description
stringlengths 2.98k
3.35M
| abstract
stringlengths 94
10.6k
| cpc
int64 0
8
|
|---|---|---|
TECHNICAL FIELD
[0001] The present invention relates generally to electronic devices, particularly portable electronic devices and more specifically to portable electronic devices having multiple body elements configurable to predetermined fixed orientations each of which define a respective different operative position.
BACKGROUND OF THE INVENTION
[0002] The demand by users and the purchasing public that portable electronic devices, particularly mobile telephone devices, become increasing smaller and lighter while at the same time providing an increasing number of different functions in addition to the basic telephone communication functions places a premium on available surface space for the user interfaces necessary to carryout the intended functions and operations of the associated features. In addition, there is also a demand for larger size screens for displaying images, for example, taken with a camera built into the mobile telephone or for displaying received images such as streaming video. This demand has required the manufacturer of such devices to design and develop innovative device enclosures capable of reconfiguration from one operative position to another to provide the necessary user interface to operate the device and to accommodate larger size screens. One such commonly known prior art mobile telephone device enclosure is the “flip” phone wherein the cover of the device is hinged to a main body element which carries a user interface relative to usage and the cover is “flipped” to open the device to make the user interface assessable to the user. The inside surface of the cover carries a screen to display alphanumeric characters, graphics, images and other representations common to such mobile telephone devices and which are commonly known in the trade and by the consuming public. The “flip” phone enclosure configuration provides one method to expand the user interface surface and provide a larger screen display area while maintaining a relatively smaller size device enclosure compared to other mobile telephone devices wherein the user interface and the screen share a common surface area.
[0003] Another prior art mobile telephone device enclosure as illustrated, for example, in FIGS. 1A-1C is the “slide” phone generally designated 10 wherein the cover 12 overlays a main body element 14 and is arranged for sliding engagement with the main body element 14 . The cover 12 carries a screen 16 and may include keys 18 to carry out various intended functions of the device when the cover 12 is in its overlying operative position as shown in FIG. 1A . The device is configured to a second operative position when the cover 12 is slid by a user in the direction shown by arrow 20 to expose a surface 22 of the main body element 14 as shown in FIG. 1B wherein the surface 22 carries a user interface 24 which may be an arrangement of keys 26 in a desired pattern to carry out the intended function such as inputting a telephone number or entry of alphanumeric characters to the device in a well known manner. The device is returned to its closed operative position by sliding the cover 12 in the direction shown by the arrow 21 . Although such “slide” phones provide ease of usage in changing from one operative position to another operative position, the increase in effective user interface area provided by prior art “slide” phones is not as effective as “flip” phones because of the limited movement of the cover 12 with respect to the main body element 14 . As schematically illustrated in FIG. 1C , an overlap of the cover 12 and main body element 14 represented by the length 28 is typically a 50 percent overlap and results in a hidden area 30 between the cover 12 and main body element 14 to maintain rigidity of the “slide” phone in its extended open position and thus the hidden area 30 of the main body element surface 22 is not available for usage as a user interface or for any other function.
[0004] Accordingly, there is a need to provide a portable electronic device that overcomes the limitations and disadvantages of the prior art portable electronic devices wherein one body element is arranged to move relative to another body element to increase the effective user interface area.
[0005] It is an object of the present therefore to provide a portable electronic device wherein one body element is arranged to move relative to another body element from an overlapping closed operative position to a non-over lapping operative position to maximize the surface area relative to usage of each body element.
[0006] It is a further object of the present invention to provide a portable electronic device wherein one body element is arranged to move relative to another body element to maximize the surface area relative to usage of each body element for use as a user interface.
[0007] It is a yet further object of the present invention to provide a portable electronic device wherein one body element is arranged for relative movement with respect to another body element to configure the body elements in a number of different predetermined fixed orientations each of which define a different operative position.
SUMMARY OF THE INVENTION
[0008] In a first aspect of the invention, a portable electronic device is presented and has a first main body element having a first major surface relative to usage and a second body element having a first major surface relative to usage. The second body element is mechanically coupled and arranged for relative movement with respect to the first main body element to configure the first main body element and the second body element in a number of different predetermined fixed orientations, each of which predetermined fixed orientations define a corresponding different operative position of the portable electronic device.
[0009] In a second aspect of the invention, the first main body element and the second body element are in overlying relationship with one another and the second body element includes a display constructed in at least a portion of its first major surface, and the first main body element includes a first keypad arrangement in at least a portion of its first major surface. The first main body element and the second body element are further arranged for slidable movement with respect to one another between a first operative position and a second operative position wherein in the first operative position the first keypad arrangement is covered by the second body element and not accessible by a user and wherein in the second operative position the second body element is slidably moved along a linear path in a first direction to expose the first keypad arrangement for access and use by a user.
[0010] In a third aspect of the invention, the first main body element includes a second keypad arrangement in a different portion of its first major surface from the portion of the first keypad arrangement. The first main body element and the second body element are further arranged for relative slidable movement to a third operative position wherein the second body element is slidingly movable along a linear path in a second direction opposite to the first direction to cover the first keypad arrangement and to expose the third keypad arrangement for access and use by a user.
[0011] In a fourth aspect of the invention, the second body element further includes a second major surface disposed opposite the second body element first major surface and in facing relation to the first main body element first major surface. The second body element further includes a camera imaging lens constructed in an end marginal portion of the second major surface whereby the camera imaging lens is exposed for taking pictures when the portable electronic device is in its third operative position.
[0012] In a fifth aspect of the invention, a mechanism is provided for coupling the first main body element to the second body element whereby movement of one of the first main body element and the second body element in one direction causes the other of the first main body element and the second body element to move in the opposite direction.
[0013] In a sixth aspect of the invention, the second body element is nested within the first main body element in the first operative position. The second body element includes a first and second portion with each respective portion extending from opposite ends of the first main body element when the portable electronic device is in its second operative position. The first and second portions are further arranged for carrying respective portions of the first major surface whereby the first and second portions of the first major surface are exposed and accessible by a user.
[0014] In a seventh aspect of the invention, the first and second portions of the first major surface are further constructed to carry a keypad arrangement.
[0015] In an eighth aspect of the invention. a first sliding mechanism is provided for coupling the first main body element to the second body element wherein the first sliding mechanism has a major surface relative to usage and includes a keypad arrangement constructed in at least a portion of the sliding mechanism major surface. The first main body element and the first sliding mechanism and the second body element are in an overlying stacked relationship with respect to one another in a first operative position. The second body element is arranged for slidable movement in a lengthwise direction with respect to the first main body element and the first sliding mechanism to uncover the keypad arrangement constructed in the at least a portion of the sliding mechanism major surface for access by a user in a second operative position when moved from the first operative position. The second body element and the sliding mechanism are further arranged for slidable movement in a direction perpendicular to the lengthwise direction whereby the second body element and the sliding mechanism move together to uncover the first main body element first major surface for access by a user in a third operative position when moved from the first operative position.
[0016] In a ninth aspect of the invention, the second body element includes a display constructed in at least a portion of its first major surface.
[0017] In a tenth aspect of the invention, the first main body element includes a keypad arrangement constructed in a least a portion of its first major surface.
[0018] In an eleventh aspect of the invention, the keypad arrangement is a QWERTY keypad arrangement.
[0019] In a twelfth aspect of the invention, a second sliding mechanism is provided for coupling the first main body element to the second body element and includes a major surface relative to usage wherein a first portion is exposed and accessible by a user when the second body element is in a fully extended configuration in a first direction defining a first operative position wherein a first portion of the first major surface of the first main body element is exposed and accessible by a user, and wherein the second sliding mechanism major surface further includes a second portion that is exposed and accessible by a user when the second body element is in a fully extended configuration in a second direction opposite the first direction defining a second operative position wherein a second portion of the first major surface of the first main body element is exposed and accessible by a user.
[0020] In a thirteenth aspect of the invention, the second body element has a second major surface relative to usage disposed on the opposite side of the second body element first major surface. A foldable hinge frame is provided for coupling the first main body element and the second body element. In a first operative position the first main body element and the second body element are in an overlying stacked relationship with one another and the second body element second major surface is exposed and accessible by a user and the first main body element first major surface is covered by the second body element. In a second operative position the second body element is unfolded along a first hinge axis to a first fully extended position whereby the second body element first major surface and the first main body element first major surface are exposed and accessible by a user. In a third operative position the second body element is unfolded along a second hinge axis to a second fully extended position whereby the second body element first major surface and the first main body element first major surface are exposed and accessible by a user.
[0021] In a fourteenth aspect of the invention, the foldable hinge frame has a peripheral marginal surface area defining a window to permit access and viewing of the first main body element first major surface when the portable electronic device is in its second operative position, and to permit access and viewing of the second body element first major surface when the portable electronic device is in its third operative position.
[0022] In a fifteenth aspect of the invention, the foldable hinge frame includes a keypad arrangement constructed in a portion of the foldable hinge frame marginal surface area on one side of the foldable hinge frame. The keypad arrangement is active and operative when the portable electronic device is in its second operative position.
[0023] In a sixteenth aspect of the invention, the foldable hinge frame includes a keypad arrangement constructed in a portion of the foldable hinge frame marginal surface area on both sides of the foldable hinge frame. The keypad arrangement is active and operative when the portable electronic device is in a respective operative position wherein the keypad arrangement is exposed and accessible by a user.
[0024] In a seventeenth aspect of the invention, a swivel arm mechanism sandwiched between the first main body element and the second body element is provided for coupling the first main body element to the second body element. In a first operative position the first main body element and the second body element are in an overlying stacked relationship with one another and the second body element first major surface is exposed and accessible by a user and the first main body element first major surface is covered by the second body element. In a second operative position the second body element moves in a plane along a first arcuate path in a first direction from its overlying stacked relationship with the first main body element to a fully open orientation to uncover the first main body element first major surface for access by a user. In a third operative position the second body element moves in a plane along a second arcuate path in a second direction opposite the first direction from its overlying stacked relationship with the first main body element to a lengthwise extended orientation to uncover a portion of the first main body element first major surface for access by a user.
[0025] In an eighteenth aspect of the invention, a keypad arrangement is constructed in the first main body element first major surface.
[0026] In a nineteenth aspect of the invention, the keypad arrangement is a QWERTY keypad arrangement.
[0027] In a twentieth aspect of the invention, a screen display is constructed in the second body element first major surface.
[0028] In a twenty-first aspect of the invention, a pair of swivel arms are sandwiched between the first main body element and the second body element.
[0029] In a twenty-second aspect of the invention, a swivel plate mechanism made up of a pair of swivel plates sandwiched between the first main body element and the second body element is provided for coupling the first main body element to the second body element. Each of the swivel plates has a major surface relative to usage. In a first operative position the first main body element and the second body element are in an overlying stacked relationship with one another and the second body element first major surface is exposed and accessible by a user and the first main body element first major surface is covered by the second body element. In a second operative position the second body element moves in a plane along a first arcuate path in a first direction from its overlying stacked relationship with the first main body element to a fully open orientation to uncover the first main body element first major surface for access by a user. One of the swivel plates is arranged for rotation along a second arcuate path and the other of the swivel plates is arranged for rotation along a third arcuate path with each of the swivel plates rotating from its respective sandwiched position as the second body element moves to the fully open orientation whereby each swivel plate major surface is exposed and accessible to a user when the portable electronic device is in its second operative position.
[0030] In a twenty-third aspect of the invention, an input device is constructed in the swivel plate major surface.
[0031] In a twenty-fourth aspect of the invention, a swivel arm mechanism sandwiched between the first main body element and the second body element is provided for coupling the first main body element to the second body element. The swivel arm mechanism has a major face surface relative to usage and has two pivot points spaced along a central lengthwise axis wherein the first pivot point is coupled to a first cooperating pivot located along a central lengthwise axis of the second body element and wherein the second pivot point is coupled to a second cooperating pivot located along a central lengthwise axis of the first main body element. In a first operative position the first main body element and the swivel arm mechanism and the second body element are in an overlying stacked relationship with one another and the second body element first major surface is exposed and accessible by a user and the first main body element first major face surface and the swivel arm major face surface are covered. In a second operative position the swivel arm mechanism and the first main body element are in an overlying stacked relationship with one another and rotated about the swivel arm mechanism first pivot point and the second body element first cooperating pivot whereby a portion of the swivel arm mechanism major face surface is exposed and accessible by a user and the first main body element first major surface is covered by the swivel arm mechanism. In a third operative position the first main body element is rotated about the swivel arm mechanism second pivot point and the first main body element second cooperating pivot along an arcuate path in a direction toward the second body element wherein a portion of the first main body element major face surface and the portion of the swivel arm mechanism major face surface are exposed and accessible by a user.
[0032] In a twenty-fifth aspect of the invention, a first keypad arrangement is constructed in the first main body element major face surface, a second keypad arrangement is constructed in the portion of the swivel arm mechanism major face surface, and a display screen is constructed in the major face surface of the second body element.
[0033] In a twenty-sixth aspect of the invention, the first keypad arrangement is a QWERTY keypad arrangement.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Additional features, objects and advantages of the present invention will become readily apparent from the following written description taken in conjunction with the drawings wherein:
[0035] FIG. 1A is a top plan view of a prior art slide mobile telephone in its closed operative position;
[0036] FIG. 1B is a top plan view of the slide mobile telephone of FIG. 1A in its open operative position;
[0037] FIG. 1C is a schematic side view of the mobile telephone of FIG. 1B illustrating the overlapping area between the cover and main body element.
[0038] FIG. 2A is a schematic perspective view of a first embodiment of the present invention showing a mobile telephone in a first operative position;
[0039] FIG. 2B shows the mobile telephone of FIG. 2A in a second operative position;
[0040] FIG. 2C shows the mobile telephone of FIG. 2A in a third operative position;
[0041] FIG. 2D is a rear schematic perspective view of the mobile telephone shown in FIG. 2C ;
[0042] FIG. 3A is a schematic perspective view of a second embodiment of the present invention showing a mobile telephone in a first operative position;
[0043] FIG. 3B is a schematic side view of the mobile telephone shown in FIG. 3A ;
[0044] FIG. 3C shows the mobile telephone of FIG. 3A in a fully open second operative position;
[0045] FIG. 3D is a schematic side view of the mobile telephone shown in FIG. 3C ;
[0046] FIGS. 4A-4I illustrate schematically a third embodiment of the present invention showing a mobile telephone having a sliding mechanism sandwiched between the first main body element and the second body element whereby the mobile telephone has a closed operative position ( FIG. 4A ), a vertically open operative position ( FIG. 4D ) and a horizontally open operative position ( FIG. 4G ).
[0047] FIGS. 5A-5H illustrate schematically a fourth embodiment of the present invention showing a mobile telephone having a sliding mechanism sandwiched between the first main body element and the second body element whereby the mobile telephone has a closed operative position ( FIG. 5A ), a first vertically open operative position in a first direction ( FIG. 5E ) and a second vertically open operative position in a second direction ( FIG. 5G ) opposite the first direction;
[0048] FIGS. 6A-6E illustrate schematically a fifth embodiment of the present invention showing a mobile telephone having a foldable hinge frame sandwiched between the first main body element and the second body element whereby the mobile telephone has a vertical operative position ( FIG. 6B ) and a horizontal operative position ( FIG. 6C );
[0049] FIGS. 7A-7D illustrate schematically a sixth embodiment of the present invention showing a mobile telephone having a pair of swivel arms sandwiched between the first main body element and the second body element whereby the mobile telephone has an open horizontal operative position ( FIG. 7C ) and an open vertical operative position ( FIG. 7D );
[0050] FIGS. 8A-8D illustrate schematically a seventh embodiment of the present invention showing a mobile telephone having a pair of swivel plates sandwiched between the first main body element and the second body element whereby the mobile telephone has a closed operative position ( FIG. 8A ) and an open horizontal operative position ( FIG. 8D ).
[0051] FIGS. 9A-9F illustrate schematically an eighth embodiment of the present invention showing a mobile telephone having a single swivel arm sandwiched between the first main body element and the second body element whereby the mobile telephone has a closed operative position ( FIG. 9A ), an open vertical operative position revealing a first user interface area carried by the swivel arm ( FIG. 9E ) and a horizontal operative position revealing a second user interface area carried on the first main body element and the first user interface area carried on the swivel arm ( FIG. 9F ).
DESCRIPTION OF PREFERRED EMBODIMENTS
[0052] Turning now to the drawings and considering the invention in further detail, a schematic perspective view of a first embodiment of the portable electronic device of the present invention is illustrated schematically in FIGS. 2A-2D and shows for purposes of explanation of the invention a mobile telephone generally designated 32 in FIG. 2A in a first or closed operative position. As shown in FIG. 2A , the mobile phone 32 includes a first main body element 34 and a stacked or overlying second body element generally designated 36 arranged for relative movement with respect to the main body element 34 along a linear path in a first direction represented by arrow 38 and in an opposite second direction indicated by arrow 40 as discussed in further detail below. The second body element 36 includes a first major surface generally designated 42 relative to usage. The first major surface 42 of the second body element 36 may include a screen generally designated 44 constructed in at least a portion generally designated 46 of the first major surface 42 . The second body element 36 may also include a second keypad arrangement generally designated 48 in at least another portion generally designated 50 of the first major surface 42 . As illustrated in FIG. 2B , the second body element 36 is shown slid in the direction of arrow 38 with respect to the main body element 34 to a second or open operative position to reveal and expose a first keypad arrangement generally designated 52 carried in at least a portion 54 of a first major surface 56 relative to usage of the first main body element 34 . As can be seen, the first keypad arrangement 52 is covered by the second body element 36 and not accessible by a user when the mobile telephone 32 is in its first operative position. In its second operative position as illustrated in FIG. 2B , the first keypad arrangement 52 is available as a user interface to operate the mobile telephone and any associated functions such as PDA functions in a manner well known to those skilled in the art and by the consuming public. FIG. 2C shows the mobile telephone 32 of FIG. 2A in an open or third operative position wherein the second body element 36 is slid in the direction shown by arrow 40 to reveal and expose a third keypad arrangement generally designated 58 constructed in the first major surface 56 of the main body element 34 in a portion 60 at the end 62 opposite the portion 54 of the main body element carrying the first keypad arrangement 52 . The third keypad arrangement 56 is usable as a further user interface to operate additional features and function of the mobile telephone 32 . For example, as illustrated in FIG. 2D , the mobile telephone 32 in its open or third operative position may reveal a camera imaging lens generally designated 64 carried in a second major surface 66 disposed opposite the first major surface 42 of the second body element 36 . A user may aim the camera imaging lens 64 in the direction of the object or person whose image is to be captured and view the captured image on the screen 44 and operate one of the designated keys of the keypad arrangement 48 or 58 as required to activate the camera imaging function of the mobile telephone 32 . The second body element 36 may be directly attached for slidable movement with respect to the first main body element 34 as shown in a schematic side view in FIG. 2E which represents the closed or first operative position. FIG. 2F is a schematic representation of the open or second operative position of the mobile telephone 32 wherein the second body element 36 is shown extended in one direction relative to the first main body element 34 . FIG. 2G is a schematic representation of the mobile telephone 32 in its open or third operative position wherein the second body element 36 is shown extended in the opposite direction with respect to the second operative position. Alternately, the second body element 36 may be arranged for slidable movement with respect to the first main body element 34 by means of a sliding mechanism 68 sandwiched between the first main body element 34 and the second body element 36 to couple the first main body element and the second body element for relative movement with respect one another between the first, second and third operative positions as illustrated in FIGS. 2H, 2I and 2 J respectively. The sliding mechanism may be arranged such that movement of one of the second body element or first main body element causes the other of the second body element and first main body element to move in the opposite direction of the element being moved by the user. Such a mechanism may be motor driven and mechanically couple the second body element and first main body element through a set of gears, belts or other mechanical coupling devices well known to those skilled in the art.
[0053] Turning now to FIGS. 3A-3D , a schematic perspective view of a second embodiment of the portable electronic device of the present invention shows a mobile telephone generally designated 70 in a closed or first operative position in FIGS. 3A and 3D . The mobile telephone 70 includes a first main body element 72 having a first major surface 74 relative to usage in an upwardly facing exposed configuration. A screen generally designated 76 is constructed in at least a portion of the first major surface 74 . Keys 78 are constructed in at least a further portion of the first major surface 74 and which keys are operated by a user to carry out the intended function. The keys 78 are shown carried in one end region 82 although other locations and placements are contemplated in accordance with the particular design and function to be carried out. In addition, the mobile telephone 70 may include a user input device generally designated 80 which operates in a well known manner to control the direction of movement of a cursor for example on the display shown on the screen 76 or to carry out other intended functions as well known and understood to those skilled in the art. The mobile telephone 70 includes a second body element further comprising a first portion 90 and a second portion 94 nested within the first main body element 72 and unexposed and inaccessible with respect to usage in the closed or first operative position. In the second operative position as illustrated in FIG. 3B and FIG. 3D , the first portion 90 and second portion 94 extend from opposite end regions 82 and 84 respectively of the main body element 72 . The mobile telephone 70 is reconfigured from its closed or first operative position to its open or second operative position the second body element first portion 90 is slid or extended away from the main body element in the direction as indicated by the arrow 88 and the second body element second portion 94 is slid or extended from the main body element in the opposite direction as shown by direction arrow 86 . The second body element first portion 90 has a first major surface 92 relative to usage which may include an arrangement of keys 98 to carry out an intended function and which first major surface 92 is exposed and accessible by a user in the open or second operative position. The second body element second portion 94 also includes a first major surface 96 relative to usage and which first major surface is exposed and accessible by a user and may carry an arrangement of keys 100 to carry out an intended function. The major surfaces 92 , 96 do not have to carry keys and may be alternatively configured and arranged as required as an intended user interface to carry out the intended function.
[0054] A third embodiment of the portable electronic device of the present invention is illustrated schematically in FIGS. 4A-4I which show a mobile telephone generally designated 102 having a sliding mechanism 112 sandwiched between the first main body element 110 and the second body element 104 and for mechanically coupling the body elements 110 and 104 to on another. The mobile telephone 102 has a closed or first operative position as illustrated in FIGS. 4A, 4B and 4 C wherein the first main body element 110 and the sliding mechanism 112 and the second body element 104 are in an overlying stacked relationship with respect to one another. The second body element 104 has a first major surface 106 relative to usage and includes a screen 108 constructed in at least a portion of the first major surface 106 . The second body element 104 is arranged for sliding engagement with the first main body element 110 in the direction as shown by the arrow 116 by means of oppositely disposed marginal legs 130 , 130 extending lengthwise of the second body element 104 . The legs 130 , 130 are received in and co-act with respective oppositely disposed channels 132 , 132 located lengthwise in the marginal areas of the sliding mechanism 112 . The mobile telephone 102 has a vertically open or second operative position schematically illustrated in FIGS. 4D, 4E and 4 F wherein the second body element 104 is slid or extended in a vertical direction as indicated by the arrow 116 with the lengthwise marginal legs 130 sliding lengthwise in the channels 132 of the sliding mechanism 112 as illustrated in FIG. 4E . The second body element 104 is slid vertically in the direction of arrow 116 to reveal a portion 134 of the sliding mechanism 112 and expose a major surface 120 of the sliding mechanism for use as a user interface. As illustrated in FIG. 4D , the major surface 120 may carry keys 122 arranged to carry out an intended function.
[0055] As illustrated schematically in FIGS. 4G, 4H and 41 , the second body element 104 and the sliding mechanism 112 are also arranged for slideable movement in a direction indicated by arrow 118 perpendicular to the lengthwise direction whereby the second body element 104 and the sliding mechanism 112 move together to uncover the first main body element 110 which exposes a first major surface 124 for access by a user in the horizontal open or third operative position. The first major surface 124 carries an arrangement of keys 126 configured to carry out an intended function and is illustrated for example as a QWERTRY keyboard in FIG. 4G . The slide mechanism 112 includes leg portions 114 , 114 which are slidingly engaged for movement in slide tracks 128 , 128 along the marginal opposite end regions 136 , 136 of the slide mechanism 112 .
[0056] A fourth embodiment of the portable electronic device of the present invention is illustrated schematically in FIGS. 5A-5I wherein a mobile telephone 160 has a sliding mechanism generally designated 168 sandwiched between the first main body element 166 and the second body element 162 . The second body element 162 has a major surface 163 relative to usage and may carry a screen 164 . As illustrated in the side view shown in FIG. 5B , the first main body element 166 has an upper or top edge portion 180 and a lower or bottom edge 186 . The second body element has an upper or top edge portion 184 and a lower or bottom edge portion 182 . The main body element 166 and the second body element 162 are arranged for sliding engagement with respect to one another by means of a sliding mechanism 168 in the form of a plate sandwiched between the two elements. Oppositely disposed legs 176 , 176 formed in the second body element are received in a lengthwise channel 170 formed by oppositely disposed tabs 172 and 174 extending from the ends of the sliding mechanism 168 as illustrated in the fragmentary view shown in FIG. 5D . The main body element 166 is likewise mechanically coupled to the sliding mechanism 168 by means of oppositely disposed legs 178 , 178 received in the lengthwise channel 170 of the sliding mechanism 168 as illustrated in the fragmentary view shown in FIG. 5D . It will be seen that such an arrangement allows relative lengthwise movement between the main body element 166 , the sliding plate mechanism 168 and the second body element 162 . As illustrated in FIGS. 5E and 5F , the second body element 162 is slid or extended in a first vertical lengthwise direction as indicated by the direction arrow 165 relative to the main body element 166 and the sliding mechanism 168 and which sliding movement of the second body element 162 also causes the sliding mechanism 168 to move in the direction indicated by arrow 165 to the first vertically open operative position. In the first vertically open operative position, the lower edge 182 of the second body element is in approximately alignment with the upper edge 180 of the first main body element wherein approximately 50% of the upper portion 167 of the sliding mechanism 168 supports the second body element 162 . The other half portion 169 of the sliding mechanism 168 supports the first main body element 166 . The sliding mechanism includes a first major surface portion relative to usage generally designated 188 and which portion is revealed or exposed when the second body element is extended fully in the direction shown by the arrow 165 with respect to the first main body element 166 . The first surface portion 188 may provide a user interface area and carry keys arranged as keypad or other desirable user input device to carry out an intended function. Also in the fully open vertical operative position, a first surface portion 190 of the first main body element 166 is revealed and accessible to a user. The first major surface 190 may function as a further user interface area and carry a keypad or other desired user input device in accordance with the intended function. The second body element 162 may also be moved in an opposite direction with respect to the first main body element 166 and the sliding mechanism 168 as indicated by the direction arrow 195 to a second vertical open operative position as illustrated in FIG. 5G . In the second vertically open operative position, a second surface portion 192 of the sliding mechanism 168 is revealed and may be arranged as a further user interface and include a desired user input device to carry out an intended function of the mobile telephone 160 . Also in the second vertically open operative position, a second surface portion 194 of the main body element 166 is revealed and accessible to a user and likewise may carry a further user interface or user input device to carry out the intended function. Accordingly, the embodiment illustrated in FIGS. 5A-5H provides for at least four different user interface areas in the mobile telephone 160 .
[0057] A fifth embodiment of the portable electronic device of the present invention is illustrated schematically in FIGS. 6A-6E which show a mobile telephone generally designated 200 having a foldable hinge frame 212 sandwiched between a first main body element 202 and a second body element 206 . The second body element 206 is arranged for relative movement with respect to the first main body element 202 between a first or closed operative position as illustrated schematically by end and side views in FIGS. 6D and 6E respectively, and a vertical open operative position as shown in the top plan view in FIG. 6B and a third or horizontal open operative position as illustrated in the top plan view in FIG. 6C . The first main body element 202 has a first major surface 204 relative to usage and may carry an arrangement of keys forming a keypad generally designated 224 to carry out an intended function. The second body element 206 includes a first major surface 208 and an oppositely disposed second major surface 210 . A screen 226 may be constructed in a portion of the surface 208 . The second body element 206 is hingedly connected to the folding hinge frame 212 by means of a hinge 211 along the first hinge axis 214 passing through the intersection of one end 209 of the second body element 206 and one end 215 of the hinge frame 212 . The second body element 206 is arranged for rotation about the hinge axis 214 in a direction indicated by the rotation direction arrow 230 as the second body element 206 is moved as indicated by the arrow 232 toward and away from the hinge frame first major surface 220 . The first main body element 202 is hingedly connected to the foldable hinge frame 212 by means of a hinge 219 formed between the intersection of one side 221 of the hinge frame 212 and one side 207 of the first main body element 202 . The first main body element 202 is arranged for rotation about the hinge axis 216 as indicated by the rotation direction arrow 228 when the hinge frame 212 is moved toward and away from the first major surface 204 of the first main body element 202 as indicated by the direction arrow 234 . As illustrated in FIGS. 6D and 6E , in the closed position the major surface 208 of the second body element 206 is rotated about the axis 214 into a facing face-to-face relationship with the surface 220 of the hinge frame 212 . The hinge frame 212 is rotated about the axis 216 in the direction of rotation arrow 228 such that the surface 222 of the hinge frame is in a face-to-face orientation with respect to the first major surface 204 of the first main body element 202 . When the second body element 206 is rotated about the axis 214 to the vertical operative position as illustrated in FIG. 6B the major surface 208 of the second body element 206 lies in substantially the same plane as the major surface 220 of the hinge frame 212 and the keys 224 are accessible by a user through a window 218 defined in the hinge frame. When the second body element 206 and the hinge frame 212 are rotated together about the axis 216 to the horizontal operative position as illustrated in FIG. 6C the major surface 222 of the hinge frame 212 lies substantially in the same plane as the major surface 204 of the first main body element 202 . The screen 226 is viewable through the window 218 in the hinge frame 212 . The keys forming the keypad arrangement 224 are arranged to carry out the intended function and may be for example a QEWTRY keyboard. Further, the device includes appropriate electronics to orient the display shown on the screen 226 from a vertical to horizontal orientation as required depending on the operative position of the mobile telephone 200 .
[0058] A sixth embodiment of the present invention is illustrated in FIGS. 7A-7D which show a mobile telephone generally designated 250 having swivel arms 262 , 264 sandwiched between a first main body element 252 and a second body element 254 for mechanically coupling the first main body element to the second body element. The second body element 254 includes a first major surface 256 . A screen 258 is constructed in at least a portion of the surface 256 . Keys 260 , 260 are also provided in another portion of the surface 256 for use in operating and carrying out the intended functions of the mobile telephone. In the first operative closed position as illustrated in FIGS. 7A and 7B , the second body element is in an overlying stacked relationship with the first main body element 252 such that the first major surface 256 of the second body element 254 is exposed and accessible by a user and the first major surface 276 of the first main body element 252 is covered by the second body element. The second body element 254 is moved from the first or closed operative position to a second or horizontal operative position as illustrated in FIG. 7C by moving or swiveling the second body element in a direction indicated by the arrow 274 . The second body element 254 follows along a curved path and retains its orientation relative to the closed operative position as illustrated in FIG. 7A . The second body element 254 is in a top-bottom configuration with respect to the first main body element 252 in the second horizontal operative position as illustrated in FIG. 7C . An arrangement of keys forming a keypad 278 is constructed in the major surface 276 of the first main body element 252 and which keys are exposed and accessible to a user when the second body element is swiveled to its open horizontal position. The second body element 254 may be moved or swiveled with respect to the first main body element 252 and follow along a curved path indicated by the direction arrow 280 to a third or vertical open operative position as illustrated in FIG. 7D . A portion of the key arrangement 278 is exposed for access and operation by a user in the vertical open operative position. The pivot arms 262 and 264 may be used to carry power and data connections between the first main body element 252 and the second body element 254 . Alternately, the data connection may be made via an optical link established and constructed between the first main body element 252 and the second body element 254 .
[0059] Turning now to FIGS. 8A-8D , a sixth embodiment of the present invention is illustrated schematically therein showing a mobile telephone generally designated 290 wherein a pair of swivel plates 302 , 304 are sandwiched between the first main body element 292 and a second body element 296 for mechanically coupling the first main body element to the second body element. The swivel plate 302 is pivotally connected at the pivot point 301 to the first main body element 292 . The swivel plate 302 is pivotally connected to the second body element 296 at the pivot point 303 . In a similar manner, the swivel plate 304 is coupled to the first main body element 292 at the pivot point 305 and coupled to the second body element 296 at the pivot point 307 . It can be seen that the connection arrangement between the second body element 296 , swivel plates 302 and 304 and the first main body element 292 form a parallelogram such that movement of the second body element 296 along the arcuate path indicated by the direction arrow 310 causes the swivel plate 302 to follow along the arcuate path as indicated by the direction arrow 312 and the swivel plate 304 to follow an arcuate path as indicated by the direction arrow 314 as the second body element 296 moves in the same plane maintaining its orientation as in the closed position illustrated in FIG. 8A to the open horizontal operative position as illustrated in FIG. 8D . The swivel plates 302 and 304 move with the second body element 296 until the mobile telephone is in the horizontal operative position. The second body element 296 includes a major surface 298 which may carry a screen 300 . The first main body element 292 includes a first major surface 294 relative to usage and may carry an arrangement of keys arranged to carryout the intended function and may be a keyboard for example, a QWERTY keyboard. The swivel plate 302 includes a major surface 306 relative to usage and provides an area for a user interface such as a keypad arrangement or other user input device. The swivel plate 304 also includes a major surface 308 relative to usage and likewise may carry an arrangement of keys or other user input device. Power and data connections between the main body element 292 , swivel plates 302 and 304 and the second body element 296 may be carried via the pivot connections. Alternately, the data connection may be via an optical link between the main body element 292 , swivel plates 302 and 304 and the second body element 296 .
[0060] An eighth embodiment of the portable electronic device of the present invention is illustrated schematically in FIGS. 9A-9F and show a mobile telephone 330 having a swivel arm body 338 sandwiched between a first main body element 346 and a second body element 332 such that the swivel arm body 338 mechanically couples the main body element 346 to the second body element 332 . The mobile telephone 330 has a first operative position as illustrated in FIG. 9A wherein the second body element 332 and the swivel arm body 338 and the main body element 346 are in an overlying stacked relationship with one another and the second body element major surface 334 is exposed and accessible by a user and the first main body element major face surface 348 and the swivel arm body major face surface 340 are covered. The second body element 332 is pivotally coupled at the pivot point 354 to the swivel arm body 338 at the pivot point 356 . The swivel arm body 338 is pivotally coupled at the pivot point 358 to the main body element 346 at the pivot point 360 . The second body element pivot point 354 lies on a lengthwise center axis 366 and is spaced a distance D 1 from the edge 372 . The pivot point 360 of the main body element lies on a lengthwise center axis 370 and is spaced a distance D 1 from the edge 374 . The pivot points 356 and 358 lie on a lengthwise center axis 368 . The pivot point 356 is spaced a distance D 1 from the edge 376 and the pivot point 358 is spaced a distance D 1 from the edge 378 . A user interface 342 is defined in at least a portion of the major surface 340 of the swivel arm body and may carry an arrangement of keys 344 to carryout an intended function. A user interface 350 is defined in at least a portion of the major surface 348 of the main body element 346 and may carry an arrangement of keys 352 to carryout an intended function. The mobile telephone 330 has a second or vertically open operative position as illustrated in FIG. 9E wherein the swivel arm body 338 and main body element 346 are rotated about the second body element 332 pivot point 354 and the cooperating pivot point 356 along an arcuate path as indicated by the direction arrow 362 to expose the keypad 334 for access and use by a user. The swivel arm body 338 is in an overlying stacked relationship with the main body element 346 in the vertical operative position as shown in FIG. 9E . The mobile telephone 330 has a third or horizontal operative position as illustrated in FIG. 9F wherein the main body element 346 is rotated about the pivot point 360 and the cooperating pivot point 358 of the swivel arm body 338 along an arcuate path as indicated by direction arrow 364 to expose the keypad arrangement 352 for access and use by a user. The second body element 332 is rotated about the pivot point 354 and cooperating pivot point 356 of the swivel body 338 along an arcuate path as indicated by the direction arrow 364 whereby the orientation of the screen 336 is in a horizontal orientation. Power and data connections are made between the main body element 346 , swivel arm body 338 and second body element 332 via the pivot point connections. Further, the keys of the keypad arrangement 352 may be arranged to carry out an intended function such as for example a QWERTY keyboard.
|
Multiple body element portable electronic devices are configurable to predetermined fixed orientations each of which define a respective different operative position wherein one body element is arranged to move relative to another body element from an overlapping closed operative position to a non-overlapping operative position to maximize the surface area relative to usage of each body element. The multiple body elements may be arranged for slidable, hinged and swivel movement with respect to one another.
| 6
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims under 35 U.S.C. §119(a) the benefit of Korean Patent Application No. 10-2012-0024182 filed Mar. 9, 2012, the entire contents of which are incorporated herein by reference.
BACKGROUND
[0002] (a) Technical Field
[0003] The present invention relates to an apparatus and method for recovering energy after carbon dioxide capture. More particularly, it relates to an apparatus and method for recovering energy after carbon dioxide capture, which can recover energy from a discharge pressure of captured carbon dioxide when the captured carbon dioxide is treated by a method such as fixation or conversion.
[0004] (b) Background Art
[0005] Generally, methods for capturing carbon dioxide include an absorption method, an adsorption method, and a separation membrane method. Absorption methods can treat a large amount of exhaust gas compared to adsorption methods and separation membrane methods, and provides a high removal efficiency even in cases when the CO 2 concentration condition is about 7% to about 30%. Further, adsorption methods have a high economical efficiency and are easy to apply.
[0006] The carbon dioxide, once captured, can then be stored, or can be treated by fixation and conversion methods. Among these, the method of storing CO 2 in the ground or deep sea is easy even with a large amount of CO 2 , in contrast to the other treatment methods. Such storage methods are currently available are have been commercialized. However, the cost for storing CO 2 in the ground or deep sea is high, and the stored CO 2 cannot be fundamentally removed, making additional profit-making difficult.
[0007] The methods of converting captured CO 2 into other chemical substances using CO 2 as a carbon source, and fixing CO 2 using plants and seaweeds are both being studied. If such methods reach a commercialization stage, CO 2 can be fundamentally removed, and useful products produced thereby can allow for additional profit-making. Accordingly, these methods are being evaluated as more economical and preferable technologies.
[0008] Among the absorption methods for capturing carbon dioxide, a chemical absorption method is currently being most widely developed. In a chemical absorption method, CO 2 is selectively separated from exhaust gas by a chemical reaction. With chemical absorption, the amount of absorption is not significantly affected by the CO 2 partial pressure. Accordingly, there is an advantage in that the CO 2 removal efficiency is high even when the CO 2 partial pressure is low. However, the chemical absorption method is limited because high energy consumption is required in a subsequent recovery process in which CO 2 is separated from an absorbent. For example, it is known that the energy cost for recovery accounts for about 60% or more of the total CO 2 recovery cost of a CO 2 capturing apparatus. In particular, it is known that the energy cost for separating CO 2 from absorbent in a recovery tower accounts for about 80% of the energy cost for CO 2 recovery, and the energy cost for maintaining process equipment such as a pump accounts for about 20% of the energy cost for CO 2 recovery.
[0009] Accordingly, an improved absorption technology is needed for capturing carbon dioxide wherein energy consumed in absorbent recovery is reduced, thereby reducing the cost for collecting carbon dioxide.
[0010] Hereinafter, a typical carbon dioxide capturing processing will be described in brief.
[0011] As shown in FIG. 2 , an exhaust gas containing CO 2 is supplied to an absorption tower 10 that has a wide surface area for smooth gas-liquid contact and which is filled with filling substances.
[0000] In this case, a liquid absorbent is supplied from an absorbent storage tank 12 to an upper part of the absorption tower 10 , and an exhaust gas is supplied to a lower part of the absorption tower 10 . the exhaust gas contacts the liquid absorbent (absorption solution) at an atmospheric pressure in the upper end of the absorption tower 10 , allowing CO 2 in the exhaust gas to be absorbed into the absorption solution, generally within a temperature range of 40° C. to 70° C.
[0012] The absorbent that absorbs CO 2 is discharged from the absorption tower 10 and is supplied to a recovery tower 14 where it undergoes a recovery process in which the absorbent is heated to a temperature of 100° C. to 160° C. Thereafter, the absorbent is discharged from the lower part of the recovery tower 14 (“used CO 2 absorbent”) and it is resupplied to the absorption tower 10 through an absorbent supplying line 22 .
[0013] Absorbent that is resupplied to the absorption tower 10 is heated by passing through a heat exchanger 16 . As shown, absorbent newly supplied to the recovery tower 14 from the absorbent storage tank 12 can be preheated by heat exchange with the heated absorbent that is resupplied from the lower part of the recovery tower 14 . This combined heated absorbent is then supplied to the upper part of the recovery tower 14 .
[0014] During the recovery process in which absorbent is heated to a temperature of 100° C. to 160° C. in the recovery tower 14 , evaporated absorbent and CO 2 is discharged from the upper part of the recovery tower 14 . Absorbent with CO 2 is discharged from the lower part of the recovery tower 14 and is heated to a temperature range of 100° C. to 160° C. by a heater 18 , such as a boiler, to separate CO 2 from the absorbent.
[0015] CO 2 separated in the recovery tower 14 is discharged through a condenser to locations for storage, fixation, and conversion, and the evaporated absorbent is condensed in the condenser 20 then fed back to the recovery tower 14 .
[0016] The CO 2 separated in the recovery tower 14 is a high concentration of gaseous CO 2 (90% to 100%), and is discharged from the recovery tower 14 at a pressure range of 1.9 atm to 6 atm to be finally treated by a storage, fixation, or conversion method.
[0017] In order to store captured CO 2 in the ground or deep sea, the pressure of a high concentration of CO 2 discharged from the upper end of the recovery tower 14 must be increased to a high pressure of about 70 atm to about 100 atm. For this pressure increase, additional energy is required.
[0018] On the other hand, when captured CO 2 is directly treated by fixation or conversion instead of storage, the captured CO 2 can be treated by a pressure of just 1.2 atm or less and, thus, a process of increasing the pressure of CO 2 with a compressor is unnecessary.
[0019] The above information disclosed in this Background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known in this country to a person of ordinary skill in the art.
SUMMARY OF THE DISCLOSURE
[0020] The present invention provides an apparatus and method for recovering energy after carbon dioxide capture, which reduces a discharge pressure of captured CO 2 to a pressure necessary for fixation or conversion. The apparatus and method further simultaneously generates energy (e.g. in a generator connected to a turbine), wherein the energy is generated by fixation or conversion of the captured CO 2 instead of storing the captured CO 2 in the ground or deep sea. This generated energy can be supplied to process operating units of the present apparatus and, thus, can be used by any of the operating units to capture CO 2 .
[0021] In one aspect, the present invention provides an apparatus for recovering energy after carbon dioxide capture, including an energy recovery unit at a carbon dioxide discharge part of a carbon dioxide capturing apparatus, wherein the energy recovery unit reduces a discharge pressure of the carbon dioxide to a pressure level suitable for a fixation or conversion treatment. According to various embodiments, energy generated during the pressure reduction can be simultaneously recovered by the energy recovery unit.
[0022] In an exemplary embodiment, the energy recovery unit may be in connection with one or more process operating units of the carbon dioxide capturing apparatus to supply the recovered electrical energy to the desired process operating units.
[0023] In another exemplary embodiment, the energy recovery unit may include: a turbine disposed at an outlet of a condenser, wherein the outlet is a discharge part of the carbon dioxide capturing apparatus; and a generator connected to the turbine.
[0024] In another aspect, the present invention provides a method for recovering energy after carbon dioxide capture, including: capturing, by a carbon dioxide capturing apparatus, carbon dioxide from an exhaust gas; discharging, by the carbon dioxide capturing apparatus, the captured carbon dioxide; reducing a discharge pressure of the discharged carbon dioxide to a pressure level suitable for a fixation or conversion treatment; and recovering energy generated during the pressure reduction.
[0025] In an exemplary embodiment, the method may further include supplying the recovered energy to one or more desired process operating units of the carbon dioxide capturing apparatus to utilize the recovered energy.
[0026] In another exemplary embodiment, the energy recovery may include: rotating a turbine using the discharge pressure of the carbon dioxide captured by the carbon dioxide capturing apparatus; continually reducing a final discharge pressure of the carbon dioxide that has passed the turbine to the pressure level suitable for the fixation or conversion treatment; and delivering a rotary force of the turbine to a generator connected to the turbine to enable generation of energy by the generator.
[0027] In still another exemplary embodiment, when the discharge pressure of the carbon dioxide captured by the carbon dioxide capturing apparatus ranges from about 1.8 atm to about 6 atm, the final discharge pressure of the carbon dioxide that has passed the turbine may be reduced to a pressure of less than about 1.8 atm, less than about 1.6 atm, less than about 1.4 atm, or a pressure of about 1.2 atm which is suitable for the fixation or conversion treatment.
[0028] Other aspects and exemplary embodiments of the invention are discussed infra.
BRIEF DESCRIPTION OF THE DRAWINGS
[0029] The above and other features of the present invention will now be described in detail with reference to certain exemplary embodiments thereof illustrated the accompanying drawings which are given hereinbelow by way of illustration only, and thus are not limitative of the present invention, and wherein:
[0030] FIG. 1 is a diagram illustrating an apparatus for recovering energy after carbon dioxide capture according to an embodiment of the present invention; and
[0031] FIG. 2 is a diagram illustrating a typical carbon dioxide capturing apparatus.
[0032] Reference numerals set forth in the Drawings includes reference to the following elements as further discussed below:
10 : absorption tower 12 : absorbent storage tank 14 : recovery tower 16 : heat exchanger 18 : heater 20 : condenser 22 : absorbent supplying line 30 : energy recovery unit 32 : turbine 34 : generator
[0043] It should be understood that the appended drawings are not necessarily to scale, presenting a somewhat simplified representation of various preferred features illustrative of the basic principles of the invention. The specific design features of the present invention as disclosed herein, including, for example, specific dimensions, orientations, locations, and shapes will be determined in part by the particular intended application and use environment.
[0044] In the figures, reference numbers refer to the same or equivalent parts of the present invention throughout the several figures of the drawing.
DETAILED DESCRIPTION
[0045] Hereinafter reference will now be made in detail to various embodiments of the present invention, examples of which are illustrated in the accompanying drawings and described below. While the invention will be described in conjunction with exemplary embodiments, it will be understood that present description is not intended to limit the invention to those exemplary embodiments. On the contrary, the invention is intended to cover not only the exemplary embodiments, but also various alternatives, modifications, equivalents and other embodiments, which may be included within the spirit and scope of the invention as defined by the appended claims.
[0046] It is understood that the term “vehicle” or “vehicular” or other similar term as used herein is inclusive of motor vehicles in general such as passenger automobiles including sports utility vehicles (SUV), buses, trucks, various commercial vehicles, watercraft including a variety of boats and ships, aircraft, and the like, and includes hybrid vehicles, electric vehicles, plug-in hybrid electric vehicles, hydrogen-powered vehicles and other alternative fuel vehicles (e.g., fuels derived from resources other than petroleum). As referred to herein, a hybrid vehicle is a vehicle that has two or more sources of power, for example both gasoline-powered and electric-powered vehicles.
[0047] The above and other features of the invention are discussed infra.
[0048] Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.
[0049] The present invention provides an apparatus and method that improves the economical efficiency of CO 2 capture by reducing the CO 2 absorption cost, particularly by reducing energy costs.
[0050] According to the present invention, a CO 2 capturing apparatus is designed to discharge captured CO 2 for conversion or fixation after reducing the discharge pressure of the CO 2 to a pressure level suitable for fixation or conversion treatment, wherein energy is recovered during the pressure reduction, and the recovered energy is supplied to one or more of process units of the CO 2 capturing apparatus.
[0051] According to an exemplary embodiment, as shown in FIG. 1 , an energy recovery unit 30 may be disposed around a location where CO 2 captured by the CO 2 capturing apparatus is discharged. For example, the energy recovery unit 30 may be disposed at the side of an outlet of a condenser 20 connected to a recovery tower 14 of the CO2 capturing apparatus.
[0052] When CO 2 captured in the CO 2 capturing apparatus is discharged from the outlet of the condenser 20 , the energy recovery unit 30 may be configured and arranged to reduce the discharge pressure of CO 2 to a pressure level suitable for fixation or conversion treatment, and to recover energy generated during the pressure reduction.
[0053] More specifically, the energy recovery unit 30 according to an embodiment of the present invention may include a turbine 32 disposed at an outlet of the condenser 20 that is a discharge part of the CO 2 capturing apparatus. A generator 34 can be provided in connection with the turbine 32 , for example, by concentrically connecting the generator 34 to the turbine 32 or by other suitable arrangements.
[0054] The generator 34 of the energy recovery unit 30 may be connected to one or more process operating units (e.g., pump and blower disposed in each capture process, which are typically driven by electrical energy) of the CO 2 capturing apparatus so as to supply generated electrical energy to the respective process operating units.
[0055] Hereinafter, a method of recovering energy after CO 2 capture according to an embodiment of the present invention will be described as follows.
[0056] As shown in FIG. 1 , exhaust gas containing CO 2 may be supplied into an absorption tower 10 , and absorbent, typically liquid absorbent, may be supplied from an absorbent storage tank 12 to an upper part of the absorption tower 10 .
[0057] The exhaust gas supplied into the absorption tower 10 may contact liquid absorbent (absorption solution), typically at an atmospheric pressure, in the absorption tower 10 (e.g. in the upper part of the absorption tower 10 ), and CO 2 within the exhaust gas may be absorbed by the absorbent.
[0058] The absorbent that absorbs CO 2 (“used CO 2 absorbent”) is discharged from the absorption tower 10 , and is supplied to a recovery tower 14 where it may then undergo a recovery process. In particular, in the recovery process the absorbent is heated to a suitable temperature (such as a temperature of about 100° C. to about 160° C.) in the recovery tower 14 .
[0059] The absorbent recovered in the recovery process is discharged from the lower part of the recover tower 14 , and may then be resupplied to the absorption tower 10 via an absorbent supplying line 22 which connects the absorbent storage tank 12 and the absorption tower 10 .
[0060] As shown, the resupplied absorbent passes through a heat exchanger 16 , and thereafter combines with CO 2 absorbent newly supplied from the absorption tower 10 . As such, the newly supplied CO 2 absorbent may be preheated by heat exchange with the heated resupplied absorbent, and the combined absorbent (newly supplied absorbent and resupplied absorbent) may then be supplied to the upper part of the recovery tower 14 .
[0061] During the recovery process in which absorbent is heated to a suitable temperature, such as a temperature of about 100° C. to about 160° C., evaporated absorbent with CO 2 may be discharged from the upper part of the recovery tower 14 . Further, liquid absorbent with CO 2 may be discharged from the lower part of the recovery tower 14 , may pass through a heater 18 (e.g. a boiler or the like) where it is heated to a suitable temperature range, such as a temperature of about 100° C. to about 160° C., so as to separate CO 2 from the absorbent.
[0062] CO 2 separated in the recovery tower 14 , i.e., CO 2 with evaporated absorbent, may be discharged to a condenser 20 . From the condenser, condensed absorbent may be resupplied to the recovery tower 14 , while separated CO 2 may be discharged to a location for fixation or conversion treatment.
[0063] When separated CO 2 is discharged from the condenser 20 to the location for the fixation or conversion treatment, the pressure of CO 2 may range from about 1.8 atm to about 6 atm. A suitable discharge pressure of CO 2 necessary for the fixation or conversion treatment may be less than this discharge pressure, and, for example, may be less than 1.8 atm, less than 1.6 atm, less than 1.4 atm, and in some embodiments, may be about 1.2 atm.
[0064] As shown in the embodiment of FIG. 1 , separated CO 2 discharged from the condenser 20 at a pressure of about 1.8 atm to about 6 atm is passes through the turbine 32 of the energy recovery apparatus 30 . As the separated CO 2 passes through the turbine, the turbine 32 may be rotated, and the rotary force of the turbine 32 may be delivered to the generator 34 .
[0065] While the separated CO 2 discharged from the condenser 20 passes through the turbine 32 , the pressure of CO 2 may be reduced to a suitable pressure level for the fixation or conversion treatment. In particular, according to an exemplary embodiment, separated CO 2 is discharged from the condenser 20 at a pressure of about 1.8 atm to about 6 atm, and passes through the turbine 32 where the pressure of the CO 2 is constantly or continuously reduced as needed to a suitable pressure level for fixation or conversion treatment.
[0066] For example, the final discharge pressure of CO 2 that has passed through the turbine 32 may be reduced to a pressure of about 1.2 atm, which is a suitable pressure for the subsequent fixation or conversion treatment.
[0067] As the CO 2 passes through the turbine and is reduced in pressure, the rotary force of the turbine 32 may be delivered to the generator 34 , enabling the generation of energy by the generator 34 . Electrical energy generated in the generator 34 may be supplied to and consumed in one or more of the process operating units (e.g., pump and blower disposed in each capture process and driven by electrical energy) of the CO 2 capturing apparatus.
[0068] As a result, the amount of energy that must be supplied (i.e. external energy) to operate the CO 2 capturing apparatus can be significantly reduced, and costs can be saved by utilizing electrical energy generated in the generator 34 of the energy recovery unit 30 as energy for powering one or more of the process operating units of the CO 2 capturing apparatus.
[0069] As a test example of the present invention, a test of energy recovery was performed using a process simulation program in which the amount of CO 2 capture (removal) was about 1000 ton/day. The CO 2 absorption process conditions are shown in Table 1 below.
[0000]
TABLE 1
Gas-liquid flow ratio
125
150
175
200
225
Flow rate of exhaust gas,
2,125.6
2,125.6
2,125.6
2,125.6
2,125.6
m3/min
CO 2 concentration,
20
20
20
20
20
mol %
Flow rate of absorbent,
17.0
14.2
12.1
10.7
9.4
m3/min
MEA concentration in
35
35
35
35
35
absorption tower, wt %
[0070] The consumed energy kW of a reboiler (e.g., heater 18 connected to the lower part of the recovery tower 14 ) for each gas-liquid flow ratio and the flow rate of CO 2 gas discharged from the condenser are shown in Table 2 below.
[0000]
TABLE 2
Gas-Liquid Flow Ratio
125
150
175
200
225
Amount of
1,000
1,000
1,000
1,000
1,000
CO 2
Removal,
ton/day
Energy Used
697.2
577.2
489.8
425.0
376.0
in Absorbent
Pump, kW
Flow Rate of
77.95
79.50
80.88
81.97
83.50
CO 2
discharged
from
Condenser,
m3/min
Pressure of
4.41
4.32
4.25
4.20
4.12
CO 2
discharged
from
Condenser,
atm
[0071] The simulation results of energy generated through the turbine for each gas-liquid flow ratio according to the above test conditions are shown in Table 3 below.
[0000]
TABLE 3
Division
Wet radical flow
Dry radical flow
Gas-Liquid Flow Ratio
125
150
175
200
225
125
150
175
200
225
Pressure of
4.41
4.32
4.25
4.20
4.12
4.41
4.32
4.25
4.20
4.12
CO 2 injected
into turbine,
ata
Pressure of
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
CO 2
discharged
from turbine,
atm
Turbine
0.75
0.75
0.75
0.75
0.75
0.85
0.85
0.85
0.85
0.85
efficiency
Generated
177.3
176.1
175.1
174.2
173.0
223.9
222.4
221.0
220.0
218.5
energy, kW
Reduction rate
25.4
30.5
35.7
41.0
46.0
32.1
38.5
45.1
51.8
58.1
of energy used
in absorbent
pump, %
[0072] As shown in Table 3, the pressure of CO 2 inputted into the turbine ranged from about 4.12 atm to about 4.41 atm regardless of a wet or dry flow, and the pressure of CO 2 discharged into a fixation or conversion treatment unit through the turbine is constantly reduced to about 1.20 atm. Also, as energy generated by the generator increased according to the turbine efficiency, energy used in the absorbent pump of the CO 2 capturing apparatus was reduced.
[0073] According to the embodiments of the present invention, when CO 2 captured by the CO 2 capturing apparatus are processed by fixation or conversion treatment instead of a method of storing CO 2 in the ground or deep sea, the discharge pressure of CO 2 captured by the CO 2 capturing apparatus can be reduced to a pressure necessary for the fixation or conversion treatment. An energy recovery unit can be provided to generate energy from the pressure reduction, particularly wherein a turbine is positioned through which captured CO 2 passes such that the rotary force of the turbine can be delivered to a generator to obtain an energy recovery effect in which electrical energy is produced.
[0074] Also, since electrical energy produced in the generator can be utilized as energy for driving various process operating units (e.g., pump and blower) of the CO 2 capturing apparatus, energy (i.e., externally supplied energy) necessary for operating the apparatus to capture CO 2 can be significantly saved.
[0075] The invention has been described in detail with reference to exemplary embodiments thereof. However, it will be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
|
Disclosed are an apparatus and a method for recovering energy after carbon dioxide capture. The apparatus includes an energy recovery unit at a discharge part of a carbon dioxide capturing apparatus through which captured carbon dioxide is discharged. The energy recovery unit reduces a discharge pressure of the carbon dioxide to a pressure level suitable for a fixation or conversion treatment, and simultaneously generates and recovers energy generated during the pressure reduction.
| 8
|
This is a division of application Ser. No. 591,194, filed Mar. 16, 1984, now U.S. Pat. No. 4,577,572.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention generally relates to a fully rotary or rotating hook for a sewing machine and more particularly, to an improved construction of a fully rotating hook for eliminating disadvantages due to rotational friction between an inner shuttle member or bobbin case and an outer shuttle member or loop taker.
2. Description of the Prior Art
In FIGS. 1 and 2 illustrating a prior art arrangement, there is shown a vertically fully rotating hook 1 which is held at a needle descending position, with an inner shuttle member or bobbin case 3 accommodated in an outer shuttle member or rotary loop taker 2. In the inner bobbin case 3, there is mounted a bobbin 11 for winding a bobbin thread therearound. The inner bobbin case 3 is stopped against rotation by an inner loop taker retaining member (not shown) which is fixed to a machine body. Along an outer peripheral surface of the inner bobbin case 3, there is formed an externally directed flange-like track projection 5 extending in a circumferential direction partially throughout the circumference. This projection 5 is fitted into an internally directed flange-like track groove 6 extending in a circumferential direction along a portion of the inner peripheral surface of the outer loop taker 2. The outer loop taker 2 may be driven for rotation in one direction about an axis by a drive means (not shown) connected to a rotary shaft 16. For rotating the outer loop taker 2 in the state where the inner bobbin case 3 is stopped from rotation as described above, a lubricating oil or the like is supplied between contact faces 4 of the track projection 5 of the inner bobbin case 3 and the track groove 6 of the outer loop taker 2 so as to reduce friction between such two elements.
In this prior art device, however, during high speed rotation of the vertical fully rotating hook 1, friction still exists between the outer loop taker 2 and the inner bobbin case 3, even when the lubricating oil or the like is applied thereto, thus resulting in abrasion of the rotary hook 1. Moreover, the thread or the like tends to be soiled by the lubricating oil, and thus it has been difficult to carry out a sewing operation smoothly in an efficient manner.
SUMMARY OF THE INVENTION
Accordingly, it is a primary object of the present invention to provide an improved fully rotating hook in which smooth movements between an outer shuttle member or rotary loop taker and an inner shuttle member or bobbin case can be achieved without employment of lubricating oil, thereby eliminating the technical problems described above.
In accomplishing the above object, the fully rotating hook for a lock stitch sewing machine according to the present invention includes an outer shuttle member or rotary loop taker having formed therein a track groove, with at least one air blast hole formed in the track groove. A spaced relation is maintained between the track groove and a projection of the inner bobbin case by jetting compressed air from the air blast hole into a clearance between the surfaces of the groove and the projection.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top plan view of a conventional fully rotating hook,
FIG. 2 is a cross section taken along the line II--II in FIG. 1,
FIG. 3 is a longitudinal sectional view of a fully rotating hook according to one preferred embodiment of the present invention,
FIG. 4 is a view similar to a portion of FIG. 3, but of another embodiment of the invention,
FIG. 5 is a fragmentary cross sectional view on an enlarged scale of a section V in FIG. 4,
FIG. 6 is a top plan view of an inner shuttle member or bobbin case according to a further embodiment of the present invention,
FIG. 7 is a fragmentary cross section taken along the line VI--VI in FIG. 6, and
FIG. 8 is a fragmentary cross section taken along the line VIII--VIII in FIG. 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 3, there is shown a longitudinal sectional view of one preferred embodiment according to the present invention, in which portions corresponding to like parts in the prior art arrangement of FIG. 2 are designated by similar reference numerals, but followed by the suffix "a".
In the arrangement of FIG. 3, an upper bobbin case member 8 is mounted within an inner shuttle member or lower bobbin case member 3a. A bobbin 9 having wound therearound thread 7 is accommodated within members 3a and 9. A track projection 5a extends outwardly in the circumferential direction, partially through out the circumference as in the prior art arrangement described above, from an outer peripheral surface of member 3a, and projection 5a is fitted into a circumferentially extending track groove 6a formed in an inner peripheral surface 11 of outer shuttle member or rotary loop taker 2a, partially throughout the circumference thereof. In the track groove 6a of the outer loop taker 2a, one or more air blast holes 12 are formed to confront an outer portion 13 of the projection 5a of member 3a. These air blast holes 12 are communicated with a hollow portion or passages 14 of the outer loop taker 2a.
Into a bottom portion 15 of the outer loop taker 2a is fitted one end of a cylindrical rotary shaft 16a which is positioned coaxially with the axis of outer loop taker 2a. The hollow portion 14 of the outer loop taker 2a is communicated with a hollow portion or passage 19 of the rotary shaft 16a, while a fitting 20 between the outer loop taker 2a and the rotary shaft 16a is fixed by fixing members 17 and 18 so as to achieve airtightness.
In the vicinity of a central portion of the rotary shaft 16a, there are provided vent holes 22 and 23. A cylindrical pipe joint 21 is coaxially mounted about the rotary shaft 16a in a manner to cover vent holes 22 and 23. The pipe joint 21 has an inner diameter slightly larger than an outer diameter of the rotary shaft 16a, and a clearance 24 between the pipe joint 21 and the rotary shaft 16a is communicated with the hollow portion 19 of the rotary shaft 16a through the vent holes 22 and 23. At positions bridging the vent holes 22 and 23 of the rotary shaft 16a in the clearance 24, there are mounted O rings 25, 26, 27 and 28 which contact the outer peripheral surface of the rotary shaft 16a in circumferential directions. These O rings 25 to 28 are respectively fitted into concave grooves 29, 30, 31 and 32 extending in circumferential directions along the inner peripheral surface of the pipe joint 21. Concave grooves 29 to 32 prevent displacement of the positions of the O rings 25 to 28. Owing to the O rings 25 to 28 mounted to bridge the vent holes 22 and 23 in the manner described above, it is possible to prevent air leakage through the clearance 24 between the pipe joint 21 and the rotary shaft 16a. Moreover, at opposite axial ends 33 and 34 of the pipe joint 21, there are provided bearings 35 and 36 which rotatably support the rotary shaft 16a extending through the pipe joint 21.
The clearance 24 between the rotary shaft 16a and the pipe 21 leading to the hollow portion 19 of the rotary shaft 16a is communicated with a hollow portion or passage 38 of an air feed pipe 37 extending from the pipe joint 21, with the end portion of the air feed pipe 37 being connected to an air compressor pump, not shown.
The compressed air fed from the air compressor pump passes through the air feed pipe 37 and is fed from clearance 24 through vent holes 22 and 23 into the hollow portion 19 of the rotary shaft 16a. The compressed air is further fed from the hollow portion 19 of the rotary shaft 16a through the hollow portion 14 of the outer loop taker 2a and through the air blast holes 12. Thus, the compressed air is jetted from the air blast holes 12 into a clearance 4a between the track groove 6a and the projection 5a. As a result, an air film is formed in the clearance 4a, and thus, the sliding resistance or friction between the rotating track groove 6a and the stationary projection 5a are eliminated.
By providing the air blast mechanism as described above in the outer loop taker 2a, high speed operations at speeds of more than 5000 to 6000 stitches per minute, which are considered to be a limit in sewing machines employing conventional fully rotating hooks, may be advantageously realized. Moreover, through elimination of the sliding resistance between the outer loop taker 2a and the inner bobbin case 3a, sliding noises occurring in conventional hooks are eliminated, with a consequent elimination of an unpleasant atmosphere for operators of the sewing machine. Furthermore, since air under high pressure is directed towards the inner bobbin case 3a at all times, it is possible to simultaneously obtain a cleaning effect and cooling effect for the fully rotating hook 1a. It is to be noted that materials for the inner bobbin case 3a may be light weight alloys, plastics, etc.
FIG. 4 is a longitudinal sectional view of another embodiment according to the present invention, while FIG. 5 is a cross sectional view showing a section V in FIG. 4 on an enlarged scale. The construction of FIG. 4 resembles that of FIG. 3, with corresponding parts being designated by similar reference numerals, but followed by the suffix "b". A track projection 5b of the inner shuttle member or bobbin case 3b is fitted into the track groove 6b of the outer shuttle member or loop taker 2a. In the track groove 6b are formed air blast holes 43, 45 and 44 respectively confronting side portions 40 and 41 and outer portion 42 of the projection 5b. Blast holes 43 to 45 are communicated with a hollow portion 14b of the outer loop taker 2a. By jetting the compressed air in the three illustrated directions shown in FIG. 5, the surfaces of the projection 5b and the track groove 6b may be positively maintained in spaced relation from each other, and the functions of the fully rotating hook 1b further will be improved.
FIG. 6 is a top plan view of an inner shuttle member or bobbin case 3c according to a further embodiment of the present invention, FIG. 7 is a cross section taken along the line VII--VII in FIG. 6, and FIG. 8 is also a cross section taken along the line VIII--VIII in FIG. 6. In an outer portion 51 of a track projection 5c of the inner bobbin case 3c is formed a circumferential concave groove 52. At least one or more elongated openings 12c are provided in a track groove 6c to confront groove 52. Also, exhaust holes 50 connected with concave groove 52 are formed in projection 5c to extend in vertical upward and downward directions. The exhaust holes 50 are provided at spaced intervals in the circumferential direction of the projection 5c.
