easily be destroyed by shock and vibration forces. Because it is both costly and difficult to mount an expensive large screen display equipment in a condition that is free of harmful shocks or vibrations the safe course has been to sacrifice the quality of the more costly equipment for the lesser quality of less costly alternative equipment. For example, rear projection units are used in place of large screen digital displays in order to avoid putting a costly large screen digital display at risk from harmful shocks and vibration forces. Unfortunately, the result is that in many cases the overall system quality suffers since such systems do not provide the user the sharp image of higher quality display systems. The tradeoff of quality for costs is addressed by the present invention that provides a fixture for supporting sensitive equipment with the fixture isolating the sensitive equipment from the effects of shock and vibration forces to avoid putting the sensitive equipment at risk.
SUMMARY OF THE INVENTION
[0009] A wall mounted display including a system for isolation of wall hung equipment from harmful shock and vibration forces including a wall mountable support or fixture having a first member for securing to a wall and a second member for securing to equipment with a plurality of triad elastomers mounted therebetween to cantileverly support the weight of the equipment and at the same time isolate the equipment from shock and vibration forces through a shearing action within the elastomer mounts. The elastomer mounts, while permitting displacement of the members with respect to one another inhibit the members from contacting each other when one or the other is subject to shock or vibration.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] [0010]FIG. 1 is a front view of a wall mountable fixture with a portion of the one of the members cut away to reveal a triad elastomer used with the present invention.
[0011] [0011]FIG. 2 is a side view showing one of the members of the wall mountable fixture secured to a wall and the other member supporting a digital display system.
[0012] [0012]FIG. 3 is the perspective view of a double triad elastomer used in the wall mountable fixture of FIG. 1.
[0013] [0013]FIG. 4 is a side view of wall mounted elastomers cantileverly supporting an equipment operators chair.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] [0014]FIG. 1 shows a front view of a wall mountable fixture or isolator 10 having a first rigid plate member 11 positioned rearward of a second rigid plate member 12 . Extending between rigid plate member 11 and rigid plate member 12 are a plurality of triad elastomers 13 , 14 , 15 , 16 , 17 and 18 . The Triad elastomers are more fully described in copending application titled Double Triad Elastomer Mount filed Feb. 8, 2001, Ser. No. 09/779,423 and is herein incorporated by reference. A feature of the triad elastomers is that the compressive forces on opposite ends of the triad elastomer produce a shearing action within the elastomer mount rather than a material compression. The result is that the elastomer mounts, which act in shear mode rather than compression mode, provide effective damping of shock and vibration forces.
[0015] [0015]FIG. 2 is a side view showing fixture 11 secured to wall to 9 by fastening members 19 and 21 , which may be screws bolts or the like. Secured to member 12 by fasteners 21 , which may be screws bolts or the like, is a large screen display 20 . Large screen display systems are known in the art and will not be described herein except to point out that such high systems are generally costly and lack the ability to withstand shocks and vibrations encountered in various environments.
[0016] [0016]FIG. 2 illustrates that the double triad elastomers provide the sole cantilever support between plate member 11 and plate member 12 . With the wall mountable fixture 10 located in the position shown the weight of the large screen display 20 acts downward as indicated by force arrow F 1 thereby inducing a shear force to each of the cantileverly extending triad elastomers. In addition, large screen display 10 produces a slight torque as indicated by arrows F 2 and F 3 . Although the torque produces a compression force on elastomer 18 and a tension force on elastomer 13 the triad elastomer responds to a compressive force by providing shear resistance. In the embodiment shown the shear forces within the elastomer mounts absorb the static weight of the large screen display 20 . In addition the elastomer mounts, which are under tension or compression forces, utilize the shear resistance of the elastomer mounts to absorb energy from shock and vibration forces. While a large screen display has been illustrated the wall mountable member is suitable for use with other sensitive equipment that need to be isolated from shock and vibration.