The compressed air fed from the compressor pump is jetted from the elongated openings 12c of the outer loop taker into the concave groove 52 of the projection 5c of the inner bobbin case 3c, and is discharged through the exhaust holes 50 connected with the concave groove 52. By discharging the compressed air from the exhaust holes 50 extending in the upward and downward directions of the projection 5c as described above, a spaced relation between the surfaces of projection 5c and the track groove 6c may be positively achieved.
The vertical fully rotating hook according to each embodiment of the present invention may be readily coupled with the air jetting device 60 shown in FIG. 3, without requiring a large-scale remodeling of the conventional sewing machine. Moreover, the present invention may also be applied to a horizontal fully rotating hook as well.
As is clear from the foregoing description, according to the present invention it is possible to prevent the rotating hooks from being abraded due to high speed rotation by eliminating the undesirable sliding resistance or friction between the inner shuttle member or bobbin case and the outer shuttle member or loop taker through employment of compressed air. Furthermore, owing to the elimination of soiling of threads and the like by oil as experienced in conventional arrangements, the fully rotating hook according to the present invention provides marked improvements of the sewing performance and productivity.
The invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present 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 by 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.
|
A fully rotating hook includes an outer member or rotary loop taker having a track groove therein and an inner shuttle member or bobbin case a projection extending into the groove. A spaced relation between the track groove and the projection is maintained by feeding compressed air into a clearance therebetween. The compressed air is fed through a plurality of air holes opening into the track groove to direct air jets to upper, lower and radially outermost surfaces of the projection on the bobbin case. Furthermore, the loop taker is rotated on a hollow shaft which has an air passage therethrough for feeding compressed air to the plurality of air holes which open into the track groove of the loop taker.
| 3
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method for manufacturing a helium metal vapor laser tube.
2. Description of the Prior Art
The state of the prior art, as to helium cadmium lasers, is exemplified by the article "Simplified Low Noise Helium Cadmium Laser With Segmented Bore" by W. T. Silfvast and L. H. Szeto, Applied Physics Letters, Vol. 19, No. 10, pgs. 445-447, Nov. 15, 1971. That article describes the use of segmented bores to obtain a low noise helium cadmium laser and indicates that when a single cadmium element is used and positioned near the anode, a uniform cadmium density over the entire bore region cannot be obtained through cataphoresis pumping. The article further notes that when instabilities occur near the cadmium source, the instabilities tend to propagate over the entire length of the discharge tube, thereby causing large fluctuations in laser output signals. Based upon these observations, the article recommends the use of a plurality of cadmium elements segmented throughout the bore so as to overcome the fluctuation problem.
In addition, U.S. Pat. No. 3,755,756, entitled "Gaseous Laser Employing A Segmented Discharge Tube" by W. T. Silfvast, generalizes the specific teachings of the above-described article and describes the use of the segmented bore structure to overcome the disadvantages of a single cadmium source.
Other prior art descriptions of helium cadmium lasers are included in articles entitled "Efficient CW Laser Oscillation At 4416°A in Cadmium (II)" by W. T. Silfvast, Applied Physics Letters, Vol. 13, No. 5, pgs. 169-171, Sept. 1, 1968 "Cataphoresis In The Helium Cadmium Laser Discharge Tube" by T. P. Sosnowski, Journal of Applied Physics, Vol. 40, No. 13, pgs. 5138-5144, December 1969, "Discharge Current Noise In Helium Neon Laser And Its Suppression", by Takeo Suzuki, Japanese Journal of Applied Physics, Vol. 9, No. 3, Mar. 1970, "Helium Clean-Up In The Helium-Cadmium Laser Discharge" by T. P. Sosnowski and M. B. Klein, Journal of Quantum Electronics, Vol QE-7, No. 8, August 1971, pgs. 425-426.
The teachings as to helium-cadmium lasers are representative of the state of the art of other helium metal vapor lasers.
SUMMARY OF THE PRESENT INVENTION
It is therefore an object of this invention to provide a novel method of manufacturing a helium metal vapor discharge tube which uses only a single metal source and provides for a stable output and an extended life characteristic.
The process contains three major areas which singly and in combination extend the useful life of the helium metal vapor laser tube. The first processing area is directed toward steps for baking the tube after assembly for a period greater than ten hours under vacuum and at a temperature less than the sublimation temperature of the metal used. The second area of processing is the melting of the metal in the metal reservoir while the tube is filled with argon. The third area of processing is the final burn-in procedure wherein the manufactured tube is mounted in a resonator and operated for a period of 20-40 hours.
An advantage of this process is that it allows for the manufacturing of helium metal vapor laser tubes having extended life expectancies which may extend to more than 1,000 usable hours.
Another advantage of this process of manufacturing is that the resulting helium metal vapor laser tube is characterized by low noise and a stabilized output.
Another advantage of this process is that the tube may be of simple construction and of low cost.
The foregoing and other objects, features and advantages of the invention will be apparent from the following, more particular, description of the preferred embodiment of the invention as illustrated in the accompanying drawings.
IN THE DRAWING
FIG. 1 is a side elevational view of a helium metal vapor laser tube in its basic form;
FIG. 2 is a side elevational view of an assembled helium metal vapor laser tube connected to a vacuum system for further processing;
FIG. 3 is a side elevational view of a completed helium metal vapor laser tube mounted in a resonant chamber forming a helium metal vapor laser for final processing; and
FIG. 4 is a flow diagram showing the nine major steps of the process for manufacturing helium metal vapor laser tubes.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The process for manufacturing a helium metal vapor laser tube of the invention begins with selecting a tube which has been developed through the glass-blowing stage. A selected tube A, as shown in FIG. 1, is comprised of a gas ballast 1, a pair of window mounting surfaces 2 and 3, a pair of diffusion traps 4 and 5, a pair of shields 6 and 7, a vacuum port 8, a barium strontium carbonate cathode 10 having cathode lead 12 extending to the exterior, a tube 16 forming a bore 18 therein, a metal reservoir 19 having metal filler tube 20 extending therefrom, a cataphoretic shield 21 forming a bore 22, and a tungsten anode 23 having an anode lead 24 extending therefrom to the exterior.
The selected tube A, in completing the manufacturing process is passed through nine major steps. FIG. 4 is a flow diagram illustrating the major steps within the process. Each of the major steps will be discussed in detail and are comprised of a series of substeps. The process will be described using cadmium, however, other metals may be used in the process. These other metals include cadmium, selenium, zinc, tellerium and other low temperature high vapor pressure metals.
Step 1 - Cleaning and Assembly of Tube
The tube A, when received from the glass-blower, is first examined for assurance that the window angles and orientation of the surfaces 2 and 3 are proper and that the bore 18 of the tube 16 and the bore 22 of the cataphoretic shield 21 are of the proper size and aligned. The tube A is then cleaned to remove all dust particles. Next, the tube A is air-baked at approximately 250°C for approximately 1/2 hour so as to remove water vapor from within the tube A. After the tube A cools, three grams of cadmium shot 25 are placed in the metal reservoir 19, through the metal filler tube 20. As illustrated by FIG. 2, a pair of radial heat sinks 27 and 28 is then placed on the tube A. (NOTE: The numeral designations of FIG. 1 are not repeated in FIG. 2.) A pair of Brewster windows 30 and 32 are attached to the window surfaces 2 and 3, respectively. It is necessary to take precautions for cleanliness throughout the procedure. The tube A is next connected to a vacuum system (not shown) through the vacuum port 8 by means of a vacuum clamp 34 and a vacuum tube 36 of the vacuum system. During various steps of the process, the vacuum port 8 is used for the purpose of evacuating the tube A and for inserting various gases. Also, as hereinafter discussed, the tube 36 has an electrode 38 extending to the exterior.
The shields 6 and 7 are held in place in front of the openings of the diffusion traps 4 and 5, respectively, so as to prevent the forming of any films on the inside surfaces of the Brewster windows 30 and 32. The shields 6 and 7 are comprised of magnetic material and are held in place by magnets (not shown) positioned outside of the tube A. The final substep within this major step of cleaning and assembly of the tube is the sealing off of the metal filler tube 20. The filler tube 20 is sealed off at the top most position to prevent the heat from effecting the cadmium shots 26 in the metal reservoir 19. Accordingly, FIG. 2 illustrates the status of the helium metal vapor laser tube as of the end of this first major processing step.
Step 2 - Bake Evacuated Tube at 100°C for 12 hours
The tube A is next evacuated to a pressure of less than 5 × 10.sup. -5 Torr. Heater tapes are wrapped around portions of the tube and the entire tube is covered with aluminum foil. Next, the tube is baked for a period greater than 10 hours at a temperature that is less than the sublimation temperature of the cadmium shots 26 within the cadmium reservoir 19. Vapor pressure curves of cadmium which illustrate the variation of vapor pressure with respect to temperature are found in Rosebury, Electron Tube and Vacuum Techniques, Addison-Wesley (1965) at page 143. Experiments have shown that a temperature of 100°C for a period greater than 12 hours is sufficient to obtain the desired results of enhancing the useful life of the helium metal vapor laser tube. It should be noted that the cadmium temperature must be kept lower than its sublimation point during this process. It is realized that if caution is taken to keep the cadmium shot 26 below its sublimation temperature, that the overall temperature of the rest of the tube might be raised and that the bake period could be less than 10 hours. However, as a general rule, a bake period of greater than 10 hours has been found to be required.
Step 3 - Heat Tube Cathode In Oxygen Atmosphere
After the tube A has cooled off from its bake operation of Step 2, all foils and heating tapes are removed. The tube is then backfilled (at a slow rate) with 0.5 Torr of oxygen. A voltage is applied between the cathode lead 12 and the lead 38 to cause the cathode 10 to be heated such that the barium strontium carbonate cathode material is transformed into barium oxide and strontium oxide. The tube A is then cooled, and evacuated to a pressure less than 5 × 10.sup. -5 Torr.
Step 4 - Strike Discharge In Neon Helium Atmosphere
This step removes moisture remaining in the bores 18 and 22 as well as any other moisture within the tube A. The tube is first backfilled with 300 microns of neon plus a quantity of helium 4 such that the total pressure within the tube is 3 Torr. Voltage is applied across the anode lead 24 and the cathode lead 12. A discharge then begins. The current flowing through the tube at this time is held to 20 milliamperes. This step should continue until the blue-color discharge in the tube is gone and the entire tube glows a reddish color. The normal time for this step is approximately 15 minutes.
The tube is then cooled and evacuated again to a pressure less than 5 × 10.sup. -5 Torr.
Step 5 - Melt Cadmium In Argon Atmosphere
The tube is next backfilled with 12 Torr of argon. Heat sinks are clamped on both sides of the metal reservoir 19. It is highly desirous to melt the cadmium shot 26 and to prevent the cadmium from depositing on surfaces within the tube. Heat sinks are placed on both sides of the reservoir 19 during the heating of the cadmium shot 26 within the reservoir 19 to prevent the travel of cadmium vapor through the bores 18 and 22 and other portions of the tube. The interjection of argon into the tube for the heating process has been found to be extremely useful in maintaining and localizing the travel of cadmium atoms, such that the deposition of the cadmium atoms remains nearly entirely within the metal reservoir 19. The metal reservoir 19 is heated at the bottom with a cold flame having no oxygen. After approximately 45 seconds, a small amount of oxygen is added to the flame in order to melt the cadmium. After the cadmium has melted and formed a pool within the bottom of the reservoir 19, the metal filler tube 20 is again sealed off at a point 40 as close as possible to the metal reservoir 19 as illustrated in FIG. 3. The tube is then cooled and the argon evacuated. Finally, the tube should be evacuated to a pressure of less than 5 × 10.sup. -5 Torr.
Step 6 - Strike Discharge In Helium 4 Gas
The tube is wrapped with asbestos 42 or other insulating material, along the laser tube 16, the cathode 10, the evacuation port 8 and the metal condenser area 12 as illustrated in FIG. 3. The asbestos 42 acts as a thermal blanket and prevents cadmium from depositing within the bore 18 of the tube 16. The cadmium will deposit on the glass area near the ends of the asbestos 35 since that area is cool enough to allow deposition. The tube A is then backfilled with 6 Torr of helium 4 gas. A 50 milliampere current is passed from the cathode 10 to the anode 23 resulting in a bluish discharge within the tube. After 10 minutes the current is increased to 70 milliamperes and run at this rate for a period of 3 hours. This step is the initial burn-in portion of the burn-in cycle of the helium cadmium laser tube.
Step 7 - Fill Tube With Helium 3 Gas And Seal Tube
The tube A is evacuated to a pressure less than 5 × 10.sup. -5 Torr and then backfilled with helium 3 gas to a pressure of 5.5 Torr. The tube is then heated by again passing current of 70 milliamperes from the cathode 10 to the anode 23. When the tube has been heated, vacuum port 8 is sealed at a point 44 as shown in FIG. 3. The tube is now free of the vacuum system and is allowed to cool.
Step 8 - Mount And Align The Tube In The Resonator
The helium cadmium tube A is then mounted on a resonator 46 which holds a mirror structure 48 and 50 at opposite ends to form the helium cadmium laser. The shields 6 and 7 are removed to positions such that they will not interfere with the discharge path during the laser operation of the helium cadmium laser. The shields 6 and 7 are respectively held in these positions by means of a pair of magnets 52 and 54 respectively. FIG. 3 shows the final structure of the helium cadmium laser comprising the helium cadmium tube. The helium cadmium tube is placed with the resonator 46 and held by a pair of posts 56 and 58. The tube is then aligned with a set of mirrors 60 and 62 such that lasing operation will occur.
Step 9 - Run Laser For 20-40 Hours
Within 1 hour from the completion of Step 7, the helium cadmium laser formed in Step 8 should be turned on. The laser should be operated for a period of time of 20-40 hours. It is interesting to note that during this period of time, fluctuations in power as reported by Silfvast in his referenced articles can be noted. However, as the burn-in period increases in length, the fluctuations decrease and the power output becomes stabilized. While at first it might appear wasteful to have a burn-in period which can be as long as 43 hours, it has been found that by utilizing this long burn-in procedure, the average lifetime of the tube is greater than 1,000 hours of useful output. It has also been noted that during this burn-in period the cadmium within the reservoir 19 will constantly redistribute itself around the entire surface of the cadmium reservoir 19 to form a thin layer of cadmium on the surface of cadmium reservoir 19. This redistribution continues during the operational lifetime of the tube utnil the source of cadmium has been depleted.
In essence, a circular source of cadmium is constantly being formed which acts as a uniform sublimation source. An additional advantage has been found in that depositing the cadmium on the surface of the reservoir 19, results in the cadmium being maintained at approximately the same temperature as that of the reservoir 19 and the reduced occurrence of fluctuations of power due to variations in temperature of the cadmium. Further, the discharge current also heats the cadmium element to supply the cadmium vapor in the bore region of the laser. At the completion of the 20-40 hour burn-in period, the laser is turned off and is ready for distribution and use.
While the invention has been particularly shown and described with reference to a preferred embodiment thereof, it would be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
|
A process for manufacturing helium metal vapor laser tubes having an extended life characteristic. Three main areas of processing are presented which extend the life expectancy of a helium metal vapor laser tube. The first area of processing is directed to a time bake under vacuum of the tube to be used; the second is directed to the melting of the metal in an argon atmosphere; and the third area is directed to a final burn-in procedure of the helium metal vapor laser using the manufactured helium metal vapor tube.
| 7
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of application Ser. No. 10/701,957, filed Nov. 5, 2003, now U.S. Pat. No. 6,932,077, issued Aug. 23, 2005, which is a divisional of application Ser. No. 09/978,480, filed Oct. 17, 2001, now U.S. Pat. No. 6,691,696, issued Feb. 17, 2004, which is a divisional of application Ser. No. 09/753,159, filed Jan. 2, 2001, now U.S. Pat. No. 6,427,676, issued Aug. 6, 2002, which is a continuation of application Ser. No. 09/434,147, filed Nov. 4, 1999, now U.S. Pat. No. 6,196,096, issued Mar. 6, 2001, which is a continuation of Ser. No. 09/270,539, filed Mar. 17, 1999, now U.S. Pat. No. 6,155,247, issued Dec. 5, 2000, which is a divisional of application Ser. No. 09/069,561, filed Apr. 29, 1998, now U.S. Pat. No. 6,119,675, issued Sep. 19, 2000, which is a divisional of application Ser. No. 08/747,299, filed Nov. 12, 1996, now U.S. Pat. No. 6,250,192, issued Jun. 26, 2001.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to a method and apparatus for sawing semiconductor substrates such as wafers and, more specifically, to a wafer saw and a method of using the same employing multiple indexing techniques and multiple blades for more efficient sawing and for sawing multiple die sizes and shapes from a single semiconductor wafer.
2. Background of Related Art
An individual integrated circuit or chip is usually formed from a larger structure known as a semiconductor wafer, which is usually comprised primarily of silicon, although other materials such as gallium arsenide and indium phosphide are also sometimes used. Each semiconductor wafer has a plurality of integrated circuits arranged in rows and columns with the periphery of each integrated circuit being rectangular. Typically, the wafer is sawn or “diced” into rectangularly shaped discrete integrated circuits along two mutually perpendicular sets of parallel lines or streets lying between each of the rows and columns thereof. Hence, the separated or singulated integrated circuits are commonly referred to as dice.
One exemplary wafer saw includes a rotating dicing blade mounted to an aluminum hub and attached to a rotating spindle, the spindle being connected to a motor. Cutting action of the blade may be effected by diamond particles bonded thereto, or a traditional “toothed” type blade may be employed. Many rotating wafer saw blade structures are known in the art. The present invention is applicable to any saw blade construction, so further structures will not be described herein.
Because semiconductor wafers in the art usually contain a plurality of substantially identical integrated circuits arranged in rows and columns, two sets of mutually parallel streets extending perpendicular to each other over substantially the entire surface of the wafer are formed between each discrete integrated circuit and are sized to allow passage of a wafer saw blade between adjacent integrated circuits without affecting any of their internal circuitry. A typical wafer sawing operation includes attaching the semiconductor wafer to a wafer saw carrier, mechanically, adhesively or otherwise, as known in the art, and mounting the wafer saw carrier on the table of the wafer saw. A blade of the wafer saw is passed through the surface of the semiconductor wafer by moving either the blade relative to the wafer or the table of the saw and the wafer relative to a stationary blade, or a combination of both. To dice the wafer, the blade cuts precisely along each street, returning back over (but not in contact with) the wafer while the wafer is laterally indexed to the next cutting location. Once all cuts associated with mutually parallel streets having one orientation are complete, either the blade is rotated 90° relative to the wafer or the wafer is rotated 90°, and cuts are made through streets in a direction perpendicular to the initial direction of cut. Since each integrated circuit on a conventional wafer has the same size and rectangular configuration, each pass of the wafer saw blade is incrementally indexed one unit (a unit being equal to the distance from one street to the next) in a particular orientation of the wafer. As such, the wafer saw and the software controlling it are designed to provide uniform and precise indexing in fixed increments across the surface of a wafer.
It may, however, be desirable to design and fabricate a semiconductor wafer having various integrated circuits and other semiconductor devices thereon, each of which may be of a different size. For example, in radio-frequency ID (RFID) applications, a battery, chip and antenna could be incorporated into the same wafer such that all semiconductor devices of an RFID electronic device are fabricated from a single semiconductor wafer. Alternatively, memory dice of different capacities, for example, 4, 16 and 64 megabyte DRAMs, might be fabricated on a single wafer to maximize the use of silicon “real estate” and reduce thiefage or waste of material near the periphery of the almost-circular (but for the flat) wafer. Such semiconductor wafers, in order to be diced, however, would require modifications to and/or replacement of existing wafer saw hardware and software.
SUMMARY OF THE INVENTION
Accordingly, an apparatus and method for sawing semiconductor wafers, including wafers having a plurality of semiconductor devices of different sizes and/or shapes therein are provided. In particular, the present invention provides a wafer saw and method of using the same, capable of “multiple indexing” of a wafer saw blade or blades to provide the desired cutting capabilities. As used herein, the term “multiple indexing” contemplates and encompasses both the lateral indexing of a saw blade at multiples of a fixed interval and at varying intervals which may not comprise exact multiples of one another. Thus, for conventional wafer configurations containing a number of equally sized integrated circuits, the wafer saw and method herein can substantially simultaneously saw the wafers with multiple blades and, therefore, cut more quickly than single blade wafer saws known in the art. Moreover, for wafers having a plurality of differently sized or shaped integrated circuits, the apparatus and method herein provide a multiple indexing capability to cut nonuniform dice from the same wafer.
In a preferred embodiment, a single-blade, multi-indexing saw is provided for cutting a wafer containing variously configured integrated circuits. By providing multiple-indexing capabilities, the wafer saw can sever the wafer into differently sized dice corresponding to the configuration of the integrated circuits contained thereon.
In another preferred embodiment, a wafer saw is provided having at least two wafer saw blades spaced a lateral distance from one another and having their centers of rotation in substantial parallel mutual alignment. The blades are preferably spaced apart a distance equal to the distance between adjacent streets on the wafer in question. With such a saw configuration, multiple parallel cuts through the wafer can be made substantially simultaneously, thus essentially increasing the speed of cutting a wafer by the number of blades utilized in tandem. Because of the small size of the individual integrated circuits and the correspondingly small distances between adjacent streets on the wafer, it may be desirable to space the blades of the wafer saw more than one street apart. For example, if the blades of a two-blade saw are spaced two streets apart, a first pass of the blades would cut the first and third laterally separated streets. A second pass of the blades through the wafer would cut through the second and fourth streets. The blades would then be indexed to cut through the fifth and seventh streets, then sixth and eighth, and so on.
In another preferred embodiment, at least one blade of a multi-blade saw is independently raisable relative to the other blade or blades when only a single cut is desired on a particular pass of the carriage. Such a saw configuration has special utility where the blades are spaced close enough to cut in parallel on either side of larger integrated circuits, but use single blade capability for dicing any smaller integrated circuits. For example, a first pass of the blades of a two-blade saw could cut a first set of adjacent streets defining a column of larger integrated circuits of the wafer. One blade could then be independently raised or elevated to effect a subsequent pass of the remaining blade cutting along a street that may be too laterally close to an adjacent street to allow both blades to cut simultaneously, or that merely defines a single column of narrower dice. This feature would also permit parallel scribing of the surface of the wafer to mutually isolate conductors from, for example, tie bars or other common links required during fabrication, with subsequent passage by a single blade indexed to track between the scribe lines to completely sever or singulate the adjacent portions of the wafer.
In yet another preferred embodiment, at least one blade of a multi-blade saw is independently laterally translatable relative to the other blade or blades. Thus, in a two-blade saw, for example, the blades could be laterally adjusted between consecutive saw passes of the sawing operation to accommodate different widths between streets. It should be noted that this preferred embodiment could be combined with other embodiments herein to provide a wafer saw that has blades that are both laterally translatable and independently raisable, or one translatable and one raisable, as desired.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1 is a schematic side view of a first preferred embodiment of a wafer saw in accordance with the present invention;
FIG. 2 is a schematic front view of the wafer saw illustrated in FIG. 1 ;
FIG. 3 is a schematic front view of a second embodiment of a wafer saw in accordance with the present invention;
FIG. 4 is a schematic view of a prior art silicon semiconductor wafer having a conventional configuration to be diced with the wafer saw of the present invention;
FIG. 5 is a schematic view of a silicon semiconductor wafer having variously sized semiconductor devices therein to be diced with the wafer saw of the present invention;
FIG. 6 is a schematic front view of a third embodiment of a wafer saw in accordance with the present invention;
FIG. 7 is a schematic view of a silicon semiconductor wafer having variously sized semiconductor devices therein to be diced with the wafer saw of the present invention;
FIG. 8 is a top elevation of a portion of a semiconductor substrate bearing conductive traces connected by tie bars; and
FIG. 9 is a top elevation of a portion of a semiconductor substrate bearing three different types of components formed thereon.
DETAILED DESCRIPTION OF THE INVENTION
As illustrated in FIGS. 1 and 2 , an exemplary wafer saw 10 according to the invention is comprised of a base 12 to which extension arms 14 and 15 suspended by support 16 are attached. A wafer saw blade 18 is attached to a spindle or hub 20 which is rotatably attached to the extension arm 15 . The wafer saw blade 18 may be secured to the hub 20 and extension arm 15 by a threaded nut 21 or other means of attachment known in the art. The wafer saw 10 also includes a translatable wafer table 22 movably attached in both X and Y directions (as indicated by arrows in FIGS. 1 and 2 ) to the base 12 . Alternatively, wafer saw blade 18 may be translatable relative to the wafer table 22 to achieve the same relative X-Y movement of the wafer saw blade 18 to the wafer table 22 . A silicon wafer 24 to be scribed or sawed may be securely mounted to the wafer table 22 . As used herein, the term “saw” includes scribing of a wafer, the resulting scribe line 26 not completely extending through the wafer substrate. Further, the term “wafer” includes traditional full semiconductor wafers of silicon, gallium arsenide, or indium phosphide and semiconductor materials, partial wafers, and equivalent structures known in the art wherein a semiconductor material table or substrate is present. For example, so-called silicon-on-insulator, or “SOI,” structures, wherein silicon is carried on a glass, ceramic or sapphire (“SOS”) base, or other such structures as known in the art, are encompassed by the term “wafer” as used herein. Likewise, “semiconductor substrate” may be used to identify wafers and other structures to be singulated into smaller elements.
The wafer saw 10 is capable of lateral multi-indexing of the wafer table 22 or wafer saw blade 18 or, in other words, translatable, from side-to-side in FIG. 2 and into and out of the plane of the page in FIG. 1 , various nonuniform distances. As noted before, such nonuniform distances may be mere multiples of a unit distance, or may comprise unrelated varying distances, as desired. Accordingly, a wafer 24 having variously sized integrated circuits or other devices or components therein may be sectioned or diced into its nonuniformly sized components by the multi-indexing wafer saw 10 . In addition, as previously alluded, the wafer saw 10 may be used to create scribe lines or cuts 26 that do not extend through the wafer 24 . The wafer 24 can then subsequently be diced by other methods known in the art or sawed completely through after the wafer saw blade 18 has been lowered to traverse the wafer 24 to its full depth or thickness.
Before proceeding further, it will be understood and appreciated that design and fabrication of a wafer saw according to the invention having the previously referenced, multi-indexing capabilities, independent lateral blade translation and independent blade raising or elevation, are within the ability of one of ordinary skill in the art and that, likewise, the control of such a device to effect the multiple-indexing (whether in units of fixed increments or otherwise), lateral blade translation and blade elevation may be effected by suitable programming of the software-controlled operating system, as known in the art. Accordingly, no further description of hardware components or of a control system to effectuate operation of the apparatus of the invention is necessary.
Referring now to FIG. 3 , another illustrated embodiment of a wafer saw 30 is shown having two laterally spaced blades 32 and 34 with their centers of rotation in substantial parallel alignment transverse to the planes of the blades. For a conventional, substantially circular silicon semiconductor wafer 40 (flat omitted), as illustrated in FIG. 4 , having a plurality of similarly configured integrated circuits 42 arranged in evenly spaced rows and columns, the blades can be spaced a distance D substantially equal to the distance between adjacent streets 44 defining the space between each integrated circuit 42 . In addition, if the streets 44 of wafer 40 are too closely spaced for side-by-side blades 32 and 34 to cut along adjacent streets 44 , the blades 32 and 34 can be spaced a distance D substantially equal to the distance between two or more streets. For example, a first pass of the blades 32 and 34 could cut along streets 44 a and 44 c and a second pass along streets 44 b and 44 d . The blades could then be indexed to cut the next series of streets 44 and the process repeated for streets 44 e , 44 f , 44 g , and 44 h . If, however, the integrated circuits of a wafer 52 have various sizes, such as integrated circuits 50 and 51 , as illustrated in FIG. 5 , at least one blade 34 is laterally translatable relative to the other blade 32 to cut along the streets 44 , such as street 56 , separating the variously sized integrated circuits 50 , 51 . The blade 34 may be variously translatable by a stepper motor 36 having a lead screw 38 ( FIG. 3 ) or by other devices known in the art, such as high precision gearing in combination with an electric motor or hydraulics or other suitable mechanical drive and control assemblies. For a wafer 52 , the integrated circuits, such as integrated circuits 50 and 51 , may be diced by setting the blades 32 and 34 to simultaneously cut along streets 56 and 57 , indexing the blades, setting them to a wider lateral spread and cutting along streets 58 and 59 , indexing the blades while monitoring the same lateral spread or separation and cutting along streets 60 and 61 , and then narrowing the blade spacing and indexing the blades and cutting along streets 62 and 63 . The wafer 52 could then be rotated 90°, as illustrated by the arrow in FIG. 5 , and the blade separation and indexing process repeated for streets 64 and 65 , streets 66 and 67 , and streets 68 and 69 .
As illustrated in FIG. 6 , a wafer saw 70 according to the present invention is shown having two blades 72 and 74 , one of which is independently raisable (as indicated by an arrow) relative to the other. As used herein, the term “raisable” includes vertical translation either up or down. Such a configuration may be beneficial for situations where the distance between adjacent streets is less than the minimum lateral achievable distance between blades 72 and 74 , or only a single column of narrow dice is to be cut, such as at the edge of a wafer 80 . Thus, when cutting a wafer 80 , as better illustrated in FIG. 7 , the two blades 72 and 74 can make a first pass along streets 82 and 83 . One blade 72 can then be raised, the wafer 80 indexed relative to the unraised blade 74 and a second pass performed along street 84 only. Blade 72 can then be lowered and the wafer 80 indexed for cutting along streets 85 and 86 . The process can be repeated for streets 87 (single-blade pass), 88 , and 89 (double-blade pass). The elevation mechanism 76 for blade 72 may comprise a stepper motor, a precision-geared hydraulic or electric mechanism, a pivotable arm which is electrically, hydraulically or pneumatically powered, or by other means well known in the art.
Finally, it may be desirable to combine the lateral translation feature of the embodiment of the wafer saw 30 illustrated in FIG. 3 with the independent blade raising feature of the wafer saw 70 of FIG. 6 . Such a wafer saw could use a single blade to cut along streets that are too closely spaced for dual-blade cutting or in other suitable situations, and use both blades to cut along variously spaced streets where the lateral distance between adjacent streets is sufficient for both blades to be engaged.
It will be appreciated by those skilled in the art that the embodiments herein described, while illustrating certain embodiments, are not intended to so limit the invention or the scope of the appended claims. More specifically, this invention, while being described with reference to semiconductor wafers containing integrated circuits or other semiconductor devices, has equal utility to any type of substrate to be scribed or singulated. For example, fabrication of test inserts or chip carriers formed from a silicon (or other semiconductor) wafer and used to make temporary or permanent chip-to-wafer, chip-to-chip and chip-to-carrier interconnections and that are cut into individual or groups of inserts, as described in U.S. Pat. Nos. 5,326,428 and 4,937,653, may benefit from the multi-indexing method and apparatus described herein.
For example, illustrated in FIG. 8 , a semiconductor substrate 100 or portions thereof may have traces 102 formed thereon by electrodeposition techniques that require connection of a plurality of traces 102 through a tie bar 104 . A two-blade saw in accordance with the present invention may be employed to simultaneously scribe semiconductor substrate 100 along parallel lines 106 and 108 flanking a street 110 in order to sever tie bars 104 of adjacent substrate segments 112 from their associated traces 102 . Following such severance, the two columns of adjacent substrate segments 112 (corresponding to what would be termed “dice” if integrated circuits were formed thereon) are completely severed along street 110 after the two-blade saw is indexed for alignment of one blade therewith, and the other blade raised out of contact with semiconductor substrate 100 . Subsequently, when either the saw or the substrate carrier is rotated 90°, singulation of the substrate segments 112 is completed along mutually parallel streets 114 . Thus, substrate segments 112 for test or packaging purposes may be fabricated more efficiently in the same manner as dice and in the same sizes and shapes.
Further and as previously noted, RFID modules may be more easily fabricated when all components of a module are formed on a single wafer and retrieved therefrom for placement on a carrier substrate providing mechanical support and electrical interconnection between components.
As shown in FIG. 9 , a portion of a substrate 200 is depicted with three adjacent columns of varying-width segments, the three widths of segments illustrating batteries 202 , chips 204 and antennas 206 of an RFID device. With all of the RFID components formed on a single substrate 200 , an RFID module may be assembled by a single pick-and-place apparatus at a single work station. Thus, complete modules may be assembled without transfer of partially assembled modules from one station to the next to add components. Of course, this approach may be employed to any module assembly wherein all of the components are capable of being fabricated on a single semiconductor substrate. Fabrication of different components by semiconductor device fabrication techniques known in the art is within the ability of those of ordinary skill in the art and, therefore, no detailed explanation of the fabrication process leading to the presence of different components on a common wafer or other substrate is necessary. Masking of semiconductor device elements not involved in a particular process step is widely practiced and so similar isolation of entire components is also easily effected to protect the elements of a component until the next process step with which it is involved.
Further, the present invention has particular applicability to the fabrication of custom or nonstandard ICs or other components, wherein a capability for rapid and easy die size and shape adjustment on a wafer-by-wafer basis is highly beneficial and cost-effective. Those skilled in the art will also understand that various combinations of the preferred embodiments could be made without departing from the spirit of the invention. For example, it may be desirable to have at least one blade of the independently laterally translatable blade configuration be independently raisable relative to the other blade or blades, or a single blade may be both translatable and raisable relative to one or more other blades and to the target wafer. In addition, while, for purposes of simplicity, some of the preferred embodiments of the wafer saw are illustrated as having two blades, those skilled in the art will appreciate that the scope of the invention and appended claims are intended to cover wafer saws having more or less than two blades. Thus, while certain representative embodiments and details have been shown for purposes of illustrating the invention, it will be apparent to those skilled in the art that various changes in the invention disclosed herein may be made without departing from the scope of the invention, which is defined in the appended claims.
|
A saw for dicing substrates, such as semiconductor wafers, that has one or more variable indexing capabilities and two or more blades. One of the blades may be moved laterally or vertically, independent of one or more other blades.
| 8
|
BACKGROUND OF THE INVENTION
This invention is in the field of nonwoven fabrics and methods of treating the same.
Nonwoven fabrics include those commonly termed spun-bonded fabrics, which are well known and comprise generally fabrics formed by spinning continuous filaments of suitable materials and laying them in web form with the filaments randomly arranged so that portions extend in all directions. The webs are then treated to cause the filaments to bond to each other at their intersections, either by mechanical bonding, fusion or by the use of separate bonding materials. Such fabrics and method for their manufacture are well known and one such method is described in the patent to Kinney U.S. Pat. No. 3,338,992. A further patent describing these materials is the patent to Hartmann U.S. Pat. No. 3,544,854.
As used in this application, the term nonwoven fabric is intended to refer to fabrics of the type having randomly oriented filaments bonded at their intersections by mechanical means, material fusion or separate bonding materials and whether or not the filaments are continuous.
The known nonwoven fabrics are generally considered unsatisfactory for many purposes because of their stiffness or poor drapability.
The compaction of certain types of nonwovens has traditionally been somewhat less than satisfactory in regards to the improvement in softness obtained. This has been particularly true with spun-bonded fabrics of polyester, polyamide, and polyolefins. It has been felt that the problem lies in the fact that the fiber in these fabrics will absorb very little moisture and, therefore, cannot be plasticized or softened by rewetting. Consequently, because of their greater stiffness at the time of processing, relatively high forces are required to buckle the fiber and compact these fabrics. The result has generally been that compaction of spun-bonded fabrics results in a coarse macrocrepe which results in some stiffness reduction but also an undesirable harsh surface quality. This effect is more or less pronounced depending on the fiber denier and basis weight of the material.
Previous attempts to overcome this problem involved efforts to accurately control compaction temperature so as to soften the fabric and make the fibers more pliable and susceptible to compaction. This has been a generally unsatisfactory solution. Even though the fabric may be considerably shrunk in this manner, upon cooling after compaction, the stiffness of the fabric is seldom reduced and in many instances may actually be increased. Too high a temperature is known to have a detrimental effect on softness.
Attempts were also made to reduce the compressive resistance of the fibers by the addition of chemicals known to act as swelling agents. The results were all unproductive, generally because the chemical agents acted as lubricants and hence interferred with the compaction process. In addition, none of the chemicals evaluated produced a significant reduction in the compressive modulus of the material being treated.
Considerable success has been achieved in improving softness of certain types of fabrics by conventional compaction. However, the conventional compaction process acts predominantly on those fibers and fiber segments, oriented in the longitudinal direction of the fabric. Consequently, the reduction in fabric stiffness obtained by this process is mainly limited to the longitudinal direction of the fabric while stiffness in the fabric's transverse direction is reduced only slightly.
Attempts to increase the compressive forces available also centered on the use of antilubricants to increase the friction between the blanket and the material. Mechanical embossing of the web was also evaluated as a means of increasing friction. Additionally, a harder blanket (60 Shore A Durometer va. 50 Shore A Durometer) had a significant effect. The harder blanket produced a finer compaction particularly on the heavy-weight materials.
SUMMARY OF THE INVENTION
Applicant has discovered that the compressive modulus of many nonwoven fabrics can be considerably reduced by stretching. By stretching a web of the material beyond its elastic limit in the machine direction, that is, the direction of fabric feed and applied tension, and then compacting the same, a considerably better quality compaction could be obtained. This is believed to be due to the reduced compressive modulus of the fabrics, which results in less resistance of the fabric to the compressive force of compaction.
Another very significant benefit is that as the material is stretched, it necks down or narrows in the cross direction so that lateral fiber buckling is achieved. Thus, cross direction stretch of as much as 20% has been realized along with significant reductions in stiffness.
The reference herein to compaction refers to that step or process by which fabrics are shortened in their longitudinal direction while maintaining the sheet or web against increase in thickness or "crepeing".
It is, therefore, an object of this invention to provide a method for the compaction of nonwoven fabrics rendering those fabrics softer and more flexible.
A further object is to provide such a method wherein the fabrics are rendered stretchable in two directions.
Another object is to provide such a method applicable to any material capable of having one dimension appreciably reduced by applying tensile forces at right angles to that dimension.
Further objects and advantages will become apparent from the following description which is made with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a plan view of a schematic representation of apparatus for practicing one form of the present invention;
FIG. 2 is a side elevational view of the apparatus schematically shown in FIG. 1;
FIG. 3 is a schematic plan view of a modified form of the apparatus for practicing the present invention; and
FIG. 4 is a side elevational view of the apparatus of FIG. 3.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the drawings, numeral 2 indicates a web of nonwoven fabric of the type heretofore referred to and is shown as a continuous elongated web of material. In the process as illustrated in FIGS. 1 and 2, the web 2 is fed, from any suitable source, between the nip of feed rollers 4 which are caused to rotate at a predetermined speed to thus predetermine the rate at which the web 2 is fed therepast. From the feed rollers 4 the web 2 is directed over a roller 5 to a cylinder 12 and blanket 6 trained over nip roller 8 of a compacting apparatus 10. The compacting apparatus 10 is of well known construction and operation and is exemplified by the drawings and described in the patent to Cluett U.S. Pat. No. 2,624,245. Briefly, the compacting apparatus comprises a heated cylinder 12 mounted for rotation about its axis. A nip roller 8 is customarily mounted for adjustment toward and from the roller 12 and a relatively thick elastomeric blanket 6 is trained over the nip roller, between the roller 8 and cylinder 12, then over an arcuate portion of cylinder 12 to a take-up roller 14 and then over the return roller 16 from which it is directed back to the nip roller 8. As is known, the action of the blanket 6 held in tension and pressed against the cylinder 12 results in a foreshortening or compaction of web material fed through the apparatus without permitting the web to crepe and maintaining opposed surfaces of the web parallel and of substantially the same thickness. The shortening of the web is accomplished by causing substantially all longitudinally extending filaments thereof to undergo "micro-compression" and to buckle or curve within the body of the web.
As shown in FIGS. 1 and 2, the web 2 is directed from the feed rollers 4 over roller 5 and then to the nip between blanket 6 and cylinder 12 and the speed of operation of the nip roller and cylinder 12 is such that it tends to draw the web 2 at a greater speed than permitted by the feed rollers 4. This results in actually and permanently stretching those web filaments which extend generally in the direction of material feed. At the same time the web width is reduced, as illustrated in FIG. 1, this results in lateral fiber or filament buckling of the fabric. This means that the generally longitudinally extending filaments are being stretched in the feed direction and tend to align themselves with the feed direction and crowd together in the cross direction and thus portions thereof are drawn inwardly toward the center of the web and any generally laterally extending filaments bonded thereto are caused to buckle or kink and the web width is reduced in the lateral direction. This also produces a marked improvement in MD tensile strength. As the web material enters the nip between the blanket 6 and cylinder 12, the well known compaction occurs and in the present instance, the tension of the fabric filament is not only relieved but its longitudinal filaments are actually placed under compression even though its laterally extending and longitudinally extending filaments are compacted, kinked or bent within the confines of the web.
In the apparatus and steps illustrated in FIGs. 3 and 4, the web is fed through feed rollers 4, as described with reference to FIGS. 1 and 2, and then through stretching rollers 18 which are driven at a higher speed than the rollers 4 to thus impart a permanent stretch to the web 2 with the consequent reduction in width and lateral fiber buckling already described.
As the web leaves the stretching rollers 18, all tension in the longitudinal direction is relieved and some minor increase in width occurs although the width of the web is still substantially less than it was before stretching. The web is then fed loosely to a suitable accumulator cradle 20 or the like and is fed from there over roller 19 to the nip between blanket 6 and cylinder 12 of compacting apparatus 10, which may be identical to that shown in FIGS. 1 and 2. In the apparatus 10, the web is longitudinally compacted and the product issuing therefrom has substantially identical characteristics to those issuing from the apparatus of FIGS. 1 and 2.
In general, the fabric is stretched until the desired width reduction of the web is produced before feeding the web to the compactor. It has been found that stretching from 10% to 30% reduces the modulus of the material about 35% thus making compaction much easier. It is to be noted that this process first stretches the web in the feed direction, then compacts the web longitudinally in the compactor to a length approximating the original web length before stretching. However, during the time that the longitudinal compaction takes place, the web is prevented from expanding to its original lateral dimension by the fact that it is locked between the blanket 6 and cylinder 12. The generally longitudinally extending filaments are compacted; and the generally laterally extending filament portions are permanently buckled and the resulting fabric exhibits a marked increase in softness and is readily stretchable in both directions, the lateral stretchability being sufficient to recover the original width of the web. Applicant believes that one of the reasons he is able to achieve the results he does, by essentially stretching the material and then returning it to its original length in the compactor, is that the fabric is free to neck down during stretching but it is restricted from returning to its original width when the fabric is shortened in the compactor. These restrictive forces occur because the fabric is sandwiched between the cylinder and the blanket. By this restriction of CD expansion he is actually locking in the CD fiber buckles.
While reference heretofore has been made to the supposition that spun-bonded fabrics could not be compacted in the usual way, since they were hydrophobic and would not absorb moisture, it is not intended that this invention be limited to such hydrophobic materials. It is contemplated that the process may be advantageously used with fabrics composed of other materials having filaments or fibers and wherein the filaments or fibers are bonded at their crossing points in any manner whatsoever.
It has been found that with certain types of nonwoven materials, the addition of a small amount of moisture to the material prior to tensioning of the web results in a considerable increase in the amount of necking down which is accomplished. In addition, this moisture also permits the necking down of the material to be accomplished more easily; i.e., less tensile force. The types of material which were found to be beneficially treated with moisture are those which contain hydrophylic fibers and/or binders. The addition of moisture to these fabrics tends to create a more flexible and more deformable bond so that more elongation of the fabric in the machine direction and hence greater width reduction can be accomplished without rupturing the sheet.
The optimum amount of moisture addition to the material undoubtedly depends on the type of fiber and binder present. It is probably best determined experimentally. Generally the desired moisture will be in the range of 15% to 25% of the sheet weight.
In one specific case when processing a material composed of rayon fibers bonded with an acrylic binder, applicant was able to stretch the air dry fabric only about 8%. This resulted in a cross direction width reduction of 2%. Attempting to stretch the material a greater amount resulted in the sheet being pulled apart. However, by adding 12% moisture to the web, (from 7% originally to 19% total moisture) he was able to stretch the web 20% without difficulty. This resulted in a 12% width reduction which produced a considerable improvement in the textile-like properties of the processed web.
Also, it has been found that the addition of heat during stretching is beneficial to the processing of other types of materials; specifically, materials containing thermoplastic type fibers and/or binders. In this type of material, it is believed that the heat produces the same effect as moisture does in the webs composed of hydrophylic type binders or fibers.
By way of specific examples, four types of spun-bonded polyester fabrics were obtained from E. I. DuPont, as follows:
2011: A standard straight fiber fabric of 13 lbs/3000 ft. 2
2024: Similar to 2011 but has a weight of 43#/3000 ft. 2
2431: A crimped fiber fabric.
T213: a fabric in which the fiber denier is approximately 2.9 vs. 5.5 in the above fabrics. Weight is 21#/3000 ft. 2
Each of these fabrics was processed in accordance with the present invention under several different conditions; regular compaction with 50 Shore A and 60 Shore A Durometer blankets, and stretching followed by compaction on the 50 Shore A Durometer blanket and in some cases also with the 60 Shore A Durometer blanket, the results being tabulated herebelow.
______________________________________ Basis Weight Stiffness Tensile StretchSample and (#/3000 (inches) (#/in.) (%)Treatment ft..sup.2) MD CD MD CD MD CD______________________________________2011Control 13.5 3.1 3.2 3.3 2.3 24.5 27.3Compacted 50 15.4 2.6 2.5 3.2 2.3 35.9 26.6Compacted 60 15.1 2.7 2.5 3.1 2.2 33.1 27.1S+C 50 15.0 1.9 1.3 3.5 2.4 31.8 37.12024Control 43.3 6+ 5.6 20.1 10.8 38.9 36.6Compacted 50 46.4 3.2 4.4 16.9 12.2 47.4 38.7Compacted 60 44.2 3.3 4.7 18.7 13.6 49.1 35.0S+C 50 49.2 2.4 2.4 23.3 12.0 53.5 56.7S+C 60 48.3 2.4 2.5 22.1 12.3 53.0 55.4Control 53.2 4.5 3.9 12.7 11.8 51.4 73.7Compacted 50 54.6 2.7 3.1 13.2 10.3 67.4 63.1Compacted 60 52.3 2.8 2.9 12.1 9.6 64.2 55.7S+C 50 50.5 2.4 2.5 14.3 9.4 53 77.8Control 11.3 3.6 2.3 4.0 2.2 35.3 39.3compacted 50 12.0 2.7 2.2 3.9 2.0 44.6 38.3Compacted 60 12.2 2.6 2.2 4.5 2.7 40.8 41.8S+C 50 12.8 2.1 1.2 4.7 1.9 42.7 47.4______________________________________ Note: S+C = "stretched then compacted". Compacted 50 = "50 Shore A Durometer Compacted 60 = "60 Shore A Durometer blanket".
STRETCHING
Sufficient draw was applied to the web to cause it to undergo a 12-15% reduction in width prior to entering the compactor. Speed differential necessary to accomplish this was approximately 20-25%.
COMPACTION
Compaction conditions, whether or not web stretching preceded compaction, were as follows:
______________________________________Nip 15%Cylinder Temperature* 140° FCylinder Surface "Teflon"Blanket Tension 60 pliSheet Moisture Air Dry______________________________________ *Higher temperatures were found to have a negative effect on softness.
It can be seen that in all cases significant reductions in stiffness resulted from stretching and compacting as compared to simple compaction. This is true not only of MD stiffness but is particularly true also of CD stiffness. Also, the table shows that the tensile strength of the web, in at least the machine direction (MD) was significantly increased.
In addition to the above, other types of nonwoven fabrics were treated, as follows:
EXAMPLE II
A wet formed fabric composed of a combination of 1 1/2 inch long nylon and 1/2 inch rayon fibers bonded with a thermoplastic binder.
______________________________________ Control Com- Stretched Stretched (Uncom- pacted 10% + 16% + pacted) Only Compacted Compacted______________________________________Tensile (lbs/inch)MD 5.7 5.0 5.1 5.1CD 4.1 4.2 4.0 3.7Elongation (%)MD 9.3 20.1 12.6 11.2CD 10.2 10.0 14.3 17.8Stiffness (Inches)MD 6.0 2.7 3.0 3.2CD 5.2 4.8 3.5 2.6Basis Wt. 1.35 1.47 1.44(oz/yd.sup.2)______________________________________ Note: In order to stretch this fabric by the amounts shown above, it was necessary to first increase the moisture in the material to 18%. This allowed the material to be stretched without rupture. Moisture was applie with a steam shower and material ws partially dried to approximately 10% moisture prior to compaction.
EXAMPLE III
A dry formed fabric of 1 to 1/2 inch long rayon fibers bonded with a thermoplastic binder.
______________________________________ Control Compacted Stretched 14% (Uncompacted) Only & Compacted______________________________________Tensile (lb/in)MD 2.9 3.0 3.3CD 1.8 2.1 1.7Elongation (%)MD 14.3 23.7 17.0CD 13.8 14.2 20.2Stiffness (inches)MD 4.9 2.2 2.3CD 4.2 3.6 2.3Basis Weight 2.0 2.2 2.2(oz/yd.sup.2)______________________________________ Note: Material was heated to 180° F in order to facilitate the stretching. Compaction was also accomplished at 180° F.
While the foregoing description refers to only a blanket type compactor, it is to be understood that other forms of compacting means may be used, such as two-roll devices capable of simultaneous compaction in both machine and cross directions.
|
A bonded web of nonwoven fibers is stretched beyond its elastic limit in one direction sufficiently to permanently elongate those filaments or filament portions of the web extending generally in the direction of the applied tension. This results in a narrowing or necking down of the web in the cross direction and consequent shortening or lateral buckling of those filaments or filament portions extending generally transverse to the direction of applied tension. This imparts increased softness, flexibility and resilient stretchability to the fabric, in that transverse direction. The elongated filaments are then compacted longitudinally while the web is retained in its narrowed condition to impart increased softness, flexibility and resilient stretchability in the longitudinal direction.
| 3
|
BACKGROUND OF THE INVENTION
[0001] The present invention relates to a remote controlled vehicle adapted for traversing across the surfaces of a steel shipping container. It is capable of carrying a plethora of investigative equipment such as sniffers, cameras, fibre optics, drills and the such.
[0002] Even with homeland security measures heightened the majority of shipping containers reaching American international ports go uninspected. The volume of cargo containers is beyond what the authorities can handle. It is a time consuming task and often dangerous when the contents of a shipping container have shifted and opened. While leaking contents may be visible most chemical spills remain of an unknown nature. Remote controlled vehicles have been extensively used in scientific and police work where it is impractical, impossible or too hazardous to send a person.
[0003] Henceforth, a remote controlled reconnaissance vehicle for use on a steel shipping container would fulfill a long felt need in the inspection industry. This new invention utilizes and combines known and new technologies in a unique and novel configuration to overcome the aforementioned problems and accomplish this.
SUMMARY OF THE INVENTION
[0004] The general purpose of the present invention, which will be described subsequently in greater detail, is to provide a remote controlled vehicle with magnetic wheels and a magnetic braking system to affix the vehicle to a steel surface strong enough so as to enable a drill on the vehicle to exert enough force between the vehicle and the steel surface to pierce the steel surface.
[0005] It has many of the advantages mentioned heretofore and many novel features that result in a new remote controlled reconnaissance vehicle with the ability for vertical and inverted overhead travel on these steel containers and with the capability for sampling the atmosphere or viewing the container contents from any vantage point of the container which is not anticipated, rendered obvious, suggested, or even implied by any of the prior art, either alone or in any combination thereof.
[0006] In accordance with the invention, an object of the present invention is to provide a remote controlled vehicle for traversing all orientations of metal surfaces.
[0007] It is a further objective of the present invention to provide a remote controlled vehicle for traversing all orientations of metal surfaces having magnetic wheels.
[0008] It is another objective of the present invention to provide a remote controlled vehicle for traversing all orientations of metal surfaces and capable of carrying reconnaissance equipment.
[0009] It is still another objective of the present invention to provide a remote controlled vehicle for traversing all orientations of metal surfaces and capable of utilizing a magnetic brake and magnetic wheels to secure the vehicle for drilling operations from the vehicle.
[0010] It is a final objective of the present invention to provide a remote controlled vehicle for traversing all orientations of metal surfaces, having a magnetic brake to prevent rollback of the vehicle when stopped on a vertical surface.
[0011] The subject matter of the present invention is particularly pointed out and distinctly claimed in the concluding portion of this specification. However, both the organization and method of operation, together with further advantages and objects thereof, may best be understood by reference to the following description taken in connection with accompanying drawings wherein like reference characters refer to like elements. Other objects, features and aspects of the present invention are discussed in greater detail below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 is a perspective view of the preferred embodiment six wheeled mag vehicle showing the general arrangement of all components;
[0013] FIG. 2 is a side view of the preferred embodiment six wheeled mag vehicle showing an articulation of the trailer when climbing up a vertical wall;
[0014] FIG. 3 is a side view of the preferred embodiment six wheeled mag vehicle showing an articulation of the trailer when climbing down a vertical wall;
[0015] FIG. 4 is a side view of the preferred embodiment six wheeled mag vehicle showing the vehicle on a vertical wall with the magnetic brake engaged;
[0016] FIG. 5 is a perspective view of the alternate embodiment four wheeled mag vehicle showing the general arrangement of all components;
[0017] FIG. 6 is a side view of the alternate embodiment four wheeled mag vehicle with the magnetic brake disengaged;
[0018] FIG. 7 is a perspective view of the alternate embodiment four wheeled mag vehicle with the magnetic brake engaged;
[0019] FIG. 8 is a side view of the alternate embodiment four wheeled mag vehicle with the magnetic brake engaged;
[0020] FIG. 9 is a perspective view of a wheel rim;
[0021] FIG. 10 is a perspective view of a foam insert;
[0022] FIG. 11 is a perspective view of a tire;
[0023] FIG. 12 is a perspective view of a magnetic retention ring with the magnets removed;
[0024] FIG. 13 is a perspective view of a magnetic retention ring with the magnets installed;
[0025] FIG. 14 is a perspective view of the magnetic brake in the disengaged position;
[0026] FIG. 15 is a side view of the magnetic brake in the disengaged position;
[0027] FIG. 16 is a top view of the magnetic brake in the disengaged position;
[0028] FIG. 17 is a side view of the magnetic brake in the engaged position;
[0029] FIG. 18 is a perspective view of the magnetic brake's magnet barrel;
[0030] FIG. 19 is a side cross sectional view of the magnetic brake's magnet barrel;
[0031] FIG. 20 is a perspective view of the brake housing without the magnet barrel installed;
[0032] FIG. 21 is a side view of the magnetic brake in the disengaged position; and
[0033] FIG. 22 is a side view of the magnetic brake in the engaged position.
DETAILED DESCRIPTION
[0034] There has thus been outlined, rather broadly, the more important features of the invention in order that the detailed description thereof that follows may be better understood and in order that the present contribution to the art may be better appreciated. There are, of course, additional features of the invention that will be described hereinafter and which will form the subject matter of the claims appended hereto.
[0035] In this respect, before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of descriptions and should not be regarded as limiting.
[0036] Looking at FIGS. 1 to 4 a six wheel version of a magnetic shipping container crawling apparatus 2 can best be seen. A four wheel magnetic shipping container apparatus 4 is best illustrated in FIGS. 5 to 8 . These two versions differ only by the addition of a two wheeled tractor 6 that is pivotally mounted to the four wheel version 4 which becomes a trailer. The two wheeled tractor 6 and the four wheel trailer 4 are connected by a length of adjoined chain links with a biaxial pivot at one end that allows horizontal and vertical articulation simultaneously to accommodate travel over any surface. This type of connection is well known in the art and is not illustrated. This accommodates the transition between horizontal and vertical surfaces ( FIG. 2 ) and vertical and horizontal surfaces ( FIG. 3 ).
[0037] The preferential size of each vehicle is ⅛ scale although other sizes such as ⅙ and 1/10 scale have been utilized for specific operations. The frame is connected to the magnetic wheel assemblies 8 by a set of spring and strut limiters to allow ease of multi plane articulation. The vehicles have a battery powered RF signal receiver adapted for use with a battery powered RF signal transmitter operated by the user from a remote location that serves to actuate the drive system, the magnetic braking system 20 and any reconnaissance equipment as is well known in the industry. The wheel assemblies 8 of all magnetic vehicles 4 are all driven and all steer. The magnetic wheel assemblies 8 of the tractor 6 are identical in all respects to the magnetic wheel assemblies 8 of the four wheel magnetic vehicle 4 and their frames are substantially similar in design.
[0038] It is to be noted that none of the illustrations reflect the reconnaissance equipment that the vehicles are designed to carry, the drive system, the batteries and the remote control receiver and transmitter. These are not within the scope of the claimed invention and are well known in the art. For ease of illustration these have been eliminated from the drawings. While the remote operation means and the drive system of the vehicles remain essentially off the shelf, it is the wheel design that allows the vehicles to traverse in any orientation along ferromagnetic surfaces. The magnetic wheel assembly 8 has a solid wheel rim 12 ( FIG. 9 ) upon which a foam ring 14 ( FIG. 10 ) is mounted. The wheel rim 12 is journaled for rotation about a shaft or axle coupled to the vehicle's frame and drive system. The foam ring 14 resides between the wheel rim 12 and the magnetic retention ring 16 ( FIG. 12 ) and lends support to the magnet retention ring 16 which houses a uniform series of identical permanent magnets 18 ( FIG. 13 ) arranged about the retention ring's exterior periphery. A flexible, soft tire 22 ( FIG. 11 ) that is frictionally affixed to the wheel rim 12 and encases the foam ring 14 , the magnet retention ring 16 with permanent magnets of the rare earth variety 18 , completes the wheel assembly 8 . The tire 22 and magnet retention ring 16 are each formed as unitary pieces from a suitable elastomeric material.
[0039] The magnets 18 reside at approximate 20 degree intervals about the magnet retention ring 16 being held there in matingly conformed magnet recesses 20 by friction and by a flexible cement. Opposing poles are placed adjacent to each other. In the preferred embodiment the magnets each are capable of a 50 pound attraction based on a force exerted perpendicular to the ferromagnetic surface. The force required to turn the wheels is much less as the magnetic forces are incrementally removed while the wheels turn. Although there is a plethora of suitable glues an epoxy system of a silica epoxy resin with a polyamide resin hardener has been shown to work well.
[0040] The outer half of the magnet 18 is exposed to allow friction with the inside of the tire 22 . The magnetic wheel assembly 8 is not pressurized. When assembled the portion of the soft tire 22 that lies between the ferromagnetic surface being traversed and the magnet retention ring 16 deforms under the weight of the vehicle and the magnetic affinity of the magnet laden ring 16 so as to minimize the distance between the magnets 18 and the surface, thereby maximizing the adhesive holding forces of the vehicle. In this manner a magnetic contact is maintained while the wheel assemblies 8 roll along the ferromagnetic surface.
[0041] The exterior surface of the tires 22 have a tread formation 24 to maximize traction on painted ferromagmetic surfaces, although the exterior surface could be modified for increased traction on wet or oily surfaces by the application of solvents, traction rings/chains or a different tread formation.
[0042] The disposition of the magnets 18 at approximate 20 degree intervals about the magnet retention ring 16 has shown to be an optimal spacing configuration when driving over a corrugated shipping container as more of the magnets 18 are exerting a strong magnetic field toward the ferromagnetic surface when the wheel is residing in the bottom trough of a corrugation. (Conventional corrugation of a shipping container has 3 inch wide parallel crests and troughs 1.5 inches apart with 45 degree sloped connecting walls.) It is known that smaller or larger magnets may be used with different spacing for different sized wheels and for different purposes. Generally on a flat ferromagnetic surface there is a minimum of one magnet 18 per wheel assembly in strong magnetic contact with the surface. With the 20 degree magnet spacing on a ⅛ scale wheel assembly when traversing a corrugated trough there is a minimum of six magnets 18 per wheel assembly in strong magnetic contact with the surface. It is to be noted that 10 degree interval spacing has been used with larger diameter wheels or smaller magnets. The wheel assemblies 8 are pivotally connected to a remotely controlled steering mechanism as is well known in the art and is not illustrated herein.
[0043] In operation, as the tire 22 flexes and compresses at the contact plane between the wheel assembly 8 and the ferromagnetic surface, the magnet retention ring 16 is allowed to come into close enough contact with the surface to effect a strong gripping force. During rolling contact a strong magnetic attraction is maintained orthogonally between the magnetic wheel assemblies 8 and the ferromagnetic surface. A multi wheeled shipping container crawling apparatus in the referenced scale sizes with the above wheel assembly configuration is able to ascend and descend vertical walls as well as traverse inverted on horizontal surfaces and make the transition from horizontal to vertical travel and vice versa.
[0044] Each of the 18 magnets 18 in the magnet retention ring 16 has approximately two and a half times the holding strength of the total weight of a six wheeled vehicle (with the weight of all wheels included) when on a flat ferromagnetic surface. I.E. for a ⅛ scale vehicle with a weight of 20 pounds, each of the magnets in the magnet ring can lift 50 pounds vertically in air. Since a minimum of two magnets are always in magnetic contact with the surface because of the deformation of the tires 22 , with six wheels on a flat surface the holding power of the vehicle is 600 pounds. On a corrugated surface this holding power may increase by as much as three times up to 1800 lbs depending upon the actual location of each wheel. For this reason when traversing corrugated steel shipping containers there is no need for the use of the magnetic brake system 20 . Testing has shown that the drive system requires a motor to drive train gearing of 1:70 to 1:90 through a set of worm or pinion and spur gears to develop the extra torque required when traversing a corrugated shipping container wherein there is approximately 3 times the holding force generated by each wheel.
[0045] The magnetic braking system 20 retractably pivots a brake magnet 64 housed in a cylindrical brake magnet inner housing 60 , downward from the approximate center of a magnetic shipping container crawling apparatus 2 into close proximity to the ferromagnetic surface that the crawling apparatus is traversing. The brake magnet inner housing 60 is positioned on the end of a brake arm 46 dimensioned so that its longitudinal axis forms an upwardly inclined acute angle with the ferromagnetic surface when the magnetic brake is engaged. In this configuration an integrated vehicle braking system is engaged. ( FIG. 4 ) First, the additional magnetic attraction between the brake magnet 64 and the ferromagnetic surface acts to hold the vehicle in place. Second, the acute angle design transfers the downward vertical gravitational pull on the vehicle to a horizontal pull between all of the wheel assemblies 8 sand the ferromagnetic surface. When the vehicle resides on a horizontal surface, pulling the vehicle perpendicularly off of that ferromagnetic surface requires much more force than rolling the vehicle downward as would be the case if the acute angle formed between the brake arm 46 and the surface were downwardly inclined. In the preferred embodiment the brake magnets 64 each have 170 pounds of attractive force. Thus with two magnetic brakes applied there will be 340 pounds of magnetic attraction to hold the 20 pound vehicle in place and when drilling, another 600 pounds is available from each of the magnetic wheel assemblies 20 . This additional 600 pounds being applied by virtue of the brake arm's acute upward angle.
[0046] The magnetic braking system 20 has a housing 26 ( FIG. 14 ) that mechanically supports remote controlled motor 28 through mechanical fasteners 30 . The motor's drive shaft 32 has a small drive gear 34 ( FIG. 21 ) thereon that meshingly engages a larger driven gear 36 having a drive peg 38 extending normally therefrom. The drive peg 38 extents through an arced slot 48 in brake arm 46 . ( FIG. 17 ) The driven gear 36 and brake arm 46 are pivotally supported on stub axle 40 which is held in position by an inner parallel plate 42 and an outer parallel plate 44 of the housing 26 ( FIG. 16 ) and mechanically affixed to the plates at its distal and proximate ends. A spring means 50 is attached to the stub axle 40 so as to present a counterclockwise torsional force on the stub axle 40 . ( FIG. 22 ) Although the spring means 50 is illustrated as a torsional spring, a retraction coil spring could also be connected to accomplish the same result. At the inner end of the brake arm 46 is an upper stop protrusion 52 and a lower stop protrusion 54 that limit the rotation of the brake arm 46 by abutting the side of the housing 26 . ( FIG. 17 ) The outer end of the brake arm 46 is mechanically connected to the brake magnet outer housing 56 and has a central bore formed therein that supports pivot shaft 58 which is connected to brake magnet inner housing 60 by plate 62 . ( FIG. 18 ) The brake magnet inner housing 60 is a hollow cylinder rotatably housed within cylindrical brake magnet outer housing 56 . The brake magnet inner housing 60 has a section of removed housing material 63 (magnet recess) in which the brake magnet 64 resides and is affixed. ( FIGS. 18 , 19 and 20 ) A end cap not illustrated encloses the brake magnet inner housing 60 to protect it from harsh elements. A thrust shaft 66 is connected at its ends between drive peg 38 and rotate disc 68 which is affixed to plate 62 via pivot shaft 58 . ( FIGS. 16 and 22 ) The rotate disc 68 is coupled to the thrust shaft by an off centered pin 99 so as to translate the linear motion of the thrust shaft 66 into rotational motion of the brake magnet inner housing 60 . Each end of the thrust shaft is adapted for rotatable engagement.
[0047] In the preferred embodiment there is actually two independent, identical mirror image magnetic braking systems 20 utilized on opposite sides of the vehicle as illustrated best in FIGS. 1 and 5 . The magnetic strength of each of the brakes is 170 pounds. This is not necessary in all situations but rather is dictated by the amount of downward force exerted off of the vehicle's platform, such as would be encountered through a vehicle mounted drilling device for boring holes in the surface traversed.
[0048] Looking at FIGS. 14 , 15 , 17 , 21 and 22 it can be seen how the magnetic brake system 20 works. When not actuated there is no remote drive signal sent to the remote controlled DC powered motor 28 and no rotational torque is generated by the motor 28 to overcome the torsion spring means 50 which applies a counterclockwise torque on the stub axle 40 so as to rotate the brake arm 46 counterclockwise until the upper stop protrusion 52 contacts the side plate of the housing 26 at the same time as the upper end of the actuation shaft 66 is pivoted until the drive peg 38 contacts the upper side of the arced slot 48 and the lower end of the thrust shaft 66 rotates the plate 62 so as to position the brake magnet 64 and brake arm 46 as illustrated in FIGS. 14 , 15 and 21 . Here the brake magnet 64 is too far from the ferromagnetic surface to have any holding effect and to prevent the brake magnet 64 from attraction to the magnets 18 in the wheel assembly 8 .
[0049] Operation of the magnetic brake system for engagement or disengagement is a two step process. First the brake magnet 64 must be rotated and then the brake magnet 64 must be lowered or raised. In order to engage the magnetic brake system 20 a remote signal from a remote sending unit is sent to the remote controlled motor 28 from which begins to rotate its drive shaft 32 and attached small drive gear 34 counterclockwise. This in turn rotates larger driven gear 36 clockwise overcoming the counterclockwise force of the spring means 50 . As the drive peg 38 on the larger driven gear 36 rotates clockwise it travels along the arced slot 48 in the brake arm 46 ( FIG. 15 ) and forces the thrust shaft 66 to extend slightly outward from the magnetic brake housing 26 to turn rotate disc 68 which is affixed onto pivot shaft 58 and rotates plate 62 in the direction indicated by directional arrow 70 . Since plate 62 is also affixed to the pivot shaft 58 and is housed in the end of the brake magnet inner housing 60 the inner housing 60 rotates counterclockwise within the brake magnet outer housing 56 so as to move the position of the magnet 64 out of its 9 o'clock position toward the ferromagnetic surface between 90 and 120 degrees to the approximately 5:30 position. This is accomplished when the drive peg 38 contacts the end of the arced slot 48 in the brake arm 46 . Once the drive peg 38 contacts the end of the arced slot 48 the motor 28 continues to exert torque and push the thrust shaft 66 further outward which forces the drive peg 38 to rotate the brake arm 46 clockwise which lowers the other end of the brake arm 46 and the brake magnet 64 into contact with the ferromagnetic surface. With the brake magnet 64 in close proximity to the ferromagnetic surface the remote controlled motor 28 can be shut off.
[0050] It is to be noted that an acute forward (upward if on a vertical surface) angle will always reside between the brake arm 46 and the ferromagnetic surface as the brake arm 46 can only rotate until the lower stop protrusion 54 contacts the side plate of the magnetic brake housing 26 . It is to be noted that depending where the vehicle's wheel assemblies 8 are physically located on a corrugated container the stop protrusion may not be utilized.
[0051] While the brake magnet 64 is encased within the brake magnet inner housing 60 so as to be protected, it actually sits in the magnet recess 63 which leaves only a thin amount of the brake magnet inner housing cylinder wall between the ferromagnetic surface and the brake magnet 64 . Experimentation has shown that a cylinder wall thickness of 0.010 inch is adequate to withstand the forces and support the brake magnet 64 .
[0052] To disengage the magnetic brake 20 the process is reversed. The remote controlled motor 28 is remotely signaled to reverse its rotation and turn clockwise which first rotates the inner magnetic brake housing 60 approximately 90 to 120 degrees from the 5:30 o'clock position back to the 9 o'clock position to minimize the magnetic attraction between the brake magnet 64 and the ferromagnetic surface. Then when the drive peg 38 contacts the opposite end of the arced slot 48 the motor continues to drive the brake arm 46 to its original position. Once there the motor is shut off and the brake arm 46 is held in position by spring means 50 .
[0053] This sequencing is necessary to be able to use lightweight, inexpensive and conventional components. A lightweight DC powered motor 28 although highly geared for maximum torque could not directly lift the brake arm 46 without some of the magnetic attraction removed. Increasing the motor size requires larger batteries and more mass which is very undesirable.
[0054] In the preferred embodiment, the brake arm 46 rotates over approximately 45 degrees by virtue of the arced slot 48 . The brake magnet inner housing 60 rotates 90 degrees by virtue of the thrust arm travel.
[0055] In another embodiment not shown, the operation of the magnetic braking system 20 works theoretically similar however the rotate disc 68 is relocated 180 degrees such that the drive post 99 resides below pivot shaft 58 . This configuration however, places the brake magnet 64 when retracted at the 3o'clock position which is closer to the magnetic wheels 8 and will cause more torque to be exerted to overcome the magnetic attraction between the brake magnet 64 and the wheel magnets 18 , but under certain situations may offer mechanical operation advantages.
[0056] The above description will enable any person skilled in the art to make and use this invention. It also sets forth the best modes for carrying out this invention. There are numerous variations and modifications thereof that will also remain readily apparent to others skilled in the art, now that the general principles of the present invention have been disclosed. As such, those skilled in the art will appreciate that the conception, upon which this disclosure is based, may readily be utilized as a basis for the designing of other structures, methods and systems for carrying out the several purposes of the present invention. It is important, therefore, that the claims be regarded as including such equivalent constructions insofar as they do not depart from the spirit and scope of the present invention.
|
A magnetic adhesive and braking system for a remote controlled vehicle adapted for traversing across ferromagnetic surfaces of a steel shipping container including the vertical walls and ceiling. The magnetic wheel system allows the vehicle to traverse vertical grades. The magnetic braking system both securely holds the vehicle when stopped on a vertical surface, and exerts enough attractive force between the vehicle and the shipping container to allow a vehicle mounted drill to operate. The magnetic brake design uses mechanical advantage such that the force required to roll the vehicle vertically downward is heightened to the force required to detach the vehicle in a perpendicular vector from the container's surface.
| 0
|
[0001] This is a continuation application of copending application Ser. No. 13/733,398 filed on Jan. 3, 2013; which is a continuation of application Ser. No. 13/047,061 filed on Mar. 14, 2011 and issued Jan. 15, 2013 as U.S. Pat. No. 8,353,365; which is a continuation of application Ser. No. 11/742,668 filed on May 1, 2007 and issued Apr. 19, 2011 as U.S. Pat. No. 7,926,589; which is a continuation of application Ser. No. 11/168,814 filed on Jun. 28, 2005 and issued Jun. 5, 2007 as U.S. Pat. No. 7,225,885; which is a continuation of application Ser. No. 09/898,989 filed on Jul. 3, 2001 and issued Aug. 30, 2005 as U.S. Pat. No. 6,935,439; which is a continuation of application Ser. No. 09/562,503 filed on May 1, 2000 and issued Aug. 28, 2001 as U.S. Pat. No. 6,279,668; which is a continuation of application Ser. No. 09/066,964 filed on Apr. 27, 1998 and issued Jun. 27, 2000 as U.S. Pat. No. 6,079,506; the disclosures of which are incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates generally to underground boring tool guidance and, more particularly, to a remote walk over locator/controller configured for determining the underground location of a boring tool and for remotely issuing control commands to a drill rig which is operating the boring tool.
[0003] Installing underground utility cable using a steerable boring tool is well known in the art. Various examples are described in U.S. Pat. Nos. 5,155,442, 5,337,002, 5,444,382 and 5,633,589 as issued to Mercer et al (collectively referred to herein as the Mercer Patents), all of which are incorporated herein by reference. An example of the prior art Mercer technique is best illustrated in FIG. 1 herein which corresponds to FIG. 2 in the Mercer Patents. For purposes of clarity, the reference numerals used in the Mercer Patents have been retained herein for like components.
[0004] As seen in FIG. 1 , an overall boring machine 24 is positioned within a starting pit 22 and includes a length of drill pipe 10 , the front end of which is connected to the back end of a steerable boring head or tool 28 . As described in the Mercer Patents, the boring tool includes a transmitter for emitting a dipole magnetic field 12 which radiates in front of, behind and around the boring tool, as illustrated in part in FIG. 1 . A first operator 20 positioned at the starting pit 22 is responsible for operating the boring machine 24 ; that is, he or she causes the machine to let out the drill pipe, causing it to push the boring tool forward. At the same time, operator 20 is responsible for steering the boring tool through the ground. A second locator/monitor operator 26 is responsible for locating boring tool 28 using a locator or receiver 36 . The boring tool is shown in FIG. 1 being guided beneath an obstacle 30 . The locator/monitor operator 26 holds locator 36 and uses it to locate a surface position above tool head 28 . Once operator 26 finds this position, the locator 36 is used to determine the depth of tool head 28 . Using the particular locator of the present invention, operator 26 can also determine roll orientation and other information such as yaw and pitch. This information is passed on to operator 20 who then may use it to steer the boring tool to its target. Unfortunately, this arrangement requires at least two operators in order to manage the drilling operation, as will be discussed further.
[0005] Still referring to FIG. 1 , current operation of horizontal directional drilling (HDD) with a walkover locating system requires a minimum of two skilled operators to perform the drilling operation. As described, one operator runs the drill rig and the other operator tracks the progress of the boring tool and determines the commands necessary to keep the drill on a planned course. In the past, communication between the two operators has been accomplished using walkie-talkies. Sometimes hand signals are used on the shorter drill runs. However, in either instance, there is often confusion. Because an operating drill rig is typically quite noisy, the rig noise can make it difficult, if not impossible, to hear the voice communications provided via walkie-talkie. Moreover, both the walkie-talkie and the hand signals are awkward since the operator of the drill rig at many times has both of his hands engaged in operation of the drill rig. Confused steering direction can result in the drill being misdirected, sometimes with disastrous results.
[0006] The present invention provides a highly advantageous boring tool control arrangement in which an operator uses a walk-over locator unit that is configured for remotely issuing control commands to a drill rig. In this way, problems associated with reliable communications between two operators are eliminated. In addition, other advantages are provided, as will be described hereinafter.
SUMMARY OF THE INVENTION
[0007] As will be described in more detail hereinafter, there is disclosed herein a locator/control arrangement for locating and controlling underground movement of a boring tool which is operated from a drill rig. An associated method is also disclosed. The boring tool includes means for emitting a locating signal. In accordance with the present invention, the locator/control arrangement includes a portable device for generating certain information about the position of the boring tool in response to and using the locating signal. In addition to this means for generating certain information about the position of the boring tool, the portable device also includes means for generating command signals in view of this certain information and for transmitting the command signals to the drill rig. Means located at the drill rig then receives the command signals whereby the command signals can be used to control the boring tool.
[0008] In accordance with one aspect of the present invention, the means located at the drill rig for receiving the command signals may include means for indicating the command signals to a drill rig operator.
[0009] In accordance with another aspect of the present invention, the means located at the drill rig for receiving the command signals may include means for automatically executing the command signals at the drill rig in a way which eliminates the need for a drill rig operator.
[0010] In accordance with still another aspect of the present invention, drill rig monitoring means may be provided for monitoring particular operational parameters of the drill rig. In response to the particular operational parameters, certain data may be generated which may include a warning that one of the parameters has violated an acceptable operating value for that parameter. In one feature, the certain data regarding the operational parameters may be displayed at the drill rig. In another feature, the certain data regarding the operational parameters may be displayed on the portable device. The latter feature is highly advantageous in embodiments of the invention which contemplate elimination of the need for a drill rig operator.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The present invention may be understood by reference to the following detailed description taken in conjunction with the drawings, in which:
[0012] FIG. 1 is a partially broken away elevational and perspective view of a boring operation described in the previously recited Mercer Patents.
[0013] FIG. 2 is an elevational view of a boring operation being performed in accordance with the present invention in which a portable locator/controller is used.
[0014] FIG. 3 is a diagrammatic perspective view of the portable locator/controller which is used in the boring operation of FIG. 2 , shown here to illustrate details of its construction.
[0015] FIG. 4 is a partial block diagram illustrating details relating to the configuration and operation of the portable locator/controller of FIG. 3 .
[0016] FIG. 5 is a partial block diagram illustrating details relating to the configuration and operation of one arrangement of components located at the drill rig for receiving command signals transmitted from the portable locator/controller of the present invention.
[0017] FIG. 6 is a partial block diagram illustrating details relating to the configuration and operation of another arrangement of components located at the drill rig for receiving command signals transmitted from the portable locator/controller and for, thereafter, executing the commands signals so as to eliminate the need for a drill rig operator.
DETAILED DESCRIPTION OF THE INVENTION
[0018] Turning again to the drawings, attention is immediately directed to FIG. 2 which illustrates a horizontal boring operation being performed using a boring/drilling system generally indicated by the reference numeral 70 . The drilling operation is performed in a region of ground 72 including a boulder 74 . The surface of the ground is indicated by reference numeral 76 .
[0019] System 70 includes a drill rig 78 having a carriage 80 received for movement along the length of an opposing pair of rails 82 which are, in turn, mounted on a frame 84 . A conventional arrangement (not shown) is provided for moving carriage 80 along rails 82 . During drilling, carriage 80 pushes a drill string 86 into the ground and, further, is configured for rotating the drill string while pushing, as will be described. The drill string is made up of a series of individual drill string sections or pipes 88 , each of which includes a suitable length such as, for example, ten feet. Therefore, during drilling, sections 88 must be added to the drill string as it is extended or removed from the drill string as it is retracted. In this regard, drill rig 78 may be configured for automatically adding or removing the drill string sections as needed during the drilling operation. Underground bending of the drill string sections enables steering, but has been exaggerated for illustrative purposes.
[0020] Still referring to FIG. 2 , a boring tool 90 includes an asymmetric face 92 and is attached to the end of drill string 86 . Steering of the boring tool is accomplished by orienting face 92 of the boring tool (using the drill string) such that the boring tool is deflected in the desired direction. Boring tool 90 includes a mono-axial antenna such as a dipole antenna 94 which is driven by a transmitter 96 so that a magnetic locating signal 98 is emanated from antenna 94 . Power may be supplied to transmitter 96 from a set of batteries 100 via a power supply 102 . A control console 104 is provided for use in controlling and/or monitoring the drill rig. The control console includes a drill rig telemetry transceiver 106 connected with a telemetry receiving antenna 108 , a display screen 110 , an input device such as a keyboard 112 , a processor 114 , and a plurality of control levers 116 which, for example, hydraulically control movement of carriage 80 along with other relevant functions of drill rig operation.
[0021] Still referring to FIG. 2 , in accordance with the present invention, drilling system 70 includes a portable locator/controller 140 held by an operator 141 . With exceptions to be noted, locator 140 may be essentially identical to locator 36 , as described in the Mercer Patents.
[0022] Turning to FIG. 3 in conjunction with FIG. 2 , the same reference numerals used to describe locator 36 in the Mercer Patents have been used to designate corresponding components in locator/controller 140 . In order to understand and appreciate the present invention, the only particular components of locator 36 that form part of locator 140 and that are important to note here are the antenna receiver arrangement comprised of orthogonal antennas 122 and 124 and associated processing circuitry for measuring and suitably processing the field intensity at each antenna and roll/pitch antenna 126 and associated processing circuitry 128 for measuring the pitch and roll of the boring tool. Inasmuch as the Mercer patents fully describe the process by which locator 140 is used to find the position of boring tool 90 , the reader is referred to the patents for a detailed description of the locating method.
[0023] Referring to FIGS. 2-4 , in accordance with the present invention, locator/controller 140 includes a CPU 144 , interfaced with a remote telemetry transceiver 146 , a joystick 148 and a display 150 . Remote transceiver 146 is configured for two-way communication with drill rig transceiver 106 via an antenna 152 . Joystick 148 is positioned in a convenient location for actuation by operator 141 . In accordance with one highly advantageous feature of the present invention, operator 141 is able to remotely issue control commands to drill rig 78 by actuating joystick 148 . Commands which may be issued to the drill rig by the operator include, but are not limited to (1) roll orientation for steering direction purposes, (2) “advance” and (3) “retract.” It should be appreciated that the ability to issue these commands from locator/controller 140 , in essence, provides for complete boring tool locating and control capability from locator/controller 140 . A locator/controller command is implemented using CPU 144 to read operator actuations of the joystick, interpret these actuations to establish the operator's intended command, and then transfer the command to remote transceiver 146 for transmission to the command drill rig telemetry transceiver 106 at the drill rig, as will be described immediately hereinafter.
[0024] Still referring FIGS. 2-4 , control commands are entered by using display 150 in conjunction with joystick 148 . Display 150 includes an enhanced roll orientation/steering display 154 having a clock face 156 which shows clock positions 1 through 12 . These clock positions represent the possible steering directions in which boring tool 90 may be set to travel. That is, the axis of the boring tool is assumed to extend through a center position 158 of the clock display and perpendicular to the plane of the figure. The desired roll orientation is established by moving joystick 148 either to the left or right. As the joystick is moved, a desired roll orientation pointer 160 incrementally and sequentially moves between the clock positions. For instance, if the desired roll pointer was initially located at the 12 o'clock position (not shown), the locator/controller operator may begin moving it to the 3 o'clock position by moving and holding the joystick to the right. CPU 144 detects the position of the joystick and incrementally moves the desired roll pointer to the 1 o'clock, then 2 o'clock, and finally the 3 o'clock position. At this point, the operator releases the joystick. Of course, at the 3 o'clock position, the command established is to steer the boring tool to the right. Similarly, the 6 o'clock position corresponds to steering downward, the 9 o'clock position corresponds to steering to the left and the 12 o'clock position corresponds to steering upward. As mentioned previously, steering is accomplished by setting face 92 of the boring tool in an appropriate position in accordance with the desired roll of the boring tool. With regard to boring tool steering, it is to be understood that boring tool steering has been implemented using concepts other than that of roll orientation and that the present invention is readily adaptable to any steering method either used in the prior art or to be developed.
[0025] Having established a desired steering direction, operator 141 monitors an actual roll orientation indicator 162 . As described in the Mercer patents, roll orientation may be measured within the boring tool by a roll sensor (not shown). The measured roll orientation may then be encoded or impressed upon locating signal 98 and received by locator/controller 140 using antenna 126 . This information is input to CPU 144 as part of the “Locator Signal Data” indicated in FIG. 4 . CPU 144 then causes the measured/actual roll orientation to be displayed by actual roll orientation indicator 162 . In the present example, operator 141 can see that the actual roll orientation is at the 2 o'clock position. Once the desired roll orientation matches the actual roll orientation, the operator will issue an advance command by moving joystick 148 forward. Advancement or retraction commands for the boring tool can only be maintained by continuously holding the joystick in the fore or aft positions. That is, a stop command is issued when joystick 148 is returned to its center position. If the locating receiver were accidentally dropped, the joystick would be released and drilling would be halted. This auto-stop feature will be further described in conjunction with a description of components which are located at the drill rig.
[0026] Still referring to FIGS. 2-4 , a drill string status display 164 indicates whether the drill rig is pushing on the drill string, retracting it or applying no force at all. Information for presentation of drill string status display 164 along with other information to be described is transmitted from transceiver 106 at the drill rig and to transceiver 146 in the locator/controller. Once the boring tool is headed in a direction which is along a desired path, operator 141 can command the boring tool to proceed straight. As previously described, for straight drilling, the drill string rotates. In the present example, after having turned the boring tool sufficiently to the right, the operator may issue a drill straight command by moving joystick 148 to the left and, thereafter, immediately back to the right. These actuations are monitored by CPU 144 . In this regard, it should be appreciated that CPU 144 may respond to any suitable and recognizable gesture for purposes of issuance of the drill straight command or, for that matter, CPU 144 may respond to other gestures to be associated with other desired commands. In response to recognition of the drill straight gesture, CPU 144 issues a command to be transmitted to the drill rig which causes the drill string to rotate during advancement. At the same time, CPU 144 extinguishes desired roll orientation indicator 160 and actual roll orientation indicator 162 . In place of the roll orientation indicators, a straight ahead indication 170 is presented at the center of the clock display which rotates in a direction indicated by an arrow 172 . It is noted that the straight ahead indication is not displayed in the presence of steering operations which utilize the desired or actual roll orientation indicators. Alternatively, in order to initiate straight drilling, the locator/controller operator may move the joystick to the left. In response, CPU 144 will sequentially move desired roll indicator 160 from the 3 o'clock position, to the 2 o'clock position and back to the 1 o'clock position. Thereafter, the desired roll indicator is extinguished and straight ahead indication 170 is provided. Should the operator continue to hold the joystick to the left, the 12 o'clock desired roll orientation (i.e., steer upward) would next be presented.
[0027] In addition to the features already described, display 150 on the locator/controller of the present invention may include a drill rig status display 174 which presents certain information transmitted via telemetry from the drill rig to the locator/controller. The drill rig status display and its purpose will be described at an appropriate point below. For the moment, it should be appreciated that commands transmitted to drill rig 78 from locator/controller 140 may be utilized in several different ways at the drill rig, as will be described immediately hereinafter.
[0028] Attention is now directed to FIGS. 2 and 5 . FIG. 5 illustrates a first arrangement of components which are located at the drill rig in accordance with the present invention. As described, two-way communications are established by the telemetry link formed between transceiver 106 at the drill rig and transceiver 146 at locator/controller 140 . In this first component arrangement, display 110 at the drill rig displays the aforedescribed commands issued from locator/controller 140 such that a drill rig stationed operator (not shown) may perform the commands. Display 110 , therefore, is essentially identical to display 150 on the locator/controller except that additional indications are shown. Specifically, a push or forward indication 180 , a stop indication 182 and a reverse or retract indication 184 are provided. It is now appropriate to note that implementation of the aforedescribed auto-stop feature should be accomplished in a fail-safe manner. In addition to issuing a stop indication when joystick 148 is returned to its center position, the drill rig may require periodic updates and if the updates were not timely, stop indication 182 may be displayed automatically. Such updates would account for loss of the telemetry link between the locator/controller and the drill rig.
[0029] Still referring to FIGS. 2 and 5 , the forward, stop and retract command indications eliminate the need for other forms of communication between the drill rig operator and the locator/controller operator such as the walkie-talkies which were typically used in the prior art. At the same time, it should be appreciated that each time a new command is issued from the locator/controller, an audible signal may be provided to the drill rig operator such that the new command does not go unnoticed. Of course, the drill rig operator must also respond to roll commands according to roll orientation display 154 by setting the roll of the boring tool to the desired setting. In this regard, it should be mentioned that a second arrangement (not shown) of components at the drill rig may be implemented with a transmitter at the locator/controller in place of transceiver 146 and a receiver at the drill rig in place of transceiver 106 so as to establish a one-way telemetry link from the boring tool to the drill rig. However, in this instance, features such as operations status display 174 and drill string status display 164 cannot be provided at the locator/controller.
[0030] It should be appreciated that the first and second component arrangements described with regard to FIG. 5 contemplate that the drill rig operator may perform tasks including adding or removing drill pipe sections 88 from the drill string and monitoring certain operational aspects of the operation of the drill rig. For example, the drill rig operator should insure that drilling mud (not shown) is continuously supplied to the boring tool so that the boring tool does not overheat whereby the electronics packaged housed therein would be damaged. Drilling mud may be monitored by the drill rig operator using a pressure gauge or a flow gauge. As another example, the drill rig operator may monitor the push force being applied to the drill string by the drill rig. In the past, push force was monitored by “feel” (i.e., reaction of the drill rig upon pushing). However, push force may be directly measured, for instance, using a pressure or force gauge. If push force becomes excessive as a result of encountering an underground obstacle, the boring tool or drill string may be damaged. As a final example, the drill rig operator may monitor any parameters impressed upon locating signal 98 such as, for instance, boring tool temperature, battery status, roll, pitch and proximity to an underground utility. In this latter regard, the reader is referred to U.S. Pat. No. 5,757,190 entitled A SYSTEM INCLUDING AN ARRANGEMENT FOR TRACKING THE POSITIONAL RELATIONSHIP BETWEEN A BORING TOOL AND ONE OR MORE BURIED LINES AND METHOD which is incorporated herein by reference.
[0031] Referring to FIG. 5 , another feature may be incorporated in the first and second component arrangements which is not requirement, but which nonetheless is highly advantageous with regard to drill rig status monitoring performed by the drill rig operator. Specifically, a rig monitor section 190 may be included for monitoring the aforementioned operational parameters such as drilling mud, push force and any other parameters of interest. As previously described, proper monitoring of these parameters is critical since catastrophic equipment failures or damage to underground utilities can occur when these parameters are out of range. In accordance with this feature, processor 114 receives the status of the various parameters being monitored by the rig monitor section and may provide for visual and/or aural indications of each parameter. Visual display occurs on operations status display 174 . The display may provide real time indications of the status of each parameter such as “OK”, as shown for drilling mud and push force, or an actual reading may be shown as indicated for the “Boring Tool Temperature”. Of course, visual warnings in place of “OK” may be provided such as, for example, when excessive push force is detected. Audio warning may be provided by an alarm 192 in the event that threshold limits of any of the monitored parameters are violated. In fact, the audio alarm may vary in character depending upon the particular warning being provided. It should be mentioned that with the two-way telemetry link between the drill rig and locator/controller according to the aforedescribed first component arrangement, displays 164 and 174 may advantageously form part of overall display 150 on locator/controller 140 , as shown in FIG. 4 , which may also include alarm 192 . However, such operational status displays on the locator/controller are considered as optional in this instance since the relevant parameters may be monitored by the drill rig operator. The full advantages of rig monitor section 190 and associated operations status display 174 will come to light in conjunction with a description of a fully automated arrangement to be described immediately hereinafter.
[0032] Referring to FIGS. 2 and 6 , in accordance with a third, fully automated arrangement of the present invention, a drill rig control module 200 is provided at drill rig 78 . Drill rig control module 200 is interfaced with processor 114 . In response to commands received from locator/controller 140 , processor 114 provides command signals to the drill rig control module. The latter is, in turn, interfaced with drill rig controls 116 such that all required functions may be actuated by the drill rig control module. Any suitable type of actuator (not shown) may be utilized for actuation of the drill rig controls. In fact, manual levers may be eliminated altogether in favor of actuators. Moreover, the actuators may be distributed on the drill rig to the positions at which they interface with the drill rig mechanism. For reasons which will become apparent, this third arrangement requires two-way telemetry between the drill rig and locator/controller such that drill string status display 164 and operations status display 174 are provided as part of display 150 on the locator/controller. At the same time, these status displays are optional on display 110 at the drill rig.
[0033] Still referring to FIGS. 2 and 6 , in accordance with the present invention, using locator/controller 140 , operator 141 is able to issue control commands which are executed by the arrangement of FIG. 6 at the drill rig. Concurrent with locating and controlling the boring tool, operator 141 is able to monitor the status of the drill rig using display 150 on the locator/controller. In this regard, display 174 on the locator/controller also apprises the operator of automated drill rod loading or unloading with indications such as, for example, “Adding Drill Pipe.” In this manner, the operator is informed of reasons for normal delays associated with drill string operations. Since push force applied by the drill rig to the drill string is a quite critical parameter, the present invention contemplates a feature (not shown) in which push force is measured at the drill rig and, thereafter, used to provide push force feedback to the operator via joystick 148 for ease in monitoring this critical parameter. The present invention contemplates that this force feedback feature may be implemented by one of ordinary skill in the art in view of the teaching provided herein. Still other parameters may be monitored at the drill rig and transmitted to locator/controller 140 . In fact, virtually anything computed or measured at the drill rig may be transmitted to the locator/controller. For example, locator/controller 140 may display (not shown) deviation from a desired path. Path deviation data may be obtained, for example, as set forth in U.S. Pat. No. 5,698,981 entitled BORING TECHNIQUE which is incorporated herein by reference. Alternatively, path deviation data may be obtained by using a magnetometer (not shown) positioned in the boring tool in combination with measuring extension of the drill string. With data concerning the actual path taken by the boring tool, the actual path can be examined for conformance with minimum bend radius requirements including those of the drill string or those of the utility line which, ultimately, is to be pulled through the completed bore. That is, the drill string or utility line can be bent too sharply and may, consequently, suffer damage. If minimum bend radius requirements for either the drill string or utility are about to be violated, an appropriate warning may be transmitted to locator/controller 140 . It should be appreciated that with the addition of the drill rig control module, complete remote operation capability has been provided. In and by itself, it is submitted that integrated locating capability and remote control of a boring tool has not been seen heretofore and is highly advantageous. When coupled with remote drill rig status monitoring capability, the present invention provides remarkable advantages over prior art horizontal directional drilling systems.
[0034] The advantages of the fully automated embodiment of the present invention essentially eliminate the need for a skilled drill rig operator. In this regard, it should be appreciated that the operator of a walkover locator is, in most cases, knowledgeable with respect to all aspects of drill rig operations. That is, most walkover locator operators have been trained as drill rig operators and then advance to the position of operating walkover locating devices. Therefore, such walkover locator operators are well versed in drill rig operation and welcome the capabilities provided by the present invention.
[0035] It should be understood that an arrangement for remotely controlling and tracking an underground boring tool may be embodied in many other specific forms and produced by other methods without departing from the spirit or scope of the present invention. Therefore, the present examples are to be considered as illustrative and not restrictive, and the invention is not to be limited to the details given herein, but may be modified within the scope of the appended claims.
|
A drilling system performs underground boring using a drill rig and a boring tool which is configured for moving through the ground under control of the drill rig to form an underground bore. A monitoring arrangement, forming part of the system, includes a detection arrangement at the drill rig for monitoring at least one operational parameter to produce a data signal relating to at least one of a utility to be installed in the underground bore, the drill rig and the boring tool. A portable device forms another part of the system for receiving the data signal relating to the operational parameter for use by the portable device. A communication arrangement, for example using telemetry, transfers the data signal from the drill rig to the portable device. The operational parameter may be monitored for the purpose of preventing equipment failure.
| 4
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. patent application Ser. No. 13/030,257, filed Feb. 18, 2011, which claims the benefit of U.S. Provisional Application No. 61/338,897 filed Feb. 25, 2010.
[0002] This application also claims priority to German Patent Application No. 10 2011 003 824.8, filed Feb. 9, 2011, said priority claim being limited to additional disclosure not set forth in U.S. patent application Ser. No. 13/030,257.
FIELD OF THE INVENTION
[0003] The present invention relates to clutch housings for automotive transmissions in automotive vehicles such as, but not limited to, passenger vehicles, motor cycles, rough-terrain vehicles and trucks.
BACKGROUND OF THE INVENTION
[0004] Many, if not most, automotive clutch housings are fabricated from a cylindrical work piece. Spline teeth are then formed or cut into the cylindrical work piece. It is desirable to provide a clutch housing where the spline teeth of the clutch housing can be formed on a generally flat work piece that is later formed into a cylinder.
SUMMARY OF THE INVENTION
[0005] In a preferred embodiment, the present invention provides a clutch housing that is formed from a work piece of sheet strip material. The work piece has spline teeth form folded thereon. The form folded work piece is then formed into a cylinder body and is connected with a hub portion of the clutch housing.
[0006] 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
[0007] The present invention will become more fully understood from the detailed description and the accompanying drawings, wherein:
[0008] FIG. 1 is a perspective view of a cylindrical body of A clutch housing according to the present invention;
[0009] FIG. 2 is a schematic view of a generally flat metallic sheet metal work piece utilized to form THE cylindrical body of the clutch housing of the present invention;
[0010] FIG. 3 is a schematic view of a work piece shown in FIG. 2 being form folded by press brake tooling into a cylindrical BODY for the clutch housing of the present invention;
[0011] FIG. 4 is a schematic view of an alternative fold forming operation wherein splined teeth of the cylindrical body are formed by a rolling operation;
[0012] FIG. 5 is a top view of a clutch housing of the present invention;
[0013] FIG. 6 is a sectional view taken along lines 6 - 6 of FIG. 5 ;
[0014] FIG. 7 is a perspective view of the clutch housing shown in FIG. 5 ;
[0015] FIG. 8 is a front perspective view of a hub utilized in the clutch housing shown in FIG. 5 ;
[0016] FIG. 9 is a rear perspective view of the hub shown in FIG. 8 ;
[0017] FIG. 10 is a front view of the hub shown in FIG. 8 ;
[0018] FIG. 11 is a sectional view of the hub shown in FIG. 8 taken along lines 11 - 11 of FIG. 10 ;
[0019] FIG. 12 is an enlargement of a portion that is circled in FIG. 10 ;
[0020] FIG. 13 is a side perspective view of the hub shown in FIG. 8 ; and
[0021] FIG. 14 is an enlargement of a portion 14 encircled in FIG. 13 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0022] The following description of the preferred embodiment(s) is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses.
[0023] Referring to FIG. 1 , cylindrical body 410 for the clutch housing 407 ( FIG. 7 ) according to the present invention is shown. The cylindrical body 410 is fabricated from a fold formed strip sheet metal work piece 16 ( FIG. 2 ). Typically, steel is the material of choice. Typical cylindrical body 410 thicknesses can be approximately 1.5 mm. The cylindrical body 410 has a series of spline teeth 414 . The spline teeth 414 of the cylindrical body has an inner flat 413 and an outer flat 417 that are joined by slope portions 419 .
[0024] To fabricate the cylindrical body from the press brake tooling 41 is utilized having a re-hit portion 43 . The press brake tooling 41 and 43 stamp the spline teeth 414 into the shape of the cylindrical body. The spline teeth 414 , as schematically shown in FIG. 4 , can also be roll formed from a continuous flat strip work piece 16 . In a subsequent operation (not shown), an individual cylindrical body 410 is cut off.
[0025] The cylindrical body 410 has along its opposite ends, a dove tail interlock joint comprising a male tab 24 ( FIG. 2 ) and a corresponding female cut out 26 . The ends of the cylindrical body 435 and 437 are brought together to form the cylindrical shape of the cylindrical body and a connective interlock is formed by the dove tail joint 24 , 26 thereafter the ends 435 , 437 are joined preferably by welding, clenching or brazing.
[0026] Referring to FIGS. 5-14 , a clutch housing 407 is provided. As shown, clutch housing 407 will support friction plates on its outer diameter but the clutch housing can be designed to mount friction plates on its inner diameter. Clutch housing 407 has a hub portion 440 . In many embodiments, the hub 440 will be fabricated from powered metal. Hub 440 has a disc or planer portion 442 integrally connected with a cylindrical portion 444 having internal spline teeth 446 . The hub 440 has a series of apertures 448 to allow for passage of rivet fasteners 450 that connects the hub 440 with the cylindrical body 410 . The hub 440 along its peripheral surface has a series of radially projecting gear like teeth 451 . Alternating teeth 451 have radial overhangs 452 . The radial overhangs 452 are continuous with radial ribs or vanes 454 that are formed by depressions 458 in an outer surface of the hub disc portion 442 . Cylindrical body spline teeth 414 have a series of axially alternating positioned oil slots 416 . The cylindrical body 410 has a generally axial portion 418 and radially inwardly bent tabs 420 . Between the generally axial portion 418 and the radially inwardly bent tabs 420 is a transition region 422 . Between the tabs 420 within the transition region 422 , there are slots 424 . Connecting the generally cylindrical body 410 with the hub 440 are a series of rivets 450 . The radial tabs 420 are aligned with the hub depressions 458 and the hub's radial gear like teeth 451 are aligned with the outer radial flat 417 of the spline teeth 414 of the cylindrical body 410 . Additionally, the gear teeth 451 aid in supporting the spline teeth 414 in the transition region 422 . The vanes 454 and their slot 424 received radial overhangs 452 provide for a circumferential interlock and torsional force transfer to the cylindrical body tabs 420 . In the transition region 422 , the aforementioned interlock inhibits a propagation of cracks in the cylindrical body 410 .
[0027] Between the radially inward bent tabs 420 of the cylindrical housing and the disc portion 442 of the hub, there is a torsional interchange facilitated by the rivets 450 and a sheer mold. The tabs 420 lateral sides 471 have an interference fit with the vanes 454 to allow a torsional interchange in a compressive contact mode between the tabs 420 and the vanes 454 . Via the overhang 458 of the vanes 454 in the slot 424 , there is also a similar compressive torsional interchange between the cylindrical body and the hub in the transition region 422 of the cylindrical body. Typically the hub 440 is also connected to the cylindrical body 410 by the interference connection of the splined teeth 414 with the hub radially projecting gear like teeth 451 . Accordingly, a maximum amount of torsional interchange between the hub and cylindrical body is achieved while allowing the material utilized to fabricate the cylindrical body 410 to be as thin as possible while at the same time preventing tears in the material of the cylindrical body. Torsional interchange between the hub and cylindrical body is achieved along the main portion of the radial tab 420 along the peripheral edges of the tab 420 within the transition region 422 and with the circumferential interlock between the hub gear teeth 541 and the cylindrical body splined teeth 414 providing a strong and enduring joint between the hub and cylindrical body.
[0028] 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.
|
An automotive clutch housing and a method of manufacture thereof is provided. The clutch housing has a cylindrical body that is formed from a form folded strip metal sheet that is later formed into a cylindrical body. The cylindrical body is then joined to a hub to form a clutch housing.
| 5
|
BACKGROUND OF THE INVENTION
[0001] This invention relates to methods and apparatus for inflating and sealing pillows in packaging.
[0002] This invention relates particularly to the construction and operation of a machine which is small enough to be installed for operation on site where articles packaged for transport are placed in shipping containers with protective inflated pillow-type strip packaging.
[0003] This invention relates particularly to a machine which is compact in overall size, which can be conveniently operated to produce varied lengths of strips of inflated pillow-type packaging as needed, which can begin production of inflated pillow-type strip packaging immediately after being held out of a production cycle for some period of time and which applies a heated sealing element directly to and in sliding contact with a web of film to securely seal the inlet port of an inflated pillow while the pillow is under pressure and as the web of film is continuously and uninterruptedly advanced through the machine.
[0004] This invention relates particularly to a machine which forms the seal complete and secure during a short path of travel and during a short interval of time. The seal is made without the need for additional pressing together of the film after the sealing and without the need for additional cooling of the seal after the sealed inlet port moves out of contact with the sealing structure.
[0005] Webs of plastic film which are constructed to permit the production of strips of air filled envelopes, cushions and pillows have (in the past ten years or so) been used extensively for cushioning objects to be transported in containers.
[0006] The thin webs of plastic film are inexpensive, tough, resilient and recyclable. Strips of inflated pillow packaging which are created from these webs of plastic film are used for void-fill packaging to replace products such as crumpled paper or polystyrene peanuts and for protective packaging to replace molded or extruded foams.
[0007] U.S. Pat. Nos. 5,454,642; 5,651,237; 5,755,328; 4,017,351; and 5,824,392 disclose methods, apparatus, and webs of plastic film used for making strips of inflated pillow packaging of this general kind. Each of these U.S. patents is incorporated by reference in this application.
[0008] Co-pending application Ser. No. 09/207,129 filed Dec. 8, 1998 and entitled “Method and Apparatus for Manufacturing Air-Filled Sheet Plastic Shipping Cushions and the Like”, Nicholas P. De Luca and Andrew Perkins, inventors and co-pending application Ser. No. 09/439,552 filed Nov. 12, 1999 and entitled “Machine and Method for Manufacturing a Continuous Production of Pneumatically Filled Inflatable Packaging Pillows”, Andrew Perkins, Philipp Borchard, and Nicholas P. De Luca, inventors also disclose methods, apparatus and webs of plastic film of this general kind. Each of these two co-pending applications is assigned to the same assignee as the assignee of this application. Each of these two co-pending applications is incorporated in this application by reference.
[0009] Sealing an inflated pillow made a web of plastic film while the air inflates the pillow under pressure and while the web of plastic film is being transported through the machine presents problems.
[0010] The seal must be secure and must not leak in order for the inflated pillow packaging to be used effectively for cushioning objects transported within a container.
[0011] The seal needs to be formed efficiently, quickly and without extensive, related pressing and/or cooling structure in order to make the machine as compact as possible in size and as efficient as possible in production rate.
[0012] To simplify machine construction and to provide a high efficiency of production, it is desirable to be able to make the seal as the web of plastic film is moved continuously and without any interruption and/or intermittent stopping of the film transport during the sealing operation.
[0013] It is a primary object of the present invention to construct and to operate a machine which is compact in size, which is efficient in production, which is continuous and uninterrupted in operation and which produces seals which are secure and which do not leak.
SUMMARY OF THE PRESENT INVENTION
[0014] In a specific embodiment of the present invention, a machine inflates and seals pillows in packaging while continuously and uninterruptedly advancing a web of film through an inflating station and a sealing station. The inflating station sequentially inflates pillows at preformed patterns in the web of film by introducing pressurized air through a narrow width inlet port of a preformed pattern. The sealing station seals each inlet port by applying a heated sealing element directly to and in sliding contact with the web of film while the air in an inflated pillow is under pressure as the inlet port moves across the heated sealing element.
[0015] The web of film has an uninflated pillow pattern and an uninflated inflation channel preformed in the film. The uninflated pillow patterns comprise multiple, spaced apart, pillow patterns aligned along one side of an inflation channel. The inflation channel extends longitudinally and continuously along the entire length of the film. Each uninflated pillow pattern has a narrow width inlet port extending generally transversely to the longitudinally extending inflation channel and connecting the uninflated pillow pattern to the uninflated inflation channel so that, when pressurized air is introduced into the inflation channel, the pressurized air can be transmitted through the inlet port to inflate the pillow pattern. In some cases the preformed pattern is also formed with outlet ports connected to the inflation channel in such a way that air entering the inflation channel can move into a pillow through an inlet port and can also exit out of the inflation channel through the outlet port. The outlet port is generally shaped smaller than the inlet port.
[0016] By allowing the air above a desired pressure to escape through an outlet port or ports, the pressure in the inflation channel is maintained at a desired level for inflating the pillows without creating over-pressurization.
[0017] The air escaping through the outlet port is also sensed to detect where the pillows are in the machine. These detected outlet port positions are then used as signals for an associated electronic unit to count the number of pillows inflated in a particular run through the machine. This also facilitates being able to stop the movement of the film through the machine after one production run of a selected number of inflated pillows at a position which is the right position to start a subsequent production run of a selected number of inflated pillows.
[0018] In a specific embodiment of the present invention, the web of film with the preformed patterns is stored on a storage roller of the machine and is advanced through the machine by a first set of nip rollers and a second set of nip rollers at a respective first film transport station and a second film transport station.
[0019] Pressurized air is introduced into the inflation channel of the web of film at an inflating station as the web of film is transported through the first film transport station. The pressurized air inflates at least one of the pillow patterns prior to the time the web of film is continuously transported through a sealing station.
[0020] Pressure is maintained in the inflated pillow pattern within a calibrated pressure range during the time that the web of film is continuously transported through the sealing station.
[0021] At the sealing station the inlet port of an inflated pillow is sealed by applying a heated sealing element directly to and in sliding contact with the web of film. The heated sealing element slides across the inlet port while the air in the inflated pillow is under pressure and as the web of film is continuously and uninterruptedly advanced throughout all components of the machine.
[0022] The heated sealing element has a relatively small longitudinal dimension in the direction of movement of the web of film. In a specific embodiment the length of the heated sealing element is about the same as the width of the inlet port of a pillow pattern. This small size of the heated sealing element helps minimize the amount of sealing heat applied to the web of film.
[0023] The sealing station includes a sealing roller disposed alongside the heated sealing element so as to permit the web of film to be advanced between the sealing roller and the heated sealing element. Adjustable biasing means provide for adjustment of the force with which the heated sealing element and the sealing roller are pressed toward engagement with one another.
[0024] The sealing roller is positioned with respect to the first and second pairs of nip rollers so as to cause the web of film to wrap around a part of the peripheral surface of the sealing roller both in a circumferential direction and also in a lateral direction. This helps create a dead and flat zone right at and adjacent to the line of sealing across the inlet port. This in turn facilitates making a secure seal without leaking while the pillow is inflated under pressure.
[0025] The axes of rotation of at least the second pair of nip rollers are preferably canted at a slight angle with respect to the axis of rotation of the sealing roller.
[0026] The second pair of nip rollers are preferably rotated at a speed slightly faster than the speed of rotation of the first pair of nip rollers so as to maintain tension in the web of film between the second and first pair of nip rollers.
[0027] In one specific embodiment of the present invention the heated sealing element is a fabric covered Nichrome wire disposed at the end of a bar element which is biased toward engagement with a sealing roller. The fabric covering of the Nichrome wire has a Teflon coating on its outer surface for facilitating sliding of the heated sealing element on the engaged surface of the film as the web of film is advanced through the machine.
[0028] The bar on which the heated sealing element is mounted is a composite bar. The very tip of the bar is a ceramic having good insulating qualities, and the remainder of the bar is a different material selected to provide enhanced mechanical durability.
[0029] The seal is formed complete and secure during a short path of travel through the sealing station.
[0030] The seal is complete and secure at the time the web of film moves out of contact with the wheel at the sealing station and without the need for additional pressing together of the film after the sealing station and without the need for additional cooling of the film across the sealed inlet port after the sealed inlet port moves out of contact with the sealing station.
[0031] In a second specific embodiment of the present invention the sealing wheel is pressure biased toward engagement with the heated sealing element.
[0032] In both the first and second specific embodiments the heated sealing element and the sealing wheel are spaced apart from one another when the machine is not transporting the web of film through the machine in a production run. This enables the heated sealing element to be maintained at a desired temperature level while preventing contact with and possible burning of the unmoving film at the sealing station.
[0033] In one specific embodiment of the invention the fabric covering for the Nichrome wire is held in a fixed position at the end of the bar element and is replaced as needed.
[0034] In another specific embodiment of the invention the heating station includes a cartridge unit which can be quickly and easily interchanged with another cartridge unit. The cartridge unit includes an elongated strip of the fabric covering. The strip is mounted on two rotatable reels. The fabric always covers the Nichrome wire, as in the first specific embodiment, and the fabric has a Teflon coating on the side which engages the film in sliding contact, as in the first specific embodiment. The elongated strip of fabric covering is wound between the two reels so as to be moved across the length of the Nichrome wire at a speed which is much slower than the speed of movement of the film through the machine but which is fast enough to ensure that the covering strip of fabric is always effective to function properly without any burn through of the fabric or damage to the film from the heated Nichrome wire. The cartridge unit permits the Nichrome wire of the heated sealing element to be easily disconnected from its power supply. The cartridge units are constructed to be readily interchanged as units, rather than having to replace individual components of the cartridge unit.
[0035] Methods and apparatus which incorporate the features noted above and which are effective to function as described above comprise further, specific objects of this invention.
[0036] Other and further objects of the present invention will be apparent from the following description and claims and are illustrated in the accompanying drawings, which by way of illustration, show preferred embodiments of the present invention and the principles thereof and what are now considered to be the best modes contemplated for applying these principles. Other embodiments of the invention embodying the same or equivalent principles may be used and structural changes may be made as desired by those skilled in the art without departing from the present invention and the purview of the appended claims.
BRIEF DESCRIPTION OF THE DRAWING VIEWS
[0037] [0037]FIG. 1 is an isometric view of a machine, constructed in accordance with one embodiment of the present invention, for inflating and sealing pillows in packaging. FIG. 1 is a general view which illustrates how a web of film is transported through the machine. FIG. 1 shows how the web of film has a preformed pattern of spaced-apart, inflatable pillows aligned along one side of a longitudinally extending inflation channel. FIG. 1 illustrates how rollers (at a first transport station, at a sealing station, and at a second transport station) are positioned to engage the underside (as viewed in FIG. 1) of the web of film.
[0038] [0038]FIG. 2 is another isometric view of the machine shown in FIG. 1, but in FIG. 2 the lower part of the figure has been revised to (in effect) see through the web of film in order to show details of certain structure of the machine. FIG. 2 shows the inflation tube of the inflating station, the nip rollers of the first transport station, the heated sealing element and the associated sealing roller at the sealing station, and the nip rollers at the second transport station.
[0039] [0039]FIG. 3 is an isometric view of the machine of FIGS. 1 and 2, but without the web of film material. FIG. 3 shows the main structural and operative features of the machine itself.
[0040] [0040]FIG. 4 is an isometric, enlarged view showing details of the features of the first film transport station, the inflation station structure, the sealing station structure, the slitting station structure, and the second film transport station structure.
[0041] [0041]FIG. 5 is an isometric, enlarged view like FIG. 4 but shows details of just the mechanism for driving the various rollers of the machine. FIG. 5 does not show the inflation station structure, the heated sealing element at the sealing station, or the slitter structure for opening up the inflation tube of the web of film after the sealing station.
[0042] [0042]FIG. 6 is an isometric view showing details of the structure of the sealing station. FIG. 6 shows the heated sealing element pressed toward engagement with the sealing wheel in the positions occupied by those two components during a production run of the inflated pillow packaging through the machine.
[0043] [0043]FIG. 7 is a top plan view, taken along the line and in the direction indicated by the arrows 7 - 7 in FIG. 6, but showing the heated sealing element retracted away from the sealing wheel in the positions occupied by those two components when no film is being transported through the machine.
[0044] [0044]FIG. 8 is a top plan view of a specific embodiment of a web of film constructed in accordance with the present invention and having a specific pattern of inflatable pillows, inlet ports for permitting inflation of the pillows, and escape ports for preventing over pressurization of the pillows and for also permitting more accurate position sensing of the pillows as the web of film moves through the machine.
[0045] FIGS. 9 A- 9 G are a series of the isometric views showing details of the structure, components and sequence of assembly of certain components of the heated sealing element at the sealing station.
[0046] [0046]FIG. 10 is an isometric view of a machine constructed in accordance with a second embodiment of the present invention. The embodiment of the machine shown in FIG. 10 includes a cartridge unit which is mounted on a separate sub-plate or sub-frame and which permits all of the components of the cartridge unit to be quickly and easily removed and replaced by another, replacement cartridge unit. The cartridge unit provides the heated sealing element components for the sealing station. FIG. 10 shows the sealing wheel of the sealing station positioned to engage the web of film in sliding contact with the heated sealing element during a production run of packaging.
[0047] [0047]FIG. 11 is an isometric view like FIG. 10 but showing the sealing wheel moved to a retracted position which permits the web of film to move out of contact with the heated sealing element when the machine is stopped between production runs and the film is not being transported through the machine.
[0048] [0048]FIG. 12 is an enlarged, isometric view of the replaceable cartridge unit itself. FIG. 12 shows the strip of covering fabric in stored positions on the reels of the cartridge unit prior to installation of the cartridge unit in the machine. When installed in the machine, a portion of the strip of covering fabric is positioned over the wire of the heating element (as illustrated in FIGS. 10 and 11).
[0049] [0049]FIG. 13 is an enlarged, isometric view of the sealing wheel and the related actuator mechanism for positioning the sealing wheel at the sealing station.
[0050] [0050]FIG. 14 is an enlarged, side elevation view of the sealing station structure with the structure in the operative position shown in FIG. 10; and,
[0051] [0051]FIG. 15 is an enlarged, side elevation view of the sealing station structure with the structure in the non-operating position shown in FIG. 11.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0052] [0052]FIGS. 1, 2 and 3 are isometric view of a machine, constructed in accordance with one embodiment of the present invention, for inflating and sealing pillows in packaging.
[0053] The machine is indicated by the general reference numeral 11 in each of FIGS. 1, 2 and 3 .
[0054] The machine 11 , as most easily viewed in FIG. 3, comprises a main plate 13 on which various structural and operational features are mounted.
[0055] A support tube 15 is mounted at the upper (as viewed in FIGS. 1 - 3 ) of the main plate 13 for supporting a roll 17 of a web of film 19 (see FIGS. 1 and 2).
[0056] Guide tubes 21 and 23 are mounted on the plate 13 below the tube 15 . The tubes 21 and 23 serve to guide the web of film 19 from the roll 17 to the operating mechanism 25 of the machine 11 . The operating mechanism 25 is described in more detail below.
[0057] The mechanism 25 is illustrated in detail in FIG. 4 and comprises a first film transport station 27 , a second film transport station 29 , an inflating station 31 , a sealing station 33 , and a slitting station 35 .
[0058] The first film transport station 27 includes a first pair of nip rollers 37 and 39 for gripping the web of film 19 (see FIG. 1) and for pulling the web of film 19 from the roll 17 and under and over the guide tubes 21 and 23 and through the first film transport station 27 when the nip rollers are rotated by associated drive gears 41 , 43 and a drive belt 45 . The nip rollers 37 and 39 are rotated in the directions indicated by the direction arrows on the drive gears 41 and 43 shown in FIG. 4.
[0059] The drive belt 45 is driven by a drive gear 47 which is in turn driven by a motor 49 (see FIG. 5).
[0060] The second film transport station 29 comprises a second pair of nip rollers 49 and 51 which grip the web of film 19 to continuously advance the web of film 19 from the first transport station 27 to and through the inflating station 25 and to and through the sealing station 33 and then to and through the second film transport station 29 .
[0061] The nip rollers 49 and 51 are driven by drive gears 53 and 55 and in the rotational directions indicated by the directional arrows on the drive gears 53 and 55 in FIG. 4.
[0062] Drive shafts 40 and 44 transmit the drive from the drive gears 41 and 43 to the nip rollers 37 and 39 .
[0063] Drive shafts 50 and 52 transmit the drive from the drive gears 53 and 55 to the nip rollers 49 and 51 .
[0064] With continued reference to FIG. 4, the drive belt 45 passes about an idler gear 57 . The drive gears 41 , 43 , 47 , 53 , 55 and idler gear 57 are all mounted for rotation on and are supported by the main plate 13 .
[0065] The inflating station 31 includes an inflation tube 59 and a generally spherically shaped and partially Teflon coated ball 61 located at the upper end (as viewed in FIG. 4) of the tube 59 . The ball 61 has a plurality of openings 63 for injecting pressurized air into an inflation channel in the web of film 19 .
[0066] As illustrated in FIGS. 1, 2 and 8 , the web of film 19 as stored on the roll 17 shown in FIG. 1 has a pattern of pillows 65 , a longitudinally extending inflation channel 67 , inlet ports 69 , and outlet ports 71 preformed in the web of film. The pillows 65 , channel 67 , ports 69 and ports 71 are uninflated in the web of film as stored on the roll 17 .
[0067] The uninflated pillow patterns 65 are longitudinally spaced apart from one another and are aligned (in the embodiment of the web of film 19 illustrated in the drawings) along one side of the inflation channel 67 .
[0068] The inflation channel 67 extends longitudinally and continuously along the entire length of the web of film 19 .
[0069] The inflation channel 67 is dimensioned to provide a close, sliding fit over the Teflon coated ball 61 .
[0070] Each pillow 65 is connected to the inflation channel 67 by an inlet port 69 . The inlet port 69 extends generally transversely to the longitudinally extending inflation channel 67 and has a narrow interior width which is positioned at the sealing station 33 (in a manner to be described more fully below) to facilitate quick and secure sealing of pressurized air within an inflated pillow 65 in a small path of travel and in a short time of continuous, uninterrupted travel through the sealing station 33 .
[0071] The outlet ports 71 are shaped to be somewhat smaller than the inlet ports 69 . These outlet ports 51 are located on the side of the channel 67 opposite the inlet ports 69 and are generally aligned with the inlet ports 69 .
[0072] As will be described in greater detail below, the outlet ports 71 allow air to escape in a way to maintain pressure in the channel 67 and in the inflated pillows at a calibrated, desired level without creating over-pressurization in the pillows.
[0073] In addition, the air that exits from an outlet port 71 can be sensed by a pressure transducer 73 (see FIG. 8) to allow for accurate position sensing of the pillows as the pillows move through the machine 11 .
[0074] The air escaping through the outlet ports is sensed to detect where the pillows are in the machine. These detected outlet port positions are then used as signals for an associated electronic unit to count the number of pillows inflated in a particular run through the machine. This also facilitates being able to stop the movement of the film through the machine, after one production run of a selected number of inflated pillows, at a position which is the right position to start a subsequent production run of a selected number of inflated pillows.
[0075] The upper end of the inflation tube 59 is formed with a small curvature so as to better follow the path of the film 19 as the film is advanced through the first transport station 27 and the sealing station 33 .
[0076] Details of the construction and mode of operation of the sealing station 33 are illustrated and will be described with reference to FIGS. 4, 6 and 7 .
[0077] The sealing station 33 comprises a sealing roller 75 mounted on a shaft 77 which is in turn mounted for rotation in a bearing assembly attached to the main plate 13 .
[0078] The sealing station 33 also comprises a heated sealing element located at the outer end (the right hand end as viewed in FIG. 7) of a bar 81 . The very tip 80 of the bar 81 is a ceramic of aluminum silicate to provide an insulation function, and the remainder of the bar 81 is a different material selected for mechanical durability.
[0079] The bar 81 is mounted for sliding motion within a support 83 .
[0080] A spring 85 and an adjustment screw 87 provide a selectable bias force for biasing the bar 81 toward the opposed periphery of the roller 75 so that the film 19 (in the longitudinally extending strip which crosses the inlet ports 69 ) is pressed in rolling contact with the outer periphery roller 75 and in sliding contact with the end surface of the bar 81 as the first and second film transport stations continuously advance the web of film 19 through the sealing station 33 .
[0081] An actuator 89 is included in the sealing station 33 for retracting the bar 81 against the bias of spring 85 and away from engagement with the roller 75 when the film 19 is not being advanced through the machine 11 . This facilitates keeping the heating element energized at the proper heating level and out of contact with the film 19 during time intervals when the machine 11 is not being used to produce inflated pillow packaging.
[0082] Details of the structure, components and sequence of assembly of components of the heated sealing element are shown in the exploded views of FIGS. 9 A- 9 F.
[0083] The heating element disposed at the end of the bar 81 , in a specific embodiment of the present invention, comprises at least one Nichrome wire 70 which runs vertically (as viewed in FIGS. 9 A- 9 G) along the right hand end of the bar 81 .
[0084] The Nichrome wire 70 at this location has a length about the same as the throat width of an outlet port 69 in the film 19 , and the Nichrome wire 70 is covered by a fabric 72 having a Teflon coating on the surface which contacts the film 19 . The fabric covering 72 helps to form the wire 70 to a preferred shape for engagement with the film 19 , and the Teflon coating facilitates sliding movement of the film 19 with respect to the heated sealing element.
[0085] The heated sealing element comprises at least one Nichrome wire 70 , but (as illustrated in FIGS. 9 A- 9 F) the present invention also encompasses using a plurality of parallel extending and laterally spaced apart Nichrome wires 70 for providing multiple seal lines across inlet ports 69 of the pillows 65 .
[0086] As best illustrated in FIGS. 6 and 7, wires 91 and 93 conduct electricity to the Nichrome wire for heating the Nichrome wire.
[0087] The slitting station 35 (see FIG. 4) includes a blade 95 attached to the inflation tube 59 and positioned to slit the inflation channel 67 in the film 19 after the outlet port 69 of a pillow 65 has been sealed at the sealing station 33 . This enables strips of inflated packaging to be removed from the machine 11 .
[0088] It is an important feature and benefit of the present invention that the components of the mechanism 25 and the coaction between those components enable a seal to be formed complete and secure in a short path of travel of the film through the sealing station 33 and in a short period of time and without the need for additional pressing together of the web of film after the sealing station and without the need for additional cooling of the seal across the inlet port after the sealed inlet port moves out of contact with the sealing station. The sealing of the inlet port at the sealing station is performed by applying the heated sealing element directly to and in sliding contact with the web of film and across the inlet port while the air and the inflated pillow is under pressure and as the web of film is continuously and uninterruptedly advanced through the mechanism 25 shown in FIG. 4.
[0089] A number of features of the present invention contribute to obtaining this efficient and beneficial sealing result.
[0090] As described above, the outermost tip of the bar 81 is a ceramic material which functions as an insulator to help confine the heat of the heating element to substantially just the linear area of contact of the fabric covered Nichrome wire with the film 19 .
[0091] The roller 75 is laterally offset outwardly (as viewed in FIGS. 1 - 5 ) and is positioned with respect to the pairs of nip rollers 37 - 39 and 49 - 51 so as to cause a bump in the film 19 at the sealing station 33 . This helps to create a dead zone adjacent the inlet port 69 to be sealed by causing the web of film 19 to wrap around a part of the peripheral surface of the sealing roller 75 both in a circumferential direction and also in a lateral direction.
[0092] Driving the second pair of nip rollers 49 - 51 at a slightly higher speed than the first pair of nip rollers 37 - 39 helps to insure that the film 19 is maintained flat and in substantially pressure sealing engagement with the periphery of the sealing roller 75 .
[0093] As best shown in FIG. 5, the axes of rotation of at least the second set of nip rollers 49 - 51 are preferably canted at a slight upward (as viewed in FIG. 5) angle with respect to the axes of rotation of the main drive gear 47 and the sealing roller 75 .
[0094] In a specific embodiment of the present invention the axes of rotation of the first set of nip rollers 37 - 39 are also canted at this same slightly upwardly inclined angle.
[0095] The inclusion and positioning of the outlet ports 71 (see FIG. 8) and the smaller size of these outlet ports contribute to allowing air to escape through the outlet ports in an amount to maintain sufficient pressure in the channel 67 without permitting over-pressurization in that channel 67 or in the pillows 65 .
[0096] The present invention permits sealing the inlet port at a sealing station by applying a heated sealing element directly to and in sliding contact with the web of film and across the inlet port while the air and the inflated pillow is under pressure and as the web of film is continuously and uninterruptedly advanced through each of the first transport station, inflating station, sealing station, second transport station and slitting station.
[0097] In FIGS. 1, 2 and 8 of the drawings the pillows 65 are shown in a generally rectangular-shaped pattern. It should be noted, however, that the pillows 65 can be any preformed pattern configuration. The patterns of the pillows 65 can, for example, include preformed seal line elements within the interior of the pillows which permit the pillows to be folded along one or more of the preformed interior seal lines. This in turn permits one pillow to cushion an object in more than one direction when placed within a shipping container.
[0098] Score lines (not illustrated in the drawings, but similar to score lines shown in webs of plastic film described in numerous ones of the prior U.S. patents incorporated by reference in this application) permit ready detachment of single ones or groups of inflated pillows from the film 19 after the pillows are inflated and sealed.
[0099] A number of different film compositions (also as noted in U.S. patents incorporated by reference in this application) can be used as the composition material for the web of film 19 .
[0100] The machines that are used to preform the patterns on the web of film 19 include conventional presses which impress multiple pillow patterns (and the related ports and inflation channel) on a strip of film 19 on each pressing operation. The pattern is formed while there is no inflation pressure anywhere in the web 19 .
[0101] The preformed pattern can also be formed by a roller arrangement in which at least one roller is heated and configured to form the desired patterns.
[0102] Pattern forming machines of these kinds are also disclosed in several of the U.S. patents incorporated by reference in this application.
[0103] Such machines for forming preformed patterns in the film 19 can be associated with the machine 11 shown in FIG. 1 to replace the storage roll 17 so that the preformed patterns can be preformed continuously at the site where the machine 11 is installed. However, in most cases it is more practical to use a storage roll 17 with preformed patterns than it is to preform the patterns at the job site where the machine 11 is to be used.
[0104] A second embodiment of a machine constructed in accordance with the present invention is illustrated in FIGS. 10 - 15 of the drawings. This second embodiment is indicated by the general reference numeral 101 .
[0105] The components and parts of the machine 101 which correspond to the machine 11 shown in FIGS. 1 - 9 are indicated by corresponding reference numerals.
[0106] The machine 101 includes a cartridge unit 103 (see FIG. 12) which is mounted on a separate sub-plate or sub-frame 105 . The sub-frame 105 is mounted on the main plate or main frame 13 . This cartridge unit technique permits the components of the entire cartridge unit to be quickly and easily interchanged (as a unit) with another replacement cartridge unit. Individual components of the cartridge unit do not have to be removed and replaced.
[0107] In the machine 101 shown in FIGS. 10 - 15 , the construction and mounting of the cartridge unit 103 permits the entire cartridge unit to be pulled out of a box and plugged in as a unit at the production site. This cartridge unit permits all of the components of the cartridge unit to be replaced as a unit. It is never necessary, for example, to replace the Nichrome wires as individual elements in the field. Instead, the entire cartridge unit is just pulled out and replaced as a unit with a replacement cartridge unit.
[0108] The structure, components and mode of operation of the first film transport station 27 , the second film transport station 29 , the inflation station 31 , and the slitting station 35 are the same as the corresponding mechanism, components and mode of operation described above with reference to the machine 11 , and will not be reviewed in more specific detail at this point.
[0109] The specific structure of the sealing station 33 of the machine 101 is different from the machine 11 and will be described in more detail below. However, the method of making seals across the inlet ports 69 in the machine 101 is the same as the method of machine 11 , as will be understood from the description to follow.
[0110] One difference between the sealing station structure of the machine 11 and the sealing station structure of the machine 101 is in the way that the heated sealing element and the sealing wheel are moved apart from one another during those times when the machine is stopped between production runs of inflated pillows.
[0111] In the machine 11 (and as illustrated in FIG. 7) the heated sealing element which is mounted on the end of the bar 81 is retracted away from the sealing wheel 75 . In the machine 11 the shaft 75 of the heated sealing wheel 75 is held in a fixed position with respect to the frame 13 in all modes of operation of the machine 11 .
[0112] In the machine 101 the heated sealing element is held in a fixed position with respect to the frame 13 . The rotational shaft 77 of the sealing wheel 75 is mounted for rotation in a movable support bracket 75 so that the sealing wheel 75 is movable toward and away from the heated sealing element.
[0113] As best illustrated in FIG. 13, the support bracket 75 is mounted on a rod 82 of an actuator 84 . The actuator 84 is mounted on a support plate 86 , and the support plate 86 is mounted on the main plate 13 of the machine 101 .
[0114] The actuator 84 extends and retracts the rod 82 to move the sealing wheel 75 between the retracted position of the rod 82 shown in FIGS. 11 and 15 and the extended position shown in FIGS. 10 and 14.
[0115] In the retracted position illustrated in FIGS. 11 and 15 the sealing wheel 75 is positioned to let the film 19 remain out of contact with the heated sealing element when the machine 101 is not operated in a production run.