[0017] [0017]FIG. 3 shows a pictorial view of a triad elastomer mount or single isolator 30 for providing shock and vibration attenuation while providing axially offset support. Isolator 30 is a two-tetrahedron shock isolator 30 for simultaneously isolating shocks and for cantileverly supporting a static load Tetrahedron shock isolator 30 comprises an elastomer material, having a set of integral side walls forming a first tetrahedron isolator 31 with a tetrahedron shaped cavity 31 c therein and a second tetrahedron shock isolator 32 with a tetrahedron shaped cavity 32 c therein. A central axis 33 is shown extending through an apex end 32 a and an apex end 31 a . Apex end 31 a and apex end 32 a are smoothly joined to each other to form a one-piece two-tetrahedron shock isolator. The top tetrahedron isolator 32 has a triangular shaped base end for forming a first support surface 32 b . Similarly, the bottom tetrahedron isolator 31 has a triangular shaped base end for forming a second support surface 31 b . The conjunction of the two-tetrahedron isolator provides an integral force transfer region with both the triangular shaped base ends 31 a and 32 a of the two-tetrahedron isolator 31 and 32 laterally offset with respect to the minimum cross-sectional area which occurs at the apex conjunction of the tetrahedron shock isolator 31 and 32 . That is, a line parallel to axis 33 that extends through first support surface 32 b does not extend through the conjoined region between the apex of the two-tetrahedron isolators 31 and 32 . Similarly, a line parallel to axis 33 that extends through the second support surface 31 b does not extend through the conjoined region between the two apexes of the two-tetrahedron isolators 31 and 32 . As can be seen from FIG. 3 the support surface 32 b even though identical in shape to support surface 31 b are rotationally displaced from each other as well as laterally displaced from each other so compressive forces on the end of elastomer mount 30 do not produce compression forces in elastomer mount 30 but instead produce shear forces which can effectively damp shock and vibration forces.
[0018] [0018]FIG. 4 is a side view of another embodiment of the invention wherein a wall 42 cantileverly connects to an operators chair 43 . A first triad elastomer 40 has one end secured to the back of chair 43 by a suitable adhesive and the other and secured to wall 42 by a suitable adhesive. Similarly, triad elastomer 41 has one end secured to the back of chair 43 by a suitable adhesive and the other and secured to wall 42 by a suitable adhesive. While only two elastomers are shown, a third triad elastomer mount (not shown) is mounted thereon to provide a three point connection between the wall and the chair 43 . If desired, more triad elastomer mounts could be used With the present invention one can obtain maximum shock and vibration damping by using elastomer mounts which are solely in a shear mode.
[0019] In operation of the cantilevered chair 43 the operator sits on cushion 45 while resting his or her back against backrest 44 . The console and keyboard 46 is positioned in front of the operator's chair 43 . In the embodiment shown one end of double triad elastomers 40 and 41 are adhesively secured directly to the chair 43 and the other end of the double triad elastomer mounts are adhesively secured directly to wall member 42 . That is, in certain applications the wall 42 or a portion of the equipment can be directly secured to the double triad elastomers without the use of separate plate members. In order to reduce torsional forces on an individual elastomer it is preferred to space the elastomer members laterally from each other.
[0020] Thus the present invention also includes a method of isolating a wall hung article from shock and vibration comprising the steps of: 1. securing a first end of a first elastomer mount to one surface of an article; 2. laterally securing a first end of a second elastomer mount to the one surface of an article; 3. securing a second end of the first elastomer to a support surface; and 4. laterally securing a second end of the second elastomer to the support surface whereby the first elastomer mount and the second elastomer mount cantileverly support the article with each of the elastomer mounts having laterally offset support surfaces to provide shear resistance to compressive forces thereon.
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A system for isolating wall hung equipment from shock and vibration including a wall mountable support or fixture having a first member for securing to a wall and a second member for securing to equipment with a plurality of triad elastomers mounted therebetween to cantleverly support the equipment and at the same time isolate the equipment from shock and vibration. The elastomer mounts while permitting displacement of the members with respect to one another inhibit the members from contacting each other when one or the other is subject to shock or vibration.
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