[0116] In the extended position shown in FIGS. 10 and 14 the sealing wheel 75 is positioned to engage the film 19 and to press that film 19 in sliding contact with the heated sealing element as the film 19 is continuously and uninterruptedly advanced through the machine during a production run of inflated pillows.
[0117] The force with which the film 19 is engaged in sliding contact with the heated sealing element is determined by selecting the pressure level within the actuator 84 .
[0118] As best illustrated in FIGS. 12, 10, and 14 , the cartridge unit 103 comprises a guide block 107 mounted in a fixed position on the sub-plate 105 , two reels 109 and 111 , each mounted for rotation on the sub-plate 105 , and a guide post 113 mounted on the sub-plate 105 .
[0119] The reels 109 and 111 are storage and take-up reels for a strip of covering fabric 72 . The fabric 72 has a Teflon coating on the side engaged in sliding contact with the film 19 .
[0120] The strip of covering fabric 72 is trained around a guide post 113 and into the guide slots 115 and 1 17 which are recessed within the outer and forward surfaces of the flanges 119 and 121 of the guide block 107 .
[0121] The way that the strip of covering fabric 72 is conveyed from the storage roller 109 , around the guide post 113 , through the guide slot 115 , over the Nichrome wires 70 , through the guide slot 117 and onto the reel 111 is best illustrated in FIGS. 10, 11, 14 and 15 .
[0122] In a specific embodiment of the machine 101 the lower reel 111 is driven, through reduction gearing, and by an electric motor (not shown), to pull the strip of covering fabric 72 across the Nichrome wires 70 at a relatively slow speed (a speed considerably slower than a speed at which the web of film 19 is transported through the machine 101 during a production run), but at a speed fast enough to insure that no part of the covering fabric 72 is ever in contact with the Nichrome wires 70 long enough to permit any burn through of the fabric by the Nichrome wires 70 . The reel storage of the covering fabric 72 and the slow movement of the fabric with respect to the Nichrome wires 70 during operation of the machine 101 thus insure that the area of the fabric engageable with the Nichrome wires is, in effect, renewed soon enough to prevent any burn through.
[0123] As best illustrated in FIGS. 12 and 15, the outer tips of the flanges 119 and 120 extend slightly beyond the outer surfaces of the Nichrome wires 70 . This insures that the covering fabric 72 is engaged with the Nichrome wires 70 only when the sealing wheel 75 is moved to the position shown in FIGS. 10 and 14 during a production run of the machine 101 .
[0124] The strip of covering fabric 72 is held out of contact with the Nichrome wires 70 when the machine 101 is not being operated in a production run of packaging.
[0125] While not illustrated in FIGS. 10 - 15 , the Nichrome wires 70 are energized by detachable leads 91 and 93 (as illustrated for the machine 11 in FIGS. 9 A- 9 G).
[0126] The sealing roller 75 of the machine 101 is laterally offset outwardly in the same way as the sealing roller 75 of the machine 11 so as to cause a bump in the film 19 at the sealing station 33 . This helps to create a dead zone adjacent the inlet port 69 to be sealed by causing the web of film 19 to wrap around a part of the peripheral surface of the sealing roller 75 both in a circumferential direction and also in a lateral direction (as described above with reference to the machine 11 ).
[0127] The machine 101 permits sealing the inlet port at a sealing station by applying a heated sealing element directly to and in sliding contact with the web of film and across the inlet port while the air in an inflated pillow is under pressure and as the web of film is continuously and uninterruptedly advanced through each of the first transport station, inflating station, sealing station, second transport station and slitting station.
[0128] While we have illustrated and described the preferred embodiments of our invention, it is to be understood that these are capable of variation and modification, and we therefore do not wish to be limited to the precise details set forth, but desire to avail ourselves of such changes and alterations as fall within the purview of the following claims.
|
A machine which inflates and seals pillows in packaging is compact in overall size, can be conveniently operated to produce varied lengths of strips of inflated pillow-type packaging as needed, can begin production of inflated pillow-type strip packaging immediately after being held out of a production cycle for some period of time, and applies a heated sealing element directly to and in sliding contact with a web of film to securely seal the inlet port of an inflated pillow while the pillow is under pressure and as the web of film is continuously and uninterruptedly advanced through the machine.
| 8
|
CROSS-REFERENCE TO A RELATED PATENT APPLICATION
This patent application is a divisional patent application of U.S. patent application Ser. No. 08/683,923, filed Apr. 19, 1996 which issued on May 19, 1998, as U.S. Pat. No. 5,753,162, and which was a divisional patent application of U.S. patent application Ser. No. 08/451,933, filed May 26, 1995 which issued on May 13, 1997, as U.S. Pat. No. 5,628,849.
This patent application is related to U.S. patent application Ser. No. 08/451,899, entitled "APPARATUS FOR IN-SITU ENVIRONMENT SENSITIVE SEALING AND/OR PRODUCT CONTROLLING", filed on May 26, 1995, assigned to the assignee of the instant patent application, and the disclosure of which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates generally to a new apparatus and method for in-situ processing of a product in an open atmosphere and then in-situ placing the product in a closed box in a second environment. More particularly, the invention encompasses an apparatus and a method that allows the binder to burn out of products, such as, substrates and then without taking the substrates out of the furnace to be able to sinter the substrates within the furnace in a closed atmosphere. The invention also generally relates to the fabrication of fired substrates and, more particularly, to the binder burn out and sintering of such substrates. Also disclosed is the in-situ application of weight on the product at the desired temperature due to the deformation or collapse of a sensitive spacer.
BACKGROUND OF THE INVENTION
Ceramic substrates are of particular importance in the microelectronics industry for the mounting, packaging and cooling of integrated devices. The fabrication of ceramic substrates is well known and is described, for example, in U.S. Pat. No. 5,130,067 issued to Philip L. Flaitz et al. on Jul. 14, 1992 and assigned to the present assignee. Burn-out and sintering comprise the final steps in the fabrication sequence. Burn-out drives off the volatile binder utilized in the ceramic slurry into a vented atmosphere. It is well known to be beneficial to apply weight to the ceramic substrate during sintering to minimize distortion due to shrinkage and cambering of the substrate.
Provision has been made in the prior art cited in the Flaitz et al patent, namely, U.S. Pat. No. 4,340,436 issued to Dubetsky et al on Jul. 20, 1982 and assigned to the present assignee, to accomplish burn out and sintering in a two step process. In the first step, the substrates are loaded into a furnace held at a temperature range and for a time sufficient to drive off the binder, cooled to room temperature, and then unloaded. The same substrates are placed into a configuration to maintain substrate flatness and then reloaded into a furnace and exposed to a higher temperature range and a longer time than were employed in the previous burn out cycle.
U.S. Pat. No. 5,130,067, cited above, teaches a process of applying an external load during sintering of a green ceramic substrate to constrain the substrate in the and Y directions and thereby control dimensional stability. The load is applied by weights that are either in place at the start of the heating cycle or remotely applied to the substrate by pneumatic, hydraulic or mechanical levers.
U.S. Pat. No. 4,259,061 issued to Derry J. Dubetsky on Mar. 31, 1981 and assigned to the present assignee describes the use of ceramic coated refractory plates used for setters onto which alumina substrates are placed to control shrinkage uniformly.
U.S. Pat. No. 5,364,608 issued to James P. Edler on Nov. 15, 1994 discloses a method to form sintered silicon nitride articles within a walled container which is vented to the furnace in which it is placed.
U.S. Pat. No. 5,376,601 issued to Yoshihiro Okawa on Dec. 27, 1994 cites the components used in the sintering of AlN components that resist deformation at high temperatures. When the sintered AlN product itself is used as setters and supports for a baking jig to hold other AlN products to be sintered, the patent states that the setters and supports of the jig are not deformed under the baking conditions and, hence, do not cause the molded articles to be deformed.
The following Japanese Patent Publications show the use of refractory boxes for sintering aluminum nitride substrates placed therein.
______________________________________Publication No. Publication Date Inventor______________________________________02-302088 December 14, 1990 Omote Koji et al.03-097682 April 23, 1991 U. Etsuro et al.04-198062 July 17, 1992 H. Michio et al.05-009076 January 19, 1993 T. Yutaka et al.05-105526 April 27, 1993 Akiyama Susumu______________________________________
This invention overcomes the above-mentioned problems and short-comings of the prior art, and provides a refractory box that remains open during a first temperature range, such as, during binder burn out, and automatically in-situ seals itself during a second temperature range, such as during the sintering cycle. It further provides a method to apply a weight onto a substrate at a predetermined temperature within the box.
PURPOSES AND SUMMARY OF THE INVENTION
The invention is a novel method and an apparatus for in-situ sealing to provide open atmosphere binder burn out and closed atmosphere sintering.
Therefore, one purpose of this invention is to provide an apparatus and a method that will provide a vented atmosphere binder burn out and sealed atmosphere sintering with a single furnace loading of components to be sintered.
Another purpose of this invention is to provide a refractory box for holding components to be sintered therein, said box permitting maximum binder removal rate at one time and automatically preventing rapid evaporation of transient liquid sintering aid at a later time in the sintering cycle.
Still another purpose of this invention is to provide a refractory box for holding components to be sintered therein, said box being vented during a first phase of the sintering cycle and being sealed automatically during a second phase of the sintering cycle.
Yet another purpose of this invention is to provide an automatic means located entirely within a refractory holding components to be sintered therein whereby weight is applied to said components only after a selected phase of the sintering cycle.
These and other purposes of the present invention are achieved in a best mode embodiment by the provision of a refractory box which is vented initially to the surrounding atmosphere of a sintering furnace. The box later seals itself from said atmosphere upon the attainment of a predetermined sintering temperature. Stacked setters within the box support the ceramic components to be sintered. The successive setters initially are spaced from each other by an amount greater than the thickness of said components. Said spacing is reduced at the aforesaid temperature so that the weight of an overlying setter thus is applied uniformly to the underlying ceramic components to help control camber and dimensional stability during sintering. Temperature sensitive collapsible spacers are used to change the venting and the weight pressure that is applied on top of the components.
Therefore, in one aspect this invention comprises a refractory box having at least one in-situ closeable cover comprising; a frame, a first cover and a second cover, wherein said first cover and said second cover sandwich said frame, and at least one control means connects at least a portion of said frame to at least a portion of at least one of said covers, and wherein said control means deforms at a predictable temperature in a thermal environment and thereby forms said refractory box having at least one in-situ closeable cover.
In another aspect this invention comprises a method for heating a product in a thermal environment with in-situ closeable cover comprising the steps of:
(a) placing said product in a box, wherein said box has a first cover a frame and a second cover,
(b) separating said first cover from said frame with at least one sensitive spacer,
(c) placing said box in said thermal environment, and wherein said sensitive spacer deforms at a predictable temperature and reduces the distance between said first cover and said frame.
BRIEF DESCRIPTION OF THE DRAWINGS
The features of the invention believed to be novel and the elements characteristic of the invention are set forth with particularity in the appended claims. The drawings are for illustration purposes only and are not drawn to scale. Furthermore, like numbers represent like features in the drawings. The invention itself, however, both as to organization and method of operation, may best be understood by reference to the detailed description which follows taken in conjunction with the accompanying drawings in which:
FIG. 1, illustrates a preferred embodiment of this invention, which is a simplified exploded view of the best mode embodiment of the refractory box and the contents thereof in accordance with the present invention.
FIG. 2, illustrates a cross-sectional view of the assembled refractory box of FIG. 1.
FIG. 3, illustrates a cross-sectional view after the refractory box of this invention has gone through binder burn out and is in the sintering cycle in a furnace.
FIG. 4, illustrates another preferred embodiment of this invention, which is a simplified cross-sectional view of an optional implementation of the refractory box of FIG. 1.
FIG. 5, illustrates another preferred embodiment of the invention where at least one collapsible spacer is on the bottom cover to hold the frame and at least one collapsible spacer is on the frame to hold the top cover, and a plurality of collapsible spacers hold a plurality of products inside the frame.
DETAILED DESCRIPTION OF THE INVENTION
In the sintering of metallized ceramic substrates, it has been found that ideally the substrate initially should be fully exposed to the furnace atmosphere during the binder burn-out (BBO) phase to allow maximum binder removal rates. Thereafter, it may be desired to apply weight onto the substrate to minimize distortion. In some applications which use a transient liquid phase sintering aid or where the substrate to be heated has components with high vapor pressure which are to be retained within the substrate, the substrate may need additional processing with the enclosed container. These desiderata are currently practiced as a two step process that extends the overall cycle time considerably, as well as requiring the loading and unloading of the furnace twice.
In accordance with the present invention, an in situ box sealing technique is provided which uses fusible or collapsible or deformable spacers that allow for the venting of BBO products but deform or collapse at higher temperatures to close a lid on the box to retain volatile species during the subsequent sintering cycle after binder burn-out has been completed.
AlN, for example, typically is sintered at high temperatures using volatile sintering aids to produce the highest thermal conductivity. Compositions have -been developed that sinter to high thermal conductivities at less than 1700° C. using various combinations of Al, B, Ca, F, Y, etc. These compositions all require processing using a binder which must be removed slowly during the BBO phase. This is accomplished in the above-mentioned two step process by first loading the substrates into a furnace for a BBO cycle exposed to furnace ambient at between about 1200 to about 1300° C. for a few hours, cooling to room temperature and then unloading the substrates. The same substrates are then reloaded in a stack sinter configuration to maintain flatness between the setter tiles, such as, Mo setter tiles, and sintered at about 1625° C. while sealed from the furnace ambient for more than 10 hours in a sealed refractory box. Without using the box the substrate only sinters to about 80 percent of theoretical density. With the sealed box about 98 to 99 percent of theoretical density can be obtained.
However, with this invention the BBO and sintering steps are combined into one furnace loading cycle using the inventive box configuration shown in FIG. 1, and wherein FIG. 2, illustrates a cross-sectional view of the assembled inventive box of FIG. 1. Products 25, such as, substrates 25, are placed on a first or lower setter tile 12. A second or upper setter tile 14, is then placed over the lower setter tile 12, and is raised sufficiently above the substrates 25, by fusible or deformable or collapsible or sensitive spacers 16, to allow for minimally impeded BBO gas evolution.
At the required time/temperature schedule, sensitive spacers 16, collapse to allow the upper setter tile 14, to drop onto underlying substrates 25. The dropping of the setter tile 14, onto the substrate 25, could be gradual or sudden depending upon the material characteristics of the sensitive spacer 16. The upper setter tile 14, can now be used to apply a uniform load on the substrate 25, such as, for example, to help in controlling the camber and dimensional stability of the underlying substrate 25.
A second set of fusible or deformable or collapsible or sensitive spacers 18, which could be made from material similar to the spacers 16, are provided to initially hold up the top cover 20, for sealable refractory box 7. Spacers 18, are preferably mounted in recesses 17, in frame 15. Base 10, is secured to frame 15, by methods well known in the art. Spacers 18, are tall enough to raise top cover 20, above the frame 15, during the BBO cycle so that the volatilized binder within the substrates 25, may vent into the furnace atmosphere. As earlier stated, however, spacers 18, collapse when the furnace temperature is raised to begin the sintering cycle to allow the top cover 20, to lower and seal itself to the frame 15, thereby retaining the volatile sintering aids within the sealable refractory box 7. It has been found that sealing of the box 7, is important for achieving high density and thermal conductivity. Cover 20, should be thick enough to remain flat during temperature processing and to provide a good seal to the box 7, after spacers 18, have collapsed.
FIG. 3, illustrates a cross-sectional view after the inventive box 7, of this invention has gone through binder burn out and is in the sintering cycle in a furnace. As can be clearly seen that the spacer 16, has either fused or collapsed or evaporated and has left behind residual material 26. The residual material 26, could be in a liquid state or could be in a shape of a shrunk slug. Similarly, the spacer 18, has also either fused or collapsed or evaporated and has left behind residual material 28, within the cavity 17. The residual material 28, could be in a liquid state or could be in a shape of a shrunk slug. As stated earlier that once the spacer 16, collapses the upper setter tile 14, drops and applies pressure onto the substrates 25. While, upon the collapse of the spacer 18, the cover 20, provides a good seal for the box 7, and prevents the volatile material inside the box 7, from escaping into the furnace.
An alternative embodiment of this invention is to use the spacer materials which may be allowed to melt into a liquid form in order to achieve very specific collapse temperatures is shown in FIG. 4. In this embodiment the inventive box 29, has a hollowed-out support pit or blind hole or cavity 17 and 27, made in the frame 15, and the first or lower setter tile 22, respectively. The spacers 16 and 18, are then mounted in the blind hole 27 and 17, respectively, so that the molten material from the spacers 16 and 18, respectively, is collected inside the cavities 27 and 17, respectively, and is not free to spill about in the furnace.
In order to ensure that the material from the spacer is contained within the inventive box of this invention a piston having a stop could be provided. One such piston 23, having a stop 24, is shown in FIG. 4, which forces the material from the collapsing spacer 18, to stay inside the cavity 17. A similar piston with a stop could also be provided for the spacer 16, so that the material from the collapsing spacer 16, could be forced to stay inside the cavity 27. Of course the piston 23, having the stop 24, could be integrated and made a part of the cover 20. Similarly, a piston having the stop could be integrated and made a part of the upper or second setter tile 14.
FIG. 5, illustrates another preferred embodiment of the invention where a refractory box 59, having sensitive or collapsible or deformable spacers 58, on the bottom cover 50, hold the frame 55, and sensitive spacers 18, on the frame 55, hold the top cover 20. Also, shown are a plurality of collapsible spacers 16, that hold a plurality of products 25, inside the frame 55. As can be clearly seen that once the sensitive spacers 16, collapse or deform the tile 14, comes to rest on top of the product 25, and applies weight pressure. One could also have a product 52, where a weight pressure is not desired or required and in that case it could be placed on top of the tile 14, or on top of the bottom cover 50, without the tiles 14.
It should be noted that the product 25 or 52, could be anything that needs to go through a controlled thermal environment. The range of the thermal environment could be below 0° C. to above 0° C.
Sensitive spacers 16, 18 and 58, are preferably made from ceramic, refractory metal, cermet material or other metal material. For a specific application, such as BBO, the spacers should be made from a material that can survive the BBO cycle, usually between about 1200 and about 1330° C., for about 4 hours, without any significant deformation during the heating process.
The spacers 16, 18 and 58, can also be made from the family of metals such as Mo and W which are stable in H 2 atmospheres or from ceramics such as Al 2 O 3 , ZrO 2 , and AlN which can be sintered in the range of between about 1400° C. to about 1600° C. range.
The spacers 16, 18 and 58, preferably can be fabricated from a pressed, cast or extruded mixture that can be processed to form a pellet or disc shape or any other shape. Care should be taken that the materials that are selected for the spacers 16, 18 and 58, are stable, so as not to melt and react with their underlying support or have high vapor pressure that can interact with the furnace, hardware or substrate.
The material of fusible spacers 16, 18 and 58, is preferably selected based upon its shrinkage after the BBO cycle has been completed. Such shrinkage can be varied by changing the particle size of the constituent powder (finer powders sinter earlier), adding sintering aids to accelerate shrinkage (Pt, Pd activate sintering of Mo and W at less than 1200° C.) or adding sintering inhibitors such as AlN, Al 2 O 3 . Once the amount of shrinkage is determined that occurs after BBO has been completed, the composition of the material for the spacers 16, 18 and 58, can be determined to provide the proper spacer height that will shrink enough after BBO to allow the upper setter tiles 14, to drop onto the substrates 25, or to close the box lid 20, as the case may be. The spacers 16, 18 and 58, can be pre- or partially sintered to provide strength, if needed. A pressing operation appears to be the most cost efficient manufacturing method to manufacture the deformable or collapsible spacers 16, 18 and 58.
An example of shrinkage values for pressed pellets made of different starting material powder sizes is shown in Table 1. These tungsten powders were pressed into 1/2 inch cylinders and heated in a furnace in 10 percent hydrogen in nitrogen atmosphere at 4° C./min up to the indicated temperature and hold time.
TABLE 1______________________________________ Height Shrinkage AfterPowder Type 1300° C./4 hr 1300° C./4 hr-1625° C./24______________________________________ hrWA25 3.0 percent 16.0 percentWA10 8.0 percent 22.6 percentHC40 16.4 Percent 26.3 percent______________________________________
As can be clearly seen in Table 1, at least a 10 percent change in height can be obtained between the low and high temperature holds, providing an indication of the amount of the shrinkage available to allow a setter plate or cover to be lowered onto a substrate or box to provide flattening or sealing, respectively.
The rate of collapse of the sensitive spacer is gradual and is primarily controlled by the composition of the spacer material. Other factors that can also have a direct impact on the rate of collapse or sensitivity of the spacer is its processing history, such as, for example, the ambient atmosphere that it was prepared in, supported load and the heating rate to which the spacer was subjected during its manufacturing, etc.
Examples of spacer materials with a very specific collapse temperature would be those made from high purity elements or eutectic metals, including low temperature solders. Table 2, for example, provides data for low to medium temperature metals that could be used for very specific collapse temperatures.
TABLE 2______________________________________Collapse Temperature Spacer Composition(° C.) (percent)______________________________________-32 1,2 Dichloroethane30 Phenyl Ether100 46 Bi, 34 Sn, 20 Pb145 51.2 Sn, 30.6 Pb, 18.2 Cd199 91 Sn, 9 Zr525 45 Ag, 38 Au, 17 Ge780 72 Ag, 28 Cu1,063 100 Au.______________________________________
The sensitive spacers could also be made from materials which respond to changes in atmosphere to affect a change in the shape of the spacer. For example, a reducible metal oxide powder could be prepared as a spacer which will tolerate an oxidizing or neutral atmosphere without significant collapse or change in shape. However, at the desired time in the process, for instance, after BBO in an oxidizing atmosphere, the ambient could be changed to reduce the metal oxide and cause the spacer to collapse or melt. This deformation of the sensitive spacer from one atmosphere to another could be used to actuate the motion of the cover closing onto the frame or the application of applying weight/pressure onto a product. Copper oxide, for example, undergoes about 40 volume percent reduction during reduction to a metal. Therefore, the spacers used in this invention could be selected from a group comprising of materials that are sensitive to the change in ambient oxygen partial pressure.
Another application which could utilize this invention would be the use of a self actuating sealing process, such as, the process of contamination sensitive devices in controlled ambients as well as the containment of hazardous materials.
While the present invention has been particularly described, in conjunction with a specific preferred embodiment, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. It is therefore contemplated that the appended claims will embrace any such alternatives, modifications and variations as falling within the true scope and spirit of the present invention.
|
A single furnace loading cycle method for sintering at least one product comprises placing at least one product into a ventable/sealable box, and placing the box within the furnace. The box is vented inside the furnace at a first temperature range and the product is sealed inside the box in a second temperature range, wherein the second temperature range is higher than the first temperature range. The box includes a closeable top cover and a control means that comprises a first set of collapsible spacers which hold open the cover at temperatures below the first temperature range and collapse to lower the cover into sealing engagement with the box at temperatures above the first temperature range. The box further comprises a substrate to be sintered with a lower and an upper setter on opposite sides of the substrate. The substrate rests on the lower setter, and a second set of collapsible spacers rest on the lower setter and have heights sufficient to lift the upper setter above the height of the substrate, and wherein the second set of spacers collapse to lower the upper setter to rest upon the substrate at temperatures above the first temperature range.
| 5
|
BACKGROUND TO THE INVENTION
The present invention relates to coated abrasives and particularly to abrasive products adapted to perform in an improved fashion when used under moderate to low pressure grinding conditions.
In the production of coated abrasives a backing material, which may be treated to modify the absorptive properties, is provided with a make coat comprising a curable binder resin and abrasive grains are deposited on the make coat before the binder is at least partially cured. Thereafter a size coat comprising a curable binder resin is deposited over the abrasive grain to ensure the grains are securely anchored to the backing.
When the coated abrasive is used to abrade a workpiece, the tips of the abrasive grains lying in the plane of the surface contact the workpiece and begin the work of abrasion. The grains thus contacting the workpiece are subjected to great stresses and, if the grain is not adequately held by the size coat it can be plucked from the surface before it has completed abrading. The bond therefore should hold the grain securely. As abrading continues the grain can become polished, in which case significant frictional heat is generated and little removal of the workpiece occurs. In addition the stresses build up further and eventually the grain is either plucked out completely of it fractures so that a large portion is lost. This however generates new sharp edges such that abrading can resume. Ideally the mode of fracture should be as small as possible such that each grain will last a long time. This is achieved using sol-gel alumina abrasive grains which each comprises micron-sized or smaller crystallites which, under grinding conditions, can break off to reveal new cutting edges. However this occurs under moderate to heavy grinding pressure and only a reduced amount of self-sharpening occurs at lower pressure grinding conditions. There is therefore a need for a highly effective abrasive particle that operates very efficiently at moderate to low pressure grinding conditions.
One option that has been explored is the use of agglomerated abrasive grains in which an abrasive particle made up of a number of finer abrasive particles is held together by a bond material that can be organic or vitreous in nature. Because the bond is in general more friable than the abrasive particles, the bond fractures under grinding conditions that would otherwise lead to polishing or wholesale fracture of the abrasive grain.
Agglomerated abrasive grain generally permit the use of smaller particle (grit) sizes to achieve the same grinding efficiency as a larger abrasive grit size. Agglomerated abrasive grains have also been reported to improve grinding efficiency.
U.S. Pat. No. 2,194,472 to Jackson discloses coated abrasive tools made with agglomerates of a plurality of relatively fine abrasive grain and any of the bonds normally used in coated or bonded abrasive tools. Organic bonds are used to adhere the agglomerates to the backing of the coated abrasives. The agglomerates lend an open-coat face to coated abrasives made with relatively fine grain. The coated abrasives made with the agglomerates in place of individual abrasive grains are characterized as being relatively fast cutting, long-lived and suitable for preparing a fine surface finish quality in the work-piece.
U.S. Pat. No. 2,216,728 to Benner discloses abrasive grain/bond agglomerates made from any type of bond. The object of the agglomerates is to achieve very dense wheel structures for retaining diamond or CBN grain during grinding operations. If the agglomerates are made with a porous structure, then it is for the purpose of allowing the inter-agglomerate bond materials to flow into the pores of the agglomerates and fully densify the structure during firing. The agglomerates allow the use of abrasive grain fines otherwise lost in production.
U.S. Pat. No. 3,048,482 to Hurst discloses shaped abrasive micro-segments of agglomerated abrasive grains and organic bond materials in the form of pyramids or other tapered shapes. The shaped abrasive micro-segments are adhered to a fibrous backing and used to make coated abrasives and to line the surface of thin grinding wheels. The invention is characterized as yielding a longer cutting life, controlled flexibility of the tool, high strength and speed safety, resilient action and highly efficient cutting action relative to tools made without agglomerated abrasive grain micro-segments.
U.S. Pat. No. 3,982,359 to Elbel teaches the formation of resin bond and abrasive grain agglomerates having a hardness greater than that of the resin bond used to bond the agglomerates within an abrasive tool. Faster grinding rates and longer tool life are achieved in rubber bonded wheels containing the agglomerates.
U.S. Pat. No. 4,355,489 to Heyer discloses an abrasive article (wheel, disc, belt, sheet, block and the like) made of a matrix of undulated filaments bonded together at points of manual contact and abrasive agglomerates, having a void volume of about 70-97%. The agglomerates may be made with vitrified or resin bonds and any abrasive grain.
U.S. Pat. No. 4,364,746 to Bitzer discloses abrasive tools comprising different abrasive agglomerates having different strengths. The agglomerates are made from abrasive grain and resin binders, and may contain other materials, such as chopped fibers, for added strength or hardness.
U.S. Pat. No. 4,393,021 to Eisenberg, et al, discloses a method for making abrasive agglomerates from abrasive grain and a resin binder utilizing a sieve web and rolling a paste of the grain and binder through the web to make worm-like extrusions. The extrusions are hardened by heating and then crushed to form agglomerates.
U.S. Pat. No. 4,799,939 to Bloecher teaches erodable agglomerates of abrasive grain, hollow bodies and organic binder and the use of these agglomerates in coated abrasives and bonded abrasives. Higher stock removal, extended life and utility in wet grinding conditions are claimed for abrasive articles comprising the agglomerates. The agglomerates are preferably 150-3,000 microns in largest dimension. To make the agglomerates, the hollow bodies, grain, binder and water are mixed as a slurry, the slurry is solidified by heat or radiation to remove the water, and the solid mixture is crushed in a jaw or roll crusher and screened.
U.S. Pat. No. 5,129,189 to Wetscher discloses abrasive tools having a resin bond matrix containing conglomerates of abrasive grain and resin and filler material, such as cryolite.
U.S. Pat. No. 5,651,729 to Benguerel teaches a grinding wheel having a core and an abrasive rim made from a resin bond and crushed agglomerates of diamond or CBN abrasive grain with a metal or ceramic bond. The stated benefits of the wheels made with the agglomerates include high chip clearance spaces, high wear resistance, self-sharpening characteristics, high mechanical resistance of the wheel and the ability to directly bond the abrasive rim to the core of the wheel. In one embodiment, used diamond or CBN bonded grinding rims are crushed to a size of 0.2 to 3 mm to form the agglomerates.
U.S. Pat. No. 4,311,489 to Kressner discloses agglomerates of fine (≦200 micron) abrasive grain and cryolite, optionally with a silicate binder, and their use in making coated abrasive tools.
U.S. Pat. No. 4,541,842 to Rostoker discloses coated abrasives and abrasive wheels made with agglomerates of abrasive grain and a foam made from a mixture of vitrified bond materials with other raw materials, such as carbon black or carbonates, suitable for foaming during firing of the agglomerates. The agglomerate “pellets” contain a larger percentage of bond than grain on a volume percentage basis. Pellets used to make abrasive wheels are sintered at 900° C. (to a density of 70 lbs/cu. ft.; 1.134 g/cc) and the vitrified bond used to make the wheel is fired at 880° C. Wheels made with 16 volume % pellets performed in grinding with an efficiency similar to that of comparative wheels made with 46 volume % abrasive grain. The pellets contain open cells within the vitrified bond matrix, with the relative smaller abrasive grains clustered around the perimeter of the open cells. A rotary kiln is mentioned for firing the green foam agglomerates.
U.S. Pat. No. 5,975,988 teaches conventional abrasive agglomerates comprising abrasive particles dispersed in a binder matrix but in the form of shaped grains deposited in a precise order on a backing and bonded thereto.
U.S. Pat. No. 6,319,108 describes a rigid backing with, adhered thereto by a metal coating, a plurality of abrasive composites comprising a plurality of abrasive particles dispersed throughout a porous ceramic matrix.
None of these prior art developments suggest the manufacture of coated abrasives using porous agglomerated abrasive grain as the term is used herein and a bond. Neither do they suggest the production of a product with abrasive particles held together by a relatively small amount of bond such that the particle binder phase is discontinuous. The methods and tools of the invention yield new structures and benefits from the use of such agglomerated abrasive grains, yet they are sophisticated in permitting the controlled design and manufacture of broad ranges of abrasive article structures having beneficial interconnected porosity characteristics. Such interconnected porosity enhances abrasive tool performance in large contact area, precision grinding operations, and in general relatively medium to low pressure grinding applications.
SUMMARY OF THE INVENTION
The present invention provides a coated abrasive article comprising a backing material and adhered thereto by a binder material, abrasive agglomerate grains characterized in that the grains used in the production of the coated abrasive comprise a plurality of abrasive particles adhered together in a three dimensional structure in which each particle is joined to at least one adjacent particle by a particle binder material which is present in the agglomerate as a discontinuous phase within the agglomerate grain and is located essentially completely in the form of bond posts linking adjacent particles, such that the agglomerate has a loose pack volume that is at least 2% lower than that of the abrasive particles in the individual state.
In this application the term “grains” will be reserved for agglomerates of a plurality of abrasive “particles”. Thus the grains will have the above identified porosity characteristics whereas the particles will have essentially zero porosity. Further the binder holding the particles together is identified as a “particle binder” which may be the same, (or more often different from), the binder by which the grains are attached to the backing material.
The particle binder in the agglomerate grains is located essentially completely in the form of bond posts and this means that at least 70% of the binder, and preferably in excess of 80%, is used to form bond posts linking adjacent particles. A bond post is formed under agglomerate forming conditions when the particle binder is in a fluid condition and tends first to coat the particles and then to flow to points of contact or closest approach of adjacent particles and to merge with the binder associated with such adjacent particles. When the temperature is lowered and the binder solidifies the binder forms a solid contact between the particles that is known as a “bond post”. Naturally each bond post is also attached to the surface of the particles it connects but this binder is considered part of the bond post for the sake of this description. This does not exclude the possibility that some relatively small amount is present as a coating on at least part of the particle surface not associated with a bond post. It is intended however to exclude the situation in which the particles are embedded in a matrix of binder as occurs in conventional aggregate abrasive grains. As is apparent from examination of FIGS. 5-7 of the Drawings the individual abrasive particles making up the agglomerate grain are individually identifiable and indeed are essentially all that can be seen in typical agglomerate grains according to the invention. It is therefore possible to describe the particles as being “agglomerated” implying being linked together rather than being held in a matrix which fills the larger portion of the space between the particles. Naturally when larger numbers of particles are agglomerated some individuals within the agglomerate will not be individually visible, but if it were possible to take a cross-section, the same pattern of individual particle visibility would be evident.
Clearly when the number of particles agglomerated becomes large, there will necessarily be substantial volumes of porosity created by this agglomeration. This can be as much as 70% of the total apparent volume of the agglomerate. However when the numbers of particles agglomerated are small, perhaps in the single figures, the concept of “porosity” becomes less useful in describing the agglomerates. Examples of such agglomerates showing the kind of structures involved are illustrated in FIGS. 5-7.
For this reason the term “loose pack volume” (LPV) is adopted. The LPV value is obtained by dividing the solid volume, (that is the total actual volume of the solids in the abrasive grain or particle, including the bond component) by the apparent volume of the agglomerate grain. The highest possible figure will be obtained from the particles themselves without any agglomeration having taken place. The larger the number of particles agglomerated, the greater the divergence from the maximum figure. Thus while the difference can be as low as 2% it can rise to 40% or even higher when larger numbers of particles are agglomerated together in the manner taught herein.
The calculation of the LPV is exemplified using the following data which represent actual agglomerate made using 60 grit particles of a seeded sol-gel alumina as the abrasive particles and a conventional vitreous bond suitable for use with such particles using a process substantially as described in Example 2 below.
The products are identified by the agglomerate grain size shown at the head of each column. In each case the measurements were made of the basis of a fixed volume of the agglomerate abrasive grains, referred to here as the “Apparent Volume”.
Particles 60
grit
−40 +45
−30 +35
−25 +30
−20 +25
Weight
25.1
23.1
19.73
18.3
16
Density (of solid)*
3.9
3.759
3.759
3.759
3.759
Vol. of grit + bond
6.436
6.145
5.249
4.868
4.256
Apparent Volume
12.797
12.797
12.797
12.797
12.797
LPV
0.503
0.480
0.410
0.380
0.333
*Density estimated according to the rule of mixtures.
As will be appreciated from the above, the larger the agglomerate grain, the smaller the LPV by comparison with that of the unagglomerated particles. The smallest grains showed a 4.6% drop in LPV whereas the largest (−20+25) showed a drop of nearly 34% by comparison with the LPV of the 60 grit particles.
The agglomerate grains generally have a diameter, (defined as the size of the aperture in a sieve (of series of standard sieves) with the coarsest mesh on which the grains are retained), that is at least two times the diameter of the individual abrasive particles contained therein. The shape of the agglomerate abrasive grains is not critical and they can therefore be random somewhat blocky shapes or, more preferably, somewhat elongated shapes. They can also have an imposed shape this is often advantageous for some applications.
The abrasive particles present in the agglomerates of the invention may include one or more of the abrasives known for use in abrasive tools, such as aluminas, including fused alumina, sintered and sol gel sintered alumina, sintered bauxite, and the like, silicon carbide, alumina-zirconia, garnet, flint, diamond, including natural and synthetic diamond, cubic boron nitride (CBN), and combinations thereof. Any size or shape of abrasive particle may be used. For example, the grain may include elongated sintered sol gel alumina particles having a high aspect ratio of the type disclosed in U.S. Pat. No. 5,129,919 or the filamentary shaped abrasive particles described in U.S. Pat. No. 5,009,676.
The abrasive particles can comprise blends of abrasives of different qualities since often the performance of a premium quality particles is only marginally diminished by dilution with minor amounts of inferior particles. It is also possible to blend the abrasive particles with minor amounts of non-abrasive materials such as grinding aids, pore formers and filler materials of conventional sorts.
Particle sizes suitable for use herein range from regular abrasive grits (e.g., 60 to 7,000 micrometers) to microabrasive grits (e.g., 2 to 60 micrometers), and mixtures of these sizes. For any given abrasive grinding operation, it is generally preferred to use an agglomerate grain with a grit size smaller than a conventional abrasive grain (non-agglomerated) grit size normally selected for this abrasive grinding operation. For example, when using agglomerate grains, 80 grit size is substituted for 54 grit conventional abrasive, 100 grit for 60 grit abrasive and 120 grit for 80 grit abrasive and so on.
The abrasive particles within the agglomerate are bonded together by a metallic, organic or vitreous bond material and these are referred to generically as “particle binders”.
Particle binders useful in making the agglomerates include vitreous materials, (defined herein to include both conventional glass materials as well as glass-ceramic materials), preferably of the sort used as bond systems for vitrified bonded abrasive tools. These may be a pre-fired glass ground into a powder (a frit), or a mixture of various raw materials such as clay, feldspar, lime, borax, and soda, or a combination of fritted and raw materials. Such materials fuse and form a liquid glass phase at temperatures ranging from about 500 to 1400° C. and wet the surface of the abrasive particles and flow to points of closest contact between adjacent particles to create bond posts upon cooling, thus holding the abrasive particles within a composite structure. The particle binder is used in powdered form and may be added to a liquid vehicle to insure a uniform, homogeneous mixture of coating with abrasive particles during manufacture of the agglomerate grains.
Temporary organic binders are preferably added to powdered inorganic coating components, whether fritted or raw, as molding or processing aids. These binders may include dextrins, starch, animal protein glue, and other types of glue; a liquid component, such as water or ethylene glycol, viscosity or pH modifiers; and mixing aids. Use of such temporary binders improves agglomerate uniformity and the structural quality of the pre-fired or green agglomerates. Because the organic binders burn off during firing of the agglomerate grains, they do not become part of the finished grain.
An inorganic adhesion promoter, such as phosphoric acid, may be added to the mixture to improve adhesion of the particle binder to the abrasive particles as needed. The addition of phosphoric acid to alumina grains greatly improves the mix quality when the particle binder comprises a fritted glass. The inorganic adhesion promoter may be used with or without an organic particle binder in preparing the agglomerate grains.
The preferred particle binder is an inorganic material such as a vitreous bond material. This has a distinct advantage over organic particle binders because it permits the agglomerate grains to be deposited on a substrate in the formation of a coated abrasive using a UP technique. The UP deposition technique is also very suited to use when the particles are bonded together using a metallic binder. Since this process is somewhat more effective and controllable than a gravity deposition technique this represents a significant advance over conventional aggregate grains made using an organic resin binder matrix.
The particle binder can also be an organic binder such as a thermosetting resin such as a phenolic resin, an epoxy resin, a urea/formaldehyde resin, or a radiation-curable resin such as an acrylate, a urethane/acrylate, an epoxy-acrylate, a polyester-acrylate and the like. In general thermosetting resins are preferred as organic binders.
The particle binder is present at about 2 to 25 volume %, more preferably 3 to 15 volume %, and most preferably 3 to 10 volume % based on the combined volume of the particles and binder.
It is also foreseen that the particle binder component can be eliminated altogether if the abrasive particles are caused to sinter together in a controlled fashion such that, by material transport between contacting particles, the bond-posts would be autogenously generated. Alternatively where the abrasive particles are alumina, these could be mixed with a sol of relatively small amount of an alpha alumina precursor such as boehmite. Upon firing this would convert to the alpha phase and would serve the same function as bond posts by connecting adjacent particles.
The invention includes coated abrasives incorporating agglomerated abrasive grain wherein the grains are made by a process which comprises the steps of:
a) feeding abrasive particles and a particle binder material, selected from the group consisting essentially of vitrified bond materials, vitrified materials, ceramic materials, inorganic binders, organic binders, water, solvent and combinations thereof, into a rotary calcination kiln at a controlled feed rate;
b) rotating the kiln at a controlled speed;
c) heating the mixture at a heating rate determined by the feed rate and the speed of the kiln to temperatures from about 145 to 1,300° C.,
d) tumbling the particles and the particle binder in the kiln until the binder adheres to the particles and a plurality of the particles adhere together to create sintered agglomerate grains; and
e) recovering the sintered agglomerates from the kiln,
whereby the sintered agglomerate grains have an initial three-dimensional shape, a loose packing volume that is at least 2% below the corresponding loose pack volume of the constituent particles and comprise a plurality of abrasive particles.
The invention also includes coated abrasives incorporating sintered abrasive agglomerate grains that have been made by a method comprising the steps:
a) feeding abrasive particles along with a particle binder material into a rotary calcination kiln at a controlled feed rate;
b) rotating the kiln at a controlled speed;
c) heating the mixture at a heating rate determined by the feed rate and the speed of the kiln to temperatures from about 145 to 1,300° C.,
d) tumbling the abrasive particles and the particle binder in the kiln until the binder adheres to the grain and a plurality of grains adhere together to create sintered abrasive agglomerate grains; and
e) recovering the sintered agglomerate grains from the kiln,
whereby the sintered agglomerate grains have an initial three-dimensional shape, comprise a plurality of particles and have a loose packing volume that is at least 2% below the corresponding loose pack volume of the constituent particles.
DESCRIPTION OF DRAWINGS
FIG. 1 is a rotary calcination apparatus that may be used to produce agglomerates according to the invention.
FIG. 2 is a graph showing amount of metal cut in the evaluations of four abrasive discs carried out according to Example 1.
FIG. 3 is a graph showing amount of metal cut in the evaluations of four abrasive discs carried out according to Example 2.
FIG. 4 is a graph showing amount of metal cut in the evaluations of four abrasive discs carried out according to Example 3.
FIGS. 5-7 are enlarged photographs of agglomerates used to produce coated abrasives according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
In this section the nature and production of the abrasive agglomerate grains and the coated abrasives made with such grains are explored and illustrated with the assistance of several Examples illustrating the surprisingly improved properties that are obtained by the use of the abrasive agglomerate grains as components of coated abrasives.
Manufacture of Abrasive Agglomerates
The agglomerate grains may be formed by a variety of techniques into numerous sizes and shapes. These techniques may be carried out before or after firing the initial (“green”) stage mixture of grain and particle binder. The step of heating the mixture to cause the particle binder to melt and flow, thus adhering the binder to the grain and fixing the grain in an agglomerated form is referred to as firing, calcining or sintering. Any method known in the art for agglomerating mixtures of particles may be used to prepare the abrasive agglomerate grains.
In a first embodiment of the process used herein to make agglomerate grains, the initial mixture of particles and particle binder is agglomerated before firing the mixture so as to create a relatively weak mechanical structure referred to as a “green agglomerate” or “pre-fired agglomerate.”
To carry out a first embodiment, the abrasive particles and an inorganic particle binder are agglomerated in the green state by any one of a number of different techniques, e.g., in a pan pelletizer, and then fed into a rotary calcination apparatus for sintering. The green agglomerates can also be placed onto a tray or rack and oven fired, without tumbling, in a continuous or batch process.
In an another process the abrasive particles are conveyed into a fluidized bed, then wetted with a liquid containing the particle binder to adhere the binder to the surface of the particles, screened for agglomerate size, and then fired in an oven or calcination apparatus.
Pan pelletizing is often carried out by adding particles to a mixer bowl, and metering a liquid component (e.g., water, or organic binder and water) containing the particle binder onto the grain, with mixing, to agglomerate them together. Alternatively a liquid dispersion of the particle binder, optionally with an organic binder, is sprayed onto the particles, and then the coated particles are mixed to form agglomerates.
A low-pressure extrusion apparatus may be used to extrude a paste of particles and particle binder into sizes and shapes which are dried to form agglomerate grains. A paste may be made of the particle binder and the particles optionally with an organic temporary binder and extruded into elongated particles with the apparatus and method disclosed in U.S. Pat. No. 4,393,021.
In a dry granulation process, a sheet or block made of abrasive particles imbedded in dispersion or paste of the particle binder is dried and then broken up using a roll compactor to form precursors of the agglomerate grains.
In another method of making green or precursor agglomerate grains, the mixture of the particle binder and the particles are added to a molding device and the mixture molded to form precise shapes and sizes, for example, in the manner disclosed in U.S. Pat. No. 6,217,413.
In another embodiment of the process useful herein for making agglomerate grains, a mixture of the abrasive particles, particle binder and a temporary organic binder system is fed into an oven, without pre-agglomeration and heated. The mixture is heated to a temperature high enough to cause the particle binder to melt, flow and adhere to the particles, after which the mixture is cooled to make a composite. The composite is crushed and screened to make the sintered agglomerate grains.
It is further possible to sinter the agglomerates while the particles and the binder are contained in a shaped cavity such that the agglomerates as produced have a specific shape such as a square-based pyramid. The shapes need not be exact and indeed because the amount of particle binder is relatively small, the sides of the shapes will often be relatively rough. However such agglomerated grains can be extremely useful in producing coated abrasives with the ability to produce a very uniform surface in a very aggressive abrading operation.
Preferred Manufacture of Abrasive Agglomerates
In a preferred process for making agglomerates, a simple mixture of the particles and an inorganic particle binder (optionally with an organic temporary binder) is fed into a rotary calcination apparatus of the type shown in FIG. 1 . The mixture is tumbled at a predetermined rpm, along a predetermined incline with the application of heat. Agglomerate grains are formed as the particle binder heats, melts, flows and adheres to the particles. The firing and agglomeration steps are carried out simultaneously at controlled rates and volumes of feeding and heat application. The feed rate generally is set to yield a flow occupying roughly 8-12%, by volume, of the tube of the rotary calcination apparatus. The maximum temperature exposure within the apparatus is selected to keep the viscosity of the particle binder materials in a liquid state at a viscosity of at least about 1,000 poise. This avoids excessive flow of the particle binder onto the surface of the tube and a resulting loss from the surface of the abrasive particles.
A rotary calcination apparatus of the type illustrated in FIG. 1 may be used to carry out the agglomeration process for agglomerating and firing the agglomerates in a single process step. As shown in FIG. 1, a feed hopper ( 10 ) containing the feedstock ( 11 ) mixture of particle binder and abrasive particles is fed into a means ( 12 ) for metering the mixture into a hollow heating tube ( 13 ). The tube ( 13 ) is positioned at an incline angle ( 14 ) of approximately 0.5-5.0 degrees such that the feedstock ( 1 ) can be gravity fed through the hollow tube ( 13 ). Simultaneously, the hollow tube ( 13 ) is rotated in the direction of the arrow (a) at a controlled rate to tumble the feedstock ( 11 ) and the heated mix ( 18 ) as they pass along the length of the hollow tube.
A portion of the hollow tube ( 13 ) is heated. In one embodiment, the heating portion may comprise three heating zones ( 15 , 16 , 17 ) having a length dimension (d 1 ) of 60 inches (152 mm) along the length (d 2 ) of 120 inches (305 mm) of the hollow tube ( 13 ). The heating zones permit the operator to control the processing temperature and to vary it as needed to sinter the agglomerate grains. In other models of the apparatus, the hollow tube may only comprise one or two heating zones, or it may comprise more than three heating zones. Although not illustrated in FIG. 1, the apparatus is equipped with a heating device and mechanical, electronic and temperature control and sensing devices operative for carrying out the thermal process. As can be seen in the cross-sectional view of the hollow tube ( 13 ), the feedstock ( 11 ) is transformed to a heated mix ( 18 ) within the tube and it exits the tube and is collected as agglomerate granules ( 19 ). The wall of the hollow tube has an inner diameter dimension (d 3 ) which may range from 5.5 to 30 inches (14-76 mm) and a diameter (d 4 ) which may range from 6 to 36 inches (15-91 mm), depending upon the model and the type of material used to construct the hollow tube (e.g., refractory metal alloy, stainless steel, refractory brick, silicon carbide, mullite). The material selected for the construction of the tube depends largely on the temperatures reached. Temperatures up to 1000° C. can usually be accommodated by a stainless steel tube but over this temperature a silicon carbide tube is often preferred.
The incline angle of the tube may range from 0.5 to 5.0 degrees and the rotation of the tube may operate at 0.5 to 10 rpm. The feed rate for a small scale rotary calciner may range from about 5 to 10 kg/hour, and an industrial production scale feed rate may range from about 227 to 910 kg/hour. The rotary calciner may be heated to a sintering temperature of 800 to 1400° C., and the feed material may be heated at a rate of up to 200° C./minute as the feedstock enters the heated zone. Cooling occurs in the last portion of the tube as the feedstock moves from a heated zone to an unheated zone. The product is cooled, e.g., with a water cooling system, to room temperature and collected.
Suitable rotary calcination machines may be obtained from Harper International, Buffalo, N.Y., or from Alstom Power, Inc., Applied Test Systems, Inc., and other equipment manufacturers. The apparatus optionally may be fitted with electronic, in-process control and detection devices, a cooling system, various designs of feed apparatus and other optional devices.
Manufacture of Coated Abrasives
The coated abrasive according to the invention can have the form of an abrasive belt, sheet, individual abrasive disc or a composite abrasive in any structure or format. Thus the substrate to which the abrasive agglomerate grains are adhered can be a film, paper, textile, fiber (both in the non-woven web form or as a lofty fibrous structure) or even a foam material. The term “coated abrasive” as used herein therefore embraces both conventional abrasive products such as belts and discs using a planar substrate made of conventional materials and in addition products in which the abrasive agglomerates of the invention are adhered to a lofty fibrous structure of the type often called “composite abrasives” and those in which they are dispersed in and adhered within the surface layers of an open-celled foam structure.
The coated abrasive of the invention can be formed in any of the conventional techniques know in the prior art. These include application over a make coat deposited on a substrate followed by deposition of a size coat, as well the deposition of the abrasive agglomerate grains dispersed within a suitable curable binder on a substrate. The curable binder can be cured as applied or the surface can be treated by known techniques to impose a surface structure thereon.
Likewise coated abrasives in which the abrasive agglomerate grains are deposited on lofty fibrous structures or in at least the surface layers of a polymer foam can be obtained using processes know in the art.
A coated abrasive can be formed by deposition of the abrasive agglomerate grains on to a substrate that has been coated with a maker coat in the conventional way. In this event the deposition can be by gravity feed or by a UP process. When a vitreous particle binder is used to form the agglomerates, it becomes possible to use the UP deposition technique which is generally preferred for coated abrasives. This technique is less well adapted for depositing agglomerates made using an organic resin as the particle binder since such grains do not project well under the influence of an electrostatic field.
The abrasive agglomerate grain can be deposited alone or in admixture with other conventional abrasive grains. The level of application can provide for a closed coat, (100% coverage of the surface area of the substrate to which the grains are applied), or a more open coat wherein the grains are separated to some degree depending on the degree of “openness”. In some case it is desirable to apply the abrasive agglomerate grains over a previously deposited layer of another abrasive, perhaps one of lesser quality, to provide better support for the abrasive agglomerate grains.
Where the coated abrasive is formed in the conventional way using make and size coats to anchor the agglomerate grains, it is often preferred that the application of the size coat does not have the effect of significantly reducing the porosity of the abrasive agglomerate grains. The size coat is typically a relatively fluid curable resin formulation and if this is applied under some pressure, for example by a roll application technique, the curable formulation can be forced into the pores of the grain thereby reducing an important property of the abrasive agglomerate grains. It is therefore preferred that the size coat be applied using a non-contact technique such as spray application. In addition or alternatively, it is often desirable to modify the size coat resin properties to increase the viscosity, perhaps by the addition of fillers such as silica, to minimize the tendency of the resin to penetrate the grain structure. Preferably the viscosity in adjusted to a value of at least 1000 centipoise and more preferably to at least 1500 centipoise or higher. Where the binder is used as a matrix to hold the agglomerate grain and simultaneously attach it to the backing a similar viscosity adjustment is preferred.
In the manufacture of a coated abrasive using a maker coat, the grains do not become immersed in the maker coat which is in any case usually partially cured and therefore not very fluid when it receives the abrasive agglomerates. However the size coat is usually applied over the agglomerate grain and therefore has significantly greater opportunities for penetration of the structure of the agglomerate. While an a excessive loss of the openness of an agglomerate structure comprising many particles may be undesirable, a limited amount of penetration of the structure of the agglomerate need not necessarily be a bad thing since the effect is to increase the surface area of the grain in contact with the size coat and thereby strengthen the grip on the grain exerted by the size coat.
The coated abrasive can also be formed by application of a slurry comprising the abrasive agglomerate grains, dispersed in a curable binder formulation, to a suitable backing material. In this case also the binder can be treated to reduce penetration of the structure of the abrasive agglomerate grains by the binder resin. Application of the slurry can be accomplished in two or more operations, optionally using different formulations in the successive depositions. This allows a certain flexibility to vary the nature of the abrasive action as the coated abrasive wears.
Coated abrasive belts according to the invention may need to be flexed before use as is usual with belts made using a binder resin that sets to an inflexible layer. In addition it is often desirable to dress the grinding surface before use to ensure uniform high cut rates from the start.
Lofty fibrous structures according to the invention can be made for example by treating a lofty mat of fibers with a binder material, frequently using a spray technique, and then depositing the abrasive agglomerate grains thereon before curing the binder resin. The products according to the invention in this form have particular utility for polishing and finishing of metal surfaces.
EXAMPLES
The Invention is now illustrated using the following Examples which are intended to show the surprisingly advantageous properties of the products according to the invention.
Manufacture of Vitreous Bonded Abrasive Agglomerate Grains
The agglomerate grains evaluated in the following Examples were made by a process corresponding to the “Preferred Manufacture of Abrasive Agglomerates” described above and using the equipment illustrated in FIG. 1 .
The first six Examples illustrate the production of the abrasive agglomerates used in the invention. The agglomerate grains made in this fashion were incorporated into coated abrasives to evaluate their performance by comparison with conventional high quality commercial abrasive grains. The results are documented in the Examples 7-9 which are provided by way of illustration of the invention, and not by way of limitation.
Example 1
A series of agglomerated abrasive grain samples were prepared in a rotary calcination apparatus (electric fired model # HOU-5D34-RT-28, 1,200° C. maximum temperature, 30 KW input, equipped with a 72″ (183 cm) long, 5.5″ (14 cm) inner diameter refractory metal tube, manufactured by Harper International, Buffalo, N.Y.). The refractory metal tube was replaced with a silicon carbide tube of the same dimensions, and the apparatus was modified to operate at a maximum temperature of 1,550° C. The process of agglomeration was carried out under atmospheric conditions, at a hot zone temperature control set point of 1,180° C., with an apparatus tube rotation rate of 9 rpm, a tube incline angle of 2.5 to 3 degrees, and a material feed rate of 6-10 kg/hour. The apparatus used was substantially identical to the apparatus illustrated in FIG. 1 . The yield of usable free-flowing granules (defined as −12 mesh to pan) was 60 to 90 % of the total weight of the feedstock before calcination.
The agglomerate samples were made from a simple mixture of abrasive particles and water mixtures described in Table 1-1. The vitrified bond particle binder used to prepare the samples are listed in Table 2. Samples were prepared from three types of abrasive particles: alumina 38A, fused alumina 32A and sintered sol gel alpha-alumina Norton SG grain, obtained from Saint-Gobain Ceramics & Plastics, Inc., Worcester, Mass., USA, in the grit sizes listed in Table 1.
After agglomeration in the rotary calcination apparatus, the agglomerated abrasive grain samples were screened and tested for loose packing density (LPD), size distribution and agglomerate strength. These results are shown in Table 1.
TABLE 1-1
Agglomerated Grain Characteristics
Binding
Sample No
material
pressure at
grain
Weight
Volume
LPD
Average
50%
liquid
Weight
% (on
% of
g/cc
Average size
size
Average %
crushed
particle
lbs (Kg)
grain
binding
−12/
distribution
distrib
relative
fraction
binder
of mix
basis)
material
pan
microns
mesh size
density
MPa
1
30.00
2.0
3.18
1.46
334
−40/+50
41.0
0.6 ± 0.1
60 grit 38A
(13.6)
water
0.60
A binder
(0.3)
0.64
(0.3)
2
30.00
6.0
8.94
1.21
318
−45/+50
37.0
0.5 ± 0.1
90 grit 38A
(13.6)
water
0.90
E binder
(0.4)
1.99
(0.9)
3
30.00
10.0
13.92
0.83
782
−20/+25
22.3
2.6 ± 0.2
120 grit 38A
(13.6)
water
1.20
C binder
(0.5)
3.41
(1.5)
4
30.00
6.0
8.94
1.13
259
−50/+60
31.3
0.3 ± 0.1
120 grit 32A
(13.6)
water
0.90
A binder
(0.4)
1.91
(0.9)
5
30.00
10.0
14.04
1.33
603
−25/+30
37.0
3.7 ± 0.2
60 grit 32A
(13.6)
water
1.20
E binder
(0.5)
3.31
(1.5)
6
30.00
2.0
3.13
1.03
423
−40/+45
28.4
0.7 ± 0.1
90 grit 32A
(13.6)
water
0.60
C binder
(0.3)
0.68
(0.3)
7
30.00
10.0
14.05
1.20
355
−45/+50
36.7
0.5 ± 0.1
90 grit SG
(13.6)
water
1.20
A binder
(0.5)
3.18
(1.4)
8
30.00
2.0
3.15
1.38
120
−120/+140
39.1
—
120 grit SG
(13.6)
water
0.60
E binder
(0.3)
0.66
(0.3)
9
30.00
6.0
8.87
1.03
973
−18/+20
27.6
—
60 grit SG
(13.6)
water
0.90
C binder
(0.4)
2.05
(0.9)
a The volume % binder is a percentage of the solid material within the grain (i.e., binding material and particles) after firing, and does not include the volume % porosity.
The volume % binder of the fired agglomerate grains was calculated using the average LOI (loss on ignition) of the binder raw materials.
The sintered agglomerate grains were sized with U.S. standard testing sieves mounted on a vibrating screening apparatus (Ro-Tap; Model RX-29; W. S. Tyler Inc. Mentor, Ohio). Screen mesh sizes ranged from 18 to 140, as appropriate for different samples. The loose packed density of the sintered agglomerate grains (LPD) was measured by the American National Standard procedure for Bulk Density of Abrasive Grains.
The initial average relative density, expressed as a percentage, was calculated by dividing the LPD (ρ) by a theoretical density of the agglomerate grains (ρ 0 ), assuming zero porosity. The theoretical density was calculated according to the volumetric rule of mixtures method from the weight percentage and specific gravity of the particle binder and of the abrasive particles contained in the agglomerates.
The strength of the agglomerate grains was measured by a compaction test. The compaction tests were performed using one inch (2.54 cm) in diameter lubricated steel die on an Instron® universal testing machine (model MTS 1125, 20,000 lbs (9072 Kg)) with a 5 gram sample of agglomerate grain. The agglomerate grain sample was poured into the die and slightly leveled by tapping the outside of the die. A top punch was inserted and a crosshead lowered until a force (“initial position”) was observed on the recorder. Pressure at a constant rate of increase (2 mm/min) was applied to the sample up to a maximum of 180 MPa of pressure. The volume of the agglomerate grain sample (the compacted LPD of the sample), observed as a displacement of the crosshead (the strain), was recorded as the relative density as a function of the log of the applied pressure. The residual material was then screened to determine the percent crush fraction. Different pressures were measured to establish a graph of the relationship between the log of the applied pressure and the percent crush fraction. Results are reported in Table 1 as the log of the pressure at the point where the crush fraction equates to 50 weight percent of the agglomerate grain sample. The crush fraction is the ratio of the weight of crushed particles passing through the smaller screen to the weight of the initial weight of the sample.
The finished, sintered agglomerates had three-dimensional shapes varying among triangular, spherical, cubic, rectangular and other geometric shapes. Agglomerates consisted of a plurality of individual abrasive grits (e.g., 2 to 20 grits) bonded together by glass binding material at grit to grit contact points.
Agglomerate grain size increased with an increase in amount of binding material in the agglomerate grain over the range from 3 to 20 weight % of the particle binder.
Adequate compaction strength was observed for all samples 1-9, indicating that the glass particle binder had matured and flowed to create an effective bond among the abrasive particles within the agglomerate grain. Agglomerate grains made with 10 weight % particle binder had significantly higher compaction strength than those made with 2 or 6 weight % of particle binder.
Lower LPD values were an indicator of a higher degree of agglomeration. The LPD of the agglomerate grains decreased with increasing weight % particle binder and with decreasing abrasive particle size. Relatively large differences between 2 and 6 weight % particle binder, compared with relatively small differences between 6 and 10 weight % particle binder indicate a weight % particle binder of less than 2 weight % may be inadequate for formation of agglomerate grains. At the higher weight percentages, above about 6 weight %, the addition of more particle binder may not be beneficial in making significantly larger or stronger agglomerate grains.
As suggested by agglomerate grain size results, particle binder C samples, having the lowest molten glass viscosity at the agglomerating temperature, had the lowest LPD of the three particle binder. The abrasive type did not have a significant effect upon the LPD.
TABLE 2
Particle Binder used in the Agglomerates
A Particle
Binder
B
C
D
E
F
Fired
Wt %
Particle
Particle
Particle
Particle
Particle
Composition
(A-1 particle
Binder
Binder
Binder
Binder
Binder
Components b
binder) a
wt %
wt %
wt %
wt %
wt %
Alumina
15 (11)
10
14
10
18
16
Glass Formers
69 (72)
69
71
73
64
68
(SiO 2+ B 2 O 3 )
alkaline earth
5-6 (7-8)
<0.5
<0.5
1-2
6-7
5-6
(CaO, MgO)
Alkali
9-10 (10)
20
13
15
11
10
(Na 2 O, K 2 O, Li 2 O)
Spec. Gravity g/cc
2.40
2.38
2.42
2.45
2.40
2.40
Estimated Viscosity (Poise)
25,590
30
345
850
55,300
7,800
at 1180° C.
a The A-1 particle binder variation set forth in parentheses was used for the samples of Example 2.
b Impurities (e.g., Fe 2 O 3 and TiO 2 ) are present at about 0.1-2%.
Example 2
Additional samples of agglomerate grains were made utilizing various other processing embodiments and feedstock materials.
A series of agglomerate grains (sample nos. 10-13) were formed at different sintering temperatures, ranging from 1100 to 1250° C., utilizing a rotary calcination apparatus (model #HOU-6D60-RTA-28, equipped with a 120 inch (305 cm) long, 5.75 inch (15.6 cm) inner diameter, ⅜ inch (0.95 cm) thick, mullite tube, having a 60 inch (152 cm) heated length with three temperature control zones. The apparatus was manufactured by Harper International, Buffalo, N.Y.). A Brabender feeder unit with adjustable control volumetric feed-rate was used to meter the abrasive particles and particle binder mixture into the heating tube of the rotary calcination apparatus. The process of agglomeration was carried under atmospheric conditions, with an apparatus tube rotation rate of 4 rpm, a tube incline angle of 2.5 degrees, and a feed rate of 8 kg/hour. The apparatus used was substantially identical to the apparatus illustrated in FIG. 1 . Temperature selections and other variables utilized to make these agglomerates are set forth in Table 2-1.
All samples contained a mixture, on a weight % basis, of 89.86 % abrasive particles (60 grit 38A alumina obtained from Saint-Gobain Ceramics & Plastics, Inc.), 10.16% temporarye binder mixture (6.3 wt % AR30 liquid protein binder, 1.0 % Carbowax® 3350 PEG and 2.86% of particle binder A). This mixture yielded 4.77 volume % particle binder and 95.23 volume % abrasive particles in the sintered agglomerate grain. The calculated theoretical density of the agglomerate grains (assuming no porosity) was 3.852 g/cc.
Prior to placing the mixture into the feeder unit, green stage agglomerate grains were formed by simulated extrusion. To prepare extruded agglomerate grains, the liquid protein temporary binder was heated to dissolve the Carbowax® 3350 PEG. Then the particle binder was added slowly while stirring the mixture. Abrasive particles were added to a high shear mixer (44 inch (112 cm) diameter) and the prepared particle binder mixture was slowly added to the particles in the mixer. The combination was mixed for 3 minutes. The mixed combination was wet-screened through a 12 mesh box screen (US standard sieve size) onto trays in a layer at a maximum depth of one inch (2.5 cm) to form wet, green (unfired), extruded agglomerate grains. The layer of extruded agglomerate grains was oven dried at 90° C. for 24 hours. After drying, the agglomerate grains were screened again using a 12 to 16 mesh (U.S. standard sieve size) box screen.
It was observed during rotary calcination that the agglomerate grains made in the green state appeared to break apart when heated, and, then, re-formed as they tumbled out of the exit end of the heated portion of the rotary calciner tube. The larger size of the agglomerated grains made in the green state, relative to that of the agglomerated grains after firing, was readily apparent upon visual inspection of the samples.
After firing, the agglomerated grain sizes were observed to be sufficiently uniform for commercial purposes, with a size distribution over a range of about 500-1200 microns. The size distribution measurements are set forth in Table 2-2, below.
TABLE 2-1
pressure at
%
LPD
50%
%
Ave.
LPD
Sintering
Yield
Ave.
g/cc
crushed
yield
agglom
g/cc
Sample
Temp. a
−12
size
−12
fraction
−16/+35
size
−16/+35
No.
° C.
mesh
μm
mesh
MPa
mesh
μm
mesh
(10)
1100
n/a b
n/a
n/a
n/a
n/a
536
n/a
(11)
1150
97.10
650
1.20
13 ± 1
76.20
632
0.95
(12)
1200
96.20
750
1.20
9 ± 1
87.00
682
1.04
(13)
1250
96.60
675
1.25
8 ± 1
85.20
641
1.04
a Temperature of rotary calciner controller set point (for all 3 zones).
b “n/a” indicates no measurement was made.
TABLE 2-2
Size distribution for fired agglomerate grains
Sieve #
ASTM-E
Sample
Sieve # ISO
Weight % on Screen
No.
565 μm
10
11
12
13
−35
−500
41.05
17.49
11.57
14.31
35
500
22.69
17.86
14.56
17.69
30
600
18.30
24.34
21.27
26.01
25
725
12.57
21.53
24.89
23.06
20
850
3.43
13.25
16.17
12.43
18
1000
1.80
4.58
10.09
5.97
16
1180
0.16
0.95
1.44
0.54
Example 3
Agglomerate grains (sample nos. 14-23) were prepared as described in Example 2, except the temperature was maintained constant at 1000° C., and a model #KOU-8D48-RIA-20 rotary calciner apparatus, equipped with a 108 inch (274 cm) long, 8 inch (20 cm) inner diameter, fused silica tube, having a 48 inch (122 cm) heated length with three temperature control zones, was used. The apparatus was manufactured by Harper International, Buffalo, N.Y. Various methods were examined for preparation of the pre-fired mixture of abrasive particles and particle binder material. The process of agglomeration was carried under atmospheric conditions, with an apparatus tube rotation rate of 3 to 4 rpm, a tube incline angle of 2.5 degrees, and a feed rate of 8 to 10 kg/hour. The apparatus used was substantially identical to the apparatus illustrated in FIG. 1 .
All samples contained 30 lbs (13.6 Kg) abrasive particles (the same as were used in Example 2, except that sample 16 contained 25 lbs (11.3 Kg) of 70 grit Norton SG® sol gel alumina, obtained from Saint-Gobain Ceramics and Plastics, Inc.) and 0.9 lbs (0.41 Kg) particle binder A (yielding 4.89 volume % particle binder material in the sintered agglomerate grain). The particle binder material was dispersed in different temporary binder systems prior to addition to the abrasive particles. The temporary binder system of Example 2 (“Binder 2”) was used for some samples and other samples were made using AR30 liquid temporary binder (“Binder 3”) in the weight percentages listed below in Table 3. Sample 20 was used to prepare agglomerate grains in the green, unfired state by the simulated extrusion method of Example 2.
The variables tested and the test results of the tests are summarized in Table 3.
TABLE 3
Green stage binder treatments
%
wt %
Yield
binder
−12
Sample
Mix
(as % of
mesh
LPD
No.
Treatment
grain wt)
screen
g/cc
14
Binder 3
2.0
100
1.45
15
Binder 3
1.0
100
1.48
16
Binder 3;
4.0
92
1.38
SG grain
17
Binder 3
4.0
98
1.44
18
Binder 2
6.3
90
1.35
19
Binder 3
8.0
93
1.30
20
Binder 2;
6.3
100
1.37
simulated
extrusion
21
Binder 3
3.0
100
1.40
22
Binder 3
6.0
94
1.44
23
Binder 2
4.0
97
1.54
These results confirm that green stage agglomeration is not needed to form an acceptable quality and yield of sintered agglomerated grains (compare samples 18 and 20). As the wt % of Binder 3 used in the initial mix increased from 1 to 8 %, the LPD showed a trend towards a moderate decrease, indicating that the use of a binder has a beneficial, but not essential, effect upon the agglomeration process. Thus, rather unexpectedly, it did not appear necessary to pre-form a desired agglomerate grain shape or size prior to sintering it in a rotary calciner. The same LPD was achieved merely by feeding a wet mixture of the agglomerate components into the rotary calciner and tumbling the mixture as it passes through the heated portion of the apparatus.
Example 4
Agglomerate grains (sample nos. 24-29) were prepared as described in Example 2, except the temperature was maintained constant at 1200° C. and various methods were examined for preparation of the pre-fired mixture of abrasive particles and particle binder. All samples (except samples 28-29) contained a mixture of 300 lbs (136.4 Kg) abrasive particles (same as in Example 2: 60 grit 38A alumina) and 9.0 lbs (4.1 Kg) of particle binder A (yielding 4.89 volume % particle binder in the sintered agglomerate grain).
Sample 28 (same composition as Example 2) contained 44.9 lbs (20.4 Kg) of abrasive particles and 1.43 lbs (0.6 Kg) of temporary binder A. The binder was combined with the liquid binder mixture (37.8 wt % (3.1 lbs) of AR30 binder in water) and 4.98 lbs of this combination was added to the abrasive particles. The viscosity of the liquid combination was 784 CP at 22° C. (Brookfield LVF Viscometer).
Sample 29 (same composition as Example 2) contained 28.6 lbs (13 Kg) of abrasive particles and 0.92 lbs (0.4 Kg) of particle binder A (yielding 4.89 volume % particle binder in the sintered agglomerate grain). The particle binder was combined with the liquid temporary binder mixture (54.7 wt % (0.48 lbs) Duramax® resin B1052 and 30.1 wt % (1.456 lbs) Duramax resin B1051 resin in water) and this combination was added to the abrasive particles. The Duramax resins were obtained from Rohm and Haas, Philadelphia, Pa.
The process of agglomeration was carried under atmospheric conditions, with an apparatus tube rotation rate of 4 rpm, a tube incline angle of 2.5 degrees, and a feed rate of 8 to 12 kg/hour. The apparatus used was substantially identical to the apparatus illustrated in FIG. 1 .
Sample 28 was pre-agglomerated, before calcination, in a fluidized bed apparatus made by Niro, Inc., Columbia, Md. (model MP-2/3 Multi-Processor™, equipped with a MP-1 size cone (3 feet (0.9 meter) in diameter at its widest width). The following process variables were selected for the fluidized bed process sample runs:
inlet air temperature 64-70° C.
inlet air flow 100-300 cubic meters/hour
granulation liquid flow rate 440 g/min
bed depth (initial charge 3-4 kg) about 10 cm
air pressure 1 bar
two fluid external mix nozzle 800 micron orifice
The abrasive particles were loaded into the bottom apparatus and air was directed through the fluidized bed plate diffuser up and into the particles. At the same time, the liquid mixture of particle binder and temporary binder was pumped to the external mix nozzle and then sprayed from the nozzles through the plate diffuser and into the particles, thereby coating individual particles. Green stage agglomerate grains were formed during the drying of the particle binder and binder mixture.
Sample 29 was pre-agglomerated, before calcination, in a low pressure extrusion process using a Benchtop Granulator® made by LCI Corporation, Charlotte, N.C. (equipped with a perforated basket having 0.5 mm diameter holes). The mixture of abrasive particles, particle binder and temporary binder was manually fed into the perforated basket (the extruder screen), forced through the screen by rotating blades and collected in a receiving pan. The extruded pre-agglomerate grains were oven-dried at 90° C. for 24 hours and used as feed stock for the rotary calcination process.
The variables tested and the results of the tests are summarized below and in Tables 4-1 and 4-2. These tests confirm the results set forth in Example 3 are also observed at a higher firing temperature (1200 versus 1000° C.). These tests also illustrate that low-pressure extrusion and fluid bed pre-agglomeration may be used to make agglomerated granules, but an agglomeration step before rotary calcination is not necessary to make the agglomerates of the invention.
TABLE 4-1
Agglomerate characteristics
wt %
binder
%
on
Yield
particles
−12
Average
Sample
Mix
wt %
mesh
size
LPD
No.
Treatment
basis
screen
μm
g/cc
24
Binder 3
1.0
71.25
576
1.30
25
Binder 3
4.0
95.01
575
1.30
26
Binder 3
8.0
82.63
568
1.32
27
Binder 2
7.2
95.51
595
1.35
28
Binder 3
7.2
90.39
n/a
n/a
29
Duramax
7.2
76.17
600
1.27
resin
TABLE 4-2
Grit size distribution for agglomerate grains
Sieve #
ASTM-E
Sample
Sieve # ISO
Weight % on Screen
No.
565 μm
24
25
26
27
28
29
−40
−425
17.16
11.80
11.50
11.50
n/a
11.10
40
425
11.90
13.50
14.00
12.50
n/a
12.20
35
500
17.30
20.70
22.70
19.60
n/a
18.90
30
600
20.10
25.20
26.30
23.80
n/a
23.70
25
725
17.60
19.00
17.20
18.40
n/a
19.20
20
850
10.80
8.10
6.40
9.30
n/a
10.30
18
1000
3.90
1.70
1.60
3.20
n/a
3.60
16
1180
0.80
0.10
0.30
1.60
n/a
1.10
Example 5
Additional agglomerate grains (sample nos. 30-37) were prepared as described in Example 3, except sintering was done at 1180° C., different types of abrasive particles were tested, and 30 lbs (13.6 Kg) of abrasive particles were mixed with 1.91 lbs (0.9 Kg) of particle binder A (to yield 8.94 volume % particle binder in the sintered agglomerate grains). Binder 3 of Example 3 was compared with water as a temporary binder for green stage agglomeration. Samples 30-34 used 0.9 lbs (0.4 Kg) of water as a temporary binder. Samples 35-37 used 0.72 lbs (0.3 Kg) of Binder 3. The variables tested are summarized below in Table 5.
The process of agglomeration was carried under atmospheric conditions, with an apparatus tube rotation rate of 8.5-9.5 rpm, a tube incline angle of 2.5 degrees, and a feed rate of 5-8 kg/hour. The apparatus used was substantially identical to the apparatus illustrated in FIG. 1 .
After agglomeration, the agglomerated abrasive grain samples were screened and tested for loose packing density (LPD), size distribution and agglomerate strength. These results are shown in Table 5.
TABLE 5
wt %
pressure at
binder
50% crushed
Sample
Abrasive
Temp.
on
Average
LPD
fraction
No.
particles
Binder
particles
size μm
g/cc
MPa
30
60 grit
water
3.0
479
1.39
1.2 ± 0.1
57A alumina
31
60 grit
water
3.0
574
1.27
2.5 ± 0.1
55A alumina
32
80 grit
water
3.0
344
1.18
0.4 ± 0.1
XG alumina
33
70 grit
water
3.0
852
1.54
17 ± 1.0
Targa ® sol gel
alumina
34
70/30 wt %
water
3.0
464
1.31
1.1 ± 0.1
60 grit 38A/
60 grit Norton
SG alumina
35
60 grit 38A
Binder 3
2.4
n/a
n/a
n/a
alumina
36
60 grit Norton
Binder 3
2.4
n/a
n/a
n/a
SG ® alumina
37
60/25/15 wt %
Binder 3
2.4
n/a
n/a
n/a
60 grit 38 A/
120 grit Norton
SG/
320 grit 57A
These results again demonstrate the utility of water as a temporary binder for the agglomerate grains in the rotary calcination process. Further, mixtures of grain types, grain sizes, or both, may be agglomerated by the process of the invention and these agglomerates can be coated at a temperature of 1180° C. in the rotary calciner. A significant increase in crush strength was observed when a high aspect ratio (i.e., ≧4:1), elongated abrasive grain was used in making the agglomerate grains (sample 33).
Example 6
Another series of agglomerate grains (sample nos. 38-45) was prepared as described in Example 3, except different sintering temperatures were used, and different types of abrasive particle grit sizes blends and different particle binders were tested. In some of the feedstock mixtures, walnut shell was used as an organic pore inducer filler material (walnut shell was obtained from Composition Materials Co., Inc., Fairfield, Conn., in US Sieve size 40/60). The variables tested are summarized below in Table 6. All samples contained a mixture of 30 lbs (13.6 Kg) abrasive particles and 2.5 wt % Binder 3, on grain weight basis, with various amounts of particle binders as shown in Table 6.
The process of agglomeration was carried under atmospheric conditions, with an apparatus tube rotation rate of 8.5-9.5 rpm, a tube incline angle of 2.5 degrees, and a feed rate of 5-8 kg/hour. The apparatus used was substantially identical to the apparatus illustrated in FIG. 1 .
After agglomeration, the agglomerated grain samples were screened and tested for loose packing density (LPD), average size and agglomerate crush strength (see Table 6). The properties of all agglomerate grains were acceptable for use in manufacturing coated abrasives. These data appear to indicate the use of organic pore inducers, i.e., walnut shells, had no significant impact on agglomerate characteristics.
TABLE 6
pressure at
Vol %
Vol %
50%
Abrasive parts.
Fired
Fired
crushed
Sample
wt % mixture
Binding
Particle
Pore
LPD
fraction
No.
grit size/type
material
Binder a
Inducer
g/cc
MPa
38
90/10 wt %
F
5.18
0
1.14
11.5 ± 0.5
60 grit 38A/
70 grit
Targa ® sol
gel alumina
39
90/10 wt %
C
7.88
2
1.00
11.5 ± 0.5
60 grit 38A/
70 grit
Targa ® sol
gel alumina
40
90/10 wt %
F
5.18
2
1.02
10.5 ± 0.5
80 grit 38A/
70 grit
Targa ® sol
gel alumina
41
90/10 wt %
C
7.88
0
0.92
n/a
80 grit 38A/
70 grit
Targa ® sol
gel alumina
42
50/50 wt %
F
5.18
2
1.16
11.5 ± 0.5
60 grit 38A/
60 grit 32A
43
50/50 wt %
C
7.88
0
1.06
n/a
60 grit 38A/
60 grit 32A
44
50/50 vol %
F
5.18
0
1.08
8.5 ± 0.5
80 grit 38A/
60 grit 32A
45
50/50 vol %
C
7.88
2
1.07
11.5 ± 0.5
80 grit 38A/
60 grit 32A
a Volume % is on the basis of total solids (grain, binding material and pore inducer) and does not include the porosity of the agglomerate. 38A and 32A are fused alumina abrasive materials.
Example 7
In this Example the performance of a 17.8 cm (7 inch) disc made using abrasive agglomerates according to the invention was compared with commercial abrasive discs made using conventional materials and abrasive grains.
The abrasive disc according to the invention was made using abrasive agglomerate grains comprising seeded sol-gel alumina abrasive particles with a grit size of 90 obtained from Saint-Gobain Ceramics and Plastics, Inc. These particles were formed into abrasive agglomerate grains as described in connection with the preparation of Sample 7 in Example 1 above. The grains were graded and a −28+40 grade fraction was retained for use.
These abrasive agglomerate grains were used to form a coated abrasive disc by deposition upon a conventional fiber disc substrate using a conventional make coat/size coat technique. The resin used to provide the make and size coats was a conventional phenolic resin. The make coat was applied at a level of 0.12 kg/m 2 , (8.3 pounds/Ream) and the abrasive agglomerate grains were deposited by a UP technique at a level of 0.28 kg/m 2 , (19 pounds/Ream). The size coat was applied using a spray technique at a level of 0.49 kg/m 2 , (33 pounds/Ream), and was a standard phenolic resin with a viscosity of 800 cps modified by the addition of Cab-O-Sil silica from Cabot Corporation to a viscosity of 2000 cps. In each case the “Ream” referred to is a sandpaper-makers ream which corresponds to 330_square feet or 30.7 square meters.
The disc according to the invention was used to abrade a fiat bar of 1008 steel. The disc was contacted with the bar for 30 seconds at a contact pressure of 13 lbs/sq.in. and the weight of the bar was measured after each contact to determine the amount of metal removed at each contact. The results were plotted in a graph which is presented as FIG. 2 .
For the sake of comparison three competitive commercial discs of the same size were subjected to the same test and the results are plotted in the same FIG. 2 . The discs tested were:
984C which a fiber-backed, 44 coated, seeded sol-gel alumina 80 grit abrasive grain sold by 3M Company;
987C which is similar to 984C except that the abrasive grit is 80 “321 Cubitron®” and the disc had received a supersize treatment. This disc too was sold by 3M Company; and
983C which is the same as 984C except that the grain is an 80 grit MgO-modified sol-gel alumina and the grain is applied by a 100% UP process. This too is available from 3M Company.
As will be apparent from FIG. 2, while all discs started cutting at about the same rate, the disc according to the invention went on cutting far longer and far better than any of the 3M comparative discs.
Example 8
In this Example the effect of using a modified size coat is studied. Two otherwise identical abrasive discs prepared in the same way of the “Invention” disc in Example 1 were made with different size coats. In the first sample the disc was exactly the same as the “Invention” sample from Example 1 and the second was exactly the same except the unmodified size coat was used. The evaluation used the same procedures as are set forth in Example 1 and the results obtained are shown in FIG. 3 of the Drawings.
As will be clearly seen, while the performance is still better than the prior art products, it is not so good as that of the product with the viscosity-modified size coat. This lends credibility to the view that the lower viscosity size to some degree reduces the beneficial effect of porosity in the abrasive agglomerate grains.
Example 9
This Example compares the performance of two discs according to the invention, each having a standard (that is unmodified to increase the viscosity as in the disc tested in Example 8) size coat. In this case the only difference between the discs lay in the binder used to bond the abrasive particles together to form the abrasive agglomerate grains. In the sample identified as “Vitrified SCA Standard Size Coat” the bond was vitreous and the sample was that tested in Example 8 as indicated above. In the sample identified as “Organic SCA Standard Size Coat.” the bond was an organic bond and the seeded sol-gel alumina abrasive particles in the agglomerates were a little coarser with a grit size of 80. However the porosity was essentially the same. The comparative data, obtained using the same test procedure used in the previous Examples, is plotted on the graph presented as FIG. 4 of the Drawings.
From the graph it will be appreciated that the vitreous bonded agglomerates performed slightly better than the organic-bonded agglomerates, even though the coarser grits in the Organic SCA Standard Size Coat disc would be expected to lead to higher metal removal rates. The difference became more significant in the later stages of the life of the disc.
From the above data it is very clear that the use of abrasive agglomerate grains results in significant improvements over prior art discs especially when the bond holding the agglomerates together is a vitreous bond and the size is given a higher viscosity than would normally be used to inhibit loss of porosity when the agglomerates are used to manufacture a coated abrasive.
|
Novel coated abrasives comprising abrasive agglomerate grains characterized by a high porosity and low ratio of solid volume to nominal volume provide exceptionally useful medium to low pressure grinding characteristics.
| 8
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of provisional patent application Ser. No. 61/516,522 filed 2011 Apr. 5 by the present inventor.
BACKGROUND
Prior Art The following is a tabulation of some prior art that presently appears relevant:
[0002]
[0000]
U.S. Patents
Pat. No.
Kind Code
Issue Date
Patentee
U.S. Pat. No. 5,738,591
B1
Apr. 14, 1998
Opsal
U.S. Pat. No. 3,881,727
B1
May 6, 1975
Olson
U.S. Pat. No. 5,866,890
B1
Feb. 2, 1999
Neuner
[0003] The United States, along with many countries in the world, relies on a first-come first-served basis for organizing people's behavior in society. The first-come, first-served rule simply means that an earlier requestor for a service or product will receive that service or product before any subsequent requestor. This concept is alternatively called queuing, with queuing being the process of 1) aligning requests first to last and then 2) servicing a request in the order received. The first-come, first-served rule works well in organizing society's behavior except when someone either ignores or intentionally violates these informal rules. Nowhere is the first-come, first-served rule more likely to break down as it is in a point-of-sale activity.
[0004] A point-of-sale activity is a consumer activity where an individual desires to purchase a particular good or service. Some examples are: waiting at a service counter at the local hardware store, waiting to pay at a bank, department store customer service center, or waiting to purchase gasoline. Point-of-sale also includes using unattended machines such as those in laundromats, car washes, and other facilities using vending machines. Point-of-sale machines also include gaming devices such as pool tables, pinball machines and video poker machines.
[0005] For attended point-of-sale activities, retailers often resorted to the “take-a-number” system. In such a system, for example, a person approaches a centralized repository of numbers, retrieves the next available number, and waits until that number is called or displayed. Consumers who approached the counter earlier have lower numbers and therefore are called for service prior to this person's number. Consumers approaching later have a higher number, so they will be called after this person is called. Such systems work well but require an attendant or clerk to monitor and assure the system is properly implemented and enforced.
[0006] Vending machines present a more difficult problem for the first-come, first-served rule. Since there is generally no attendant or clerk, individual consumers must rely on the honesty and integrity of the others desiring the same service or product. Unfortunately, others often misinterpret, misunderstand or accidently misapply the first-come, first-served rule, resulting in heightened tensions and dissatisfied consumers.
[0007] A particular type of point-of-sale vending system is a gaming system such as pool tables. These systems are often present in recreational environments such as lounges, sports bars, nightclubs and other recreational centers. Such environments are often loud and confusing, thus contributing to the failure of people to successfully apply the first-come, first-served rule. For example, the game of pool is often started by inserting quarters into a money slot, activating the drop of balls that begins a game. Only one game may be played at a time with no method of queuing built into the pool gaming system. Therefore, in an environment where several people wish to play pool, those desiring to participate will place their quarters on the rail of the pool table or write their name on a chalkboard and await their turn. After the current game ends, someone will (hopefully) announce that the game is over. The persons having quarters nearest the money slot or who are next on the chalkboard will insert their quarters and begin the next game. Unfortunately, in this often confused and active environment participants forget whose quarters are next, or may intentionally try to advance their order. A lot of times, quarters are knocked over on the billiards table or into the floor during game play. The replacement of the quarters, some marked with a penny or dime, is not in order as before. Such behavior results in heightened tensions and sometimes even violence.
[0008] I have found that chalkboards, quarter queue systems, and electronic queue systems cause problems for the owner of the establishments. Chalk boards run out of chalk and the chalk is not replaced, quarter queue systems cause fights in which owners have to break up, and electronic queue systems break down and are not repaired.
[0009] It is, therefore, the object of the present embodiments to provide an easy-to-use token with designs, or designs and table friendly material, for placement on a billiards table sequencing point of sale activities.
SUMMARY
[0010] In accordance with one embodiment a billiards table queue placement token with a design, and table friendly material.
ADVANTAGES
[0011] Accordingly several advantages of one or more aspects are as follows: a separate design distinguishes one queue placement token from another which replaces the “standard quarters on the table or chalk board” rule, each participate will understand their place in the queuing system, eliminates fights among participates over who was “first” in line, each queue placement token can be a representative of who you are and what you represent according to the queue placement token you purchase, eliminates picking up quarters knocked over on the billiards table during game play, eliminates electronic queuing systems. Other advantages of one or more aspects will be apparent from considerations of the drawing and ensuing descriptions.
DRAWING
Figures
[0012] In the drawings, closely related figures have the same number but different alphabetic suffixes.
[0013] FIG. 1A and FIG. 2A shows an overhead view of the top of the base with which a design can be engraved, and a side view which has one side.
[0014] FIG. 1B and FIG. 2B shows a bottom view of the said base with which a said design can be engraved, and said side view which has one said side.
[0015] FIG. 1C and FIG. 2C shows a said bottom view of the said base with which an optional friendly billiards table material can be applied.
[0000]
Drawings-Reference Numerals
10
top of base
12
side
14
bottom of base
16
design
18
table friendly material
DETAILED DESCRIPTION
FIGS. 1 A, 1 B and 1 C
[0016] One embodiment of the token is illustrated in FIG. 1A (overhead view) and FIG. 1B (bottom view). The token has a flat top base 10 and a flat bottom base 14 and one side 12 . The flat top base 10 with the dimensions of 1½ inch diameter circle can implement a design 16 to deviate itself from other embodiments. The flat bottom base 14 with the dimensions of 1% inch diameter circle also can implement a design 16 , or according to another embodiment FIG. 1C , a table friendly material 18 can be applied to the flat bottom base 14 to make the base table friendly. The side 12 for FIGS. 1A , 1 B, and 1 C is ⅛ inch thick.
[0017] I presently contemplate for this embodiment to have a 1 ½ inch diameter circle for the top base 10 and bottom base 14 , and ⅛ inch thick for the side 12 and be made of metal. The top base 10 would implement a design 16 and the bottom base 14 would also implement a design 16 . At present I believe that this embodiment, FIG. 1A and FIG. 1B , operates most efficiently but the other embodiments are also satisfactory.
FIGS. 2 A, 2 B, and 2 C
Alternative Embodiments
[0018] There are various possibilities with regard to shape, size and material in which an embodiment can be made. FIG. 2A shows an overhead view of a square embodiment with a flat top base 10 and four sides 12 with a design 16 on the top flat base 10 . FIG. 2B shows a bottom view of a square embodiment with a flat bottom base 14 and four sides 12 with a design 16 on the flat bottom base 14 . FIG. 2C shows a bottom view of a square embodiment with a flat bottom base 14 and four sides 12 and a table friendly material 18 applied to the bottom base 14 .
[0019] Other embodiments can have different shapes, such as oval, triangular, etc. and different materials such as plastic, wood, polycarbonate, etc. The top base 10 and bottom base 14 does not need to be flat and does not have to incorporate a design 16 . Designs 16 can be anything from animals, sports teams, hobbies, etc. Sides 12 can be unlimited. The table friendly material 18 can be placed directly on the flat bottom base 14 or flat top base 10 without a design 16 present, or over the design 16 on the flat bottom base 14 or the flat top base 10 . Licensing fees must be obtained in some designs.
Operation
FIGS. 1 A, 1 B, 1 C, 2 A, 2 B, 2 C
[0020] The manner of using the embodiment is by placing the top base 10 , bottom base 14 , or the table friendly material 18 onto the rail of a billiards table in the order of turn. When your turn to play has begun, you take the required coins from your pocket or pocketbook and place in the billiard table coin slot. Then you can place the unique embodiment at the end of the line in the queue system or return it to the place of origin in which you pulled it from if no play is desirable after your turn is up.
Advantages
[0021] From the description above, a number of advantages of some embodiments of my billiards query placement token become evident:
(a) A query system that will eliminate violence regarding billiards play. (b) A query system that will eliminate the use and spillage of quarters place on a billiards table. (c) A token that you can keep and place in line on the next game of billiards you play. (d) A token that can identify you in gameplay and keep your correct turn in the query system. (e) The elimination of any chalk boards and electronic query systems that either break down or run out of chalk slowing gameplay down.
Conclusion, Ramifications, and Scope
[0027] Accordingly, the reader will see that one embodiment of the token is convenient in size and can easily be placed in your pocket and cue case. When you decide to play a game of billiards, it can also be removed easily and be placed on the table. The reader also can see that the billiards query placement token will securely mark your turn in the query system. Furthermore, the billiards query placement token has the additional advantages in that:
The material of the embodiments can be aluminum, wood, plastic, silver, gold, other types of metal, etc. The embodiments can have other shapes such as oval, triangular, rectangular, cubed, etc. Each design on the embodiment can match a design on an article of clothing or hat that you can wear that can easily identify you in the query system. Each design of the embodiments can be a representative of who you are, where you went to school, what branch you served in the military, what you stand for, etc. The designs of the embodiments can have sports teams, hobbies, military emblems, colors, letters, etc. The embodiments are lightweight and economical, and can be used by persons of any age.
[0034] Although the description above contains many specifications, these should not be construed as limiting the scope of the embodiment but merely providing illustrations of some of the embodiments. For example, you can have an oval embodiment made of silver with your initials incorporated on the top with diamonds. The sides can be just one or unlimited. Colors are also unlimited. Table friendly material can be applied to grip the billiard rail better.
[0035] Thus the scope of the embodiments should be determined by the appended claims and legal equivalents, rather than by the examples given.
|
One embodiment of a circular flat token having a unique design on the top of the base, a unique design on the bottom of the base, and sides that are low in profile which can be placed on a billiards table to sequence participation in a point of sale activity. Other embodiments are described and shown.
| 0
|
PRIORITY CLAIMS
[0001] The present application is a continuation-in-part of U.S. patent application Ser. No. 10/861,103, filed Jun. 4, 2004 (which is, in turn, a continuation-in-part of U.S. patent application Ser. No. 10/656,457, filed Aug. 22, 2003), and the present application is also a continuation-in-part of U.S. patent application Ser. No. 10/861,320, filed Jun. 4, 2004 (which is, in turn, a continuation-in-part of U.S. patent application Ser. No. 10/656,457, filed Aug. 22, 2003).
GOVERNMENT RIGHTS
[0002] This invention was made with Government support under Contract Number HR0011-04-1-0034 awarded by the Defense Advanced Research Projects Agency (DARPA). The Government has certain rights in the invention.
FIELD OF THE INVENTION
[0003] This invention relates to semiconductor laser devices and methods, and also to a laser transistor and techniques for enhancing high speed optical signal generation.
BACKGROUND OF THE INVENTION
[0004] A part of the background hereof lies in the development of light emitters based on direct bandgap semiconductors such as III-V semiconductors. Such devices, including light emitting diodes and laser diodes, are in widespread commercial use.
[0005] Another part of the background hereof lies in the development of wide bandgap semiconductors to achieve high minority carrier injection efficiency in a device known as a heterojunction bipolar transistor (HBT), which was first proposed in 1948 (see e.g. U.S. Pat. No. 2,569,376; see also H. Kroemer, “Theory Of A Wide-Gap Emitter For Transistors” Proceedings Of The IRE, 45, 1535-1544 (1957)). These transistor devices are capable of operation at extremely high speeds. An InP HBT has recently been demonstrated to exhibit operation at a speed above 500 GHz (see W. Hafez, J. W. Lai, and M. Feng, Elec Lett. 39, 1475 (October 2003).
[0006] The art had contained an objective of light emission in a heterojunction bipolar transistor, and a theoretical striving for a laser transistor. However, for various reasons, an operational laser transistor has not heretofore been reported, and the achievement of same is one of the objectives hereof. Also, control of a laser transistor, to achieve advantageous high speed optical signals, is among the further objectives hereof.
SUMMARY OF THE INVENTION
[0007] In the prior copending U.S. patent application Ser. Nos. 10/646,457, 10/861,103, and 10/861,320 (hereinafter, collectively, “the prior copending applications”), all assigned to the same assignee as the present Application, there is disclosed a direct bandgap heterojunction transistor that exhibits light emission from the base layer. Modulation of the base current produces modulated light emission. [As used herein, “light” means optical radiation that can be within or outside the visible range.] The prior copending applications also disclose three port operation of a light emitting HBT. Both spontaneous light emission and electrical signal output are modulated by a signal applied to the base of the HBT.
[0008] Another aspect of the prior copending applications involves employing stimulated emission to advantage in the base layer of a bipolar transistor (e.g. a bipolar junction transistor (BJT) or a heterojunction bipolar transistor (HBT), in order to enhance the speed of the transistor. Spontaneous emission recombination lifetime is a fundamental limitation of bipolar transistor speed. In an embodiment of the prior copending applications, the base layer of a bipolar transistor is adapted to enhance stimulated emission (or stimulated recombination) to the detriment of spontaneous emission, thereby reducing recombination lifetime and increasing transistor speed. In a form of this embodiment, at least one layer exhibiting quantum size effects, preferably a quantum well or a layer of quantum dots, preferably undoped or lightly doped, is provided in the base layer of a bipolar transistor. At least a portion of the base layer containing the at least one layer exhibiting quantum size effects, is highly doped, and of a wider bandgap material than the at least one layer. The at least one quantum well, or layer of quantum dots, within the higher gap highly doped material, enhances stimulated recombination and reduces radiative recombination lifetime. A two-dimensional electron gas (“2-DEG”) enhances carrier concentration in the quantum well or quantum dot layer, thereby improving mobility in the base region. Improvement in base resistance permits reduction in base thickness, with attendant reduction of base transport time. As described in the prior copending applications, these advantages in speed are applicable in high speed bipolar transistors in which light emission is utilized, and/or in high speed bipolar transistors in which light emission is not utilized. In light emitting bipolar transistor devices, for example heterojunction bipolar transistors of direct bandgap materials, the use of one or more layers exhibiting quantum size effects can also be advantageous in enhancing light emission and customizing the emission wavelength characteristics of the devices.
[0009] In a further embodiment disclosed in the prior copending applications, a semiconductor laser is set forth, including: a heterojunction bipolar transistor structure comprising collector, base, and emitter of direct bandgap semiconductor materials; an optical resonant cavity enclosing at least a portion of the transistor structure; and means for coupling electrical signals with the collector, base, and emitter regions to cause laser emission from the device.
[0010] In another embodiment disclosed in the prior copending applications, a plurality of spaced apart quantum size regions (e.g. quantum wells and/or quantum dots) having different thicknesses are provided in the base region of a bipolar transistor and are used to advantageously promote carrier transport unidirectionally through the base region. As an example, the base region can be provided with several spaced apart quantum size regions of different thicknesses, with the thicknesses of the quantum size regions being graded from thickest near the collector to thinnest near the emitter. An injected electron is captured in a smaller well, tunnels into the next bigger well, and then the next bigger well, and so forth, until, at the biggest well closest to the collector, it tunnels to and relaxes to the lowest state of the biggest well and recombines. The arrangement of wells encourages carrier transport unidirectionally from emitter toward collector. Maximum recombination and light are derived from the biggest well as near as possible to the collector, which is an advantageous position, such as for optical cavity reasons. Carriers diffuse “downhill” in energy; i.e., toward the thicker wells. The asymmetry in well size provides improved directionality and speed of carrier transport. In a light emitting HBT, light emission and device speed are both enhanced.
[0011] In accordance with an embodiment of the invention, a device and technique are set forth for high speed optical signal generation with an enhanced signal to noise ratio and control of “on” and “off” time durations utilizing the stimulated emission process for the “on” state and spontaneous emission process for the “off” state. The operating point and excitation of the transistor laser are selected to obtain cycles that each have an “on” portion of stimulated emission (laser optical output, and electrical signal output) and an “off” portion of spontaneous emission (without sensible optical output, and electrical noise).
[0012] A method is set forth in accordance with an embodiment of the invention for producing controllable light pulses, including the following steps: providing a heterojunction bipolar transistor structure comprising collector, base, and emitter regions of semiconductor materials; providing an optical resonant cavity enclosing at least a portion of the transistor structure; and coupling electrical signals with respect to said collector, base, and emitter regions, to switch back and forth between a stimulated emission mode that produces output laser pulses and a spontaneous emission mode. In a preferred embodiment, the electrical signals include an AC excitation signal, and part of each excitation signal cycle is operative to produce stimulated emission, and another part of each excitation signal cycle is operative to produce spontaneous emission. In this embodiment, during said part of the cycle, the current in the base region exceeds the stimulated emission threshold of the device, and during said other part of the cycle, the current in the base region does not exceed said threshold. Also in this embodiment, the frequency of the excitation signal controls the frequency of the output laser pulses and the relative amplitude of the excitation signal controls the pulse width of the output laser pulses. In a form of this embodiment, the AC excitation signal is provided at a frequency of at least about 1 GHz, and the pulse width of the output laser pulses is controlled to be less than about 100 picoseconds.
[0013] Further features and advantages of the invention will become more readily apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 is a simplified cross-sectional diagram, not to scale, of a light emitting transistor as described in a referenced copending Application.
[0015] FIG. 2 shows, on the left, a diagram, not to scale, of the epitaxial layers of a crystal used for making a heterojunction bipolar light-emitting transistor (HBLET) in accordance with an embodiment of the invention and which can be used in practicing embodiments of the method of the invention, and, on the right, a corresponding band diagram.
[0016] FIG. 3 , shows, on the left, a processed, metallized, and cleaved HBLET laser (top view) as made using the crystal of FIG. 2 and, on the right, an image of the operating device obtained with a video CCD detector.
[0017] FIG. 4 shows the transistor I-V curves of another HBLET laser with ˜260 μm spacing between the Fabry-Perot facets.
[0018] FIG. 5 shows, in quasi-continuous operation (88% duty cycle at 60 Hz), the recombination radiation spectra of the HBLET device of FIG. 3 , but with slightly increased voltage bias V CE to increase the reverse bias on the base-collector junction.
[0019] FIG. 6 shows the transistor I C versus V CE family of curves (at 213 K) of a 450 μm HBLET of another device in accordance with an embodiment of the invention and which can be used in practicing embodiments of the method of the invention.
[0020] FIG. 7 shows, in the curves (a) and (b), respectively, the small signal current gain β ac =ΔI C /ΔI B and current gain β dc =I C /I B for V CB =0 for the device whose I C curves are shown in FIG. 6 .
[0021] FIG. 8 shows (at 213 K) the laser operation (curve (a)) and spontaneous spectrum (curve (b)) power spectra of the transistor laser biased at V CE =2 V and operating at 3 GHz.
[0022] FIG. 9 shows a picture of the transistor laser in operation at 3 GHz, captured using a CCD camera.
[0023] FIG. 10 shows, in traces (a), (b) and (c), respectively, the input signal modulated at 3 GHz, and the corresponding electrical and optical outputs.
[0024] FIG. 11 shows the output collector I-V characteristics of an HBLET. For the base current below laser threshold I bth =0.744 mA, the optical recombination process yields spontaneous emission (low optical output). For base current above laser threshold the optical recombination process is stimulated (higher optical output power).
[0025] FIG. 12 shows a Gummel plot of base current and collector current with Vce=Vbe and Vbc=0V. The current gain beta increases (spontaneous emission), and the beta decreases when laser operation of the HBLET starts, since the recombination process for stimulated emission become “faster”.
[0026] FIGS. 13 ( a ), 13 ( b ), 13 ( c ), and 13 ( d ) show, respectively, the input voltage, output voltage, optical output, and optical power spectrum for a laser transistor device operated in a stimulated emission mode.
[0027] FIGS. 14 ( a ), 14 ( b ), and 14 ( c ), show, respectively, the input voltage, optical output, and optical power spectrum for a laser transistor device operated in a spontaneous emission mode.
[0028] FIGS. 15 ( a ), 15 ( b ), 15 ( c ), and 15 ( d ) show, respectively, the input voltage, output voltage, optical output, and optical power spectrum for a laser transistor device operated in a near-threshold mode.
[0029] FIG. 16 is a schematic diagram of an example of a circuit that can be used to operate a light emitting transistor in accordance with an embodiment of the invention.
[0030] FIG. 17 shows output collector I-V characteristics of an HBLET, and signals that result when operated at different operating points.
[0031] FIG. 18 shows the electrical output for operation at each of the different operating points.
[0032] FIG. 19 shows the optical output for operation at each of the different operating points.
DETAILED DESCRIPTION
[0033] FIG. 1 illustrates a device as set forth in the above-referenced copending application Ser. No. 10/646,457. A substrate 105 has the following layers disposed thereon: subcollector 110 , collector 130 , base 140 , emitter 150 , and cap layer 160 . Also shown are collector metallization (or electrode) 115 , base metallization 145 , and emitter metallization 165 . Collector lead 117 , base lead 147 , and emitter lead 167 are also shown. As described in the referenced copending Application, the collector layer 130 comprises 3000 Angstrom thick n-type GaAs, n=2×10 16 cm −3 , the base layer 140 comprises 600 Angstrom thick p+ carbon-doped compositionally graded InGaAs (1.4% In), p=4.5×10 19 cm 3 , the emitter layer 150 comprises 800 Angstrom thick n-type InGaP, n=5×10 17 cm −3 , and the cap layer comprises 1000 Angstrom thick n+ InGaAs, n=3×10 19 cm 3 .
[0034] As described in the referenced copending Application, for conventional PN junction diode operation, the recombination process is based on both an electron injected from the n-side and a hole injected from the p-side, which in a bimolecular recombination process can be limited in speed. In the case of HBT light emission, the base “hole” concentration is so high that when an electron is injected into the base, it recombines (bimolecular) rapidly. The base current merely re-supplies holes via relaxation to neutralize charge imbalance. For a heterojunction bipolar transistor (HBT), the base current can be classified into seven components, namely: (1) hole injection into the emitter region (i Bp ); (2) surface recombination current in the exposed extrinsic base region (i Bsurf ); (3) base ohmic contact recombination current (i Bcont ); (4) space charge recombination current (i Bscr ); (5) bulk base non-radiative recombination current due to the Hall-Shockley-Reed process (HSR) (i BHSR ); (6) bulk base Auger recombination current (i BAug ); and (7) bulk base radiative recombination current (i Brad ). For a relatively efficient HBT with ledge passivation on any exposed base region, the surface recombination current can be reduced significantly. Hence, the base current and recombination lifetime can be approximated as primarily bulk HSR recombination, the Auger process, and radiative recombination. The base current expressed in the following equation (1) is then related to excess minority carriers, Δn, in the neutral base region, the emitter area, A E , the charge, q, and the base recombination lifetime, τ n as
i B =i BHSR +i BAUG +i Brad =qA E Δn/τ n (1)
The overall base recombination lifetime, τ n , is related to the separate recombination components of Hall-Shockley-Read, τ HSR , Auger, τ AUG , and radiative recombination, τ rad , as
τ n =(1/τ HSR +1/τ AUG +1/τ rad ) −1 (2)
[0035] As further described in the referenced copending Application, the light emission intensity ΔI in the base is proportional to i Brad and is related to the minority carrier electron with the majority hole over the intrinsic carrier concentration, (np−n i 2 ), in the neutral base region and the rate of radiative recombination process, B, set forth in Equation (3) below, where the hole concentration can be approximated as equal to base dopant concentration, N B . The radiative base current expressed in equation (3) is then related to excess minority carriers, Δn, in the neutral base region, and the base recombination lifetime, τ rad as
i Brad =qA E B ( np−n i 2 )= qA E Bnp=qA E Δn ( BN B )= qA E Δn/τ rad (3)
[0036] For a high speed HBT, it is easy to predict that the base recombination lifetime can be less than half of the total response delay time. Hence, the optical recombination process in the base should be at least two times faster than the speed of the HBT. In other words, HBT speed, which can be extremely fast, is limiting.
[0037] In a first illustrated embodiment, a device and data are set forth showing laser operation of an InGaP—GaAs—InGaAs heterojunction bipolar light-emitting transistor (HBLET) with AlGaAs confining layers and an InGaAs recombination quantum well incorporated in the p-type base region. The epitaxial layers of the crystal used for the HBLET laser are shown schematically in FIG. 2 , with a GaAs substrate 210 , a 4000 Å n-type heavily doped GaAs buffer layer 215 , followed by a 600 Å n-type Al 0.40 Ga 0.60 As layer 220 , a 3500 Å n-type Al 0.98 Ga 0.02 As layer 222 , and a 400 Å n-type Al 0.40 Ga 0.60 As layer 224 forming the bottom cladding layers. These layers are followed by a 400 Å n-type sub-collector layer 230 , then a 200 Å In 0.49 Ga 0.51 P etch stop layer (not shown), a 650 Å undoped GaAs collector layer 240 , and a 940 Å p-type GaAs base layer 250 (the active layer), which includes also (in the base region) a 120 Å InGaAs QW (designed for λ≈980 nm). The epitaxial HBLET laser structure was completed with the growth of the upper cladding layers, which included a 1200 Å n-type In 0.49 Ga 0.51 P wide-gap emitter layer 260 , a 300 Å n-type Al 0.70 Ga 0.30 As oxidation buffer layer 270 , a 3500 Å n-type Al 0.98 Ga 0.02 As oxidizable layer 275 (see J. M. Dallesasse, N. Holonyak, Jr., A. R. Sugg, T. A. Richard, and N. El-Zein, Appl. Phys. Lett. 57, 2844 (1990)), and a 1000 Å n-type Al 0.40 Ga 0.60 As layer 280 . Finally, the HBLET laser structure was capped with a 1000 Å heavily doped n-type GaAs contact layer 290 .
[0038] The HBLET laser fabrication was performed by first patterning 6 μm protective SiN 4 stripes on the crystal. The top n-type Al 0.98 Ga 0.02 As oxidizable layer was then exposed by wet etching (1:8:160 H 2 O 2 :H 2 SO 4 :H 2 O) to form a ˜6 μm emitter mesa. Next, a wide 150 μm protective photoresist (PR) stripe was placed over the emitter mesa and the unprotected Al 0.98 Ga 0.02 As layer was completely removed (1:4:80 H 2 O 2 :H 2 SO 4 :H 2 O), revealing the In 0.49 Ga 0.51 P wide-gap emitter layer. The protective PR stripe was then removed and the sample was oxidized for 7.5 min at 425° C. in a furnace supplied with N 2 +H 2 O, resulting in a ˜1.0 μm lateral oxidation which formed ˜4 μm oxide-defined apertures in the 6 μm emitter mesa (see, again, J. M. Dallesasse, N. Holonyak, Jr., A. R. Sugg, T. A. Richard, and N. El-Zein, supra (1990); S. A. Maranowski, A. R. Sugg, E. I. Chen, and N. Holonyak, Jr., Appl. Phys. Lett. 63, 1660 (1993)). The samples were annealed (in N 2 ) at 430° C. for 7 minutes to reactivate p-dopants before the protective SiN 4 was removed by plasma (CF 4 ) etching. A 100 μm PR window was formed over the emitter mesa and oxide layer, and Au—Ge/Au was deposited over the sample to form metal contact. After lift-off of the photoresist (PR) to remove excess metal, the In 0.49 Ga 0.51 P layer was removed using a wet etch (4:1 HCl:H 2 O), exposing the p-type GaAs base layer. An 80 μm wide PR window was then patterned ˜15 μm away from the emitter mesa edge, and Ti—Pt—Au was evaporated for contact to the base. Another lift-off process was then performed to remove excess base contact metal. A 150 μm PR window was then patterned ˜6 μm away from the base contact. The GaAs base and collector layers were removed using a selective etch (4:1 C 6 H 8 O 7 :H 2 O 2 ), and the In 0.49 Ga 0.51 P etch-stop layer was removed by a wet etch (16:15 HCl:H 2 O), exposing the heavily doped n-type GaAs sub-collector layer. Au—Ge/Au metal alloy was evaporated over the sample for contact to the exposed sub-collector layer, and another lift-off process was performed to remove excess metal. The sample was then lapped to a thickness of −75 μm and the contacts annealed. The HBLET samples were cleaved normal to the emitter stripes to form Fabry-Perot facets, and the substrate side of the crystal was alloyed onto Cu heat sinks coated with In.
[0039] A processed, metallized, and cleaved HBLET laser (top view) is shown on the left in FIG. 3 . The contact probes on the emitter (E), base (B), and collector (C) are shown schematically resembling the actual probes (E PRB , B PRB , and C PRB ) on the operating device at the right. The image on the right was obtained with a video CCD detector and shows (hν) the device laser beam (photons) scattered from a Cu platform located slightly lower than the laser crystal, which, as shown, has a −200 μm spacing between the cleaved Fabry-Perot facets. Current and bias voltage (common emitter operation) were provided using a Tektronix Model 370 high resolution curve tracer connected to the HBLET by the three probes labeled E PRB , B PRB , and C PRB in FIG. 3 . The HBLET laser was operated ˜200 K in a dry N 2 environment.
[0040] The transistor I-V curves of another HBLET laser with ˜260 μm spacing between the Fabry-Perot facets are shown in FIG. 4 . As the base current, I b , is increased in 2 mA intervals from 0 to 8 mA, the usual increase of differential current gain is observed, β=ΔI c /ΔI b , in this case from β˜2 at lower current to 6.5 at higher current. Light versus V CE measurements (I b constant, data not shown) indicate that radiative recombination improves as V CE increases and then decreases at the onset of reverse breakdown. Near I b =8 mA, and as V CE is increased, however, stimulated recombination (stimulated emission) becomes significant, and the HBLET operates both as a laser and a transistor but with a distinct decrease in the current gain β. Beyond threshold, I b equal to or greater than I th ˜8 mA, the differential gain β decreases from 6.5 to a nearly constant value of 2.5 (α=β/(β+1)=I c /I e =0.71). Since β can be approximated as the simple ratio τ n /τ t (see B. G. Streetman and S. Banerjee, Solid State Electronic Devices, 5 th ed. (Pearson, N.J., 2004), p. 328), where τ t is the average (carrier) base transit time (which is almost the same below and above threshold) and τ n is the average electron lifetime in the base, the electron lifetime is reduced by a factor of 2.6 because of the stimulated recombination of the carriers collected in the 120-Å QW. The QW operates as a unique pseudo-collector (see E. A. Rezek, H. Shichijo, B. A. Vojak, and N. Holonyak, Jr., Appl. Phys. Lett. 31, 534 (1977)), and can be adjusted to govern the base recombination and thus both the optical output and transistor gain (β). It can be noted for comparison that at room temperature there was observed (data not shown) a differential current gain β of 10 at I b =2 mA and 30 at 8 mA (or current transfer ratio, α=I x /I e of 0.91 and 0.96).
[0041] FIG. 5 shows, in quasi-continuous operation (88% duty cycle at 60 Hz), the recombination radiation spectra of the HBLET device of FIG. 3 , but with slightly increased voltage bias V CE to increase the reverse bias on the base-collector junction. At (a) I b =6 mA, the HBLET recombination radiation exhibits a peak wavelength of 954 nm and a spectral width of ˜280 Å. At (b) I b =8 mA, the onset of stimulated emission can be seen with distinct spectral narrowing and mode development. At (c) I b =10 mA the laser modes are fully developed (λ=958 nm), clearly indicating transistor laser operation, which is evident also in FIG. 3 . It can be noted that the 200 μm long HBLET laser of FIG. 3 (right side) was operated with pulsed base current (1% duty cycle at 1 MHz) to prevent saturation of the Si-CCD viewing camera.
[0042] The described results demonstrate that an HBLET, suitably modified with a resonator cavity and a recombination QW (or QWs) in the p-type base (a pseudo-collector, a second collector), can be operated simultaneously as a laser and transistor with gain β=ΔI c /ΔI b >1. At laser threshold the transistor gain decreases sharply, but still supports three-port operation (electrical input, electrical output, and optical output).
[0043] In the description of the foregoing embodiment, it is shown that a heterojunction bipolar light emitting transistor (HBLET) having certain features, can support stimulated recombination and laser operation. In the following further embodiment, a three-port transistor laser, having certain features, exhibits microwave operation and optical modulation. In this embodiment, the epitaxial layers of the crystal used for the HBLET laser include of a 100 Å n-type heavily doped GaAs buffer layer, followed by a 630 Å n-type Al 0.40 Ga 0.60 As layer, a 4000 Å n-type Al 0.98 Ga 0.02 As layer, and a 250 Å n-type Al 0.40 Ga 0.60 As layer forming the bottom cladding layers. These layers are followed by a 300 Å n-type sub-collector layer, then a 150 Å In 0.49 Ga 0.51 P etch stop layer, a 600 Å undoped GaAs collector layer, and a 850 Å p-type GaAs base layer, which includes also (in the base region) a 120 Å InGaAs QW (designed for λ≈980 nm). The epitaxial HBLET laser structure is completed with the growth of the upper cladding layers, which include a 600 Å n-type In 0.49 Ga 0.51 P wide-gap emitter layer, a 50 Å n-type GaAs buffer layer, a 200 Å n-type Al 0.35 Ga 0.65 As oxidation buffer layer, a 200 Å n-type Al 0.80 Ga 0.20 As oxidation buffer layer, a 4000 Å n-type Al 0.95 Ga 0.05 As oxidizable layer, a 300 Å n-type Al 0.80 Ga 0.20 As layer, and a 500 Å n-type Al 0.35 Ga 0.65 As layer. Finally, the HBLET laser structure is capped with a 1000 Å heavily doped n-type GaAs contact layer.
[0044] The HBLET laser fabrication was performed by first patterning 8 μm protective SiN 4 stripes on the crystal. The top n-type Al 0.98 Ga 0.02 As oxidizable layer was then exposed by wet etching (1:8:160 H 2 O 2 :H 2 SO 4 :H 2 O) to form a ˜6 μm emitter mesa. Next, 10 μm and 50 μm (40 μm apart) photoresist (PR) windows were formed with the emitter mesa placed between the two windows and ˜5 μm away from the 10 μm window. The unprotected Al 0.98 Ga 0.02 As layer was then completely removed (1:4:80 H 2 O 2 :H 2 SO 4 :H 2 O), revealing the In 0.49 Ga 0.51 P wide-gap emitter layer. The protective PR stripe was dissolved and the sample was oxidized for 6.5 min at 425° C. in a furnace supplied with N 2 +H 2 O, resulting in ˜1.0 μm lateral oxidation which forms ˜4 μm oxide-defined apertures in the 6 μm emitter mesa. (Again, see J. M. Dallesasse, N. Holonyak, Jr., A. R. Sugg, T. A. Richard, and N. El-Zein, Appl. Phys. Lett. 57, 2844 (1990); S. A. Maranowski, A. R. Sugg, E. I. Chen, and N. Holonyak, Jr., Appl. Phys. Lett. 63, 1660 (1993)). The samples were annealed (in N 2 ) at 430° C. for 6.5 minutes to reactivate p-dopants before the protective SiN 4 is removed by plasma (CF 4 ) etching. The remaining InGaP emitter was selectively etched using HCl. The base-collector contact layers were then exposed by a selective wet etch (4:1 C 6 H 8 O 7 :H 2 O 2 ) for GaAs and InGaAs, and HCl for In 0.49 Ga 0.51 P. Then, a 50 μm PR window was formed over the 10 μm base contact window and the oxidized Al 0.98 Ga 0.02 As layer. A 1 μm thick Pd—Pt—Au p-type ohmic contact was deposited on top of the partially exposed base layer to form the base metal contact (followed by a lift-off process). Next, 30 μm and 50 μm (5 μm apart) PR windows were opened for the emitter and collector metal contact deposition, and 1 μm thick n-type contact AuGe—Ni—Au metal alloy was deposited on the crystal and another lift-off process was performed to remove excess metal. The sample was then lapped to a thickness of ˜100 μm and annealed. The HBLET samples were cleaved normal to the emitter stripes to form Fabry-Perot facets, and the substrate side of the crystal was alloyed onto Cu heat sinks coated with indium.
[0045] The transistor I C versus V CE family of curves (at 213 K) of a 450 μm HBLET of this embodiment is shown in FIG. 6 . As the base current I B is increased in 2.5 mA intervals from 0 to 15 mA, the current gain (β dc =I C /I B ) increases to −5.65 for I B ≦I th and then decreases to −4.5 for I B ≧I th . At I B =7.5 mA one observes in FIG. 6 a negative slope in the differential or small signal γ (γ ac =ΔI c /ΔI B ) associated with a transistor in laser operation, as described in conjunction with the previous embodiment. The transistor's V BE curve is superimposed on the family of I C versus V CE curves to indicate the zero base-collector bias point, the boundary V CB =0. From FIG. 6 and by observing the gain characteristic, it can be seen that the transistor operates as a laser over a wide range of V CE (beyond V CB =0). Light versus base current measurements (data not shown) indicate small variation in laser light intensity when the transistor operates in the saturation mode (constant I C ), and decreases at high reverse bias and the onset of heating.
[0046] A novel technique is used for determining the threshold current of a transistor laser that is based on the electrical gain of the transistor. This eliminates the need to have an additional external feedback system (photodetector) to verify that the device is operating as a laser. The small signal current gain β ac =ΔI C /ΔI B and current gain β dc =I C /I B for V CB =0 are shown by curves (a) and (b) of FIG. 7 . From curve (a) it can be observed that the small signal gain increases as I B increases and decreases sharply at the onset of stimulated emission, or for amplified spontaneous emission (I B =6.7 mA, β ac =8.6). The peak of curve (b) in FIG. 7 can be defined as the threshold current of the transistor laser (I B =I th =7.4 mA). The transistor laser operation is fully developed when β ac reaches a minimum (β ac =3.7) at I B ≈7.9 mA. This method of threshold current measurement is verified by comparison with standard light versus intensity (L-I) measurements (data not shown) and from visual observation of the laser diffraction pattern using an infrared CCD camera. It is consistent also with spectral narrowing.
[0047] FIG. 8 shows (at 213 K) the laser operation (curve (a)) and spontaneous spectrum (curve (b)) of the transistor laser of the present embodiment biased at V CE =2 V and operating at 3 GHz. The input voltage waveform is generated using a clock signal from an HP70841A pattern generator which has a maximum clock signal of 3 GHz. The output measurements were made using an HP70951 B optical spectrum analyzer. A maximum power level of −63.4 dBm was measured at λ=966.5 nm for the spontaneous emission, and for laser operation a power output of −21.44 dBm (λ=964.4 nm). The small output power of the transistor laser was attributed to weak fiber coupling. Additional free space measurements have yielded powers at least 8 times greater. A picture of the transistor laser in operation at 3 GHz, captured using a CCD camera, is shown in FIG. 9 . The light emission from the front Fabry-Perot facet was coupled (upward in FIG. 9 ) into the optical fiber, which was connected directly into the input of the optical spectrum analyzer.
[0048] A signal generator, a wideband detector, a power meter and a digital oscilloscope were used for the three-port (electrical input, electrical output and optical output) direct modulation characterization of the transistor laser. A cold station equipped with a pair of 40 GHz ground-signal microwave probes was used to enable measurements at 213 K. The HBLET, with ˜450 μm spacing between the Fabry-Perot facets, was biased in the normal operating mode (V CE =2 V and I B =9 mA), and a small signal sinusoidal voltage waveform with a peak-to-peak amplitude of 0.75 V was supplied to the base (input port) of the device. The input voltage waveform was generated using a clock signal from the HP70841A pattern generator (maximum clock signal of 3 GHz), and the electrical output collector-emitter voltage waveform was measured using a 20 GHz digital sampling oscilloscope. The complementary output of the input waveform clock signal was measured at a second separate channel of the oscilloscope. The output of the transistor laser was coupled into a multimode fiber probe with a core diameter of 25 μm. The laser signal was fed into a high-speed (10 Gb/s) wideband (400 to 1700 nm) InGaAs detector. The detector output voltage, base input voltage, and collector output voltage were all displayed simultaneously on a four channel sampling oscilloscope. The input signal modulated at 3 GHz (top trace) and the corresponding electrical and optical outputs are shown in FIGS. 10 ( a ), (b) and (c), respectively. When the 3 GHz base current is held (decreased) below the threshold current, the optical output waveform was not observed, making evident, in contrast, that stimulated emission defines a much stronger laser output signal.
[0049] In accordance with an embodiment of the invention, a device and technique are set forth for high speed optical signal generation with an enhanced signal to noise ratio and control of “on” and “off” time durations utilizing the stimulated emission process for the “on” state and spontaneous emission process for the “off” state. The operating point and excitation of the transistor laser are selected to obtain cycles that each have an “on” portion of stimulated emission (laser optical output, and electrical signal output) and an “off” portion of spontaneous emission (without optical output, and electrical noise).
[0050] The transistor I-V curves of an HBLET laser with ˜450 μm spacing between the Fabry-Perot facets are shown in FIG. 11 . At a base current I b =0.744 mA, the HBLET reaches laser threshold and changes transistor gain, β=DI c /dI b , from β=5.5 to 4.5 or (α=1/(β+1)=0.85→0.81). As above noted, an HBLET transistor laser has an important feature in the I-V curves in the transition from spontaneous emission to stimulated emission. FIG. 12 shows a Gummel plot of base current and collector current with Vce=Vbe and Vbc=0V. The current gain beta increases (spontaneous emission), and the beta decreases when laser operation of the HBLET starts, since the recombination process for stimulated emission become “faster”.
[0051] Experiments were conducted on the transistor laser in the common emitter configuration with 3 GHz modulation of the electrical input (controllable in frequency and amplitude) at the base terminal of the device.
[0052] A mode of operation termed a stimulated emission mode had, for example, the following initial operating parameters: V be =1.67 V, V ce =2 V, I b =16 mA and I c =69.2 mA. As expected, in the stimulated emission mode (i.e., with the input consistently at a level above the threshold for stimulated emission), the electrical input and output, and the optical output as shown in graphs 13 ( a ), 13 ( b ), and 13 ( c ), respectively, of FIG. 11 , are similar to the corresponding graphs 10 ( a ), 10 ( b ) and 10 ( c ) of FIG. 10 for a similar device, and the graph 13 ( d ) of the laser power spectrum is similar to the corresponding graph of FIG. 8 for the similar device.
[0053] A mode of operation termed a spontaneous emission mode had, for example, the following initial operating parameters: V be =1.47 V, V ce =2 V, I b =5 mA, and I c =19.84 mA. The graphs of FIG. 14 show results for the spontaneous emission mode (i.e., with the input consistently at a level below the threshold for stimulated emission), the graph 14 ( a ) showing the sinusoidal electrical input, the graph 14 ( b ) showing the optical signal output, which is seen to be background noise characteristic of spontaneous emission, and the graph 14 ( c ) showing the optical output power spectrum of the spontaneous emission mode.
[0054] A mode of operation termed a near-threshold mode had, for example, the following initial operating parameters: V be =1.57 V, V ce =2 V, I b =10 mA, and I c =46.2 mA. The graphs of FIG. 15 show results for the near-threshold mode (i.e., with each cycle of the sinusoidal input signal having an “on” portion during which the base current exceeds the threshold for stimulated emission, and an “off” portion during which the base current is below the threshold for stimulated emission). The graphs 15 ( a ) and 15 ( b ) again show, respectively, the electrical input and output signals. The graph 15 ( c ) shows the optical output, which is seen to have a stimulated emission laser pulse (during the part of the cycle when the base threshold current is exceeded) and spontaneous emission (during the part of the cycle when the base threshold current is not exceeded). In this case, for the 3 GHz input signal (which, it is evident, can be readily exceeded, within the capability of the present device, with better test equipment), the laser pulses, for the conditions set forth, have a half-power pulse width of less than about 100 picoseconds. By adjusting the relative signal amplitude (e.g. by controlling bias and/or the AC signal amplitude and/or load), the pulse width can be advantageously controlled. The graph 15 ( d ) shows the optical output power spectrum for this case.
[0055] FIG. 16 is a diagram of an example of a circuit that can be used to operate the light emitting transistor (LET) 1610 , under various conditions, including conditions employed in examples of embodiments hereof. In this example, a controllable oscillator 1615 is coupled to the base terminal of the LET via a bias tee 1620 , and the middle branch of the bias tee 1620 is coupled to a controllable bias voltage V BE . The emitter terminal is coupled to ground reference potential and the collector terminal is coupled, via a bias tee 1640 , to a variable load resistor 1660 . The middle branch of the bias tee 1640 is coupled to controllable bias potential V CE .
[0056] The graph of FIG. 17 , which also illustrates exemplary electrical input (above the graph), electrical output (below the graph), and optical output (on the right side of the graph), shows how three different output DC bias conditions can be used to generate optical outputs with controllable pulse widths. FIGS. 19 and 20 respectively show the three electrical and optical outputs, for the three respective operating points, plotted together.
|
A method for producing controllable light pulses includes the following steps: providing a heterojunction bipolar transistor structure including collector, base, and emitter regions of semiconductor materials; providing an optical resonant cavity enclosing at least a portion of the transistor structure; and coupling electrical signals with respect to the collector, base, and emitter regions, to switch back and forth between a stimulated emission mode that produces output laser pulses and a spontaneous emission mode. In a form of the method, the electrical signals include an AC excitation signal, and part of each excitation signal cycle is operative to produce stimulated emission, and another part of each excitation signal cycle is operative to produce spontaneous emission.
| 7
|
CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of U.S. patent application Ser. No. 835,462, filed Mar. 3, 1986 for DEVICE FOR TREATMENT OF CUTTING TOOLS, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention has a relation to treatment of materials utilizing magnetic fields.
2. Description of the Prior Art
Magnetization and the effect of magnetic fields has been explored in various applications. However, up to now treatment for increasing the life of metal parts including cutting tools has not be advanced. Stresses can be caused by many factors, such as welding, heat treating, forming or sharpening. For example, machine tools that have been sharpened will have internal stresses on their edges which start breaks or chips. Previously items were annealed or otherwise treated for stress relief, but not using magnetic fields.
SUMMARY OF THE INVENTION
The present invention relates to an apparatus and method of treating magnetic field affected objects and materials, for example ferromagnetic parts and materials and material containing ferro magnetic components such as machine tool bits to prolong life by subjecting the material to a magnetic field during a selected time cycle to redistribute stresses to reduce highly stressed areas.
The magnetic field through the material such as a tool provides relief of the stresses from sharpening, increases strength and surface hardness, decreases the coefficient of friction on the surfaces that are so treated, provides an increase in the modulus of elasticity, strength and wear resistance and in certain types of metals, provides a change in the surface concentration of such alloying metals such as wolfram, molybdenum, and tungsten, as well as oxygen and carbon.
The structure comprises a coil into which the part or material to be treated is inserted, and a controlled source of electrical power that generates a magnetic field on the interior of the coil for achieving the desired results.
It has been determined that magnetic treatment of ferromagnetic materials, even at room temperature, affects mechanical and service properties of piece parts, including machine tool bits, as well as other products. Magnetic treatment is used for new, enhanced methods for non-cutting tool applications. In metals, the magnetic domain walls have a barrier action on movement of dislocations in the material. Intense change in the magnetic pressure causes the domain walls to move at room temperature, and such fluctuation of the domain walls results in a type of a "relay race" rearrangement of dislocations and microstresses from local overstressed areas to neighboring areas of the part. This results in more uniform distribution of internal stresses in various parts. The result of treatment can be considered to be equivalent to partial thermal stress relief (recovery), tempering or aging. Microstresses also can be created by magnetic treatment.
By proper programming, generally at programed cycles that are arrived at as shown in this application, and by using the appropriate frequency, amplitude and density of pulsing magnetic field, the treating of powdered metal materials and metal consisting composition both prior to green forming, in the green formed state and both during and after sintering, both in the process and after heat treating of sintered parts, both in the process and after sizing, forging, recompacting, shaping of sintered or half sintered parts, it is possible to reduce internal stresses, and improve compactability (which makes it possible to press more sophisticated shapes and more dense parts) and to decrease the spring-back effect. Prior to green forming, magnetic treatment improves homogenity of powder particles (for example in a process of the atomization of powder) and reduces cold working (for example, after milling). In green compacts of powdered materials, magnetic treatment decreases non-uniformity of density, reduces cold working, reduces residual stress, non-uniformity of stress and reduces the required compacting pressure. In the sintered parts magnetic treatment relieves and redistributes cold working and residual stresses.
By decreasing the spring-back effect in green powdered metal compacts and reducing crack propagation. Both in green compacts and sintered parts it is possible to obtain a more uniform distribution of internal stresses and thus better life and better operation of the part.
Additionally, magnetically treating heat treated parts, such as machine tool bits and other heat treated parts, prolongs the useful life of the part by subjecting the part, such as a tool bit, to a magnetic field during a selected time cycle to redistribute stresses and to reduce stress in highly stressed areas.
It is apparent that the pulsing magnetic field that is useful for machine tool stress reducing also can be used in other stress reducing applications such as welding, brazing and soldering to prevent distortion and/or cracking of the parts that are subjected to these processes. The magnetic field can be applied before, during or after joining, or during all three times. Material subjected to magnetic treatment before welding, or other joining operations involving heat has better weldability or ability to be joined because of lower residual stresses. Treatment during the process of welding, soldering or brazing increases the amount of grain nucleus, improves the diffusion processes, limits the growth of grains, and relieves the stress between joints.
Magnetic treatment of cold welded parts, or parts which are in the process of cooling, decreases the level of residual stresses.
Machine tool treatment aids in reducing of stress in the tools and treating the part helps machinery. For example, treating ferrites and similar brittle, ferromagnetic materials with a magnetic field reduces the problems of chipping of the ferrite in areas where the tool enters and exits, which are the regions where the dynamic input of a grinding tool, for example, is most significant.
Further, deep drawing metal also involves substantial stresses in both the tools and the work piece, and proper magnetic treatment during the deep drawing operation with a magnetic field that passes through the work piece keeps the stress levels low and aids greatly in reducing fractures and damaged and lost parts.
It does become apparent that treatment of tools and/or parts during machining and/or heat treating, cooling and other normally conducted material treatment reduces the distortions due to residual stresses, and will reduce cracking of castings or powdered metal materials, as well. The same is true if bending, twisting or truing operations are being carried out, and doing this in the presence of a magnetic field.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective representation of a device made according to the present invention showing a tool holding tray in position within an inductive coil;
FIG. 2 is a vertical sectional view of the device of FIG. 1 taken on line 2--2 in FIG. 1;
FIG. 3 is a sectional view taken on line 3--3 in FIG. 1;
FIGS. 4A to 4D are schematic representations of typical power cycle time lines that have been found useful with the present device;
FIG. 5 is a cross sectional view of a modified part holder used with the device of the present invention;
FIG. 6 is a schematic representation of typical controller that can be used for providing varying power levels and timing of power to the device of the present invention;
FIG. 7 is a schematic representation of a SCR power control used with the present invention;
FIG. 8 is a schematic representation of a typical drill bit in use with a work piece, and showing magnetic field producing means surrounding the drill bit itself, and also the work piece to provide magnetic fields during operation;
FIG. 9 is a schematic representation of a different form of magnetic field generating means for a rotating part that is being machined, or ground, wherein the part can be treated as it is being machined;
FIG. 10 is a schematic representation of a rotating part held in a schematically shown chuck and which is rotated between separate electromagnets supported adjacent one end of the part, and showing a grinding wheel schematically in position for grinding the parts;
FIG. 11 is a further modified form of a magnetic field generating means schematically shown to show the treatment of a ring type part;
FIG. 12 is a schematic representation of a magnetic treatment for tools and parts during a deep draw operation;
FIG. 13 is a schematic representation of a wire die showing magnetic field generating means built into the die for treating the wire as it is being formed, and also prior to formation;
FIG. 14 is a schematic flow diagram of treating powdered metal parts, including prior to formation, as a green compact of a part, and after sintering;
FIG. 15 is a schematic representation of magnetically treating a large gun barrel; and
FIG. 16 us a schematic representation of various magnetic field signals useful for treatment according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A material treatment device made according to the present invention is indicated generally at 10 and comprises a frame 11, on which a coil assembly 12 is mounted. The coil assembly 12 as shown has a central core 14 and end flanges 15. A coil 16 of suitable wire, and having the necessary number of turns is wound on core 14 between flanges 15. The coil 16 is connected to a power source 20 that provides a reversing DC voltage and thus, current, to the coil at a desired level and frequency, through a control shown at 21. The parameters can be varied through the use of the controller 21. The power source preferrably has a SCR controlled output and the controller that permits the application of power at a desired frequency, average voltage level and duration.
The core 14 has an internal opening 25, in which a tool holding drawer 26 is mounted. The drawer 26 can be of any desired configuration, but generally is of nonmagnetic material, so that the magnetic field generated by the coil will pass through a tool or other material indicated at 30. The tool 30 shown is a tool that has recently been sharpened, and may have internal stresses.
The controller 21 is operated to provide a power cycle through the coil, to create a magnetic field through the tool, and this magnetic field, depending on the number of cycles, the length of pauses between cycles, if the cycles are repeated, and the amplitude or power of the magnetic field, will be used to treat the tool. The cycle length is usually about 15 seconds up to 50 seconds, but the waveform can be varied within the cycle time in order to obtain the desired results. Experimentation for particular tool size and material can be carried out for typical applications.
Referring to FIGS. 4A-4D, the plots of typical types of magnetization cycles are shown.
In FIG. 4A, the power cycles or magnetic field cycles shown at 40 are of relatively low magnitude (time is to the right and voltage level, and thus current, since E=IR, is vertical), relatively high frequency, and of a continuous duration for the time t 1 . This will provide a steady state magnetization, at a relatively low level for the part.
In FIG. 4B, a different type of cycle is shown. Again, voltage is on the vertical scale with the line 41 being zero, and the cycles below the line indicating a reversal of power. In this instance, the frequency is reduced, and the first cycle indicated at 42 is only of two half cycles for a time t 2 , then there is a pause for a time indicated at T 3 , another reversal of power cycle 43 is shown. Finally, if desired a third cycle 44 can be identical to that shown at 42. The pause time t 3 would be repeated between cycles 43 and 44.
In FIG. 4C, a higher frequency cycle is shown at 45, with a cycle time t 4 and a longer pause time t 5 between the reversal of cycles when the reverse cycles 46 are used. After an additional pause time t 5 , an identical cycle indicated at 48 is applied. FIG. 4D shows another variation, where the power is of higher frequency as indicated at 50 and the on time is t 6 . The pause time t 7 is of less duration, and the same number of cycles are repeated at 51 and 52, without any reversal of magnetic field. Further, the time t 8 can be different than the time t 7 . The time for applying cycles 51 or 52 may also be different from the time of cycle 50.
It should be noted that preferably the drawer or tray 26 is of nonmagnetic material, but preferably heat conducting. Bronze material has been found acceptable and as shown in FIG. 5, the tray indicated there at 60 can be modified to include an opening 61 at one end that receives a tool 62 and a set screw 63 threaded into the outer end member of the tray can be used to tightly clamp the tool 62 in place so that when the magnetic field is applied, the tool may be bent slightly or changed in position, as indicated in exaggerated form by the dotted lines in FIG. 5. Magnetic bending of materials in sufficiently powerful magnetic fields is known. However, treating a machine tool bit as shown, has not been used for relieving stresses as a function of and directly related to magnetostrictive forces.
FIG. 6 shows a typical timer and sequencing circuit that can be varied for forwarding signals to the gates of silicon controlled rectifiers for providing power. SCR controllers are well known, and any desired controller may be used. Many commercial controllers provide adjustable timing of on-off cycles, frequency and voltage outputs that can be used to supply current to the coil 16.
Power source 20 provides an output along lines 70 and 71, respectively (usually 28 volts AC). A logic power supply indicated at 72 is used for providing a five volt DC output along a line 73 for the logic circuits that are used. A one half of a zero crossing detector circuit CD4093 indicated at 75 is provided to provide output along line 76 each time the input power crosses zero, and output signal is fed to a phase locked loop circuit, for example integrated circuit CD4046, indicated at 77. The output signal from the circuit 77 along line 78 is provided at 128 times line frequency in the form shown, to provide an adequate range of control frequencies. The output frequency signal is provided to the clock input of counter 82, which is a CD4040B counter. Counts are provided along a clock frequency line 83 from counter 84, which is 64 times the line frequency to the clock input of a latch circuit 84, type LS174. Five output signals at different frequencies (32, 16, 8, 4 and 2 times line frequency) are provided to a ROM indicated at 85 (a 2764 ROM is suitable) along a bus 83A. The ROM provides control signals along a six line bus 85A to the latch 84. A second counter 90 is provided with a start signal from a cycle control circuit which is one-half of a CD4093 circuit indicated at 91. The start switch (part of cycle control switch indicated at 91A) is manually set to provide the start signal on line 92. The clock input counter 90 is connected to a phase locked line 90A that is at input line frequency. The outputs from the second counter 90 are fed to a second ROM 94. The bus 90B has 10 lines and provides counts of 1, 2, 4, etc. The input sequence select switch 95 is set (four sequences as shown in FIGS. 4A-4D typically are provided), to control the frequency of the output and the number and length of pauses and power on cycles that are to be provided.
The output of the ROM 94 are provided to the input of ROM 85, which is programmed to provide the output signals on bus 85A to the latch 84. The output of the latch goes to the 7406 circuit 97 comprising the SCR drivers 97. The outputs along a bus 98 goes to the gates of four SCR's used in a conventional manner to provide the output configurations as shown in FIGS. 4A-4D.
The ROM's can be programmed in a known manner to select which SCR is triggered and the frequency at which they are triggered, so that various power configurations can be achieved.
One type of SCR arrangement is shown in FIG. 7, schematically, and as each of the signals is provided along the bus 98, the signals to the gates of the respective silicon controlled rectifiers shown at 101, 102, 103 and 104 will provide for conduction of power to or from a line 105 that leads to one end of the coil 16. The power is from a 24 volt transformer indicated at 110. The center tap is along a line 112 leading to the opposite end of the coil 16 and by the proper sequencing of the gates in a normal known manner the cycling of the current to the coil can be obtained. The transformer can provide power to lines 70 and 71 as well.
The nominal 24 volt power is controlled by the SCR's in time duration so that basically a reversing, DC level of approximately 12 volts (rms) is provided through the coil 16. The current is of course proportional to the coil resistance and input voltage. The timing of the control current through its complete cycle until the "complete" signal is received along a "cycle done" line 99 back to the cycle control 91 will range from 15 to 50 seconds.
It should be noted also that the cycle control 91 can provide a shut off button through the manual control switches 91A so that a disable signal along 91B is provided to the latch 84 to prevent output power from being provided when the operator decides it is necessary.
Pulse durations provided from the SCR's can range from about 16 milliseconds, to about 120 milliseconds. Because the ROMs can be programmed, various settings and cycles for operating the latch 84 and thus sequencing the signals to the gates of the SCR's can be made. Additionally, as shown in FIGS. 4A-4D there is a degausing or demagnetization portion to the cycle, and this is represented by the vertical lines at the right end of each cycle. The SCR's can be controlled to reduce the voltage (and thus current) amplitude and also reverse the direction of the voltage and current, to provide the demagnetization if desired. Commercial degausing circuits are also available at the present time. The tool can be removed from the tray and then demagnetized as desired.
The size of the tool has a significant impact on the length of and type of power cycle chosen. For example, in general a one-quarter inch steel bit can be cycled at the sequence shown in FIG. 4A, for about three seconds, or one-fifth of a 15 second cycle time. It would receive a steady magnetization, and then could be degaused by reversing the direction of current, and decreasing the current to zero during the short degausing cycle.
It has been shown that when steel is magnetized, its modulus of elasticity is raised, and thus it becomes more rigid. This provides for less likelihood of deflections and provides for increased machining efficiency as well as longer tool life. Therefore, the present invention comtemplates leaving tools magnetized after the treatment for stress relief. Such tools would be for cutting non-magnetic materials, such as plastics or non-ferrous metals. When a magnetized tool is used with magnetic materials, the chips will cling to the tool.
By of example, a coil core having a two and one-half inch internal diameter has been wound with 600 turns of No. 11 square wire, and powered with about 12 volts rms, pulsing DC, through the SCR's to provide current that forms an adequate magnetic field for magnetization treatment of machine tool bits up to about two inches in diameter.
The term "machine tool bit" as used herein means a drill bit, a cutting tool for a lathe, or other tools that are to be used for working on parts for removing material from the part.
Stresses in such cutting tools are caused by contacting with machined material and sharpening or resharpening the tools in an uncontrolled atmosphere, and in particular, the thin edge of the tool is often overheated in spots. This heating is usually accompanied by overstress.
Wearing, cracking or chipping of the cutting edge as a rule starts in the area of the overstress, and by redistribution of the stress (making it more uniform or decreasing it), the tool life can be increased significantly. While stress relief is known by way of heat treatment in an oven, mechanical vibration, cryogenic treatment, or laser or annealing, the present device uses magnetostriction, by generating a magnetic field through the magnetic material of the cutting tool. This can be used for ferrous materials, crystals and component materials. The tool is subjected to multi-directional forces during magnetostriction treatment or the magnetic treatment process of the present invention, and this provides for stresses along the surface, and most importantly along the cutting edge.
Since the stresses are a function of magnetization, which in turn is a function of the applied magnetic field and that in turn is a function of the current in the coil being used, the magnetization and the relieving stresses can be controlled by monitoring the voltage level applied to the coil and by regulating the timing of the field as to intensity, duration and frequency.
Variability of the field as described is to accomodate a variety of different tools. Generally speaking, the larger the tool the longer the treatment time that is required, and the greater current that would be applied.
In regard to the device shown in FIG. 5, the bending action is achieved by placing the tool at a location other than the axis of a coil, and then holding it securely. This means that the tray head portion where the set screw is mounted has to fit on the interior of the coil tightly, so it will not shift. It, too, can be clamped tightly in place if desired.
It is to be understood that the controls previously shown in FIGS. 1-7, can be utilized with any of the following applications of the magnetic treating apparatus, wherein the benefits have been recognized as providing stress relief in metal and metal consisting objects.
In FIG. 8, a cutting tool comprising a drill bit shown at 120 is mounted in a chuck 121 of a drill head 122, and when powered, the drill is rotated and is used for drilling holes in a work piece 123 that, as shown schematically, is supported in position below the bit.
Treatment of the drill bit may be achieved by providing a magnetic coil 125 that surrounds the drill bit in its path so that the drill is subjected to a magnetic field when the drill is retracted as shown in FIG. 8, and also during the period of time that the drill operates in the work piece.
Thus, the benefits of stress relief in the drill bit are actually achieved during operation of the drill bit. Further, the part 123 itself, which can be of suitable metal, is positioned within a ring type coil 127 that provides a magnetic field through the work piece of suitable intensity or duration, or even a pulsating field as previously described may be used to help in reducing the stresses in the work piece during the drilling operations (or other machining operations).
As was previously pointed out, this treatment of the machine tool bit increases the tool life, maintains the sharpness for a longer period of time, and prevents unnecessary down time.
Another method of treating the part 123, particularly if it is a part such as a ferrite or similar brittle ferromagnetic material can be achieved with a permanent magnet or an electromagnet used to hold the part. The piece part support indicated generally at 130 is made up of a strong permanent or electromagnet, which will not only hold the piece part 123 in position, but also will provide a magnetic field that is applied before, during and after the machining operations. The magnetic field is maintained at a high enough level throughout the machining to ensure that the part does not slip or move. This greatly enhances the machineability of ferrites and other brittle materials. A magnetic field being applied to the part during work ensures that stresses are kept at a minimum.
FIG. 9 is a modified form of the invention, comprising a yoke 133 that has a north magnetic pole 134, spaced from a south magnetic pole 135, and which yoke can be provided with a coil 136 connected to a power supply 136A for providing the magnetic field. The spaced apart poles 135 and 136 permit positioning a rotating piece part 137 therebetween, so that a magnetic field is applied as the piece part 137 rotates under control of a motor 138 that rotates a support shaft 139, for example, in the direction shown by the arrow 140. A grinding wheel or similar tool (for example, saws for cutting stones or concretes) can be used on the surface or periphery of the work piece 137 at the same time the work piece is rotated, and the work piece thus is subjected to a magnetic field while it is being worked on to minimize the problems from internal stresses and make the stresses uniform. For powdered metal parts, the presence of a magnetic field reduces the chipping or breakage during operation of the machine tool.
In FIG. 10, a further modified form of the invention is shown, wherein a chuck or other tool holding part 142 is holding a cylindrical part 144 that will be rotated about the longitudinal axis 145 of the chuck and the part. A grinding wheel 147 is provided to engage the outer surface of the part and is driven with a motor 148 at the same time that part 144 is rotated. In order to aid this type of operation, again when the part is a brittle material, a pair of spaced apart pole pieces 150 and 151, which have coils 152 and 153 thereon can be provided for forming north and south magnetic poles on opposite sides of the part 144 to form a magnetic field that treats the part. A suitable power source is used for the coils to obtain the desired magnetic field. If there is movement of the part along the axis in the direction that is indicated by the arrow 155, the introductory ends of the part will be treated with a magnetic field as it is introduced into the grinding tool, and this ensures that any tendancy for fracture or clipping of the part is minimized.
FIG. 11 shows a cup shaped magnet which can be used for treating toroidal parts, either for stress relief after heat treatment or for other types of treatment, for example, after welding, brazing or soldering; and this cup shaped magnet 160 has a peripheral wall having an edge 161 that comprises a north pole, and a center piece 162 that comprises a south pole. A toroidal or annular part 163 can be slipped into the cup portion and supported in suitable supports 164 for subjection to a magnetic field. If desired, suitable coils such as that at 165 can be used for enhancing the magnetic field as desired. This type of arrangement can be used easily with parts that are already formed, and can be adapted for supporting parts that are being worked on with machine tools, as well.
In FIG. 12, a deep drawing die 175 is shown, and includes a die base 176, and a die 177 that is supported on the base. The die 177 has a central opening 178 into which a work piece, comprising a flat metal blank 180 is formed with a punch 181 in a conventional manner. The part is held at its periphery, and is drawn into the die opening 178 for forming into a cup for example. A magnet coil 182 can be provided around the die base to provide a magnetic field that will affect (act on) the work piece 180 when it is positioned on top of the die base, and will also provide a magnetic field through the die 177 and the work piece as it is being formed to keep stresses to a minimum in the die 177. Also another coil can be added to treat the die 177 and punch 181 in the process if application to reduce stresses. The coil 182 can be located where desired.
FIG. 13 shows a similar device schematically for a wire drawing die wherein a die 190 has a draw opening 191 therein, through which a wire 192 can be drawn in a suitable manner. The magnet treatment comprises providing a coil 193 surrounding the wire on the input end of the die, and also providing a coil 194 around the die itself to ensure that the magnetic field will operate not only to anneal or reduce stresses in the wire prior to forming, but also during the forming process. Another coil can be added at the exit of the die to treat the drawn wire.
Suitable controls such as that shown at 196 which are similar to those previously described can be provided to select one or the other of the coils for operation at any time, or both of the coils can be selected for simultaneous operation, as well.
Again, the magnetic field is used for reducing internal stresses in the wire, and ensuring that the drawn wire is not under high internal stresses. The magnetic field also is used for reducing internal stresses accumulating in the die.
FIG. 14 schematically shows another typical process for handling powdered material and composite parts. A coil housing indicated at 200 is provided with a central opening 201, into which a tray 202 can be placed, and then the coil can be powered from a suitable power source 203. The tray 202 is filled with powdered material shown at 204, which is in particle form for initial treatment, to reduce stresses in the metal particles through the provision of the magnetic field similar to that shown at FIGS. 1-3. This tray of course can be any desired size or shape, including a moveable baign for a continuous process to accomodate the amount of materials necessary to be treated. Also, the powder can flow (free or under some external action) through an included or vertical magnetic field process.
The powdered metal particles can then be formed into a green compact sleeve type member such as that shown at 205, in the process, and provided inside of a toroidal or annular coil 206, which can be suitably powered to provide a magnetic field that reduces the stresses on the green compact. The treating of the compact also improves its compactability, particularly if the magnetic treatment process is carried out while the powdered metal is being compacted.
The use of the magnetic field for the powder is valuable for improving compactability, so that more sophisticated shapes can be formed. The magnetic field treatment also decreases the spring-back effect. The residual porosity is decreased in the green compacts when treating as shown, within a toroidal core 206.
After treatment, the green compact is sent to a furnace 210 for sintering. The part then can be taken out, and as shown at 211, placed in a toroidal core 212 that will treat the sintered part to relieve and redistribute residual stresses, to simplify machining or further compacting, and to in general enhance its working properties. The part can be treated effectively at elevated temperatures, so the coil 212 can be in an oven or adjacent a heater to raise the temperature of the part to a desired level. Also, heating the powdered metal before compacting while treating it with the magnetic field is beneficial. For example, heaters and controls 225 can be provided with sensor 226 adjacent any part treated, including drill bits as shown schematically.
The heater 225, when used will bring the temperature of the parts to between 200° and 400° C normally, with temperatures up to 600° C. in special situations and for special materials.
In FIG. 15, a schematic illustration of use of a magnetic coil assembly for relieving the stress in large gun barrels both during and after firing is shown. For example, a tank 230 that has a gun barrel 231 extended from a turret can be treated with a portable magnet coil 232 that can be held in place and powered through a portable power pack indicated at 233. The coil is passed down the length of the barrel 201 a number of times in order to relieve stresses in the barrel. The intensity of the magnetic field can be controlled with portable controls as desired, and the coil assembly can be hand held and moved along the barrel or can even be provided with internal rollers that ride on the barrel and permit the coil to roll along the length of the barrel and back up to the outer end of the barrel as desired.
For all suggested types of treatment, the strength of the field can be varied, the magnetic field can be pulsated, and the wave form for the magnetic field can be a square wave, sine wave or saw tooth wave, as well as being intermittent. Suitable controls and a power source are provided to obtain the desired magnetic field profile.
FIG. 16 shows typical variations in the magnetic field that can be acquired with the appropriate programing for the power supply for electromagnets used. The horizontal line represents time and the vertical scale is the voltage level of the powering signal.
Certain ferromagnetic materials (iron, nickel, carbon steels, low alloy steels, tool steels and some stainless steels) deform elastically when placed in a magnetic field. Magnetostriction causes a specimen made from a ferromagnetic material to change in physical dimensions.
When a magnetic field is applied to a magnetically permeable magnetic conductive material, the magnetization of the material does not change uniformly. Internal magnetization lags the magnetization at the specimens surface. The duration of the lag is influenced by specimen shape, material conductivity, the frequency at which the magnetic field fluctuates, and the material magnetic permeability. During the initial period of magnetization, the skin of the part or specimen experiences the full magnetic field, but the interior does not. Consequently, the outer surface of the part or specimen grows or shrinks, but the core of the specimen remains stable. At the end of a pulse period, the magnetic field will saturate the specimen, if the correct magnetostrictive cycle has been employed.
Because the core and skin of a part respond at different rates to a magnetic field, magnetostriction introduces shear forces into the piece. The shear forces relieve microstresses by causing changes in the crystal structure of the metal. Phase changes can occur because of magnetostriction. Austenite may convert to martensite, for example. Magnetostriction can function like heat treatment or vibration.
The character of the magnetic field is important, as well. The rise time to full field strength and the field collapse time also influence the effectiveness of the process.
Treatable materials include cemented carbides with a cobalt and iron nickel matrix, hot-pressed ceramics such as alumina loaded with nickel and cobalt, brazed tool assemblies and tool steels. Treatment of turbine blades and fasteners can be treated to increase strength and prolong the useful life of the parts. In particular, turbine blades can be treated after installation on a motor or starter to reduce installation stresses. Also turbine blades can be treated as a part of maintenance to relieve accumulated stresses. Treatment of castings, including continuous casting, both in process of pouring and after can be applied to improve diffussion processes, homogenization, reduce internal stresses and improve performance of cast materials, and workability and machineability of castings. High pressure valves and jets can be treated to reduce or prevent crack propogation. Other materials and parts for treatment include piercers, needles, rollers, shaving blades and screens, bearings, bimetals, mine tools and mine tool holders, journals, shafts, threads, bolts, springs, screws, pinions, toothed gearing, chains, chop knives, choppers, kitchen knives, guideways, press tools, battery cans, fiber metal composites, tubing and piping - mechanically drawn and welded, pipe (tube) joints, pipe (tube) lines (for example, for oil transportation, liquid steel transportation, for nuclear station steam and liquid transportation), dental and surgical tools, medical devices, such as valves, pacemakers, steel jacketed discs, and valves.
If the process is used for cutting tools, the work pieces can be metals, including cemented carbides, wood, stone, leather, plastic, concrete, fiber materials, metal fiber compositions, green compacts, including ceramics, and welded seams, by way of example.
|
A device for treatment of ferromagnetic materials comprising means for developing a magnetic field of a selected intensity, duration, and cycle, which field is passed through materials to be processed, such as cutting tools and drill bits that have been sharpened or resharpened and other parts that have internal stresses. The magnetic field through the material provides stress relief of the stresses from welding, forming, heating cooling or sharpening or loading. The treatment increases surface wear resistance, decreases the coefficient of friction on the surfaces that are so treated, and increases the strength and modulus of elasticity. In certain types of materials, an increase in the surface concentration of such alloying metals such as wolfram, molybdenum, and tungsten, as well as oxygen and carbon is achieved. The structure comprises a coil and a controlled source of electrical power that generates a magnetic field for achieving the desired results.
| 7
|
This application is a continuation of application Ser. No. 08/839,821, filed Apr. 18, 1997.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to an exposure method and an exposure device for transferring a mask pattern onto a photosensitive substrate during certain photolithographic processes. Such processes are typically used when manufacturing semiconductor devices, image pickup devices (CCDs, etc.), liquid-crystal display elements, thin-film magnetic heads, and so on. The use of such a method and such a process is particularly favorable when a scanning type exposure device, such as step-and-scan system, is used to perform exposure operations.
2. Description of Related Art
It is known, when manufacturing semiconductor devices, to use a reduced projection type exposure device, or stepper, in a step-and-repeat or batch exposure system for transferring a reticle pattern or mask to individual shot areas of a wafer or glass plate forming a photosensitive substrate. A projection exposure device for use in a step-and-scan system has also been proposed. In this type of system, a reduced image of the reticle pattern is successively transferred to each shot area of the wafer by scanning the reticle and wafer synchronously with respect to the projection optical system. In this way, the need for enlarging the area of the transfer target pattern is met.
In a scanning exposure type projection exposure device used in a step-and-scan system, it is necessary to move the wafer stage at a fixed scanning speed V w during exposure in order to provide a prescribed exposure value with respect to the photoresist on the wafer. It is also necessary to move the reticle stage in the corresponding direction by XW/β synchronously with the movement of the wafer stage position XW, where the projection magnification from the reticle of the optical projection system to the wafer is B, in order to keep distortion and resolution of the reticle pattern image on the wafer within a prescribed margin. Therefore, the scanning speed of the reticle stage becomes V w /β when the scanning speed of the wafer stage is V w .
FIG. 6 shows the change in speed V of the wafer stage with respect to time t when executing exposure in the one shot area with a projection exposure device for a step-and-scan system. In FIG. 6, the wafer stage is accelerated from rest to a scanning speed V w within an acceleration time TA. The positional misregistration of the reticle and wafer is held to a prescribed margin within the subsequent synchronous settling time TB. Exposure is executed by irradiating illuminating light during the next exposure time TC.
Assuming that the aforementioned acceleration time is designated TA, the exposure time is designated TC, the average time necessary for stepping between the shot areas and deceleration of the wafer stage is a shot processing time designated TS, and the loading time of the wafer is a wafer processing time designated TL, then the throughput, or exposure wafer count per unit time, N may be expressed as
N=C/{n ×( TA+TB+TC+TS )+ TL} (1)
In this equation, C is the unit time and n is the shot area count per wafer. It is apparent from equation (1) that the throughput N improves by reducing the exposure time TC during which illuminating light is actually irradiated on each shot area.
In the scanning exposure system mentioned above, the throughput N can be improved by reducing the actual exposure time TC in each shot area of the wafer. However, an inability to enhance throughput (N) to a desired level has existed since the scanning speed has had an upper limit determined by the wafer and the reticle stages.
When an exposure time with respect to any arbitrary point on the wafer is designated T w , the necessary exposure value of the photoresist on the wafer is designated E (mJ/cm 2 ), the scanning speed of the wafer stage is designated V w (mm/sec), the maximum value of the scanning speed thereof is V Wmax , the slit width, in the scanning direction, of the slit shaped exposure field on the wafer is designated D, and the illumination intensity within the exposure field is designated P (mW/cm 2 ), the following relationship must be established.
T w =E/P=D/V w ≧V Wmax (2)
If the slit width D is considered to be a fixed value in order to satisfy equation (2), then it is necessary to increase a scanning speed V w when the resist sensitivity is high and the necessary exposure value E is low. On the other hand, it is necessary to decrease the scanning speed V w when the resist sensitivity is low and the necessary exposure value E is high. The scanning speed V w , however, cannot exceed the maximum value V wmax obtained by the mechanism. When the resist sensitivity is a prescribed high sensitivity and the necessary exposure value E becomes a prescribed value E sa , the scanning speed V w reaches its maximum value V wmax . For example, when the maximum value of an illumination intensity P is P max , the prescribed value E sa of the necessary exposure value E can be described as
E sa =P max •D/V Wmax (3)
The scanning speed V w is fixed at a maximum value (V wmax ) when the resist sensitivity is high and the necessary exposure value E is less than a prescribed value E sa . It is necessary, therefore, to reduce the illumination intensity P in order to satisfy equation (2) and obtain the necessary exposure value. When the scanning speed V w is fixed at the maximum value (V wmax ), the exposure time T w to one arbitrary point on the wafer is fixed at D/V Wmax according to equation (2). The actual exposure time (TC) with respect to each shot area in equation (1) is fixed at a given minimum value, and the throughput (N) reaches an upper limit.
FIG. 7 shows the relationship of the throughput to the resist sensitivity. The horizontal axis in FIG. 7 is the necessary exposure value E (mJ/cm 2 ) of the photoresist and the vertical axis is the throughput N (in arbitrary units) obtained from equation (1). FIG. 7 shows that the throughput N is high until the necessary exposure value E reaches the prescribed value E sa . Throughput N remains at a fixed value N1 during this time. The throughput N gradually decreases when the necessary exposure value E is above the prescribed value E sa . Therefore, the throughput, up to a given level, during the exposure process of the semiconductor element cannot be improved when using a photoresist of high sensitivity.
The sensitivity and the resolution oppose each other so that as the sensitivity becomes higher, the resolution becomes lower. In the layers of the semiconductor device, a photoresist of high resolution and low sensitivity is used in what is referred to as the “critical layer”. The critical layer is a layer in the semiconductor device in which the superimposition precision of the pattern is rigorous and the minimum line width is, for example, 0.3 μm. A photoresist of low resolution and high sensitivity is used in another layer, referred to as the “noncritical layer”, in which the minimum line width is greater than 0.5 μm and the superimposition precision of the pattern is relatively relaxed. When a photoresist of high sensitivity and large line width is used, an upper limit in the throughput is created.
SUMMARY OF THE INVENTION
One object of the present invention is to provide a scanning type exposure method taking the factors mentioned above into consideration and which can enhance the throughput of the exposure process by synchronously scanning the reticle and the wafer.
Another object of the present invention is to provide a scanning type exposure device that can use this type of exposure method.
A first scanning type exposure method according to the present invention is a scanning type exposure method which successively transfers and exposes a mask pattern onto a photosensitive substrate by moving the scanning mask and the photosensitive substrate synchronously and projecting one part of the pattern formed on the mask onto the photosensitive substrate. A synchronous settling time, which is the time from completion of acceleration of the mask and the photosensitive substrate until a start of a transfer of the mask pattern onto the photosensitive substrate, is switched in accordance with the sensitivity of the photosensitive substrate, the line width of the mask pattern, or both.
According to the present invention, the synchronization settling time until the start of the transfer or, more specifically, the time required to set the relative positional misregistration (synchronization error) between the mask and the photosensitive substrate at a prescribed value, is reduced if the line width of the mask pattern is large or if the sensitivity of the photosensitive substrate is high when exposing a noncritical layer. Consequently, the time necessary for the exposure is reduced and the throughput of the exposure process is improved. The necessary superimposition precision and resolution are relatively relaxed in the noncritical layer so that the necessary precision is obtained even when the synchronization settling time is reduced.
On the other hand, when the line width of the mask pattern is small or the sensitivity of the photosensitive substrate is low, as is the case when exposing a critical layer, the synchronization settling time is set long as in the conventional technology. Consequently, the necessary resolution and so on can be obtained. The necessary resolution is maintained, and the throughput can be enhanced, by changing the synchronization settling time in accordance with the particular layer involved.
A second scanning type exposure method according the present invention is similar to first scanning type exposure method and includes varying the margin for the synchronization error between the mask and the photosensitive substrate in accordance with the sensitivity of the photosensitive substrate, the line width of the mask pattern or both, when starting a transfer of the mask pattern onto the photosensitive substrate, by accelerating the mask and the photosensitive substrate.
According to the present invention, the margin for the synchronization error is set to be wide when the sensitivity of photosensitive substrate is high or the line width of the mask pattern is large, as is the case in the noncritical layer. The margin for the synchronization error, however, is set to be narrow when the sensitivity of the photosensitive substrate is low or the line width of the mask pattern is small, as is the case in the critical layer. Consequently, the throughput is improved as a whole while obtaining the necessary superimposition precision in accordance with the layer criticality.
The scanning type exposure device according to the present invention is provided with mask stages that scan a mask formed with a transfer pattern and substrate stages which scan a photosensitive substrate by synchronizing movements with those of the mask stages. The mask pattern is successively transferred and exposed onto a photosensitive substrate by synchronously scanning the mask and the photosensitive substrate via the mask and substrate stages where one part of the mask pattern is projected onto the photosensitive substrate. A storage device is provided which stores the transfer start condition (which may be, for example, either a synchronization setting time or a margin for synchronization error) in accordance with the sensitivity of multiple photosensitive substrates, the line widths of multiple mask patterns, or both, when starting a transfer of the mask pattern onto the photosensitive substrate. A control device is provided which sets the timing for starting the transfer of the transfer target mask pattern onto the exposure target photosensitive substrate. This timing is set on the basis of the transfer start condition read from the storage device according to the sensitivity of the exposure target photosensitive substrate, the line width of the transfer target mask pattern, or both, after starting the acceleration of the mask and substrate stages.
The first and second scanning type exposure methods can be used by changing the transfer start condition in accordance with the layer exposed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a view of a projection exposure device according to the present invention.
FIG. 2 ( a ) shows a synchronization error of a wafer and a reticle during a scan exposure in a first application example of the present invention.
FIG. 2 ( b ) shows a variance for prescribed synchronization error times.
FIG. 2 ( c ) shows an average value at each of the prescribed synchronization error times.
FIG. 3 shows the relationship between a synchronization settling time and a window width of the synchronization error.
FIG. 4 ( a ) shows the relationship between a throughput and the minimum line width according to the first application example.
FIG. 4 ( b ) shows a situation in which the synchronization settling time is changed more or less continuously with respect to the minimum line width.
FIG. 5 shows the throughput as it relates to a necessary exposure value of the photoresist in a second application example of the present invention.
FIG. 6 shows a change in speed of the wafer stage when exposing a one shot area with the scan exposure system.
FIG. 7 shows a relationship between the throughput and the necessary exposure value of the photoresist.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The first application example of the present invention is illustrated in FIGS. 1-4. In this example, the present invention is used when exposure is performed with a projection exposure device of a stop-and-scan system.
FIG. 1 is a block diagram showing a projection exposure device of this example. In FIG. 1, illuminating light IL, such as i-line light (wavelength 365 nm) generated from an exposure light source 1 composed of an ultrahigh-pressure mercury lamp, is incident on a fish or fly eye lens 5 . The lens 5 uniformly distributes the illumination intensity via a luminous flux condensing system 2 , such as a collimator lens, a variable extinction filter system 3 composed, for example, of an ND filter of various transmittances, and a mirror 4 for reflecting the luminous flux. A shutter that opens and closes the optical path of the illuminating light IL is arranged in a luminous flux condensing system 2 . The higher harmonics of a YAG laser, a metal vapor laser beam, or a laser beam of an ArF excimer laser, a KrF excimer laser, etc., can be used to provide illuminating light for exposure instead of or in addition to the luminescent line of the mercury lamp.
Illuminating light IL output from the fly eye lens 5 passes through an aperture diaphragm (σ contraction) 6 . The illuminating light illuminates a rectangular illumination area 12 R on the pattern area of the reticle with a uniform distribution of illumination intensity via a beam splitter 7 having a high transmittance and a low reflectivity, a first relay lens 8 A, a field diaphragm (reticle blind) 9 , a second relay lens 8 B, and a main condenser lens 10 .
On the basis of the illuminating light IL, the pattern within the illumination area 12 R of the reticle is reduced by a projection magnification β (β is for example, ¼, ⅕, etc.) via a projection optical system PL. The projection optical system is telecentric to both sides (or at least to the wafer W side). The projection is exposed onto a rectangular exposure area 12 W of the wafer W. A fixed-sensitivity photoresist is coated onto the surface of the wafer W. An explanation will now be given with respect to the direction parallel to the optical axis AX of the projection optical system PL (the Z axis), the direction parallel to the surface of the paper in FIG. 1 in a plane perpendicular to the Z axis (the X axis), and the direction perpendicular to the surface of the paper in FIG. 1 (the Y axis). In this example, the direction along the X axis (X direction) is the scanning direction of the reticle R and the wafer W during exposure.
The luminous flux in one part of the illuminating light IL reflected by the beam splitter 7 is incident on an integrator sensor 25 composed of a photoelectric detector after passing through a condensing optical system 24 . The photoelectric conversion signal DS output from the integrator sensor 25 is fed to an exposure controller 26 . The illumination intensity target value of the illuminating light IL for providing a suitable exposure value for the photoresist on the wafer W is input to the exposure controller 26 from the main control system 30 . The main control system comprehensively controls the entire device. The exposure controller 26 controls the extinction rate of the variable extinction filter system 3 and the brightness of the exposure light source 1 so that the measured value of the photoelectric conversion signal DS complies with the target value. The exposure controller also controls the opening and the closing of the shutter within luminous flux condensing system 2 .
The driving system for the reticle R and the wafer W will now be explained. The reticle stage 13 is mounted on a reticle support stand 14 . The reticle R is adhered to and held on the reticle stage 13 . The reticle stage 13 is constructed to move at a high speed in the X direction on the reticle support stand 14 in accordance with, for example, a linear motor system. The reticle stage 13 also moves in slow motion in the X direction, the Y direction, and the rotational direction. The X position, the Y position, and the rotational angle of the reticle stage 13 are monitored by a movable mirror 18 on the reticle stage 13 and an external laser interferometer 19 . Position information S 1 relating to the reticle stage 13 and, therefore, of the reticle R, obtained with a laser interferometer 19 , is fed to a stage controller 27 . The stage controller 27 controls the position and speed of the reticle stage 13 via a driving system 20 based on input position information S 1 .
Each reticle is stored respectively in one of multiple reticle cases within a reticle library (not shown in the figure). The reticle appropriate for each layer on the wafer is selected and loaded onto the reticle stage 13 via a reticle loader (not shown in the figure) according to instructions from the main control system 30 .
The wafer X axis stage 17 is loaded on a fixed disc (not shown in the figure). The wafer Y axis stage 16 is loaded on the wafer X axis stage so that it can be stepped in the Y direction. The wafer holder 15 is loaded on top of the wafer Y axis stage, and the wafer W is adhered to and held on the wafer holder 15 . A Z stage for positioning the wafer W in the Z direction and a θ stage for adjusting the rotational angle of the wafer are integrated into the wafer holder 15 . The position in the X direction, the position in the Y direction, and the rotational angle of the sample stand 15 are monitored by the movable mirror 21 on the wafer holder 15 and an externally arranged laser interferometer 22 . Position information S 2 relating to the wafer holder 15 and, therefore, to the wafer W, obtained from the laser interferometer 22 , is fed to the stage controller 27 . The stage controller 27 controls the position and speed of the wafer Y axis stage 16 and the wafer X axis stage 17 via the driving system 23 on the basis of input position information S 2 .
A reference mark unit 28 is formed with a reference mark, etc., for aligning the wafer W and the reticle R. The reference mark unit is also attached on the wafer holder 15 . Although it is not shown in FIG. 1, an alignment system for detecting the positional relationship of each shot area of the wafer W and the reticle R is also provided. In this example, the positional relationship between each shot area and the projected image of the reticle R is measured in the alignment process prior to starting the scan exposure of each shot area of the wafer W.
A data storage part 29 is connected to the main control system 30 in this example. Synchronization settling time TB data of the stage, corresponding to the sensitivity, etc., of the photoresist on the wafer or the minimum line width of the reticle, are stored in the data storage part 29 . In the main control system 30 , the corresponding synchronization settling time TB data are read from the data storage part 29 during the exposure.
The basic operation of this example when executing a scan exposure will now be explained.
The illumination intensity of the illuminating light IL for providing a suitable exposure with respect to the photoresist on the wafer W and the scanning speed V w in the X direction of the wafer W (the speed of the wafer X axis stage 17 ) are set with the main control system 30 . The illumination intensity and scanning speed (V w ) set are fed, respectively, to the exposure controller 26 and the stage controller 27 .
As shown in FIG. 6, the speed, in the X direction, of the wafer holder 15 and, therefore, the wafer W is accelerated from 0 to the scanning speed V w in an acceleration time TA. This acceleration is performed by driving the wafer X axis stage 17 . The reticle stage 13 is also accelerated by being coupled therewith. The positional misregistration between the wafer W and the reticle R is adjusted within the synchronization settling time TB. If the X coordinates of the wafer holder 15 and the reticle stage 13 are, for example, 0 when the exposure target shot areas of the wafer W and the reticle R were positioned, then the stage position is controlled so that the X coordinate X R of the reticle stage 13 with respect to the X coordinate X W of the wafer holder 15 during the scan exposure becomes −X W /β. In this relationship, β is the projection magnification of the projection optical system PL. The position code is reversed due to the projection of a reverse image according to the projection optical system PL. Synchronization error (ΔX) in the X direction of the wafer W and the reticle R is expressed as follows.
Δ X=X R =( −X w /β)= X R +X w /β (4)
There is also a synchronization error in the Y direction, which is vertically oriented relative to the scanning direction and the rotational direction. The synchronization error in the Y direction, however, is small compared to the synchronization error in the X direction. An explanation of the Y direction synchronization error, therefore, will be omitted here. The wafer X axis stage 17 is driven at a scanning speed V w in order to approach the target value of the synchronization error ΔX in equation 4 to within the synchronization settling time TB as in FIG. 6 . Here, the target value is 0. When the synchronization error ΔX is 0 and the wafer X axis stage 17 is moved in the +X or −X direction at a scanning speed V w , the reticle stage 13 is scanned in the −X direction (or +X direction) at a scanning speed V w /β. It is possible to drive the wafer X axis stage 17 by synchronization with the scanning of reticle stage 13 .
After the synchronization settling time TB has lapsed, the exposure controller 26 shown in FIG. 1 begins to irradiate illuminating light IL. The pattern image of the reticle R is successively exposed in each relevant shot area on wafer W within the exposure time TC represented in FIG. 6 .
There is a mechanically determined upper limit to the scanning speed in the X direction of the wafer X axis stage 17 and the reticle stage 13 . The projection magnification β of this example, however, is a reduction magnification (e.g., ¼, ⅕, etc.), so the scanning speed in the X direction of the reticle stage 13 is expanded by a magnification of 1/β (e.g., magnification of 4, magnification of 5, etc.) when compared to scanning speed V w of the wafer X axis stage 17 during the scan exposure. Therefore, as one example, the upper limit to the scanning speed of the reticle stage 13 becomes the mechanical upper limit value. The maximum value V Wmax of the scanning speed V w of the wafer X axis stage 17 is a magnification factor on the order of β of the scanning speed upper limit for the reticle stage 13 .
In this example, the synchronization settling time TB is changed in accordance with the minimum line width of the pattern transferred onto the wafer W. This principle will be explained with reference to FIGS. 2 and 3.
FIG. 2 ( a ) shows one example of synchronization error ΔX (the error expressed by equation ( 4 )) corresponding to acceleration time TA, synchronization settling time TB, and exposure time TC in FIG. 6 . The synchronization error (AX) converges more or less in the vicinity of 0 within the synchronization settling time TB and is maintained more or less in the vicinity of 0 within the exposure time TC.
The result of the computation of the variance XV of synchronization error ΔX in FIG. 2 ( a ) within time T before each sampling time is shown in FIG. 2 ( b ). The time necessary for one point on wafer W to pass the width, in the scanning direction, of the exposure area 12 W on the wafer W in FIG. 1 is designated T. The result of the computation of the average value XA of the synchronization error ΔX within a time T before each sampling time is shown in FIG. 2 ( c ).
The variance XV of the synchronization error in FIG. 2 ( b ) corresponds to the resolution of the pattern image transferred onto the wafer W. The resolution, therefore, is unfavorable in an area with a large variance XV and, accordingly, the picture quality degrades. On the other hand, the average value XA of the synchronization error in FIG. 2 ( c ) corresponds to the distortion in the pattern image transferred onto the wafer W. Distortion in an area with a large average value XA is unfavorable and the fluctuation in the image position becomes large. The superimposition error is unfavorable when carrying out a superimposed exposure.
The allowable range (hereafter referred to as the “window width”) of the average value XA and the variance XV of the synchronization error is determined according to the layer on the wafer W. Within the exposure time TC in FIG. 2 ( a ), it is necessary to keep the variance XV of the synchronization error within the window width WV (refer to FIG. 2 ( b )). The window width is determined according to the resolution needed. It is also necessary to keep the average value XA within the window width WA (refer to FIG. 2 ( c )), which is determined according to the distortion characteristic needed. As is apparent from FIG. 2 ( a ), the variance XV of the synchronization error ΔX and the average value XA gradually decrease within the synchronization settling time TB. It is possible, therefore, to make the window width WA have average value XA and the window width WV have a narrow variance XV when the synchronization settling time TB is made long.
FIG. 3 shows the relationship between a settable window width WV or WA and the synchronization settling time TB. The horizontal axis in FIG. 3 represents the synchronization settling time TB, and the vertical axis represents the window width WV for the variance XV (resolution) of synchronization error ΔX. When the vertical axis is the window width WA for the average value XA (distortion) of synchronization error ΔX, the same tendency is manifested. As shown in FIG. 3, the settable window width (WV) increases and the resolution of the transferred pattern degrades as the synchronization settling time TB becomes shorter. Similarly, the settable window width WA increases and the resolution in the transferred pattern degrades as the synchronization settling time TB becomes shorter.
When the window width for the variance XV of the synchronization error ΔX necessary in the critical layer (the layer with a minimum line width of 0.3 μm requiring high superimposition precision) is WV long and the window width of the variance XV necessary in the noncritical layer (the layer with a minimum line width of over 0.5 μm and in which the superimposition precision can also be low) is WV short , the synchronization settling time TB necessary to obtain the window widths becomes TB long and TB short (<TB long ), respectively.
When the minimum line width of the pattern transferred onto the wafer in the noncritical layer is the threshold value L th , the synchronization settling time TB is set to be greater than TB long with respect to a layer with a narrower minimum line width than the threshold value L th . The synchronization settling time TB is set to be less than TB short with respect to a layer with a minimum line width greater than the threshold value L th . The threshold value L th of the minimum line width and the synchronization settling times TB long and TB short are stored in the data storage part 29 of FIG. 1 . In the main control system 30 , the minimum line width L for the projected image of the reticle pattern on the wafer is obtained from the exposure data for the reticle R before exposure. The synchronization settling time TB long is set in storage controller 27 when the minimum line width L is narrower than the threshold value L th . The synchronization settling time TB short is set when the minimum line width L is more than the threshold value (L th ). Also, as was already explained, the throughput N of the exposure process is defined as follows using the aforementioned acceleration time TA, synchronization settling time TB, exposure time TC, shot processing time TS, wafer processing time TL, shot area count n, and unit time C.
N=C/{n ×( TA+TB+TC+TS )+ TL} (5)
Therefore, the throughput N improves when the synchronization settling time TB is reduced to TB short in the noncritical layer.
FIG. 4 ( a ) shows the relationship between the throughput N and the minimum line width L when exposure is performed with the scan exposure system of this example. In FIG. 4 ( a ), the curve 31 is the throughput N when the synchronization settling time TB is set at Tb long . The curve 32 is the throughput N when the synchronization settling time TB is set at TB short . The necessary resolution also normally becomes low when the minimum line width L increases so that the sensitivity of the photoresist on wafer W can be increased. The necessary exposure value E, in other words, can be made low. The throughput N in FIG. 4 ( a ) is the result of a computation that makes the sensitivity of the photoresist high when the minimum line width (L) increases.
When the minimum line width L increases as noted above, the scanning speed V w of the wafer W can be increased. As a result, the exposure time TC during which illuminating light is irradiated is reduced, and the throughput N is enhanced in accordance with equation (5). However, the scanning speed V w has an upper limit, so that curves 31 and 32 , indicating the throughput N, show saturation when the minimum line width L reaches the prescribed width L sa . The synchronization settling time TB used is differentiated at the threshold value L th as the boundary of the minimum line width L. The throughput N, therefore, is represented by the curve 31 in a range in which the minimum line width L is narrower than the threshold value L th (the range from the critical layer to the noncritical layer). The throughput N in the noncritical layer with a minimum line width L greater than the threshold value L th is represented by the curve 32 and is enhanced.
The synchronization settling time TB is typically less than one second. The synchronization settling time TB, however, is reduced for each of the many exposures to the many shot areas on wafer W, so that the throughput improves greatly as a whole.
The synchronization settling time TB is set in two steps in this example. However, the synchronization settling time TB can be set continuously with respect to the minimum line width L.
FIG. 4 ( b ) shows an example of continuously changing the synchronization settling time TB. In FIG. 4 ( b ), the synchronization settling time TB is set to TB 0 when the minimal line width L is a line width L 0 in the critical layer. The synchronization settling time TB gradually becomes shorter, as indicated with a curve 35 , as the minimum line width L becomes wider. The slope of this curve 35 should be the same as the slope for the curve represented in FIG. 3 . By continuously changing the synchronization settling time TB, it is possible to obtain the necessary resolution and distortion characteristics in each layer and to maximally enhance the respective throughput.
It is possible to set the synchronization settling time TB according to the window width WA for the distortion or the window width WV for the resolution necessary in the relevant layer by directly utilizing the relationship in FIG. 3 instead of setting the synchronization settling time TB based on the minimum line width L. In this case, storage in the data storage part 29 is according to the corresponding synchronization settling time TB and the window width WA of the distortion or the window width WV of the resolution.
Next, the second application example of the present invention will be explained with reference primarily to FIG. 5 . The first application example switched the synchronization settling time in accordance with the minimum line width. In this example, however, the synchronization settling time is switched in accordance with the sensitivity (the necessary exposure value E) of the photoresist on the wafer. In this example, exposure is also carried out by the projection exposure device of the step-and-scan system represented in FIG. 1 .
This example also utilizes the fact that the window width WV for the variance XV (resolution) of the settable synchronization error ΔX and the window width WA for the average value XA (distortion) of the synchronization error ΔX have an inverse proportional relationship with respect to the synchronization settling time TB during the scan exposure as shown in FIG. 3 . Furthermore, considering the fact that the resolution decreases when the sensitivity of the photoresist is enhanced, a photoresist having a sensitivity complying with the resolution (or distortion) necessary in the exposure target layer is used. The synchronization settling time TB is changed in accordance with the sensitivity of the photoresist (the necessary exposure value E).
As an example, the synchronization settling time TB is set greater than TB long for a layer with a necessary exposure value E larger than the threshold value E th . The synchronization settling time TB is set less than TB short for a layer with a necessary exposure value E less than the threshold value E th if the necessary exposure value E of the photoresist used in the noncritical layer is the threshold value E th . These threshold values E th of the necessary exposure value E and the synchronization settling times TB long and TB short are stored in the data storage part 29 of FIG. 1 . In the main control system 30 , the necessary exposure value E of the photoresist on the wafer W is checked in accordance with the exposure data prior to the exposure. The synchronization settling time TB long is set at the stage controller 27 when the necessary exposure value E is greater than the threshold value E th . The synchronization settling time TB short is set when the necessary exposure value E is less than the threshold value E th .
FIG. 5 shows the relationship between the throughput N and the necessary exposure value E (resist sensitivity) of the photoresist when exposure is performed with the scan exposure system in this example. In FIG. 5, a curve 33 represents the throughput N when the synchronization settling time TB is set to TB long . The curve 34 represents the throughput N when the synchronization settling time TB is set to TB short . The throughput N improves in accordance with both curves 33 and 34 when the necessary exposure value E decreases and saturates at N 1 and N 2 , respectively, when the necessary exposure value E reaches the prescribed value E th . The use of the synchronization settling time TB is differentiated in this example with the threshold value E th as the boundary in the necessary exposure value E. The throughput N is represented by the curve 33 in a range of necessary exposure values E greater than the threshold value E th (the range from the critical layer to the noncritical layer). The throughput N in the noncritical layer with a necessary exposure value E of less than the threshold value E th is represented by the curve 34 on the high side. Therefore, the throughput in the noncritical layer is enhanced, and the throughput is improved when using a high sensitivity resist with a low necessary exposure value E.
In this example, it is also possible to set the synchronization settling time TB continuously with respect to the necessary exposure value E. In this case, the synchronization settling time TB is made long in accordance with a gradual increase in the necessary exposure value E when the synchronization settling time TB is T 1 and the necessary exposure value E is the minimum value Ea.
In the aforementioned application example, the synchronization settling time TB is changed in accordance with the layer. As is apparent from FIG. 3, the window width WA for the average value XA (distortion) of the synchronization error ΔX and the window width WV for the variance XV (resolution) of the settable synchronization error ΔX become narrow as the synchronization settling time TB becomes long. This is apparent both theoretically and experimentally. The control system starts exposure when the prescribed synchronization settling time TB lapses. Therefore, the scanning exposure system is able to set a short co-scan distance during the scan exposure and use a simple arithmetic process in its control system.
The present invention is not limited to the application examples described above and can be composed in various ways within a scope not deviating from the essence of the present invention.
|
A first scanning type exposure method provides for changes in a synchronization settling time in accordance with a sensitivity of a photosensitive substrate, a line width of the mask pattern, or both. The throughput provided by the method can be enhanced while still obtaining the necessary resolution by making the synchronization settling time short when using a mask having a pattern with wide line width or a photosensitive substrate with a high sensitivity. A second scanning type exposure method provides for changes in a margin for synchronization error when starting a transfer of the pattern after completing acceleration of the photosensitive substrate and the mask in accordance with the line width of the mask pattern, the sensitivity of the photosensitive substrate, or both. A reduction in the time until the start of the exposure and an enhancement of the throughput while obtaining the necessary resolution are provided by making the margin of the synchronization error wide when using a mask having a pattern with wide line widths or a photosensitive substrate of high sensitivity. A scanning type exposure device utilizes the first or the second scanning type exposure method by setting a timing for the start of transferring the transfer target mask pattern to the exposure target photosensitive substrate. This timing is set by a transfer start condition read from a storage device in accordance with a line width of multiple mask patterns, the sensitivity of the photosensitive substrate, or both.
| 6
|
[0001] This application is a continuation-in-part of copending application Ser. No. 09/558,822 filed Apr. 26, 2000, the disclosure of which is incorporated herein by reference.
FIELD OF THE INVENTION
[0002] This invention relates to wash cycle unit dose laundry compositions for softening or conditioning fabrics. More particularly, this invention relates to unit dose fabric softening compositions which are compacted granular compositions spherical in shape and suitable for use in the wash cycle of an automatic washing machine.
BACKGROUND OF THE INVENTION
[0003] Detergent compositions manufactured in the form of tablets of compacted detergent powder are known in the art. U.S. Pat. No. 5,225,100, for example, describes a tablet of compacted powder comprising an anionic detergent compound which will adequately disperse in the wash water.
[0004] Although detergent compositions shaped as tablets have received much attention in the patent literature, the use of such tablets to provide a unit dose fabric softener which will soften or condition fabrics without impairing detergency is not known.
[0005] One possible option for providing a unit dose softener is to introduce the softening ingredients directly into the rinse cycle. But, for this type of product to be effective several practical requirements must be met. To begin with, the size and shape of the unit dose container must be readily compatible with the geometry of a wide variety of rinse cycle dispensers designed for home washing machines in order to insure its easy introduction into the dispenser.
[0006] Further, the unit dose composition must be formulated to readily dispense its contents upon contact with water in a period of time corresponding to the residence time of the unit dose in the dispenser, namely, the period of time during which water enters and flows through the rinse cycle dispenser. The aforementioned practical requirements have to date not been successfully met and therefore there remains a need in the art for a commercially acceptable unit dose softener capable of activation in the rinse cycle.
[0007] Wash cycle softeners are known in the art which condition fabrics during the period of the wash cycle. Tablet unit doses for detergent compositions are also known. Such tablets are typically flat compacted unit compositions which conceptually offer numerous advantages to the consumer such as: ease of dosing; cleaner wash cycle dispensers resulting from not being dosed with loose powder; less bulk to carry and dispense; ease of handling relative to liquids; and environmental benefits attendant to reduced packaging requirements.
[0008] But, despite these advantages. there is a major drawback which occurs in front loading washing machines which represent at least 90% of the European market, and are gaining in consumer acceptance in North America. In front loading machines, a flat compacted object when introduced into the wash cycle often becomes trapped within a few minutes in the rubber seal surrounding the window of the washing machine. Once trapped in the seal, the tablet tends to remain trapped until the wash cycle is over and is consequently not dispersed in the wash water. To overcome this problem, different approaches have been taken.
[0009] Some tablet manufacturers provide a net or sachet designed to contain the tablet unit dose, and thereby avoid the problem of direct contact between the tablet and the seal. Another proposed solution involves providing a rapidly dispersible tablet in the wash water by incorporating an effervescent matrix and/or a disintegration agent into the tablet. But, these proposed options are generally uneconomical and often result in an unduly fragile tablet unable to readily withstand normal handling by the consumer without fracturing. Thus, there is a need for an economical unit dose tablet capable of providing conditioning of fabrics, and which retains its physical integrity during normal handling prior to being introduced into the washing machine.
SUMMARY OF THE INVENTION
[0010] The present invention provides a unit dose laundry composition for softening or conditioning fabrics which is suitable as an additive to the wash cycle of an automatic washing machine, said unit dose composition comprising a compacted granular composition comprising a fabric softener or a fabric conditioner, said compacted granular composition being characterized by having a spherical shape and having no discrete outer layer surrounding said fabric softener or conditioner, which outer layer is comprised of an alkaline material such that the pH of the wash water is increased upon the dissolution of said outer layer in said wash water.
[0011] In a preferred embodiment of the invention the fabric softener or conditioner is comprised of a fabric softening clay and an organic fatty softening material. Especially preferred fabric softeners comprise a clay mineral softener, such as bentonite, in combination with a pentaerythritol compound as further described herein. Useful combinations of such softener may very from about 83%, to about 90%, by weight, of clay, and from about 10% to about 17%, by weight, of fatty softening material such as a pentaerythritol compound (often abbreviated herein as “PEC”).
[0012] In a further preferred embodiment of the invention the fabric softener or conditioner is free of a soap surfactant.
[0013] In accordance with the process aspect of the invention there is provided a process for softening or conditioning laundry which comprises contacted the laundry with an effective amount of the unit dose laundry composition defined above.
DETAILED DESCRIPTION OF THE INVENTION
[0014] The clays that are useful components of the invented products are those which cooperate with the organic fatty softener materials to provide enhanced softening of laundry. Such clays include the montmorillonite-containing clays which have swelling properties (in water) and which are of smectite structure, so that they deposit on fibrous materials, especially cotton and cotton/synthetic blends, such as cotton/polyester, to give such fibers and fabrics made from them a surface lubricity or softness. The best of the smectite clays for use in the present invention is bentonite and the best of the bentonites are those which have a substantial swelling capability in water, such as the sodium and potassium bentonites. Such swelling bentonites are also known as western or Wyoming bentonites, which are essentially sodium bentonite. Other bentonites, such as calcium bentonite, are normally non-swelling and usually are, in themselves, unacceptable as fabric softening agents. However, it has been found that such non-swelling bentonites exhibit even better fabric softening in combination with PEC's than do the swelling bentonites, provided that there is present in the softening composition, a source of alkali metal or other solubilizing ion, such as sodium (which may come from sodium hydroxide, added to the composition, or from sodium salts, such as builders and fillers, which may be functional components of the composition). Among the preferred bentonites are those of sodium and potassium, which are normally swelling, and calcium and magnesium, which are normally non-swelling. Of these it is preferred to utilize calcium (with a source of sodium being present) and sodium bentonites. The bentonites employed may be produced in the United States of America, such as Wyoming bentonite, but also may be obtained from Europe, including Italy and Spain, as calcium bentonite, which may be converted to sodium bentonite by treatment with sodium carbonate, or may be employed as calcium bentonite. Also, other montmorillonite-containing smectite clays of properties like those of the bentonites described may be substituted in whole or in part for the bentonites described herein and similar fabric softening results will be obtained.
[0015] The swellable bentonites and similarly operative clays are of ultimate particle sizes in the micron range, e.g., 0.01 to 20 microns and of actual particle sizes in the range of No's. 100 to 400 sieves, preferably 140 to 325 sieves, U.S. Sieve Series. The bentonite and other such suitable swellable clays may be agglomerated to larger particle sizes too, such as 60 to 120 sieves, but such agglomerates are not preferred unless they include the PEC('s) too (in any particulate products).
[0016] A main component of the invented compositions and articles of the present invention, and which is used in combination with the fabric softening clay is an organic fatty softener. The organic softener can be anionic or nonionic fatty chains (C 10 -C 22 preferably C 12 -C 18 ). Anionic softeners include fatty acids soaps. Preferred organic softeners are nonionics such as fatty esters, ethoxylated fatty esters, fatty alcohols and polyols polymers. The organic softener is most preferably a higher fatty acid ester of a pentaerythritol compound, which term is used in this specification to describe higher fatty acid esters of pentaerythritol, higher fatty acid esters of pentaerythritol oligomers, higher fatty acid esters of lower alkylene oxide derivatives of pentaerythritol and higher fatty acid esters of lower alkylene oxide derivatives of pentaerythritol oligomers. Pentaerythritol compound is often abbreviated as PEC herein, which description and abbreviation may apply to any or all of pentaerythritol, oligomers, thereof and alkoxylated derivatives thereof, as such, or more preferably and more usually, as the esters, as may be indicated by the context.
[0017] The oligomers of pentaerythritol are preferably those of two to five pentaerythritol moieties, more preferably 2 or 3, with such moieties being joined together through etheric bonds. The lower alkylene oxide derivatives thereof are preferably of ethylene oxide or propylene oxide monomers, dimers or polymers, which terminate in hydroxyls and are joined to the pentaerythritol or oligomer of pentaerythritol through etheric linkages. Preferably there will be one to ten alkylene oxide moieties in each such alkylene oxide chain, more preferably 2 to 6, and there will be one to ten such groups on a PEC, depending on the oligomer. At least one of the PEC OH groups and preferably at least two, e.g., 1 or 2 to 4, are esterified by a higher fatty acid or other higher aliphatic acid, which can be of an odd number of carbon atoms.
[0018] The higher fatty acid esters of the pentaerythritol compounds are preferably partial esters. And more preferably there will be at least two free hydroxyls thereon after esterification (on the pentaerythritol, oligomer or alkoxyalkane groups). Frequently, the number of such free hydroxyls is two or about two but sometimes it may by one, as in pentaerythritol tristearate, or as many as eight, as in pentaerythritol tetrapalmitate. The higher aliphatic or fatty acids that may be employed as esterifying acids are those of carbon atom contents in the range of 8 to 24, preferably 12 to 22 and more preferably 12 to 18, e.g., lauric, myristic, palmitic, oleic, stearic and behenic acids. Such may be mixtures of such fatty acids, obtained from natural sources, such as tallow or coconut oil, or from such natural materials that have been hydrogenated. Synthetic acids of odd or even numbers of carbon atoms may also be employed. Of the fatty acids lauric and stearic acids are often preferred, and such preference may depend on the pentaerythritol compound being esterified.
[0019] Examples of some esters (PEC's) within the present invention follow:
Monopentaerythritol Esters
[0020] [0020]
[0021] Monopentaerythritol Dilaurate
[0022] R 1 ═CH 3 —(CH 2 ) 10 —COO—
[0023] R 2 ═CH 3 —(CH 2 ) 10 —COO—
[0024] R 3 ═—OH
[0025] R 4 ═OH
[0026] Monopentaerythritol Monostearate
[0027] R 1 ═CH 3 —(CH 2 ) 16 —COO—
[0028] R 2 ═OH
[0029] R 3 ═OH
[0030] R 4 ═OH
[0031] Monopentaerythritol Distearate
[0032] R 1 ═CH 3 —(CH 2 ) 16 —COO—
[0033] R 2 ═CH 3 —(CH 2 ) 16 —COO—
[0034] R 3 ═OH
[0035] R 4 ═OH
[0036] Monopentaerythritol Tristearate
[0037] R 1 ═CH 3 —(CH 2 ) 16 —COO—
[0038] R 2 ═CH 3 —(CH 2 ) 16 —COO—
[0039] R 3 ═CH 3 —(CH 2 ) 16 —COO—
[0040] R 4 ═OH
[0041] Monopentaerythritol Monobehenate
[0042] R 1 ═CH 3 —(CH 2 ) 20 —COO—
[0043] R 2 ═OH
[0044] R 3 ═OH
[0045] R 4 ═OH
[0046] Monopentaerythritol Dibehenate
[0047] R 1 ═CH 3 —(CH 2 ) 20 —COO—
[0048] R 2 ═CH 3 —(CH 2 ) 20 —COO—
[0049] R 3 ═OH
[0050] R 4 ═OH
Dipentaaerythritol Esters
[0051] [0051]
[0052] Dipentaerythritol Tetralaurate
[0053] R 1 ═CH 3 —(CH 2 ) 10 —CO
[0054] R 2 ═CH 3 —(CH 2 ) 10 —CO
[0055] R 3 ═CH 3 —(CH 2 ) 10 —CO
[0056] R 4 ═CH 3 —(CH 2 ) 10 —CO
[0057] Dipentaerythritol Tetrastearate
[0058] R 1 ═CH 3 —(CH 2 ) 16 —CO
[0059] R 2 ═CH 3 —(CH 2 ) 16 —CO
[0060] R 3 ═CH 3 —(CH 2 ) 16 —CO
[0061] R 4 ═CH 3 —(CH 2 ) 16 —CO
Pentaerythritol 10 Ethylene Oxide Ester
[0062] [0062]
[0063] with n+n′═10
[0064] Monopentaerythritol 10 Ethylene Oxide Distearate
[0065] R 1 ═CH 3 —(CH 2 ) 16 —COO—
[0066] R 2 ═CH 3 —(CH 2 ) 16 —COO—
Pentaerythritol 4 Propylene Oxide Esters
[0067] [0067]
[0068] Monopentaerythritol 4 Propylene Oxide Monostearate
[0069] R 1 ═CH 3 —(CH 2 ) 16 —COO—
[0070] R 2 ═OH
[0071] Monopentaerythritol 4 Propylene Oxide Distearate
[0072] R 1 ═CH 3 —(CH 2 ) 16 —COO—
[0073] R 2 ═CH 3 —(CH 2 ) 16 —COO—
[0074] Although in the formulas given herein some preferred pentaerythritol compounds that are useful in the practice of this invention are illustrated it will be understood that various other such pentaerythritol compounds within the description thereof herein may be employed too, including such as pentaerythritol dihydrogenated tallowate, pentaerythritol ditallowate, pentaerythritol dipalmitate, and dipentaerythritol tetratallowate.
[0075] Other fabric softening materials may be incorporated into the presently described unit dose laundry compositions provided they are not ecologically unacceptable and if they do not interfere with the fiber softening action of the clay and organic fatty softener material. In fact, sometimes, when antistatic action is desirable in the product, such additions may be important because although PEC's, for example, have some antistatic properties it is generally insufficient for the intended purposes. Thus, it is possible to formulate fabric softening compositions and articles with the PEC supplemented by other antistatic agents and also by fabric softeners. The foremost of such antistatic materials are the quaternary ammonium salts but when they are present there can be ecological problems, due to their alleged toxicities to aquatic organisms. Other antistats and fabric softeners include: higher alkyl neoalkanamides, e.g., N-stearyl neodecanamide; isostearamides; amines, such as N,N-ditallowalkyl N-methyl amine; esterified quaternary salts or esterquats: amidoamines; amidoquats; imidazolines; imidazolinium salts.
[0076] Other useful ingredients for the unit dose laundry compositions of the invention include disintegration materials to enhance the disintegration of the unit dose in the wash water. Such materials include an effervescent matrix such as citric acid combined with baking soda, or materials such as PVP polymer and cellulose. Granulating agents may be used such as polyethylene glycol; bactericides, perfumes, dyes and materials to protect against color fading, dye transfer, anti-pilling and anti-shrinkage. For purposes of enhancing the aesthetic properties of the final composition, cosmetic ingredients such as dyes, micas and waxes may be used as coating ingredients to improve the appearance and feel of the unit dose.
EXAMPLE 1
[0077] A unit dose composition was prepared from the following ingredients:
Weight Percent Clay/Pentaerythritol ditallowate (PDT) in a 80% ratio of 83%:17% Effervescent matrix of baking soda and citric 17% acid Polyvinylpyrrolidone 1% Perfume 2% Dye 0.03%
[0078] This method of manufacture consisted of mixing all the ingredients with the exception of perfume in a Loedige-type mixer. The resulting blend was dried in an oven and perfume was then added to the dried powder. The powder was then compacted using an alternative or rotative press mounted with appropriate dyes. The weight of the spherical unit dose was 60 g and such unit dose dispersed in water within 20 minutes when introduced in the wash load at the beginning of the wash in a European Miele W832 front loading washing machine set a Program White Colors at 40° C.
[0079] The softness provided by the unit dose compositions on terry towels, cotton tee-shirts and cotton kitchen towels was evaluated after cummulative washes and compared with a commercial liquid fabric softener. A 3 Kg laundry ballast was used in the machine. Softness was evaluated by a panel of six judges using 9 replicates. The results were as follows:
SOFTNESS EVALUATION Laundry Item Softness Comparison Terry towels 1 unit dose softener composition of the invention provided equivalent softness to commercial liquid FS after 10 cumulative wash cycles Cotton tee-shirts 1 unit dose softener provided equivalent softness to commercial liquid FS after one wash cycle Cotton kitchen towels 1 unit dose softener provided enhanced softening relative to commercial liquid FS after one wash cycle
EXAMPLE 2
[0080] Unit dose softener compositions were prepared as described in Example 1 to provide 60 gram spherical softeners having a diameter of 44 mm. The typical range of spherical dose diameters is from about 5 to about 60 mm; preferably from about 20 to about 40 mm; and
[0081] most preferably from about 30 to about 35 mm. The dissolution behavior of the unit dose softener in the washing machine was compared to a compacted tablet of 35 grams. The European washing machine and conditions of laundering were as described in Example 1. The spherical unit dose softener of the invention and the tablet were introduced into the washing machine before the start of the wash. Results were as follows:
Dispersion Evaluation
[0082] Both the spherical unit dose and the tablet became entrapped in the rubber gasket of the washing machine within a few minutes of the wash cycle. However, the spherical unit dose was able to readily disengage itself from the gasket and return to the laundry while the tablet remained trapped in the gasket.
[0083] Out of ten wash cycles, the tablet was trapped in the rubber gasket of the machine every time (ten times). The average time to get stuck was about 10 minutes. In contrast thereto, out of ten wash cycles, the spherical unit dose softener never was trapped in the rubber gasket and dissolved in the wash water without difficulty.
|
A unit dose laundry composition for softening or conditioning fabrics which is suitable as an additive to the wash cycle of an automatic washing machine, said unit dose composition comprising a compacted granular composition comprising a fabric softener or a fabric conditioner, said compacted granular composition being characterized by having a spherical shape and having no discrete outer layer surrounding said fabric softener or conditioner, which outer layer is comprised of an alkaline material such that the pH of the wash water is increased upon the dissolution of said outer layer in said wash water.
| 2
|
This application is a continuation in part of PCT Application NO. PCT/US01/14200 filed on May 3, 2001, which claims priority to also provisional patent application Nos. 60/201,391 filed on May 3, 2000; 60/234,432 filed on Sep. 21, 2000 and 60/235,828 filed on Sep. 27, 2000. The PCT Application was published under PCT Article 21(2) in English.
BACKGROUND OF THE INVENTION
The present invention relates generally to an exhaust gas recirculation (EGR) system for regulating the flow of an exhaust gas.
EGR systems are increasingly being utilized to improve the efficiency of engines and reduce the harmful effects of the exhaust gas on the environment. As an engine burns fuel, it produces an exhaust gas which contains unburned fuel and other impurities. In an EGR system, the exhaust gas is redirected through the engine to burn any unburned fuel remaining in the exhaust gas. Reburning the exhaust gas before it is released reduces the harmful effects of the exhaust gas on the atmosphere and enables the vehicle to meet government emission standards.
In order to recirculate the exhaust gas, EGR systems typically include a valve and a cooler. The valve regulates the amount of exhaust gas that is introduced back into the engine. The cooler cools the exhaust gas to a specified temperature which condenses the unburned fuel.
Prior EGR systems utilize a vacuum source with a diaphragm actuator to open and close the valve. The diaphragm actuator has a slow response time and is either open or closed with no intermediate valve position. One drawback to the prior art is that the slow response time of valves reduce the horsepower and efficiency of the engine, limiting the amount the EGR system may be used.
Hence, there is a need for an improved exhaust gas recirculation system for regulating the flow of an exhaust gas.
SUMMARY OF THE INVENTION
The present invention relates to an exhaust gas recirculation system for regulating the flow of an exhaust gas.
The exhaust gas recirculation system includes an EGR valve apparatus which regulates the amount of exhaust gas that is recirculated in the system. In one embodiment, a motor rotates a shaft which opens or closes a plurality of valves. The amount of exhaust gas flowing through the EGR valve apparatus is proportional to the amount the valves are opened or closed.
In a second embodiment, a force balanced rotary EGR valve assembly including balance seat valves is utilized. When more exhaust is to enter a chamber, the shaft is rotated, moving a downward balanced seat rotary EGR valve downwardly out of the chamber against the flow of exhaust and an upward balanced seat rotary EGR valve upwardly into the chamber with the flow of exhaust. Rotating the shaft in the opposite direction reverses the movement of the valves, allowing less exhaust gas to enter the chamber.
A third embodiment includes an inline poppet located on each valve which opens to allow gas to enter the chamber before the EGR valve is opened to overcome the pressure in the system. A cam translates the rotary motion of the motor shaft to the linear motion of a valve shaft to open the EGR valve.
Alternatively, the motor rotates the motor shaft to pivot a balance arm in a fourth embodiment. A first end of the arm moves upwardly to raise an EGR valve, and a second end of the arm moves downwardly to lower an EGR valve, allowing more exhaust gas to enter the chamber. Reverse rotation of the shaft reverses the movement of the valves, allowing less exhaust gas to enter the chamber.
In a fifth embodiment, an air venturi apparatus is employed. The motor rotates a shaft of a poppet, separating a pintle from an orifice. The degree of separation of the pintle from the orifice allows a proportional amount of a fresh air/exhaust gas mixture to return to the system.
Accordingly, the present invention provides an exhaust gas recirculation system for regulating the flow of an exhaust gas.
These and other features of the present invention will be best understood from the following specification and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The various features and advantages of the invention will become apparent to those skilled in the art from the following detailed description of the currently preferred embodiment. The drawings that accompany the detailed description can be briefly described as follows:
FIG. 1 illustrates a flow diagram for an exhaust recirculation system which regulates the flow of an exhaust gas;
FIG. 2 is a perspective view of a first embodiment of the valve apparatus of the present invention;
FIG. 3 illustrates a perspective view of a second embodiment of the valve apparatus employing a forced balanced seat EGR valve assembly;
FIG. 4 illustrates a cross sectional side view of the valves of the force balanced rotary EGR valve assembly of the second embodiment;
FIG. 5 illustrates an interior cross sectional view of a third embodiment of the valve apparatus with the force balanced rotary valves opened;
FIG. 6 illustrates an interior cross sectional view of a fourth embodiment of the valve apparatus;
FIG. 7 illustrates a perspective internal view of an air venturi assembly of a fifth embodiment of the present invention; and
FIG. 8 illustrates an interior cross-sectional view of an alternate fourth embodiment of the valve apparatus.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The exhaust gas recirculation (EGR) system, illustrated in FIG. 1, comprises an engine control unit (ECU) 10 which transits a pulse width modulated (PWM) signal 20 to a printed circuit board (PCB) pilot circuit 12 . A PWM signal 20 is not strong enough to operate a motor 14 , the pilot circuit 12 is connected to a second current source 18 , such as a battery, which increases the strength of the PWM signal 20 . The pilot circuit 12 then transmits a second signal 22 to the motor 14 , which actuates a valve apparatus 16 to control the flow of a fresh air/exhaust gas mixture back into the system. It is preferred that the motor 14 is an electric D/C motor 14 , preferably a monophase electromagnetic actuator.
The ECU 10 is programmed to operate the EGR system at certain customer specified duty cycles. As a vehicle travels at a constant speed, the ECU 10 transmits a signal to operate the EGR system at full capacity. However, when the vehicle requires maximum horsepower, such as during acceleration, the ECU 10 transmits the PWM signal 20 to close the valves apparatus 16 , to step exhaust gas recirculation. The ECU 10 is limited by being able to transmit a signal of no more than 1.3 amps.
FIG. 2 illustrates a first embodiment of the EGR valve apparatus 16 of the present invention. A non-contact sensor of the motor 14 receives a signal from the pilot circuit 12 and in response rotates a shaft 30 to proportionally open or close a plurality of valves 28 . The motor 14 is attached to a housing 42 by a bracket 34 , which provides support for the shaft 30 and withstands the torque produced as the shaft 30 rotates.
Each of the valves 28 includes an arm 44 connected to a disc 46 by a pin. As the shaft 30 rotates, the arm 44 pivots and the disc 46 moves, opening and closing the valves 28 . In this embodiment, each of the valves 28 are substantially positioned on the same side of the shaft 30 .
After the valves 28 have been opened, exhaust gas flows from the engine, which is fastened to the housing 42 at a first mounting face 24 , through an exhaust gas inlet 40 . The exhaust gas enters a chamber 36 and exits the valve assembly 16 through the outlet 38 . The exhaust gas then flows into a cooler, which is fastened to the housing 42 at a second mounting face 26 . While multiple valves are shown for increased exhaust gas flow, only one may be used if desired.
In a second embodiment, as illustrated in FIG. 3, a valve assembly 116 including force balanced seat rotary EGR valves 128 is utilized. As the motor 114 operates, the shaft 130 rotates to proportionally raise and lower the rotary EGR valves 128 allowing exhaust to enter the chamber 136 from the engine. While a pair of force balanced rotary EGR valves 128 are illustrated, any number may be utilized. In this embodiment, the rotary EGR valves 128 are positioned on opposite sides of the shaft 130 .
As illustrated in FIG. 4, each rotary EGR valve 128 includes a pintle 148 attached to a bottom portion 150 of a valve shaft 144 . When more exhaust is to enter the system, the shaft 130 is rotated so that the downward rotary EGR valve 128 a moves downwardly out of the chamber 136 against the flow of exhaust, and the upward rotary EGR valve 128 b moves upwardly into the chamber 136 with the flow of exhaust. The degree of rotation of the shaft 130 determines the amount the rotary EGR valves 128 a , 128 b are opened. It is preferred that the shaft 130 be rotated 20°, although other degrees of rotation are possible depending on system requirements. When less exhaust is to enter the system, the shaft 130 is rotated in the opposite direction, reversing the abovementioned movement of the valves 128 a , 128 b . When no exhaust is to enter the system, the pintles 148 of the rotary EGR valves 128 fit securely into an orifice 146 cut into the first mounting face 24 of the housing 42 , preventing exhaust from being recirculated into the system.
As further illustrated in FIG. 4, an upper portion 152 of each valve shaft 144 is attached to a curved arm 154 secured to the motor shaft 130 by a pin 158 , the valve shaft 144 being positioned within an orifice 164 in the pin 158 . Wave washers 160 are utilized to reduce wear. A threaded nut 162 positioned on the upper portion 152 of the valve shaft 144 secures the assembly.
As the motor 114 rotates the shaft 130 according to the required input, the arms 154 pivot and transfer the rotational movement of the shaft 130 into the linear movement of the rotary EGR valves 128 a , 128 b . A spring can be employed on the motor shaft 130 proximate to the motor 114 to prevent vibrations and to act as a fail safe mechanism to close the valves 128 a , 128 b if the motor 114 loses power.
FIG. 5 illustrates a third embodiment of the EGR valve assembly 216 in an open position. An inline poppet 266 located on the pintle 248 opens to allow gas to enter the chamber 236 before the EGR valve 228 is opened. This overcomes the pressure in the system, reducing the force needed to open the EGR valve 228 . The motor 214 rotates a shaft 230 which is connected to a cam 268 , the cam 268 translating the rotary motion of the motor shaft 230 to the linear motion of the valve shaft 244 and opens the EGR valve 228 . The degree of rotation of the motor shaft 230 determines the degree of the opening of the EGR valve 228 . Rotation of the motor shaft 230 moves the pintle 248 towards or away from the orifice 246 to allow the desired amount of exhaust gas to enter the chamber 236 .
FIG. 6 illustrates a fourth embodiment of valve assembly 316 . The motor 314 rotates a motor shaft 330 , pivoting a balance arm 372 so that a first end 374 b of the arm 372 moves upwardly to raise the rotary EGR valve 328 b , and the second end 374 a of the arm 372 moves downwardly to lower the rotary EGR valve 328 a . As the valves 328 a , 328 b move away from their respective orifices 346 , more exhaust gas is allowed to enter the chamber 336 . Reverse rotation of the shaft 330 reverses the movement of the valves 328 a , 328 b . The degree of the opening of the valves 328 a , 328 b is determined by the ECU 10 .
FIG. 8 illustrates an alternate valve assembly 516 including a balance arm 572 moveable about a motor shaft 530 . A first valve 528 b is attached to a first end 574 b of the balance arm 572 , and a second valve 528 a is attached to a second end 574 a of the balance arm 572 . The motor (not shown) rotates the motor shaft 530 to pivot the balance arm 572 . Preferably, the valves 528 a and 528 b are covered by a plastic cover 566 . In one example, the plastic cover 566 is made of zytel. Shaft bushings (not shown) are preferably positioned around the shaft 530 to assist in alignment of the valves 528 a and 528 b.
The first mounting face 524 of a housing 542 including a chamber 536 is fastened to an engine. When more exhaust gas is to enter the chamber 536 , the shaft 530 is rotated to pivot the balance arm 572 to open the valve assembly 516 such that the first end 574 b of the arm 572 moves upwardly to raise the first valve 528 b , and the second end 574 a of the arm 572 moves downwardly to lower the second valve 528 a . After the valves 528 a and 528 b have been opened, exhaust gas flows from the engine into the chamber 536 through exhaust gas inlets 540 a and 540 b in a cooler. The exhaust gas exits the chamber 536 through an outlet 538 for cooling.
When less exhaust is to enter the chamber 536 , the shaft 530 is rotated in the opposite direction to pivot the balance arm 72 to close the valve assembly 516 such that the first end 574 b of the arm 572 moves downwardly to lower the first valve 528 b , and the second end 574 a of the arm 572 moves upwardly to raise the second valve 528 a . The degree of rotation of the shaft 530 determines the amount the valves 528 a and 528 b are opened or closed.
Each valve 528 a and 528 b includes a pintle 548 a and 548 b , respectively, attached to a bottom portion 550 of a valve shaft 544 . When no exhaust is to enter the housing 536 , the pintles 548 a and 548 b of the valves 528 a and 528 b fit securely into an orifice 546 a and 546 b , respectively, in the first mounting face 524 of the housing 542 , preventing exhaust from entering the housing 536 through the inlets 540 a and 540 b and from being recirculating into the system.
As the valves 528 a and 528 b are moved and fluid flows through the orifices 546 a and 546 b into the chamber 536 , the valve 528 a moves with the flow of the exhaust fluid and the valve 528 b moves against the flow of exhaust fluid. As these forces are balanced, no additional forces are provided on the motor during movement of the valves 528 a and 528 b.
The outer edge of the pintle 548 b includes is angled upwardly. When the valve 528 b is closed, the outer edge of the pintle 548 b contacts the orifice 546 b , breaking off any soot from the exhaust that collects on the pintle 548 b . The outer edge of the pintle 548 a is angled downwardly. Any soot accumulating on the pintle 548 b will drain off the pintle 548 b . By eliminating the buildup of soot on the pintles 548 a and 548 b , the sticking of the pintles 548 a and 548 b in the orifices 546 a and 546 b is reduced, creating a better seal between the pintles 548 a and 548 b and the orifices 546 a and 546 b.
An arm 576 is received in a hole 578 in each end 574 a and 574 b of the balance arm 572 . An upper portion 558 of each valve shaft 544 is secured to each arm 576 . In one example, the upper portion 558 of each valve stem 544 is orbital riveted to the arm 576 , reducing and eliminating vibrations. As the balance arm 572 moves about the shaft 530 , the arms 576 pivot in the holes 578 , translating the rotary motion of the shaft 530 into the linear motion of the valves 528 a and 528 b.
Each valve shaft 544 further includes a reduced diameter portion 554 received in a stem shield 556 . Each stem shield 556 includes an aperture 557 sized to receive the reduced diameter portion 554 . As the valves 528 a and 528 b are opened and closed, the interaction of the reduced diameter portion 554 and the stem shield 556 rubs off any soot and condensation, reducing any soot and condensation that forms at the interface 559 .
A portion of the valve shafts 544 are positioned in a cooling chamber 552 . The coolant enters a path 551 around the cooling chamber 552 through an inlet 550 and circulates around the valve shafts 544 to provide cooling. The coolant exits the cooling chamber 552 through an outlet (not shown) located next to the inlet 550 . The cooling chamber 552 is secured to the housing 542 by attachment members 567 to eliminate any vibrations. Preferably, the attachment members 567 are bolts.
A bushing 560 positioned around the each of the valve shafts 554 is received in the coolant chamber 552 . The bushing 560 is preferably made of sintered bronze or vespel to reduce friction between the bushing 560 and the valve shaft 544 . The interaction of the bushing 560 and the valve shaft 544 also reduces and eliminates soot and condensation that build up on the valve stem 544 and bushing 560 interface. A lip seal 562 is fitted on the top of the bushing 560 and is retained by a seal retainer 564 .
The valve apparatus 516 further includes a resilient member 568 positioned around the shaft 530 . In one example, the resilient member 568 is a spring. The resilient member 568 biases the valves 528 a and 528 b to the closed position. In the event of a power loss, the resilient member 568 closes the valve assembly 516 and acts as a fail-safe mechanism.
FIG. 7 illustrates an air venturi valve apparatus 416 . Fresh air enters from a fresh air inlet 432 in a first elongated tube 424 and exhaust gas enters from an exhaust gas inlet, mixing in a chamber 436 of a housing 442 . The fresh air/exhaust gas mixture exits the housing 442 through a fresh air/exhaust gas mixture outlet 438 in a second elongated tube 426 , leading back to the system.
When the fresh air/exhaust gas mixture is to be released back into the system, the motor 414 rotates a shaft 444 of a poppet 430 threaded in the first elongated tube 424 , separating a pintle 448 from an orifice 446 . As the pintle 448 moves away, the fresh air/exhaust gas mixture passes through the orifice 446 and into the system. The farther away the pintle 448 is positioned from the orifice 446 , the more fresh air/exhaust gas mixture is allowed to pass through the orifice 446 and back into the system.
By rotating the threaded valve shaft 444 , the pintle 448 of the poppet 430 can be repositioned depending on the system requirements. When no fresh air/exhaust gas mixture is to be allowed back into the system, the valve shaft 444 is rotated such that the pintle 448 is secured in the orifice 446 , blocking the flow of fresh air/exhaust gas into the second elongated tube 426 and into the system.
There are many advantages to operating the EGR system with the electric D/C motor 14 . First, the motor 14 can proportionally open the valves 28 , allowing for various flow ranges. Secondly, the motor 14 achieves a faster response than the vacuum actuators of the prior art. Additionally, this EGR system reduces space requirements within the engine compartment due to the compact size of the motor 14 .
The foregoing description is exemplary rather then defined by the limitations within. Many modifications and variations of the present invention are possible in light of the above teachings. The preferred embodiments of this invention have been disclosed, however, so that one of ordinary skill in the art would recognize that certain modifications would come within the scope of this invention.
|
An EGR valve apparatus regulates the amount of exhaust gas recirculated in an EGR system. The EGR valves are opened or closed by a rotatable shaft which is actuated by a motor. Alternatively, the valves can be balanced on the shaft, the valves moving in opposing direction during rotation. An inline poppet can be employed to overcome pressure in the system prior to movement of the valves. In another alternative embodiment, the motor rotates threaded shaft to move a pintle towards and away from an orifice.
| 5
|
RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 62/176,378 filed on Feb. 13, 2015.
BACKGROUND
[0002] a. Field of the Invention
[0003] The present invention relates generally to frames and similar structures that support growing plants, and, more particularly, to a spring-shaped frame that trains the plant in a manner that allows control of apical dominance to be achieved in an efficient, cost-effective and low stress manner.
[0004] b. Related Art
[0005] Farmers and gardeners look for ways of increasing conditions and improving quality in their plants. Providing a plant with optimum environmental (e.g., water, light, soil/medium, CO 2 ) and nutritional support can go a long way towards achieving these goals. Beyond meeting a plant's environmental and nutritional needs, gardeners also often explore and employ methods of training to take a plant's yield and quality to a higher level. Certain fast growing plants, such as tomatoes for example, can benefit from increased branching. Also it can be advantageous to have evenly proportioned branches, as compared to apical dominance. Apical dominance refers to the process wherein the axillary buds (side or lateral shoots) remain dormant and are reserved by the auxin (plant hormone) that is produced by the apical shoot. When a plant's apical shoot is left intact and unbent the plant tends to take on a conical shape much like a Christmas tree, which is unsatisfactory for production of many vegetables and other crops.
[0006] Removing apical dominance is achieved by either cutting (also referred to as pinching, pruning, topping and heading off) or bending of the plant's apical shoot. Cutting or bending the apical shoot removes the auxin's inhibitory effect on the axillary shoots so that growth of the latter is enhanced. Depending on the desired size of plant, and in order to distribute hormones and resources as evenly as possible among the branches/shoots, further pinching or bending may be necessary. This results in an increased number of equally proportioned branches and aids in training the plant for improved quality and increased yield. The shape of a plant trained in this manner is often that of an inverted cone.
[0007] Removing growing shoots by cutting and pinching is perhaps the least time consuming method of training plants commonly employed by growers. Gardeners often use a form of shears to remove a growing tip (some may use only their hands and/or finger nails for smaller shoots). However, there are significant drawbacks to cutting a stem or stalk of a plant. First, an open wound left behind where cutting took place, leaving a plant exposed to infection or disease until the wound is healed. Second, growth vigor is lost while the plant repairs the injury and redirects growth hormone to other shoots/branches. In combination this results in lost time and growth opportunity during healing and redistribution of growth/hormone, which in turn may reduce yield and quality (if dealing with natural growing seasons), or may increase the time to harvest (if climate and environmental controls are in effect). As an additional drawback, auxins are transported down the stem to the roots; loss of auxin, due to removing an apical shoot, may result in less stimulated root growth and root branching.
[0008] An alternative to pinching/cutting is bending. This can take various forms, from simply folding a growth shoot over, to attaching it to stakes trellis, netting or wires (e.g., an espalier), wrapping and bending with wire (e.g. bonsai), pulling it down and applying hanging weights, tying it down with cordage and stakes, and so on. After a growth shoot is bent it will immediately begin turning itself vertical again due to the effect of gravitropism (plant shoots display negative gravitropism; when placed on its side, a plant shoot will grow up against gravity) and will soon require further bending. Bending is advantageous relative to cutting in that it does not create an open wound and no auxin is lost. The main drawback of bending is that when using conventional techniques it is often much more time-consuming than cutting. This is a particular problem in commercial operations dealing with large numbers of relatively fast-growing plants, where the labor intensive aspects of conventional bending approaches become greatly compounded.
[0009] Commercial growers also often use artificial lighting, in whole or in part, to expedite growth as compared with the natural growing season, and the cost of electricity creates the need to use the artificial light efficiently. Reducing the amount of time and electricity to produce crops requires that plants not be subjected to cutting for controlling apical dominance, in order to retain auxin and shorten the time from seed to harvest. Being able to adjust the orientation/angle of the plants may also help maximize utilization of light sources. Furthermore, for a variety of reasons pots or other containers are conventionally used to grow plants in commercial environments, and in order for a training technique/device to be most useful it is desirable that the containers remain individually mobile, rather being attached to trellises or other structures that interconnect plants such that they and their containers are not easily moved about.
[0010] Thus, while prior methods of pruning and training are effective in increasing the number of evenly proportioned branches and therefore productivity, the drawbacks/limitations that are inherent to such methods leave a significant void when it comes to overcoming apical dominance in a rapid and efficient manner.
[0011] Therefore, a need exists for a method and apparatus that overcomes apical dominance while reducing the amount of stress placed on the plant from training. Furthermore, there exists a need for such a method and apparatus that is easy to learn and that can be implemented in a rapid and efficient manner, especially when working with multiple plants. Still further, there exists a need for such a method and apparatus that facilitates efficient and economical use of lighting and other growing resources. Still further, there exists a need for such a method and apparatus that may be implemented using structural components that are economical to manufacture and transport, and that are adequately durable and long-lasting to permit reuse if desired.
SUMMARY OF THE INVENTION
[0012] The present invention addresses the needs noted above, and concerns the growing and training of climbing, vining, branching, flowering, and fruiting plants, such as tomatoes or other vegetables or fruits, for example.
[0013] The invention controls apical dominance and achieves a number of relatively evenly proportioned branches/growing shoots, without the drawbacks of cutting/pinching and without the labor-intensive and time-consuming aspects of conventional bending practices. The structure employed is mobile and if desired can be set up in an individual pot or other container so plants may be moved about as needed or desired. Apical shoots are not cut off, so auxin is not lost and growth vigor is maintained, resulting in shortened time frames from seed to harvest and minimization of resource consumption and days/hours of labor. In a preferred embodiment the invention is self-guiding/instructing in design and is therefore easily learned and implemented in small- or large-scale applications.
[0014] In a first aspect the invention provides a spring-shaped frame, suitably formed of wire, referred to from time to time herein as simply a “spring.” The spring may take the shape of a Fibonacci or Golden Spiral that expands from a first center/starting point for a determined number of quarter turns, from which point the spring may contract by a similar number of quarter turns to a second center point so as to create two substantially symmetrical mirrored/opposed Golden Spirals. Preferably, the entire spring, including both Golden Spirals, may be formed of a single length of wire. A pitch may be applied to the spirals, for example by elevating one of the center points while the other remains fixed. Both the pitch and number of quarter turns the spirals make may be increased or decreased to accommodate various applications, uses and types of plants.
[0015] Depending dimensions and use of the spring, attachment portions may be applied to the center point of each spiral that permit the spring to be attached to a stake or pole member that is inserted through both center points and into the soil or medium below. The attachment points may be continuations of the wire spring, and may be angled out from both the bottom and top spiral center points. The stake may be oriented at a selected angle to the soil line, for example, by an angle of approximately 80° off the soil line in a preferred embodiment. The proximity of the spring to the soil line may be adjusted by sliding the spring up or down the angled stake; once the desired position is reached, the attachment points may be secured to the angled stake, using cable ties or other connectors, for example. The angled stake may be supported by a second stake by positioning a second slake to meet with the top of the angled stake so that the arrangement results in a triangle, with the stakes making up two sides and the soil line the third.
[0016] The present invention also provides a method for enhanced production from plants using controlled apical growth. In one aspect, a young plant may be positioned in the soil/medium near the center point of the spring closest to the soil/medium line and the plant allowed to grow vertically until its apical growth tip is above where it is to be attached to the spring frame as described above. Since bending the very tip of a growth shoot could result in snapping or splitting of the stem, it is preferable to bend further down the stem where tissues are more durable and hardened. At the point where the stem is sufficiently durable and in the proper position, a movement it may be made to bend the plant and the tip is then attached to the spring, using clips, twist ties or other connectors, for example. After the bend is made the plant may be left alone for a period of time so as to allow the plant to reorient to the new position and harden before bending again. As the growth rate of the plant increases, the wait time between bends may be reduced. The original apical shoot may be tied back down to the spring again and again while the axillary shoots are exposed to the light and their growth is thereby enhanced. Training to the spring may be continued until the plant has the desired number of shoots and the original apical shoot may then be allowed to grow vertically for the remainder of the plant's life cycle.
[0017] These and other features and advantages of the present invention will be more fully appreciated form a reading of the following detailed description in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIG. 1 is a schematic representation of an example Fibonacci spiral, namely, an approximation of the Golden Spiral created by drawing circular arcs connecting the opposite corners of squares in the Fibonacci tiling, the example in FIG. 1 using squares of sizes 1 , 1 , 2 , 3 , 5 , 8 , 13 , 21 and 34 ;
[0019] FIG. 2 is a schematic view of two example Fibonacci spirals arranged in mirrored positions with points placed along the arcs of the spirals lettered from A-I, the lettered points being used for reference in FIGS. 3 and 4 ;
[0020] FIG. 3 is a schematic view of the two example Fibonacci spirals without tiling squares, and with lettered points for reference, the spirals being continuous and having arrows to show the direction of spiral expansion and spiral contraction, the arrows also being used for reference with respect to FIG. 4 where a pitch is applied to the spirals;
[0021] FIG. 4 is a side schematic view of expanding and contracting Fibonacci spirals having an example 30° pitch, with lettered points and arrows corresponding to FIG. 2 and FIG. 3 ;
[0022] FIG. 5 is a side view of a spring-shaped frame in accordance with the present invention, having a pitched Fibonacci spiral configuration that correlates to that of FIGS. 2-4 , with the lettered points and arrows having been removed and with stakes connected to attachment points at each end of the spring-shaped frame;
[0023] FIG. 6 is a front perspective view of the spring-shaped frame of FIG. 5 , attached to an angled stake, supported by an additional stake and set in a pot with soil and no plant;
[0024] FIG. 7 is a side perspective view of the spring-shaped frame of FIG. 5 , attached to an angled stake, supported by an additional stake and set in a pot with soil and no plant;
[0025] FIG. 8 is a top plan view of the spring-shaped frame of FIG. 5 , attached to an angled stake and set in a pot with soil and no plant;
[0026] FIG. 9 is an enlarged perspective view of the spring-shaped frame of FIG. 5 , showing the lower attachment point in greater detail;
[0027] FIG. 10 is a second enlarged perspective view of the spring-shaped frame of FIG. 5 , showing in greater detail the upper attachment point and the joint formed by the angled stake and support stake;
[0028] FIG. 11 is a perspective view of the spring-shaped frame of FIG. 5 attached to an angled stake and supported by an additional stake, and set in a pot with soil together with a plant;
[0029] FIGS. 12-15 are perspective views of the spring-shaped frame of FIG. 5 , attached to an angled stake and supported by an additional stake, and set in a pot with soil and a plant attached thereto and growing up the frame;
[0030] FIG. 16 is an enlarged perspective view of the spring shaped frame of FIG. 5 attached to an angled stake, showing in greater detail the first attachment of the plant to the spring shaped frame; and.
[0031] FIG. 17 is an enlarged perspective view of a plant attached to and growing up the spring-shaped frame of FIG. 5 .
DETAILED DESCRIPTION
[0032] In nature growth frequently occurs in geometrically proportionate ways or patterns. These growth patterns have been linked to a mathematical expression referred to as Fibonacci Sequence or Golden Ratio. As shown in FIG. 1 Fibonacci Sequence 10 ( 1 , 1 , 2 , 3 , 5 , 8 , 13 , 21 , 34 ) squares 14 and Spiral 12 grow at a rate similar to that of PHI 1.618 for each quarter turn from the center point 20 . The Fibonacci Spiral and the Golden Spiral are very close approximations of one another and are considered equivalents for purposes of the present invention.
[0033] These natural growth patterns are often expressed in the spiral shape, for example, as seen in the nautilus shell, snail shell, fern, arrangement of sunflower seeds on a sunflower, and so on, a spiral being a curve on a plane that winds around a fixed center point at a continuously increasing distance from the center point. In natural growth of plants there is no simpler law than this, namely that it shall widen and lengthen in the same unvarying proportions.
[0034] It has been found, through the use of the present invention, that by applying the Fibonacci Spiral to a wire, which is then pitched to a desired degree to form a double-spiral spring-shaped support as shown in FIG. 4 , an effective means of overcoming apical dominance without removal of the apical shoot is provided. Furthermore, the arc 15 of the spring 38 opens up the plant in accordance with natural growth patterns and increases exposure to axillary shoots 58 and leaves. As the plant grows larger the Fibonacci Spiral continues to open up, increasing space for more and larger leaves, stems and shoots. The pitch applied to the arc 15 of the spring 38 provides control in overcoming apical dominance. Thus the desired pitch of the spring 38 relates to independent growth behaviors/patterns of various plant type (e.g. slow growing plants may prefer a lower pitch and fast growing plants a higher pitch). When the appropriate pitch is applied to the Fibonacci. Spiral for the plant being grown upon it, a harmonizing of growth is found. That is, the apical growth tip 54 and the axillary shoots 58 find an even pace of vertical growth 64 that continues to increase the number of evenly proportioned shoots/branches as long as the apical growth tip 54 is continually attached back to the spring 38 . This technique can for purposes of the present invention be referred to as “Apical Tuning” or “Tuning the Apex”. Once the desired plant size is achieved, bending may be discontinued and the apical growth tip 54 is allowed to continue vertically.
[0035] FIG. 2 shows two Fibonacci Spirals in a mirrored position 13 with tiling squares. This arrangement of the Fibonacci Spirals provides the mathematical basis for the dimensions for the spring-shaped frame 38 whether scaled up or down in size. Points A-I 16 are points of reference to be used in FIG. 3 and FIG. 4 .
[0036] FIG. 3 shows the Fibonacci Spirals with the tiling squares removed. The arrows 18 show the direction of the spirals' expansion and contraction and that they are continuous from center point 20 to center point 22 .
[0037] FIG. 4 shows a side view of the Fibonacci Spirals with a pitch applied. The arrows 18 show the direction of spiral expansion and contraction. Beginning with the lower center point 20 the Fibonacci Spiral 26 expands until it crosses the center line 24 at point E 16 a. The Fibonacci Spiral 28 then contracts the same or approximately the same number of turns before ending at the upper center point 22 . The pitch applied in the example in FIG. 4 is 30° or 33%, though other pitches may be applied, depending for example on the type of plant. It should be noted that FIG. 4 is 2-dimensional and therefore does not describe the depth of the spirals' arcs 15 , shortening the distance between points A-I 16 , having the effect of increasing the appearance of the applied pitch.
[0038] In accordance with an exemplary embodiment of the present invention, FIG. 5 shows a spring-shaped frame 38 . As shown, the spring-shaped frame 38 includes upper and lower Fibonacci Spiral portions 26 and 28 that correspond to the configuration of the Fibonacci segments shown back in FIG. 4 . The frame 38 is suitably constructed of bent wire, though other materials may be used, such as extruded plastic, composites, wood, bamboo, or tubing, for example. Furthermore, while the frame may be in the form of a self-supporting coil as shown, it will be understood that some embodiments may include spokes, struts, webs, and other forms of internal and/or external structure as well.
[0039] In FIG. 5 The spring-shaped frame 38 is shown attached to an angled support stake or rod 30 that parallels/passes alongside the attachment points 32 , 34 at each end. The stake 30 is preferably angled between 1-89° with respect to vertical as indicated by the vertical axis 24 , with an angle of about 80° being preferred to maximize utilization of light resources in many applications. The second stake 36 extends from the soil 52 generally vertically and meets at 40 the apex of the angled stake 30 . Using a cable tie 44 or other connector a joint is formed at the point 40 where the second stake 36 and the angled stake 30 meet, thus forming a triangular shaped configuration 42 that provides stability and ease of use.
[0040] In accordance with a method of the present invention a plant 46 may be trained to spring 38 as follows. As can be seen in FIG. 11 a young plant is first planted in the soil or other medium. Before any training is applied a period of time is allowed to pass so that the plant 46 may become established and begin to expand its roots into the newly available soil/medium 52 , in its new location/pot 48 . However, setup of the spring 38 may be done at this point rather than later, which will reduce the possibility of driving a stake through the newly formed roots. The angled stake 30 is set into the soil 52 so the spring 38 will be positioned in a manner that the spring 38 and plant 46 will intersect as the plant 46 grows vertical. It is preferable to have this intersection between plant 46 and spring 38 take place as close to the soil line 50 as possible, and also as close to the center point 20 of the base of the spring 38 as possible. In so doing, care should be exercised that the stake 30 is not inserted into the root ball in order to avoid injuring the young plant 46 . The spring 38 may be slid down the angled stake 30 by guiding the stake 30 through the bottom and top center points 20 and 22 of the spring 38 until the preferred distance between the soil line 50 and the bottom center point 20 of the spring 38 is reached. The spring 38 is rotated around the stake 30 until the pitch of the spring 38 is in proper relationship to the soil line 50 . For example; if the pitch of the spring 38 is set at 30° then it is attached to the stake 30 so that the 30° pitch is maintained in relation to the soil line 50 .
[0041] The spring 38 is then attached, using cable ties or other connectors 44 , to the angled stake 30 by way of the attachment portions 32 and 34 located at the top and bottom center points 20 and 22 . In the illustrated embodiment the attachment portions 32 and 34 are a continuation of the spring 38 using the same material, although separate pieces may be employed in some instances. The attachment portions 32 and 34 are angled out the top and bottom center points 20 and 22 and aligned with the angled stake 30 for accessibility, attachment and removal. The second stake 36 is positioned in the soil 52 at or near vertical and so the uppermost portion of the stake 36 intersects 40 with the uppermost portion of the angled stake 30 . The second stake 36 stabilizes the position of the angled stake 30 and the spring 38 . Before attaching the second stake 36 to the angled stake 30 , check for proper positioning of the pitch of the spring in relation to the soil line 50 .
[0042] After the plant 46 has begun to establish new roots and shoots an assessment of the plant's 46 readiness for bending is conducted. First the apical growth tip 54 is ascertained to be above the position on the spring 38 where attachment 56 and training/tuning is to begin. Bending may be carried out at a location spaced down from the tender growing tip where the stem has begun to harden but is still receptive to bending without breaking. It is when this hardened yet supple part of the stem is directly across from the selected position on the spring that the movement of bending the stem is to be carried out. As can be seen in FIGS. 12 and 16 , the stem 60 is bent so that the arc of the bend is as open as possible. Sharp bends are preferably avoided as these could cause unnecessary damage to the plant 46 . The arc of the bend may be from the soil line 50 to the position on the spring 38 where training/‘apical tuning’ is to begin. Using a form of wire, clip, string 56 or other connector the hardened/supple portion of the plant 46 is tied down/attached 56 to the spring 38 . Again it is preferable to leave the fragile growing tip 54 alone and that it not be tied down to the spring 38 .
[0043] The plant 46 is then observed as it reorients to its new position so that the apical growing tip 54 begins to grow vertical 64 again due to the effects phototropism and gravitropism. This new position overcomes the apical dominance of the apical growing tip 54 and the effect of auxin on the axillary shoots 58 is diminished while the increased exposure to light enhances axillary shoot 58 growth, and thus the axillary shoots 58 turn vertical 64 as well. Axillary shoots 58 may be thinned out 62 as shown in FIG. 16 , or left alone as determined/decided by the grower. Subsequently as shown in FIG. 13 , the apical growth tip 54 (what was the original apical shoot) is attached further up the arc of spring 38 . Readiness for bending is again assessed in the manner described above, and another bend is then applied to appropriate spot in the stem. The second bend, training the plant 46 up the arc and pitch of the spring 38 , continues to overcome apical dominance and exposes new axillary shoots 58 to light, thus enhancing their growth as can be seen in FIGS. 14-15 . A sequence of additional bends are applied to the original apical shoot 54 , in the same manner up the arc of the spring 38 , continually overcoming apical dominance and exposing more axillary shoots 58 to light. Finally the original apical shoot 54 may be allowed to continue its vertical growth when the desired number of evenly proportioned branches and shoots has been obtained and apical dominance is sufficiently overcome.
[0044] The above steps for training the apical tip can be applied to any desired stage in the life cycle of the plant (e.g. flowering and fruiting) and to any growing tip on the plant that may benefit from training to overcome apical dominance. Springs 38 of varying scale/dimension/pitch, while maintaining the Fibonacci/Golden Spiral pattern, can be applied to a wide range of growing situations where apical dominance is of concern.
[0045] The method steps described above can be carried out rapidly with minimal labor, and require very little training to understand and perform. The system is therefore well suited to use by a large-scale commercial growing facility having multiple employees. The training of the plant can maximize utilization of artificial light and other resources supporting growth of the plants and consequently reduce costs as compared with traditional growing techniques. Furthermore, the spring-shaped support of the invention is exceptionally economical to fabricate and when compressed can be transported/stored compactly in large numbers, contributing to low cost, and can be made sufficiently durable for reuse in applications where this may be desired.
[0046] It will be understood that the scope of the appended claims should not be limited by particular embodiments set forth herein, but should be construed in a manner consistent with the specification as a whole.
|
An apparatus and method for controlling apical growth of plants without cutting or pinching so as to increase productivity and efficiently utilize growth resources. A spring-shaped frame is provided having the form of mirror image/opposed Fibonacci or Golden Spirals that expand from a first starting point and then contract back to a second starting point by an approximately similar number of quarter-turns, the spring suitably being formed of a single length of wire. The apical growth tip of the plant is bent to meet the frame at selected locations and attached progressively as growth proceeds, using ties or other connectors. A stake inserted through the starting points of the spiral attaches the frame to the medium in which the plant is rooted. The stake is preferably angled so that the plant maximizes utilization of available light, for example, approximately 80° to the surface of the medium.
| 0
|
CROSS REFERENCE TO RELATED APPLICATION
[0001] The present application is a continuation of international application PCT/DE03/05170, filed 16 May, 2003, and which designates the U.S. The disclosure of the referenced application is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The invention relates to an apparatus and method for spinning and depositing a tow of the general type disclosed in EP 0 875 477 A2.
[0003] In the production of staple fibers, it is known to spin an individual tow from a polymer melt in a first processing step, and to deposit it into a can. In a second processing step, a plurality of individual tows are withdrawn from the respective cans and combined to a common tow and cut to staple fibers by means of a fiber cutter. The apparatus which is used exclusively for carrying out the first process step, forms the basis of the present invention.
[0004] For spinning and depositing a tow, the known apparatus comprises a spinning device for spinning a plurality of fiber bundles, a withdrawal system with a plurality of rolls for withdrawing the tows formed by the fiber bundles, and a depositing device for laying the tow into a can. To apply the necessary withdrawal forces, the withdrawal system comprises a plurality of rolls, one following the other in offset relationship, so that the tow advances through the withdrawal system along an S-shaped path by partially looping the rolls. In so doing, the tow advances over the intermediate rolls with a partial looping of preferably at most 180°. These deflections are needed on the one hand for producing high withdrawal forces. On the other hand, they lead to significant problems with threading the tow at the beginning of the process. In this connection, the tow must be manually inserted into the predefined S-shaped guide path, which requires applying accordingly great manual forces in particular in the case of relatively thick tows.
[0005] It is therefore an object of the invention to further develop an apparatus as well as a method of the initially described type in such a manner that the tow can be pieced and threaded at the beginning of the process by a more simple handling procedure.
[0006] It is a further object of the invention to make the withdrawal of the tow from the spinning device as flexible as possible.
SUMMARY OF THE INVENTION
[0007] The above and other objects and advantages of the invention are provided by a spinning apparatus and method of the described type and wherein at least one of the rolls of the withdrawal system is supported form movement on the machine frame in such a manner to permit changing of the guide path of the tow between the rolls. Thus the degree of looping between the tow and the rolls of the withdrawal system can be varied and adjusted. With that, it is possible to adjust to configurations with a high degree of looping for building up high withdrawal forces, or to configurations with a small degree of looping for building up correspondingly low withdrawal forces, or for threading and piecing the tow.
[0008] The range of adjustment of the looping angles is preferably from 0° to 180° on the intermediate rolls of the withdrawal system. To this end, at least some of the rolls in the withdrawal system are mounted for displacement to the machine frame in such a manner that they permit changing the guide path of the tow. The movability of the rolls in the withdrawal system serves only for adjusting a defined guide path of the tow or a defined looping angle. During the spinning and depositing of the tow, the movable rolls are secured in their respective positions on the machine frame, so that no undesired change of the guide path or the looping angle can occur.
[0009] A particularly advantageous further development of the invention provides for making the movable rolls adjustable between a threading position and an operating position. In this case, the tow advances in the threading position substantially without partial looping along a straight path between the rolls of the withdrawal system. Only after the movable rolls have been adjusted and secured in their operating position, will the tow advance with a corresponding partial looping over the rolls along an S-shaped path for applying the withdrawal forces.
[0010] To be able to thread the tow during the piecing step in a simplest possible manner, a spacing is formed between the stationary rolls and the movable rolls in the threading position, so that the tow can be inserted into the withdrawal system with no significant contact.
[0011] After the insertion of the tow into the withdrawal system, the rolls that are mounted for displacement to the machine frame are moved from their threading position to their respective operating position. To this end, the movable rolls can be adjusted synchronously, namely at the same time. With that, it is possible to obtain short times for piecing and threading the tow.
[0012] However, it is also possible to bring the movable rolls sequentially, i.e., one after the other, from their threading positions to their operating positions. With that, the withdrawal tension in the tow is prevented from rising suddenly, and is instead allowed to build up in the tow slowly.
[0013] The apparatus and method for the invention further includes a depositing device for laying the withdrawn tow into a can. The depositing device preferably comprises two cooperating conveying rolls, of which at least one of the conveying rolls is made movable for displacement between an operating position and a threading position. This is especially suited for automating the threading and piecing steps of the tow. In this connection, a spacing between the conveying rolls is formed in the threading position of the conveying rolls, which facilitates the insertion of the tow.
[0014] Advantageously, the withdrawal system and the depositing device are successively arranged such that in the threading position of the movable rolls of the withdrawal system and in the threading position of the movable conveying roll of the depositing device, it is possible to insert the tow into a common, straight line guide path.
[0015] In an arrangement wherein the spinning device, the withdrawal system, and the depositing device are arranged in tiers one on top of the other, it is easy to advance the tow from the spinning device automatically through the withdrawal system and the depositing device into an available can. As soon as the piecing and threading steps of the tow are completed, both the movable rolls and the movable conveying roll are moved to their respective operating position, and production can start.
[0016] The apparatus and the method of the invention are suited in particular for spinning and depositing thick tows with coarse deniers of the fiber bundles of, for example, >12,000 dtex. The spinning device may comprise a plurality of spinnerets arranged in parallel side-by-side relationship for producing a plurality of fiber bundles, or one spinneret with, for example, at least 8,000 spin holes. Spinnerets of this type allow realizing high melt throughputs of more than 500 kg/h, which result in a correspondingly thick tow. Thus, the apparatus of the invention is also suited for being combined with a plurality thereof to form a complete production line.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] In the following, several embodiments of the apparatus according to the invention and the method of the invention are described in greater detail, with reference to the attached drawings, in which:
[0018] FIG. 1 . 1 and are schematic views of a first embodiment of the apparatus according to the invention; and
[0019] FIG. 2 is a schematic view of a further embodiment of the apparatus according to the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0020] FIG. 1 . 1 shows the apparatus during the piecing and threading steps of the tow, and FIG. 1 . 2 shows the apparatus in operation during the production of the tow. The following description will apply to both Figures, unless express reference is made to one of the Figures.
[0021] The apparatus comprises a spinning device 1 , a withdrawal system 2 extending downstream of the spinning device 1 , a subsequent depositing device 3 , and a can 4 arranged downstream of the depositing device 3 . The can 4 is supported on a can traversing device 5 .
[0022] The spinning device comprises two spinnerets 6 . 1 and 6 . 2 , which are arranged in a parallel, side-by-side relationship. Each of the spinnerets 6 . 1 and 6 . 2 connects via a melt supply line 17 . 1 and 17 . 2 to a melt source (not shown). On their underside, the spinnerets 6 . 1 and 6 . 2 comprise a plurality of spin holes, from each of which a fiber is extruded. The spinnerets 6 . 1 and 6 . 2 may comprise more than 80,000 spin holes. Thus, each of the spinnerets 6 . 1 and 6 . 2 extrudes a fiber bundle 7 . 1 and 7 . 2 . Downstream of the spinnerets, the spinning device 1 normally comprises cooling devices, which generate a cooling air stream for cooling the fiber bundles. In the present embodiment, the cooling device has been omitted. Likewise the number of the spinnerets of spinning device 1 is exemplary. Thus, three, four, five, or even more spinnerets may be arranged in a parallel, side-by-side relationship, with their fiber bundles being each combined to a tow.
[0023] To combine the fiber bundles 7 . 1 and 7 . 2 to a tow 15 , a plurality of fiber lubrication elements 8 . 1 - 8 . 4 are arranged between the spinning device 1 and the withdrawal system 2 . During the process, the fiber lubrication elements 8 . 1 - 8 . 4 apply a lubricant to the fiber bundles 7 . 1 and 7 . 2 or the tow 15 . In the present embodiment, the fiber lubrication elements 8 . 1 - 8 . 4 are lubrication rolls. However, it is also possible use lubrication pins.
[0024] Arranged downstream of the lubrication rolls 8 . 1 - 8 . 4 is the withdrawal system 2 . The withdrawal system 2 comprises a plurality of rolls 9 . 1 - 9 . 3 that extend one after the other in a vertical plane. The rolls 9 . 1 - 9 . 3 are rigidly mounted to a machine frame 12 . Between the rolls 9 . 1 and 9 . 2 , the machine frame 12 includes a linear guideway 11 . 1 , in which a roll 10 . 1 is arranged for displacement. Between the rolls 9 . 2 and 9 . 3 , the machine frame likewise includes a linear guideway 11 . 2 , in which a roll 10 . 2 is arranged for displacement. In their respective linear guideways 11 . 1 and 11 . 2 , the rolls 10 . 1 and 10 . 2 can be moved between a threading position and an operating position. In this process, the rolls 10 . 1 and 10 . 2 are moved transversely to the direction of the advancing tow 15 .
[0025] FIG. 1 . 1 illustrates the situation, in which the movable rolls 10 . 1 and 10 . 2 of the withdrawal system 2 are held in a threading position on the machine frame 12 . To this end, the movable rolls 10 . 1 and 10 . 2 are displaced in their respective linear guideways 11 . 1 and 11 . 2 to the right side of the machine frame, so that the tow 15 advances along a straight path without partially looping the rolls 10 . 1 and 10 . 2 . Between the stationary rolls 9 . 1 , 9 . 2 , and 9 . 3 and the movable rolls 10 . 1 and 10 . 2 , a spacing is formed, so that the tow 15 is able to advance substantially without contact in the center of the withdrawal system 2 between the stationary rolls 9 . 1 - 9 . 3 and the movable rolls 10 . 1 - 10 . 2 . This arrangement is especially advantageous for inserting the tow 15 after piecing in a simple manner into the withdrawal system 2 .
[0026] After the tow 15 has been inserted into the withdrawal system 2 , the movable rolls 10 . 1 and 10 . 2 are displaced to the left in the linear guideways 11 . 1 and 11 . 2 on the machine frame 12 , so that the movable rolls 10 . 1 and 10 . 2 extend through the vertical plane of the stationary rolls 9 . 1 - 9 . 3 , and form an S-shaped guide path which is needed for withdrawing the tow 15 . This situation is shown in FIG. 1 . 2 . The stationary rolls 9 . 1 - 9 . 2 and the movable rolls 10 . 1 and 10 . 2 are arranged one after the other in offset relationship, so that the tow 15 passes each of the roll with a predetermined partial looping. In this situation, the movable rolls 10 . 1 and 10 . 2 are locked in position on the machine frame 12 .
[0027] For advancing the tow 15 , the rolls 9 . 1 - 9 . 3 as well as the rolls 10 . 1 and 10 . 2 are driven. In this connection, it is preferred to drive each of the rolls by a separate drive unit. However, it is also possible to drive groups of rolls by a group drive unit.
[0028] Downstream of the withdrawal system 2 is the depositing device 3 . The depositing device 3 is formed by two cooperating conveying rolls 13 . 1 and 13 . 2 . The conveying rolls 13 . 1 and 13 . 2 are driven at the same speed, so that the tow 15 uniformly advances into the can 4 that is placed below the depositing device 3 .
[0029] The can 4 may be moved by a traversing device 5 such that when depositing the tow 15 , the can 4 is evenly filled.
[0030] FIG. 2 illustrates a further embodiment of the apparatus according to the invention. The construction of the apparatus shown in FIG. 2 is largely identical with that of the foregoing embodiment of FIG. 1 , so that the foregoing description is herewith incorporated by reference, and that only differences will be described in greater detail.
[0031] In the embodiment shown in FIG. 2 , the spinning device 1 comprises only one spinneret 6 for producing a fiber bundle 7 . The fiber bundle 7 is combined via fiber lubrication elements 8 . 1 - 8 . 4 to the tow 15 .
[0032] The withdrawal system 2 is made identical with the foregoing embodiment. The present embodiment shows the situation, in which the movable rolls 10 . 1 and 10 . 2 are held in the threading position.
[0033] Downstream of the withdrawal system is the depositing device 3 . The depositing device 3 of the present embodiment is formed by a stationary conveying roll 13 and a movable conveying roll 14 . The movable conveying roll 14 is mounted in a guideway 18 , which permits displacing the movable conveying roll 14 between an operating position and a threading position. FIG. 2 shows the situation, in which the movable conveying roll 14 remains in the threading position. In this position, a spacing exists between the conveying rolls 13 and 14 , so as to permit inserting the tow 15 along a straight guide path from the spinning device 1 as far as the can 4 . This embodiment of the apparatus according to the invention is therefore especially suited for permitting an automatic piecing and threading of the tow 15 . In this instance, an operator needs to monitor only the piecing of the fiber bundle. The threading of the tow 15 into the withdrawal system 2 and depositing device 3 can occur automatically by falling into place.
[0034] As soon as the tow 15 advancing from the spinning device 1 enters the can 4 , the movable rolls 10 . 1 and 10 . 2 of the withdrawal system 2 and the movable conveying roll 14 of the depositing device 3 are returned to their respective operating position and secured therein. The adjustment of the rolls 10 . 1 and 10 . 2 and of the conveying roll 14 can occur by a common drive, which permits a synchronous adjustment of the withdrawal system and the depositing device. However, it is also possible to adjust the conveying roll 14 independently of the rolls 10 . 1 and 10 . 2 of the withdrawal system 2 .
[0035] In the case of the embodiments of the apparatus according to the invention and as shown in FIGS. 1 . 1 , 1 . 2 , and 2 , there basically also exists the possibility that during the operation, the movable rolls of the withdrawal system are previously moved to any position for adjusting defined degrees of looping. Thus, one could predetermine a plurality of operating positions, which are selected as a function of the denier of the tow for obtaining, for example, defined withdrawal forces.
[0036] The embodiments shown in the Figures are suited for adjusting on the rolls 10 . 1 and 10 . 2 different operating positions with looping angles greater than 0° and smaller than 180°.
[0037] The construction of the illustrated embodiments is likewise exemplary. Thus, they may comprise additional treatment devices as well as similar variants of configuration. For example, all rolls of a withdrawal system could be made movable for realizing a still greater flexibility in the configuration of the guide path and in the selection of the looping angles. Likewise, the adjustment of the depositing device may be realized by two movable conveying rolls.
|
An apparatus and a method for spinning and depositing a tow ( 15 ). To this end, one or more fiber bundles ( 7 ) are melt spun by means of a spinning device ( 1 ), and withdrawn as a tow by a withdrawal system ( 2 ). Subsequently, the tow ( 15 ) is laid by means of a depositing device ( 3 ) into a can ( 4 ). To be able to apply the necessary withdrawal forces to the tow ( 15 ), the tow ( 15 ) advances along an S-shaped guide path by partially looping the rolls ( 9, 10 ) of the withdrawal system ( 2 ). To be able to change the degree of the looping on the rolls, in particular for piecing and threading the tow ( 15 ), some of the rolls ( 10 ) of the withdrawal system ( 2 ) are mounted for displacement on the machine frame in such a manner that they permit changing the guide path of the tow ( 15 ).
| 3
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a PTC heating element with at least one PTC resistance element that is arranged between two electrically conductive plates in a housing opening of a housing and that, with at least one of the electrically conductive plates as an intermediate layer, is pressed with an initial tension against a heat-emitting element that is held by the housing.
[0003] 2. Description of the Related Art
[0004] Such a PTC heating element is known, for example, from EP 0 350 528, which is traced back to the applicant. In this state of the art, a number of PTC heating elements are arranged in a frame in a number of planes with heat-emitting elements, in the form of metal strips curved in a meandering manner, layered between. Located within the frame is a spring, which presses the two electrically conductive plates lying on the exterior of the PTC heating element against the PTC element for good thermal and electrical contacting and the heat-emitting elements against the adjacent electrically conductive plate for good heat transfer of the heat generated by the PTC resistance element. In the mentioned state of the art, the PTC heating element is used for heating air. There are, however, other embodiments also known in which the PTC resistance element heats a heating plate. Such embodiments are particularly known for heating or keeping warm foods, for example, baby food.
[0005] The problem forming the basis of the present invention is to specify a heating element of this category that can be manufactured simply and therefore economically.
[0006] To solve this problem, the present invention specifies a PTC heating element with the characteristics of Claim 1 . This differs from the category-defining state of the art by a housing opening, whereby attachment tabs that are arranged around the edge of the housing opening protrude from it and whereby the heat-emitting element has tab cuts behind which the tabs engage when a heat-emitting element is mounted on the housing.
[0007] As a result of this engaging, the heat-emitting element is connected to the housing in a simple manner, for example, by being locked in place. Alternatively, the tabs can also have a thickening on their free end that engages behind the tab opening, whereby this thickening is formed by surface-fusing the respective tab. Such thickened tabs are achieved, for example, by hot stamping.
[0008] The tabs, however, serve more than just to attach the heat-generating element to the housing. Rather, the tabs encircle the housing opening and protrude from the exterior of the housing opening. In this way, the tabs form a guide that forms a guide of the housing in the insertion direction of the electrically conductive plates and the at least one PTC resistance element, as a result of which the assembly is simplified. In addition to this, the tabs can be formed with a funnel-shape on the upper free end, in order to facilitate simple insertion of the two strip conductors with the at least one PTC resistance element arranged between them.
OBJECT OF THE INVENTION
[0009] The tabs of the PTC heating element according to the invention accordingly take on a double function. On the one hand, because of their arrangement relative to the housing opening, they allow a simple, guided insertion of the electrically conductive plates together with the at least one PTC resistance element. Furthermore, they securely hold in position the heat-emitting element after the final assembly.
[0010] According to a preferred further development of the present invention, the tabs project beyond an upper contact surface for the heat-emitting element, whereby this contact surface is formed by the housing and is at a height that is dimensioned in such a way that the electrically conductive plate that is raised above the contact surface by the initial tension before the placement of the heat-emitting element does not extend higher than the upper end of the tabs. In this way, it becomes possible to fix in place during the assembly the layer composition that emits the heat and that is held in the housing opening. Preferably the tabs are dimensioned in such a way that the upper electrically conductive plate that is raised above the contact surface is roughly at the same height as the upper end of the tabs. With a view to the most sparing use possible of material for forming the housing and tabs, these should project beyond the upper electrically conductive plate only slightly in the raised position.
[0011] For further simplification of the PTC heating element, according to a preferred development of the present invention it is proposed that the electrically conductive plate lying opposite the heat-emitting element, i.e., that electrically conductive plate that is provided on the side other than the heat-emitting element with respect to the PTC resistance element, be provided with at least one spring element that is formed by means of stamping processing and by bending the sheet metal material that forms the electrically conductive plate as a single piece on this sheet metal material and that is supported on the housing. The spring element is preferably cut out from the sheet metal material that forms the electrically conductive plate in such a way that it initially projects beyond the outside of the contact surface of the at least one PTC resistance element at the corresponding electrically conductive plate. The projecting section is then preferably bent under the electrically conductive plate at the back of the contact surface, and it can be supported on the housing with this spring leg, whereby this housing is preferably closed on its underside lying opposite the housing opening. In the context of the present invention, a cut that opens towards the contact surface for the heat-emitting element is particularly understood as a housing opening, whereby the size of this cut roughly corresponds to the dimensions of the PTC resistance element(s) held in the housing. In other words, the housing opening, when seen from the top, has roughly the contour of the PTC resistance element(s) of the PTC heating element.
[0012] With a view to secure and simple localisation of plug sockets connected with cables to an electrical current source for the electrical connection of the PTC heating element, according to a further preferred development of the present invention it is proposed that the housing be given two plug holders, each of which has a locking opening for engaging with a snap-in pin formed on the plug socket, whereby a contact stud formed by stamping processing and bending the electrically conductive plate is arranged in the plug holder and consequently electrically connected in a permanent and simple manner to the plug socket undetachably secured in the housing by means of the locking connection.
[0013] For simple securing of the two electrically conductive plates in the housing, it has proven advantageous to guide each contact stud to the respective electrically conductive plate out of the housing through a contact stud cut that is cut outside the housing opening on the underside in a direction at right angles to the plane of the electrically conductive plate, and by deflection into the plug holder, to bring it into an alignment in which the contact stud runs essentially parallel to the electrically conductive plate and is inserted into the plug holder. In this further development, only that cut in the housing that serves to hold the PTC resistance element(s) is understood as the housing opening. Consequently, a housing opening formed with the area of a single PTC resistance element can, for example, be cut into the housing. The electrically conductive plates have a contact section lying on the PTC resistance element, whereby a connection section that has been punched free protrudes on its exterior circumferential surface. This connection section initially lies in the plane of the sheet metal strip that forms the electrically conductive plate. A sub-area of the connection section, i.e., the front end of the connection section forming the contact stud, is then bent by 90°, so that the contact stud essentially extends from the plane of the sheet metal material at a right angle. In this state, the electrically conductive plate, with its contact section, is introduced into the opening of the housing. The contact stud here penetrates the contact stud cut that is cut into the underside of the housing and protrudes beyond the housing from the exterior. Subsequently, the protruding section is reshaped, for example, by a slide, and introduced into the contact stud holder that runs essentially parallel to the contact surface of the contact section, i.e., parallel to the bearing surface for the heat-emitting element. After this reshaping step, the respective strip conductor is held securely in the housing. The connection section of the electrically conductive plate is preferably surrounded relatively tightly by walls of the housing for this, and consequently held in a fixed position in the housing.
[0014] Further advantages and details of the present invention result from the following description, in conjunction with the drawing. This drawing shows:
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 a top view of the upper side of an embodiment of a PTC heating element with the heating plate removed;
[0016] FIG. 2 a perspective top view of the underside of the embodiment shown in FIG. 1 ;
[0017] FIG. 3 a longitudinal sectional view along the line III-III according to the depiction in FIG. 1 with the heating plate positioned; and
[0018] FIG. 4 a longitudinal sectional view along the line IV-IV according to the depiction in FIG. 1 with the heating plate positioned.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] The embodiment depicted in the drawing is a PTC heating element for heating baby food or keeping it warm, and this PTC heating element is held inside an injection moulded housing (not shown) which forms the holder for the container holding the baby food (bottle, jar). The PTC heating element shown in the drawing is located in the base of this injection moulded housing. This, with its heating plate 2 , forms the support for the container that holds the baby food and that stands directly on the heating plate 2 .
[0020] The embodiment shown in the drawing has a housing 4 , which essentially consists of three separated segments. Consequently, the housing 4 has a holder section 6 for holding a heat-emitting layer composition comprising a lower electrically conductive plate 8 , a PTC heating element 10 arranged in between with an essentially circular shape and an upper electrically conductive plate 12 (cf. FIG. 3 ). For holding this layer composition, the holder section 6 has an essentially round opening 14 that is only slightly larger than the layer composition. In this layer composition, the lower electrically conductive plate 8 and the upper electrically conductive plate 12 each have a round contact section 16 formed according to the contour of the round PTC element.
[0021] On opposite sides, electrically conductive plate receiving chambers 18 , 20 are provided that fork off through the housing 4 from the opening 14 and that open towards the opening 14 , whereby the bases of these can be raised slightly with respect to the base of the opening 14 .
[0022] The housing 4 forms two plug holders 22 , 24 , in addition to the holder section 6 . These plug holders 22 , 24 are covered with respect to the upper side of the PTC heating element shown in FIG. 1 by a covering 26 that is located below a contact surface 28 for the heating plate 2 , whereby this contact surface 28 is formed by the upper side of the housing 4 . This contact surface 28 runs essentially across the entire contour of the housing 4 along the edge.
[0023] Each of the plug holders 22 , 24 is formed for holding one plug socket 30 . The plug socket 30 essentially has a rectangular cross-section with flat upper and undersides 32 , 33 , as well as a snap-in pin 34 that projects from the upper side 32 (cf. FIG. 3 ). Corresponding to this, each of the plug holders 22 and 24 has a locking opening 36 that is cut into the interior side of the covering 24 or 26 in the shown embodiment, without penetrating the respective covering 24 , 26 .
[0024] As the section view according to FIG. 3 shows, the exterior base 40 of the plate receiving chambers 18 , 20 is at the same height as the underside 42 of the housing 4 . In extension of the edges of the plug holder 22 , 24 , contact bars 43 form the underside 42 of the housing 2 . Between the base 40 and the underside of the covering 24 , 26 , the housing 4 forms a limit stop 44 for the plug socket 30 . Below this limit stop 44 , the cut that is formed by the plug holder 22 , 24 and that is on the underside of the housing 2 is penetrated up to the back end of the same. In other words, the plug holder 22 or 24 continues beyond the cut 46 and until the rear end of the housing 4 . A contact stud holder 48 that, as a slot, connects the base 40 , exposed at the bottom, of the housing to the interior of the holder section 40 , opens towards the cut 46 , and is provided outside the opening 14 and in extension of the plug holders 22 , 24 .
[0025] The plug holders 22 , 24 are bordered on the bottom by a partition wall 50 that is provided in the front area of the plug holder 22 or 24 in the insertion direction of the plug socket 30 and that connects the two contact bars 43 of the respective plug holders 22 , 24 . Behind this, in the insertion direction, each of the plug holders 22 , 24 has a contact stud insertion opening 52 that, for reasons of injection moulding manufacture of the housing 4 , is formed with the width of the plug holder 22 or 24 (cf. FIG. 2 ).
[0026] As can be seen in FIG. 1 , three tabs 54 project beyond the contact surface 28 , whereby these three tabs 54 are provided on the edge of the round interior circumferential area of the opening 14 . The tabs 54 can be provided as a single piece with the housing 4 by means of injection moulding.
[0027] Alternatively, when the housing 4 is manufactured by injection moulding, tab cuts can be cut out and the tabs 54 can be inserted into these. In this development, it is, for example, possible to form the tabs with protruding springs on their underside ends, whereby these protruding springs are supported in the interior on the base of the housing opening 14 and press against the lower electrically conductive plate 8 , in order to press it, together with the PTC resistance element 10 and the upper electrically conductive plate 12 , against the heating plate 2 after assembly.
[0028] In an alternative development, which is realised in the shown embodiment, the lower electrically conductive plate 8 has protruding springs 56 formed in a single piece with it (cf. FIG. 4 ). These protruding springs 56 are initially formed by cutting free the sheet metal material forming the lower electrically conductive plate 8 and, in a following manufacturing step, bending them under the underside of the lower electrically conductive plate 8 , so that protruding springs 56 provided on the interior of the base 40 in a single piece with the lower electrically conductive plate 8 are formed. Preferably, a number of protruding springs 56 are provided on the circumference of the round contact section 16 and from there guided under the lower electrically conductive plate 8 .
[0029] The tabs 54 project beyond the contact surface 28 with a height that depends on two factors: firstly, the tabs serve to hold the pre-mounted layer composition. Due to the force of the protruding springs 56 , the layer composition is pressed against the interior side of the heating plate 2 after the assembly, for good heat transfer to the heating plate 2 . This means that before the final assembly, i.e., before the attachment of the heating plate 2 to the housing 4 , the layer composition protrudes beyond the contact surface 28 . The tabs 54 provided around the opening 14 and distributed around the circumference here ensure that the upper electrically conductive plate 12 remains within the circumferential surface of the opening 14 , even in this raised position.
[0030] Furthermore, the heating plate 2 has tab cuts 58 corresponding to the tabs 54 , whereby these tabs 54 engage behind these tab cuts 58 after the heating plate 2 is positioned on the contact surface 28 . For this purpose, the tabs 54 can have snap-in projections that engage behind the tab cuts 58 . In the embodiment shown, the tabs 54 are formed with a thickening 60 by means of hot stamping after the assembly of the heating plate 2 , whereby this thickening 60 protrudes beyond the tab cut 58 . Accordingly, the housing 4 and the heating plate 2 are undetachably connected to each other by means of the thickenings 60 of the tabs 54 .
[0031] For the electrical connection of the lower and upper electrically conductive plates 8 , 12 , these have connection sections 62 that go off from the contact sections 16 at opposite sides. Each connection section 62 can be subdivided into a contact stud base 64 , which is cut out by means of stamping processing and which runs in a radial direction with respect to the contact section 16 , and a contact stud 66 , which runs perpendicular thereto. The contact stud base 64 lies within the electrically conductive plate chambers 18 or 20 ; the contact stud 66 is electrically connected to the plug socket 30 .
[0032] For assembly, first the contact stud 66 is bent out of the plane of the sheet metal material at the transition to the contact stud base 64 by 90°. A fold 68 formed in this way is dimensioned in such a way that it lies in an extension of the slot-shaped contact stud holder 48 when the electrically conductive plate 8 , 12 is introduced into the opening 14 . During the assembly, i.e., during the insertion of the layer composition into the opening 14 , the contact studs 66 are accordingly inserted through the contact stud holders 48 . Subsequently, the linear section of the contact studs 66 that protrudes beyond the base 40 is turned by 90° on to the respective plug holder 22 or 24 by a slide, so that the front end of the contact stud 66 is deviated through the contact stud insertion opening 52 and into the plug holder 20 , 24 . This reshaping step normally takes place after the heating plate 2 has been attached to the housing 4 and consequently the layer composition is held in the opening 14 with respect to the height due to the initial tension of the protruding springs 56 . In this case, the contact stud 66 can be positioned between the contact stud holder 48 and the limit stop 44 , essentially against the base 40 , without there being any grounds for fearing the loss of the desired good heat transfer due to a flat fit of the upper electrically conductive plate 12 and the underside of the heating plate 2 . After the bending of the contact stud 66 , this then runs essentially parallel to the upper or underside 42 of the housing 4 , is essentially held in place with respect to the height by the base 40 and, due to the guide within the contact stud holder 48 , is fixed in place across the width within certain limits and secured in such a way that the plug socket 20 can be slid on to the contact stud 66 and consequently electrically contacted, without it being possible for the contact stud 66 to avoid the frictional forces acting here.
|
The present invention relates to a PTC heating element with at least one PTC resistance element which is arranged between two electrically conductive plates in a housing opening of a housing and, with at least one of the electrically conductive plates as an intermediate layer, which is pressed with an initial tension against a heat-emitting element which is held at the housing. With the present invention, a PTC heating element of the type mentioned at the beginning that can be manufactured easily and economically is to be specified. To solve this problem, the present invention further develops the PTC heating element mentioned at the beginning in such a way that attachment tabs arranged on the edge of the housing opening protrude beyond the housing opening and in such a way that the heat-emitting element has tab cuts, behind which the tabs engage.
| 5
|
CROSS-REFERENCE TO RELATED APPLICATIONS
Reference is made to and priority claimed from U.S. Provisional Application Ser. No. 60/430,219 Filed on Dec. 2,2002, entitled: UNIFORM COCRYSTALS OF TITANYL FLUOROPHTHALOCYANINE AND TITANYL PHTHALOCYANINE FORMED IN TRICHLOROETHANE, AND CHARGE GENERATING LAYER CONTAINING SAME.
Reference is made to the following co-pending, commonly assigned applications, the disclosures of which are incorporated herein by reference:
U.S. Provisional Patent Application Ser. No. 60/430,922, filed on Dec. 4, 2002, in the names of Molaire, et al., entitled SELF-DISPERSING TITANYL PHTHALOCYANINE PIGMENT COMPOSITIONS AND ELECTROPHOTOGRAPHIC CHARGE GENERATION LAYERS CONTAINING SAME;
U.S. Provisional Patent Application Ser. No. 60/430,923, filed on Dec. 4, 2002, in the names of Molaire, et al., entitled TWO-STAGE MILLING PROCESS FOR PREPARING COCRYSTALS OF TITANYL FLUOROPHTHALOCYANINE AND TITANYL PHTHALOCYANINE, AND ELECTROPHOTOGRAPHIC ELEMENT CONTAINING SAME;
U.S. Provisional Patent Application Ser. No. 60/430,779, filed on Dec. 4, 2002, in the names of Molaire, et al., entitled COCRYSTALS CONTAINING HIGH-CHLORINE TITANYL PHTHALOCYANINE AND LOW CONCENTRATION OF TITANYL FLUOROPHTHALOCYANINE, AND ELECTROPHOTOGRAPHIC ELEMENT CONTAINING SAME;
U.S. Provisional Patent Application Ser. No. 60/430,777, filed on Dec. 4, 2002, in the names of Molaire, et al., entitled PROCESS FOR FORMING COCRYSTALS CONTAINING CHLORINE-FREE TITANYL PHTHALOCYANINES AND LOW CONCENTRATION OF TITANYL FLUOROPHTHALOCYANINE USING ORGANIC MILLING AID.
FIELD OF THE INVENTION
The present invention relates to electrophotographic elements and related materials. More particularly, the invention relates to a process for forming nanoparticulate pigment compositions including cocrystalline titanium phthalocyanine pigments, and further to the inclusion of these compositions in the charge generation layers of electrophotographic elements.
BACKGROUND OF THE INVENTION
In electrophotography, an image including a pattern of electrostatic potential, also referred to as an electrostatic latent image, is formed on a surface of an electrophotographic element including at least two layers: a photoconductive layer and an electrically conductive substrate. The electrostatic latent image can be formed by a variety of means, for example, by imagewise radiation-induced discharge of a uniform potential previously formed on the surface. Typically, the electrostatic latent image is then developed into a toner image by contacting the latent image with an electrographic developer. If desired, the latent image can be transferred to another surface before development.
Among the many different kinds of photoconductive materials that have been employed in electrophotographic elements are phthalocyanine pigments such as titanyl phthalocyanine and titanyl tetrafluorophthalocyanines. Electrophotographic recording elements containing such pigments as charge-generation materials are useful in electrophotographic laser beam printers because of their capability for providing good photosensitivity in the near infrared region of the electromagnetic spectrum, that is, in the range of 700–900 nm.
Flocculation of organic pigment dispersions has been a recognized problem, especially in the paint and coating industry, for some time. For example, U.S. Pat. No. 3,589,924 in the names of Giambalvo, et al., describes improved non-crystallizing, non-flocculating phthalocyanine pigment compositions formed by mixing 60–95% of a crystallization-or flocculation-susceptible phthalocyanine pigment with about 5–40% of a sulfonated phthalimidomethyl phthalocyanine derivative. The mixture is prepared by the usual methods, e.g., acid pasting or salt grinding, for converting the phthalocyanine materials to pigmentary size. However techniques that are designed primarily to provide suitable pigments for paints and industrial coatings may not yield materials of sufficient purity or the appropriate crystallinity characteristics to meet the stringent requirements of electrophotographic applications, where high purity is very important for ensuring reliable performance. The crystalline form of the final pigment also has a profound influence on the performance of an electrophotographic element containing it.
In a photoconductive layer produced from a liquid coating composition that includes the titanyl phthalocyanine pigment and a solvent solution of polymeric binder, it is necessary that the titanyl phthalocyanine pigment be in a highly photoconductive form, either crystalline or amorphous, and in a sufficiently stable dispersion to permit its application as a very thin layer having high electrophotographic speed in the near infrared region.
A variety of methods have been used to produce suitable forms of titanyl phthalocyanine having differing crystallographic characteristics. U.S. Pat. No. 5,166,339 in the names of Duff, et al., presents a table of polymorphs of unsubstituted titanyl phthalocyanine in which materials bearing multiple designations are grouped as four types. Many phthalocyanine pigments are discussed in P. M. Borsenberger and D. S. Weiss, Organic Photoreceptors for Imaging Systems , Marcel Dekker, Inc., New York, pp. 338–391.
In one type of preparation, commonly referred to as “acid-pasting”, crude titanyl phthalocyanine is dissolved in an acid solution, which is then diluted with a non-solvent to precipitate the titanyl phthalocyanine product. In another type of procedure, the crude titanyl phthalocyanine is milled, generally with particular milling media. Additionally, some preparations include a combination of techniques or modify a previously prepared titanyl phthalocyanine.
U.S. Pat. No. 5,132,197 in the names of Iuchi, et al., teaches a method in which titanyl phthalocyanine is acid pasted, treated with methanol, and milled with ether, monoterpene hydrocarbon, or liquid paraffin to produce a titanyl phthalocyanine having main peaks of the Bragg angle 2Θ with respect to X-rays of Cu Kα at 9.0°, 14.2°, 23.9°, and 27.1° (all +/−0.2°).
U.S. Pat. No. 5,206,359 in the names of Mayo, et al., teaches a process in which titanyl phthalocyanine produced by acid pasting is converted to type IV titanyl phthalocyanine from Type X by treatment with halobenzene.
U.S. Pat. No. 5,059,355 in the names of Ono, et al., teaches a process in which titanyl phthalocyanine is shaken with glass beads, producing an amorphous material having no substantial peaks detectable by X-ray diffraction. The amorphous material is stirred, with heating, in water and ortho-dichlorobenzene; methanol is added after cooling. A crystalline material having a distinct peak at 27.3° is produced.
U.S. Pat. No. 4,882,427 in the names of Enokida, et al., teaches a material having noncrystalline titanyl phthalocyanine and pseudo-non-crystalline titanyl phthalocyanine. The pseudo-noncrystalline material can be prepared by acid pasting or acid slurrying. The noncrystalline titanyl phthalocyanine can be prepared by acid pasting or acid slurrying followed by dry or wet milling, or by mechanical milling for a long time without chemical treatment.
U.S. Pat. No. 5,194,354 in the names of Takai, et al., teaches that amorphous titanyl phthalocyanine prepared by dry pulverization or acid pasting can be converted, by stirring in methanol, to a low crystalline titanyl phthalocyanine having strong peaks of the Bragg angle 2Θ with respect to X-rays of Cu Kα at 7.2°, 14.2°, 24.0°, and 27.2° (all +/−0.2°). It is stated that the low crystalline material can be treated with various organic solvents to produce crystalline materials: methyl cellosolve or ethylene glycol for material having strong peaks at 7.4°, 10.9°, and 17.9°; propylene glycol, 1,3-butanediol, or glycerine for material having strong peaks at 7.6°, 9.7°, 12.7°, 16.2°, and 26.4°; and aqueous mannitol solution for material having strong peaks at 8.5° and 10.2° (all peaks +/−0.2°).
U.S. Pat. Nos. 4,994,566 and 5,008,173 both in the names of Mimura, et al., teach a process in which non-crystalline particles produced by acid pasting or slurrying, followed by mechanical grinding or sublimation, are treated with tetrahydrofuran to produce a titanyl phthalocyanine having infrared absorption peaks at 1332, 1074, 962, and 783 cm −1 .
U.S. Pat. No. 5,039,586 in the name of Itami, teaches acid pasting, followed by milling in aromatic or haloaromatic solvent, with or without additional water or other solvents such as alcohols or ethers, at 20–100° C. In an example, crude titanyl phthalocyanine is milled with α-chloronaphthalene or ortho-dichlorobenzene as milling medium, followed by washing with acetone and methanol. The titanyl phthalocyanine produced has a first maximum intensity peak of the Bragg angle 2Θ with respect to X-rays of Cu Kα at a wavelength of 1.541 Å at 27.3°+/−0.2°, and a second maximum intensity peak at 6.8°+/−0.2°. This was contrasted with another titanyl phthalocyanine that is similarly milled, but not acid pasted. This material has a maximum peak at 27.3°+/−0.2° and a second maximum intensity peak at 7.5°+/−0.2°.
U.S. Pat. No. 5,055,368 in the names of Nguyen, et al., teaches a “salt-milling” procedure in which crude titanyl phthalocyanine is milled, first under moderate shearing conditions with milling media including inorganic salt and non-conducting particles. The milling is then continued at higher shear and temperatures up to 50° C., until the pigment undergoes a perceptible color change. Solvent is substantially absent during the milling steps.
U.S. Pat. No. 4,701,396 in the names of Hung, et al., teaches near infrared sensitive photoconductive elements made from fluorine-substituted titanylphthalocyanine pigments. While phthalocyanines having only fluorine substituents, and those being equal in number on each aromatic ring, are the preferred pigments of the invention described in that patent, various non-uniformly substituted phthalocyanines are taught.
U.S. Pat. No. 5,112,711 in the names of Nguyen, et al., teaches an electrophotographic element having a physical mixture of titanyl phthalocyanine crystals and titanyl fluorophthalocyanine crystals. The element provides a synergistic increase in photosensitivity in comparison to an expected additive combination of titanyl phthalocyanine and titanyl fluorophthalocyanine. Similar elements having physical mixtures combining titanyl phthalocyanine and chloro- or bromo-substituted titanyl phthalocyanine crystals produce results in which the photosensitivity is close to that of the least sensitive of the two phthalocyanines used.
U.S. Pat. Nos. 5,238,764 and 5,238,766, both in the names of Molaire, et al., teach that titanyl fluorophthalocyanine products of acid-pasting and salt-milling procedures, unlike unsubstituted titanyl phthalocyanine, suffer a significant reduction in near infrared sensitivity when they are dispersed in a solvent such as methanol or tetrahydrofuran, which has a gamma c hydrogen bonding parameter value greater than 9.0. These patents further teach that this reduction in sensitivity can be prevented by first contacting the titanyl fluorophthalocyanine with a material having a gamma c hydrogen bonding parameter of less than 8.0.
Molaire, et al., in U.S. Pat. No. 5,629,418, discloses a method for preparing titanyl fluorophthalocyanine that includes the steps of: dissolving titanyl fluorophthalocyanine in acid to form a solution; admixing the solution and water to precipitate out amorphous titanyl fluorophthalocyanine; washing the amorphous titanyl fluorophthalocyanine until substantially all of the acid is removed and contacting it with an organic solvent, which results in the conversion of the amorphous material to high crystallinity titanyl fluorophthalocyanine, the amorphous titanyl fluorophthalocyanine having been maintained in contact with water continuously from its precipitation to its conversion to a crystalline form.
The particle size distribution and stability of charge generation dispersions are very important for providing uniform charge generation layer in order to control generation of “breakdown spots” and minimize the granularity of prints. In U.S. Pat. Nos. 5,614,342 and 5,766,810 both in the names of Molaire and Kaeding, disclose a method for preparing cocrystals of titanyl fluorophthalocyanine and unsubstituted titanyl phthalocyanine that includes the steps of: admixing crude titanyl phthalocyanine and crude titanyl fluorophthalocyanine to provide an amorphous pigment mixture, as determined by X-ray crystallography using X-radiation characteristic of Cu Kα at a wavelength of 1.541 Å of the Bragg angle 2Θ; contacting the amorphous pigment mixture with an organic solvent having a gamma c hydrogen bonding parameter of less than 8:0; and, prior to contacting, substantially excluding the amorphous pigment mixture from contact with an organic solvent having a gamma c hydrogen bonding parameter greater than 9.0. The amorphization step must be substantially complete so as to break the large primary particles of the starting crude pigments and thereby lower the average particle size of the final cocrystalline mixture. Substantially complete amorphization of the crude pigments is also necessary to prevent degradation of the dark decay characteristics of the final cocrystal; small amounts of crude pigments having inherently high dark decay that are not amorphized would not be affected by the subsequent solvent treatment and therefore would retain their high dark decay characteristics, causing degradation of the dark decay property of the final cocrystalline product.
Molaire, et al., in U.S. Pat. No. 5,523,189, discloses an electrophotographic element including a charge generation layer that includes a binder in which is dispersed a physical mixture of a high speed titanyl fluorophthalocyanine having a first intensity peak with respect to X-rays characteristic of Cu Kα at a wavelength of 1.541 Å of the Bragg angle 2Θ at 27°±0.2°, and a second intensity peak at 7.3°±0.2°, the second peak having an intensity relative to the first peak of less than 60 percent; and a low speed titanyl fluorophthalocyanine having a first intensity peak with respect to X-rays characteristic of Cu Kα at a wavelength of 1.541 Å of the Bragg angle 2Θ at 6.7°±0.2°, and a second intensity peak at 23°±0.2°, the second peak having an intensity relative to the first peak of less than 50 percent.
Molaire, et al., in U.S. Pat. No. 5,773,181, discloses a method for preparing a phthalocyanine composition including the steps of: synthesizing a crystalline product including a mixture of five different unsubstituted or fluorosubstituted phthalocyanines, wherein a central M moiety bonded to the four inner nitrogen atoms of the phthalocyanine nuclei represents a pair of hydrogen atoms or a covalent or coordinate bonded moiety, including an atom selected from the group consisting of Li, Na, K, Be, Mg, Ca, Ba, Sc, Y, La, Ac, Ti, Zr, Hf, V, Nb, Cr, Mo, W, Mn, Tc, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Hg, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, and Sb, with M preferably representing Ti=O; increasing the amorphous character of the mixture of phthalocyanines as determined by X-ray crystallography using X-radiation characteristic of Cu Kα at a wavelength of 1.541 Å of the Bragg angle 2Θ to provide an amorphous pigment mixture; contacting the amorphous pigment mixture with organic solvent having a gamma c hydrogen bonding parameter of less than 8.0; and prior to the contacting, substantially excluding the amorphous pigment mixture from contact with organic solvent having a gamma c hydrogen bonding parameter greater than 9.0.
The procedures for the preparation of titanyl phthalocyanine pigments described in the foregoing patents, all of whose disclosures are incorporated herein by reference, suffer from various deficiencies and disadvantages. For example, the use of acid presents a shortcoming for both environmental and safety concerns, particularly in commercial scale procedures. Also, salt milling avoids the use of acid but requires extensive washing of the milled material to remove salts, which can otherwise cause high dark decay in a photoconductor.
Procedures that first contact the titanyl fluorophthalocyanine with a solvent such as methanol or tetrahydrofuran that has a gamma c hydrogen bonding parameter value greater than 9.0 cause a significant reduction in near infrared sensitivity. The preparation of titanyl fluorophthalocyanine having good photogeneration characteristics is expensive. It would be desirable to be able to produce a crystalline titanyl phthalocyanine composition that has good photogeneration characteristics when used in an electrophotographic element but is less expensive than titanyl fluorophthalocyanine. A suitable procedure would avoid deleterious contact with high gamma c hydrogen bonding parameter solvents and also not require the use of acid or of salt milling media.
The present inventors believe that the effect of particle size distribution on photo speed relates more to the breadth of the distribution than the absolute size of the pigment particles. At the same time, the lower the particle size, the less the propensity for breakdown. Thus, there is a need for dispersions with smaller and more uniform particle size distribution.
SUMMARY OF THE INVENTION
The present invention is directed to a process for forming a nanoparticulate crystalline titanium phthalocyanine pigment composition that includes contacting a titanium phthalocyanine pigment with substantially pure 1,1,2-trichloroethane (TCE) under conditions effective to convert the titanium phthalocyanine pigment to the nanoparticulate crystalline composition.
DETAILED DESCRIPTION OF THE INVENTION
Unsubstituted titanyl phthalocyanine, abbreviated herein as “TiOPc”, has the following structural formula:
Titanyl fluorophthalocyanines, abbreviated herein as “TiFOPc”, have the following structural formula:
wherein each of k, l, m, and n is independently an integer from 1 to 4.
In the process of the present invention, the titanium phthalocyanine pigment can be contacted with the substantially pure TCE in its vapor or liquid form. Preferably, the pigment is wet milled in TCE using a milling aid such as steel shot. Wet milling is carried out preferably for about 10 minutes to about 96 hours, more preferably, about 30 minutes to about 6 hours.
Also, in accordance with the present invention, the titanium phthalocyanine pigment can be contacted with the substantially pure TCE using ultrasonication for a time period preferably of about 15 minutes to about 2 hours, more preferably, about 10 minutes to about 1 hour.
The titanium phthalocyanine pigment employed in the process of the invention preferably includes a cocrystalline mixture of unsubstituted titanyl phthalocyanine (TiOPc) and titanyl fluorophthalocyanine (TiOFPc), wherein the weight ratio of TiOPc:TiOFPc is preferably about 99.5:0.5 to about 70:30, more preferably, about 95:5 to about 75:25.
Alternatively, the titanium phthalocyanine pigment employed in the process of the invention can include crystalline titanium fluorophthalocyanine (TiOFPc), which can be a mixture including titanyl 2, 9, 16, 23-tetrafluoropthaiocyanine, titanyl 2, 9, 16-trifluorophthalocyanine, titanyl 2-fluorophthalocyanine, titanyl 2, 9-difluorophthalocyanine, and titanyl 2, 16-difluorophthalocyanine.
The present inventors have discovered that the use of 1,1,2-trichloroethane (TCE) as the sole solvent affords very uniform, substantially monodisperse, nanoparticulate dispersions of cocrystalline titanyl fluorophthalocyanine and unsubstituted titanyl fluorophthalocyanine. Additionally, they have found that dispersions formed using TCE as the sole solvent exhibit unusual stability toward settling. As a further advantage, the nanoparticle dispersions of the present invention can be obtained without the use of a polymeric binder.
The following examples serve to illustrate the invention:
COMPARATIVE EXAMPLE 1
A dispersion of a cocrystalline composition of unsubstituted titanyl phthalocyanine (TiOPc) and titanyl fluorophthalocyanine (TiOFPc), using a 1.5 gallon attritor, 3300 ml of 3 mm stainless steel media, 5.9 g of the copolyester ionomer poly{2,2-dimethyl-1,3-propylene-oxydiethylene (80/20) isophthalate-co-5-sodiosulfoiisophthalate (95/5)}, (prepared as described in U.S. Pat. No. 5,523,189), 23.68 g of a cocrystalline mixture of 90/10 TiOPc-TiOFPc prepared from a mixture of the amorphous pigments according to the method described in the previously discussed U.S. Pat. No. 5,614,342, and a solvent mixture of 222.24 g of DCM and 148.16 g of TCE. The concentrated dispersion was mixed with a preformed solution consisting of 17.8 g of binder, 591.6 g of DCM, and 200.62 g of TCE. The resulting dispersion was diluted to 3% solids, and the particle size distribution was determined using a UPA Ultraparticle Analyzer.
EXAMPLE 1
A TiOPc-TiOFPc dispersion was prepared using the same procedure and materials as described in Comparative Example 1, except that the solvent consisted solely of TCE. The particle size distribution was determined and compared with that of the dispersion of Comparative Example 1. The results are shown in TABLE 1 following:
TABLE 1
Particle Size (microns)
Example
10%
50%
90%
Comparative Example 1
0.226
0.433
0.736
90/10 TiOPc-TiOFPc
in 60:40 DCM:TCE
Example 1
0.036
0.086
0.182
90/10 TiOPc-TiOFPc
in TCE
The results given in TABLE 1 illustrate the desirable reduction in particle size at both 10% and 50% when pure TCE is used in place of a mixture of DCM and TCE in the preparation of the TiOPc-TiOFPc dispersion.
COMPARATIVE EXAMPLE 2
A mixture of 0.2 g of 90/10 cocrystalline TiOPc-TiOFPc and 5 g each of DCM and TCE was mixed in a vial without any polymeric binder and ultrasonicated for 3 hours, following which the particle size distribution of the resulting dispersion was measured.
EXAMPLE 2
The procedure of Comparative Example 2 was repeated, except that 10 grams of TCE was used in place of the DCM-TCE mixture. Following ultrasonication, the particle size distribution of the resulting dispersion was determined.
EXAMPLE 3
The procedure employed in Example 2 was repeated, using acid pasted crystalline titanyl fluorophthalocyanine as the pigment in place of 90/10TiOPc-TiOFPc. The particle size distribution of the resulting dispersion was measured and compared with those of the dispersions described in Comparative Example 2 and Example 2; the results are summarized in TABLE 2 following:
TABLE 2
Particle Size (microns)
Example
10%
50%
90%
Comparative Example 2
0.1071
0.2369
0.401
90/10 TiOPc-TiOFPc
in 50:50 DCM:TCE
Example 2
0.022
0.0384
0.106
90/10 TiOPc-TiOFPc
in TCE
Example 3
0.0258
0.049
0.129
TiOFPc (ZP4)
In TCE
The results presented in TABLE 2 demonstrate that nanoparticulate dispersions can be obtained from pigments dispersed in TCE alone, in the absence of a binder polymer.
COMPARATIVE EXAMPLE 3
A dispersion was made in the same manner as described in Comparative Example 1, except that the polymeric binder was the copolyester ionomer poly{4,4-xylylene-co-2,2′-oxydiethylene (46/54) isophthalate-co-5-sodiosulfoisophthalate (85/15)} (prepared as described in U.S. Pat. No. 5,523,189). The particle size distribution of the dispersion following dilution was determined as described in Comparative Example 1.
EXAMPLE 4
The same procedure was used as that described in Comparative Example 3, except that the solvent consisted solely of TCE. The particle size distribution was determined and compared with that of the dispersion of Comparative Example 3. The results are shown in TABLE 3 following:
TABLE 3
Particle Size (microns)
Example
10%
50%
90%
Comparative Example 3
0.386
0.55
0.826
90/10 TiOPc-TiOFPc
in 60:40 DCM:TCE
Example 4
0.0385
0.0807
0.1449
90/10 TiOPc-TiOFPc
in TCE
The results presented in TABLE 3 are similar to those of TABLE 1 but illustrate the desirable reduction in particle size extending to 90%.
EXAMPLE 5
A 75/25 TiOPc-TiOFPc cocrystalline pigment, prepared as described in U.S. Pat. No. 5,614,342, was used to prepare a series of dispersions in the following solvents: ethanol, methyl ethyl ketone (MEK), toluene, tetrahydrofuran (THF), dichloromethane (DCM), and 1,1,2 trichloroethane (TCE). The dispersions were ultrasonicated for 15 minutes just prior to transfer of a sample of each to a 10-ml graduated cylinder. The meniscus of the dispersion was adjusted to the 10 ml mark, and the cylinders were sealed with a cork stopper. The dispersions were periodically inspected for settling, the results being summarized in TABLE 4 following:
TABLE 4
Percent of Settled Volume
After
After
After
Solvent
5 Hours
74 Hours
98 Hours
Ethanol
2
24
27
MEK
1
22
26
Toluene
0
18
22
THF
7
30
31
DCM
0
5
7
TCE
0
0
0
The results summarized in TABLE 4 demonstrate the very large improvement in settling tendency, even on prolonged standing, provided by dispersions prepared in TCE in accordance with the present invention.
EXAMPLE 6
Dispersions of cocrystalline compositions of unsubstituted titanyl phthalocyanine (TiOPc) and titanyl fluorophthalocyanine (TiOFPc) were prepared, using a 1.5 gallon attritor, 3300 ml of 3 mm stainless steel media, 5.9 g of the copolyester ionomer poly{2,2-dimethyl-1,3-propylene-oxydiethylene (80/20) isophthalate-co-5-sodiosulfoiisophthalate (95/5)}, (prepared as described in U.S. Pat. No. 5,523,189), and 23.68 g each of five cocrystalline TiOPc-TiOFPc compositions prepared by the method described in the previously discussed U.S. Pat. No. 5,614,342. Four amorphous pigment mixtures were dispersed either in 370 g of TCE or 370 g of a 60/40 (by wt.) mixture of DCM and TCE. The following amorphous mixtures, designated Pigment Mixtures A, B, C, and D, were used to prepare these concentrated dispersions:
Pigment Mixture A—a 90/10 mixture of crude substantially chlorine-free TiOPc and crude TiOFPc, as described in Example 1 of co-pending related application TWO-STAGE MILLING PROCESS FOR PREPARING COCRYSTALS OF TITANYL FLUOROPHTHALOCYANINE AND TITANYL PHTHALOCYANINE, AND ELECTROPHOTOGRAPHIC ELEMENT CONTAINING SAME.
Pigment Mixture B—like Pigment Mixture A, but containing an 87.5/12.5 mixture of crude substantially chlorine-free TiOPc and crude TiOFPc.
Pigment Mixture C—a 90/10 mixture of highly crystalline, substantially chlorine-free TiOPc obtained from H. W. Sands Corporation and crude TiOFPc, as described in Example 2 of co-pending related application TWO-STAGE MILLING PROCESS FOR PREPARING COCRYSTALS OF TITANYL FLUOROPHTHALOCYANINE AND TITANYL PHTHALOCYANINE, AND ELECTROPHOTOGRAPHIC ELEMENT CONTAINING SAME.
Pigment Mixture D—a 90/10 mixture of lightly chlorinated Cl—TiOPc and crude TiOFPc, as described in Example 2 of co-pending related application COCRYSTALS CONTAINING HIGH-CHLORINE TITANYL PHTHALOCYANINE AND LOW CONCENTRATION OF TITANYL FLUOROPHTHALOCYANINE, AND ELECTROPHOTOGRAPHIC ELEMENT CONTAINING SAME.
The concentrated dispersions were mixed with corresponding preformed solutions consisting of 17.8 g of binder, and 792 g of either TCE or a 60/40 DCM/TCE mixture. The resulting dispersions were diluted to 3% solids and evaluated for settling using the procedure described in Example 5. The results are summarized in TABLE 5 following:
TABLE 5
Percent of Settled Volume
Pigment
After
After
After
Dispersion
Mixture
Solvent
24 Hours
68 Hours
122 Hours
1 (Comparison)
A
60/40
5
10
22
DCM/
TCE
2 (Invention)
B
TCE
0
0
0
3 (Invention)
C
TCE
0
1
2
4 (Comparison)
D
60/40
4
5
8
DCM/
TCE
5 (Invention)
D
TCE
0
0
0
The results summarized in TABLE 5 demonstrate the resistance to settling, even on prolonged standing, exhibited by dispersions prepared in substantially pure TCE compared with dispersions prepared in a DCM/TCE mixture.
The invention has been described in detail for the purpose of illustration, but it is understood that such detail is solely for that purpose, and variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention, which is defined by the following claims.
|
In a process for forming a nanoparticulate crystalline titanium phthalocyanine pigment composition, a titanium phthalocyanine pigment is contacted with substantially pure 1,1,2-trichloroethane (TCE) under conditions effective to convert the titanium phthalocyanine pigment to the nanoparticulate crystalline composition.
| 2
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention pertains to cutters generally, and particularly to shearing type cutters as might be used, for example, to cut building construction siding.
2. Description of the Related Art
In the building construction industry, many new and diverse technologies come together to provide builders with better materials and construction techniques. Advanced materials for siding, such as aluminum, steel and vinyl, provide both builders and building owners advantages. However, tools have not yet been fully developed that allow builders to take fall advantage of these materials.
For example, aluminum, steel and vinyl siding and trim are available in large sheets, strips or continuous rolls which must be cut to the particular shape of the building frame. These strips are usually quite thin, and so are readily cut by shears, much like scissors are used to cut paper. In fact, a typical siding cutter used in the field resembles a paper cutter. However, siding is not as flexible as paper and so both sides of the cut must be sheared, leaving two finished surfaces with a small kerf sheared from the finished edges.
Steel siding is particularly challenging, owing to the galvanized zinc coating that provides corrosion protection. Cutting with a saw may remove the soft zinc, leaving exposed steel surfaces. As is well known, such exposed surfaces will corrode very quickly. In fact, the use of a saw may void the siding manufacturer's warranty. Steel siding may, however, be cut with a shearing action. When cut this way, the softer zinc is smeared over the sheared steel edge, providing necessary protection against the environment.
As noted above, these strips or rolls of stock material are cut using devices that resemble office paper cutters, with a pivoting blade which coacts with two stationary cutters to shear the material. These devices work admirably when making cuts perpendicular to the stock material. The cut is made very quickly and with very clean and precise finished edges. For the purposes of this disclosure the resulting edges are referred to as finished when no further work is required to install the material into the construction.
However, cuts made at angles different from perpendicular are extremely difficult and time consuming to make in the field during construction. As a result, the expense of applying these advanced building materials increases significantly when custom work or retrofitting is required. Generally, an installer will use a cutting shear to make the necessary perpendicular cuts. When a cut other than perpendicular is required, the strip may be sheared perpendicularly to the approximate size and then angled with hand shears. Unfortunately, hand shears leave an unfinished edge that is distorted, rough, and jagged, making the stock material hazardous to handle and difficult to install smoothly against a flat surface.
Additionally, hand shears are much slower to use to cut siding. The builder will have to pencil an angle onto the material to mark the intended cut. Next, hand shears must be worked through the stock material. In the case of lap siding such as double four or double five, where there are two or more parallel but offset surfaces separated by a small edge, as shown for example in the present application as FIG. 5, the builder must shear each flat 120 and 125 first, and then bend the siding at the cut to allow access to the small edge 130 before the cut may be completed. The entire process, even in the case of an experienced installer, may typically require seven minutes of work.
Examples of prior art siding cutters are found in U.S. Pat. Nos. 5,251,524 to Clifford; 4,510,834 to Greene et al.; 3,134,285 to Greene; 3,362,070 to Huggins; 2,355,320 to Nebel; 3,714,856 to Hall et al.; 5,010,795 to Kania; and 5,038,477 to Parrow; all incorporated herein by reference. In these prior art siding cutters, as in the present invention, a cutter blade is used to pivotally shear between two spaced apart stationary blades. Commonly in the prior art and in industry, as shown, for example in FIG. 3 of Greene '285, the entire cutter structure is rotated relative to the siding. Pegs, pins, bolts, nails or other projections are used to align the siding to the cutter. While this method is acceptable when a number of cuts are to be made at a fixed angle, this is often disadvantageous in the building industry, where, for example, siding is most desirably applied alternately from both edges to a final central region. In order to accomplish these angles which alternate from one direction to another, the prior art cutters must be moved and aligned, making this method so time consuming as to be cost prohibitive. As noted hereinabove, persons in the trade find cutting the materials with hand shears and then cleaning up the unfinished edges an easier task than frequently re-aligning the siding cutter.
Another problem encountered in the industry when using a stationary siding cutter to cut angles occurs when the stock material has not been precut to a precise predetermined length. In these instances, the siding extends beyond the cutter at an angle to the stationary blades. The siding may only be placed so that the siding edge mates perfectly with one stationary cutter, but not with both stationary cutters. Therefore, the pivoting cutter blade first contacts the siding with only one stationary cutter opposing the pivoting cutter. The siding may then deform, since there is no counter force on the second edge to ensure a shearing action. When this happens, stock material may be wasted since the resulting edge will no longer be finished and the stock material may be permanently creased or deformed.
In order to overcome these difficulties previously encountered in the field, others have designed fully rotating cutter structures, such as shown, for example, in Greene et al. '834. While the '834 patent offers a number of advantages over the prior art in handling miter cuts, the cutter becomes prohibitively large and difficult to handle. The bed 10 illustrated therein must be strong enough to support the rotatable shear throughout all cutting angles and not flex or deform during the cutting stroke. As a result, the bed becomes the single largest piece of the machine. In addition, the machine operator must move the entire cutter assembly to each desired angle. As is immediately apparent, the cutter structure is at best cumbersome.
SUMMARY OF THE INVENTION
The present invention overcomes the limitations of the prior art by providing a compact shearing type cutter structure wherein the pivotal cutter blade coacts with self-adjusting, linearly sliding opposing blades. During a perpendicular cutting stroke, these cutter blades operate the same as the prior art perpendicular pivotal shearing cutters. A fence is provided to assist in placing the stock material relative to the cutter blades, and adjustments are provided to align these first linearly sliding blades to the size and spacing of the materials. A second set of linearly sliding blades is supported directly upon the first blades and is linearly slidable with respect to the first set. The second set of linearly slidable blades cooperates with the first set to form a step, where non-flat stock materials such as stepped siding are to be sheared. The second set of blades is removable or adjustable for each particular type of stock material.
The fence is rotatable, and cooperates with a novel drive mechanism while being pivoted. The drive mechanism directly slides the linearly slidable blades that are on opposite sides of the cutting gap oppositely of each other. When the fence is pivoted, the otherwise stationary blades are automatically adjusted to the new cutting angle. The drive mechanism includes an initial adjustment to properly align the blades for a perpendicular cut, after which no further adjustment is required. The fence may be positioned repetitively to preset angles through the use of a novel stop.
OBJECTS OF THE INVENTION
An object of the present invention is to provide a shear type cutter which is continuously variable to perform miter cuts of any desired angle.
Another object of the present invention is to provide a shear type cutter which is of small size relative to the stock material, and which is readily handled by a cutter operator.
Another object of the present invention is to provide a shear type miter cutter which may be operated without any special training required for the operator prior to cutting.
Another object of the present invention is to provide a shear type miter cutter which requires no adjustment between miter cuts of different angles other than movement of the fence.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects and features of the invention will be apparent from the following description of preferred embodiments with reference to the accompanying drawings, in which:
FIG. 1 illustrates a top perspective of the preferred embodiment of the invention showing the blade removed.
FIG. 2 illustrates a side perspective of the preferred embodiment of the invention showing the blade raised prior to making a cut.
FIG. 3 illustrates a cross-section of the preferred embodiment of FIG. 1 taken along section line 3 of FIG. 2.
FIG. 4 illustrates a preferred embodiment of the cutter blade slide mechanism.
FIG. 5 illustrates a siding strip which might be cut by the present invention.
FIG. 6 illustrates a bottom perspective view of the preferred embodiment drive mechanism of the present invention.
For sake of brevity and clarity, like components and elements will bear the same designations throughout the figures.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The preferred embodiment of the present invention is illustrated in FIGS. 1-4 and 6. Therein, a sliding miter cutter 10 having the preferred features of the present invention is illustrated generally, having a cutter base 20, a fence 14 and a blade 16. Extending from base 20 is a table mounting plate 18 which may be used to attach cutter 10 to a table, saw horse or other structure. Table mounting plate 18 therefore eliminates any requirement for flat work areas, which may be difficult to find at typical construction sites. Table mounting plate 18 forms a main structural support for the remaining components of cutter 10.
FIG. 3 illustrates details of cutter base 20 most clearly. Therein, cutter base 20 includes left linear cutter support 22 and right linear cutter support 24, which are mirror images of each other. While in cross-section these cutter supports 22 and 24 are shown as comprising two separate components and maybe so formed, in the preferred embodiment it is emphasized that these are formed as integral components of cutter base 20. Each cutter support 22 and 24 comprises an elevation support 26 and a top surface 28. The top surface 28 has a notch 30 formed therein. Notch 30 is rectangular and extends the length of cutter base 20.
The top of each cutter support 22 and 24 has a channel 32 formed above and separated from notch 30. Rail 34, only visible in cross-section FIG. 3, may be automatically adjusted longitudinally within channel 32, as will be explained in greater detail hereinafter. Bottom blade 36 is supported and adjustable longitudinally on rail 34, and top blade 38 is supported and longitudinally adjustable on blade 36. Rib 40 of top blade 38 fits in groove 42 formed on the top side of bottom blade 36 to ensure longitudinal alignment therebetween.
Referring back to FIG. 1, a number of threaded fixture holes 44 are located at predetermined intervals in groove 42. Adjustment slots 46 in top blade 38 extend vertically through top blade 38 to allow top blade 38 to be adjusted longitudinally relative to bottom blade 36, and then anchored in place securely with set screws 48. This, in operation, will typically be a one-time adjustment, wherein the blades may be set one relative to the other for particular sizes of siding. To adjust for different types of siding, such as double four (D4) or double five (D5) siding, the bottom blade 36 and top blade 38 must be appropriately aligned to mesh with the siding. D4 siding has two flats 120 and 125 shown in FIG. 5 which are each four inches in length. In the case of D5 siding, the two flats 120 and 125 are each five inches in length. By providing blades 36 and 38 with longitudinal adjustment relative to each other, each different type of siding may be accommodated. Furthermore, when only one cutter is required for the siding to be cut, set screws 48 may be removed completely and top blade 38 may be removed.
As is apparent, the adjustment, or removal, of top blade 38 relative to bottom blade 36 is a one-time adjustment made in the field. The adjustment is determined by the type of siding being installed, and no further adjustment will be required until a different type of siding is to be cut. Furthermore, while a set screw has been described for element 48, one of ordinary skill will identify any number of well-known suitable alternatives, the main requirement being the adjustment or removal of top blade 38 relative to or from bottom blade 36. Where desired, guide marks or mating ridges and protrusions may be provided between top blade 38 and bottom blade 36 to quickly select standard siding dimensions.
Referring most particularly to FIGS. 3 and 6, cutter supports 22 and 24 are spaced from each other to form a gap 52 through which cutter blade 16 travels. Siding fence 14 rotates relative to base 20 about pivot point 54. Siding fence 14 is carried upon and rigidly affixed to generally round disk 81 and is rotatably mounted between top fence support plate 85 and drive plates 100, 115. Drive plates 100, 115 are retained vertically by bottom fence support plates 90, laterally by outer rails 80, and longitudinally by guide pins 95, 96.
In operation of sliding miter cutter 10, an operator will select an appropriate angle for the siding to be cut at by rotating fence 14 about pivot point 54. As the operator rotates fence 14, generally round disk 81 rotates, causing guide pins 95 and 96 to move within slots 97 and 98. In turn, guide pins 95 and 96 force relative longitudinal motion between drive plates 100 and 115. For example, as viewed in FIG. 6, when generally round disk 81 and fence 14 are rotated counterclockwise, guide pins 95 and 96 also will rotate counterclockwise. Since pin 96 moves to the left of center and thereby only engages with drive plate 115, drive plate 115 is moved downward by pin 96. Simultaneously, pin 95 is moved to the right of center, thereby only engaging drive plate 100. Since the rotation of pin 95 is counterclockwise about pivot point 54, drive plate 100 is moved upward by pin 95. One will observe that drive plate 115 is moving longitudinally in one direction, while drive plate 100 moves longitudinally opposite.
When fence 14 is transverse or perpendicular to the longitudinal axis of blade 16, rotation is accompanied by very little longitudinal motion between drive plates 100 and 115. In this instance, guide pins 95 and 96 primarily slide left and right within slots 97 and 98. However, when fence 14 is nearly parallel to the longitudinal axis of blade 16, guide pins 95 and 96 are sliding perpendicular to slots 97 and 98, thereby causing a maximum amount of longitudinal motion between drive plates 100 and 115. If one plotted the relative displacement between drive plates 100 and 115 versus the angular position of fence 14 relative to the longitudinal axis of the cutter blade 16, a sine wave function would be plotted. While a sine wave is generated by the preferred embodiment, other similar nonlinear functions may also be designed and generated in accord with the present invention.
This nonlinear function of displacement relative to angle of rotation is very important. Nonlinear displacement of cutter blades 36 and 38 maintains tracking with the rotation of fence 14, to provide a bottom blade 36 immediately at the start of any miter cut to counteract any shearing forces applied by cutter blade 16. As aforementioned, stationary cutter blades of the prior art do not engage with the pivoting cutter blade on both sides of the gap when any angle other than perpendicular cuts is selected. The prior art lack of counter force blades can result in bending and deformation of the stock siding material, resulting in large waste of valuable siding material and time.
The relative longitudinal motion of drive plates 100 and 115 causes motion to be transmitted from drive plates 100 and 115 through bolts 110 and 111 to tie rods 105 and 106. Tie rods 105 and 106 are connected through side plates 114 to rails 34 and bottom blades 36.
Tie rods 105 and 106 in the preferred embodiment are fixed in length and so are not adjustable. However, as an alternative it is contemplated that tie rods 105 and 106 could be adjustable in length to allow alignments which might be desired after the time of manufacture.
As can be seen best in FIG. 2, fence 14 will rotate and thereby cause longitudinal motion to be transmitted through tie rod 105 to bolt 112 and side plate 114 and up to rail 32 and cutter 34. Side plate 114 may traverse through cutter base 20 at slots 35 and 37 which are cut vertically through cutter base 20. Side plate 114 is fixedly attached to rail 34.
A small locking slide 140 shown in FIG. 3 may be affixed to fence 14 so as to slide upon rail 145. Locking slide 140 may have a set screw or other fastener to attach directly to rail 145, to retain fence 14 in a specified position. Alternatively, an operator may attach small clamps such as C-clamps or other similar devices to rail 145 at two predetermined positions, to allow rapid switching to the corresponding preset angles by merely rotating fence 14 until slide 140 engages the clamps.
In FIG. 4, the slide mechanism 66 and blade 16 are shown in magnified view. Therein, blade 16 is attached on an extension 67 to slide 66 through linkage 69. Extension 67 may be welded, bolted, attached with other suitable fastening means or even may be formed integrally with blade 16. Extension 67 is preferably pinned to form a rotary joint with slide 66, though any reasonable pivotal interconnection is acceptable. Stop 65 engages with blade 16 when blade 16 is rotated approximately perpendicular to slide 66, to maintain handle 70 in a roughly vertical direction. An operator may move the handle 70 until blade 16 engages stop 65, retaining handle 70 in the air.
To set up the cutter 10 for operation, bottom blades 36 and top blades 38 are set for the type of siding which is being cut. Next, stock material such as siding 135 is placed onto blades 36 and 38. Next, the operator will adjust slide 66 so that blade 16 will engage the stock material at a suitable cutting angle. Next, slide locking knob 150 is rotated to clamp slide 66 into place relative to notch 30. Then the operator may begin cutting by moving handle 70 to cause blade 16 and bottom blade 36 to engage siding 135.
Slide locking knob 150 is preferably threaded into slide 66. Rotation of slide locking knob 150 results in movement of slide locking plate 155, either into planar alignment with slide 66 or out of alignment, depending upon the direction of rotation. When slide locking plate 155 is moved out of alignment with slide 66, the enlarged combined vertical height of slide 66 and slide locking plate 155 causes slide 66 to be lifted within notch 30 to frictionally engage the upper surface thereof. The friction forces are great enough to ensure that the shear begins without further movement of slide 66 within notch 30.
Some type of rotary to linear conversion must be provided to convert the rotation of slide locking knob 150 into linear motion of slide locking plate 150. In the preferred embodiment, one or more rivets 160 may be provided. Rivets 160 serve to loosely retain slide locking plate 160 with slide 66, while allowing limited motion therebetween. When slide locking knob 150 is rotated in a first direction, the threading thereon forces knob 150 through slide 66 and against slide locking plate 155, thereby forcing slide locking plate 155 out of alignment with slide 66. This results in locking of slide 66 within notch 30. When slide locking knob 150 is rotated in a second direction opposite to the first direction, slide locking knob 150 is pulled by the threading thereon away from slide locking plate 155. This results in slide locking plate 155 being freed up to move into alignment with slide 66, thereby freeing slide 66 to slide within notch 30.
Alternatively, slide locking knob 150 may be narrowed at the end adjacent slide locking plate 155, then passed through an unthreaded hole within slide locking plate 155, and then deformed therein, so as to allow rotation of slide locking knob 150 relative to slide locking plate 155 without any other changes therebetween. As is apparent, in light of the present disclosure a number of other suitable alternatives will be suitable to form this rotary to linear interconnection.
While slide locking knob 150 and slide locking plate 155 are illustrated in the preferred embodiment, it will be clearly understood by one of ordinary skill that other alternatives may be suitable for positioning blade 16. One alternative is apurely frictional engagement whereby neither slide locking knob 150 nor slide locking plate 155 are provided, leaving the shearing force upon blade 16 pressing against siding 135 to cause slide 66 to lift within notch 30 and thereby frictionally engage notch 30.
As illustrated in FIG. 1, blades 36 and 38 have angularly tapered ends 49 and 50, respectively. These ends are tapered to accommodate the greatest angle from perpendicular that the cutter may be operated at. This is so the surfaces of blades 36 and 38 opposite blade gap 52 do not interfere with placement of the siding at these greatest angles. Obviously, no angle whatsoever would be required if only perpendicular cuts were to be required. However, if cuts down to 10 degrees from the longitudinal axis are required, then ends 49 and 50 should be tapered at that same 10 degrees from longitudinal. Similarly, fence 14 has angular cutouts 64 which are provided to prevent fence 14 from colliding with either cutter base 20 or blades 36 and 38 when fence 14 is rotated to the aforementioned greatest cut angle.
While the foregoing details what is felt to be the preferred embodiment of the invention, no material limitations to the scope of the claimed invention are intended. Further, features and design alternatives that would be obvious to one of ordinary skill in the art are considered to be incorporated herein. The scope of the invention is set forth and particularly described in the claims hereinbelow.
|
A shear type miter cutter has a pivotal blade and four linearly sliding blades. The linearly sliding blades may be manually linearly positioned to preset locations for a particular size or type of stock material. The linearly sliding blades are further linearly adjusted automatically upon rotation of a stock material support fence, to ensure optimum alignment between the pivotal blade and the linearly sliding blades. The automatic adjustment allows an operator to make rapid changes in cut angles for a given stock material, while still yielding finished cut edges of high quality and precise angular orientation. A variety of designs for rapidly manually setting the cutter to specific preset angles and specific stock materials are also disclosed.
| 1
|
RELATED FILLING
The present application is related to a patent application being filed concurrently entitled Graphical User Interface Text-based Interpolation Searching, by Robert Coyne and Steven Greenspan.
FIELD OF THE INVENTION
The present invention relates generally to devices for computer animation performance and methods and computer-readable media for implementing the same. More particularly, the present invention relates to using an interactive graphical interface for animation performance.
BACKGROUND OF THE INVENTION
Computer systems often utilize displays with icons, pictures, text, pop-up, drop-down menus and other graphical items. In these systems, individual graphical items or combinations of graphical items are typically shown on the display monitor. The graphical item is generally activated by a point and click method in which a cursor controlled by a mouse, touch device, pen or trackball is pointed at the item, and a button, keyboard command or activation unit is clicked.
Generally, three dimensional character animations are incrementally specified using high technical interfaces wherein the user adjusts one parameter at a time and then previews the result. The final animation is an immutable sequence of rendered frames. At the other end of the spectrum of animation are video games wherein the user, in real-time, triggers predefined movements, but is given very little control over the nuances of expression and movement.
Generally, in many graphics implementations, animation may be performed in three dimensions, but typically utilizes a complex process called “rendering” to provide a representation of an image. For example, physical objects such as tubes, spheres, rectangles, and the like may be used to “build” other, more visually complex objects. Such objects may be rotated, stretched, twisted, or the like. However, such modeling generally requires utilizing modifiers, which may include a stack of parametric definition for each desired geometric subclass, thus requiring a large amount of storage and a complex retrieval system.
Various three dimensional animation systems provide additive displacements as a method of combining partially defined gestures, facial expressions, or morphing targets. Such targets are generally controlled by bands of sliders.
Other related interfaces are the joystick music synthesizers, wherein the joystick is used to control various aspects of the timbre and dynamics of the sound. The joystick is moved from a first position to a second position, and the parameters are dynamically mixed based on the second position of the joystick.
In addition to automation, more generally, searches in databases are achieved by using key words or expressions so that an ordered list may be obtained. However, often the list is quite long, and thus is difficult to sort through to obtain the desired information.
Thus, there is a need for a device and method for a simplified graphical user interface that the user may utilize in an interactive fashion to provide relevance weightings for searches to facilitate re-ordering of search data and to add nuances of expression and movement in animation.
SUMMARY OF THE INVENTION
The present invention provides an electronic display system that facilitates the use of a graphic interface for interactive animation on a display device. The invention includes: a central processing unit; a memory loaded with an operation system, application programs and computer-executable instructions of using a graphical interface for achieving the animation; a display unit coupled to the system bus; a cursor control unit arranged to provide signals to control movement of a cursor on the display unit; and the system bus. The computer-executable instructions for achieving use of a graphical interface for animation include: (1) inserting a desired image onto a first window; (2) inserting anchors onto a second window by, for each anchor, selecting a desired pose from a plurality of predetermined poses; and (2) upon a cursor being dragged over the second window to a desired anchor, additively applying, for the desired anchor to the desired image based on a proximity of the cursor to the desired anchor. The characteristics for the anchors are, for animation, typically facial expressions, character poses or camera positions, and the like. The electronic display system is generally implemented as a computer display system. Inserting anchors may include combining a plurality of desired anchors to form a compound anchor, e.g., by dragging one or more anchors on top of another anchor. A palette may be shown in a third window on the display unit and may be used for selecting a desired image to be inserted onto the first window.
The present invention includes a method for facilitating use of an interactive graphical interface for animation on an electronic display system by a user. The steps of the method may include inserting a desired image onto a first window; inserting anchors onto a second window by, for each anchor, selecting a desired pose, from a plurality of preselected poses; and dragging a cursor over the second window to a desired anchor wherein characteristics for the desired anchor are additively applied to the desired image, based on a proximity of the cursor to the desired anchor. Characteristics for the anchors in the method are typically, for animation: facial expressions, character poses, orientation of an image or camera positions and the like. The electronic display system may be implemented by a computer display system. A plurality of desired anchors may be combined to form a compound anchor by dragging an anchor onto another anchor or pile of anchors. Where desired, a palette in a third window displayed on the display unit may be used for selecting a desired image to be inserted onto the first window.
Where desired, the steps of the method of the invention may be implemented by computer-executable instructions in a computer-readable medium.
BRIEF DESCRIPTION OF THE DRAWINGS
The accompanying drawings, which are incorporated into and form a part of the specifications, illustrate preferred embodiments of the present invention and, together with the description, serve to explain the principle of the invention. The drawings are only for the purpose of illustrating a preferred embodiment of the invention and are not to be construed as liming the invention. In the drawings, like numbers refer to like parts throughout and mouse clicking for a cursor is shown by a circle:
FIG. 1 is a graphical representation of a 4-way split screen depiction of one embodiment of an implementation scheme for using a graphical interface for animation in accordance with the present invention.
FIG. 2A is an illustration of a character in a dance pose based on clicking a mouse for a cursor very close to the sway-right target pose selection shown on the skeleton controller in FIG. 2B .
FIG. 3A is an illustration of a character in a dance pose based on clicking a mouse for a cursor approximately equidistant from the sway-right target pose selection and the sway-left target pose selection shown on the skeleton controller in FIG. 3B .
FIG. 4A is an illustration of a character in a dance pose based on clicking a mouse for a cursor very close to the sway-left target pose selection shown on the skeleton controller in FIG. 4B .
FIG. 5A is an illustration of a character in a dance pose based on clicking a mouse for a cursor approximately equidistant from the sway-right target pose selection, the in-between pose selection and the sway-left targetpose selection shown on the skeleton controller in FIG. 5B .
FIG. 6A is an illustration of a character in a dance pose based on clicking a mouse for a cursor very close to the in-between target pose selection shown on the skeleton controller in FIG. 6B .
FIG. 7A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area apart from the target selection shown on the facial controller in FIG. 7B .
FIG. 8A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area substantially on the surprise target selection shown on the facial controller in FIG. 8B .
FIG. 9A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area substantially halfway between the surprise target selection and the anger target selection shown on the facial controller in FIG. 9B .
FIG. 10A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area substantially on the anger target selection shown on the facial controller in FIG. 10B .
FIG. 11A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area substantially halfway between the anger target selection and the smile-big target selection shown on the facial controller in FIG. 11B .
FIG. 12A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area substantially on the smile-big target selection shown on the facial controller in FIG. 12B .
FIG. 13A is an illustration of a facial configuration based on clicking a mouse for a cursor in an area substantially equidistant between the anger target selection, the surprise target selection and the smile-big target selection shown on the facial controller in FIG. 13B .
FIG. 14A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor in an area apart from the target selection shown on the block controller in FIG. 14B .
FIG. 15A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor in an area approaching the line target selection shown on the block controller in FIG. 15B .
FIG. 16A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor in an area substantially on the line target selection shown on the block controller in FIG. 16B .
FIG. 17A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor lying intermediate between the line target selection and the spiral target selection shown on the block controller in FIG. 17B .
FIG. 18A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor in an area substantially on the spiral target selection shown on the block controller in FIG. 18B .
FIG. 19A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor in an area substantially on the star 3 target selection shown on the block controller in FIG. 19B .
FIG. 20A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor lying intermediate between the line target selection and the star 3 target selection shown on the block controller in FIG. 20B .
FIG. 21A is an illustration of a configuration of a series of blocks based on clicking a mouse for a cursor lying closer to the line target selection than to the star 3 target selection shown on the block controller in FIG. 21B .
FIG. 22 is an illustration of a recording of a series of facial expressions utilized wherein the recording may be used to re-implement the series.
FIG. 23 illustrates one embodiment of a block diagram of an electronic display system operative to facilitate interactive, expressive animation by a user in accordance with the present invention.
FIG. 24 shows one embodiment of steps for a method or computer-readable medium having computer-executable instructions for facilitating interactive, expressive, animation on an electronic display system by a user in accordance with the present invention.
FIG. 25 shows one embodiment of steps for a method or computer-readable medium having computer-executable instructions for facilitating animation using a graphics-based graphical user interface in accordance with the present invention.
FIGS. 26A-26C illustrate one embodiment of a graphic user interface in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention provides a graphical user interface which allows the user to interactively change the state of an object or objects. The interface is controlled by a pointing device (mouse or tablet) or any other input device whose output may be translated to an x,y position on a second window.
In automation: The visual changes of the object that occur as the pointer is moved create an animation sequence. Since the user may see the resulting change of the object in real-time as the pointer moves, the process of creating the animation becomes a truly interactive performance. This is much different than the more step-by-step procedures used in traditional animation interfaces.
In a search: The interface of the present invention may also be used interactively to search to find a desired state of the object. Since the user may see the resulting change of the object as he moves the pointer, the search process is guided by a tight feedback loop. In the current art, database queries are delimited through a set of key words or expressions, and the result is displayed as an ordered list of documents that contain the set of keywords or expressions. The documents are ordered by relevance, where relevance is defined algorithmically as a match between the query terms and the frequency and distribution of those terms, or semantic associations of those terms, in the documents. Modifying the query will result in a reordered list. Examples of modifications are specifying different degrees of relevance of the terms, deleting some terms, introducing new terms, and indicating which terms should be close to one. The current art for describing these modifications includes Boolean string, binary relevance operators (e.g., + or −), checklists, and graphical techniques for inserting or deleting terms. Often a query will return a large set of documents and it is difficult to determine algorithmically the appropriate relevance weightings that fit the needs of the user. In contrast, the present invention provides a novel method for rearranging the query result. Using techniques developed for real-time graphical manipulation of animated figures, a graphical user interface may be used in accordance with the present invention to rearrange the query result. Each node in a graph represents a term in the query. One advantage provided by the present invention is that the nodes may be arbitrary rearranged in a two dimensional, or simulated three dimensional, display. Thus, terms with no semantic association may be arranged near one another. Positioning a cursor in the display results in a unique ordering of the query result. Notably, the cursor need not be on a node or on the direct path between nodes. If the cursor is on a node, then the term associated with that node receives the strongest relevance weighting. As the cursor is repositioned between nodes, the distance between the cursor and each node (i.e., term) is used to calculate a new set of relevance weightings. Rearranging the graph creates new possible combinations of weights. Positioning the cursor within the graph defines a unique combination of weights. The position of the cursor may be moved within the graph, and each repositioning causes a new list to be displayed.
In its basic configuration, the user interface of the present invention consists of two windows, a display window and a target (controller) window. The target window displays a two dimensional arrangement of target points where each target represents a DISPLACEMENT of the object from some BASE STATE. As the user drags the pointer over the target window, the object is updated and redrawn in the display window. The state change in the object is determined by the proximity of the pointer to the various targets.
The user is allowed to arrange the targets as desired, thus defining the potential search or animation space. Each target has an area of influence which is used to determine (based on the mouse position) how much of that target's displacement is applied to the object. The WEIGHTING CALCULATION may use any arbitrary function, but is typically based on the distance between the pointer and the target. How the target displacements are defined or selected is defined by a preselected external interface or procedure.
The object's state is changed as follows: every time the pointer position changes, the object is first put into its default base state. Then, all the targets are applied to the object based on their weighting, which is calculated from the mouse position. Often, only a small number of targets will be close enough to the mouse to have any influence. The object (“PARAMETER OBJECT”) may then either be directly displayed or its set of parameters and values may be applied to another “DISPLAY OBJECT” which the user sees. The following Lisp pseudo-code shows what happens every time the user moves the pointer:
(defun PROCESS-NEW-INPUT (window targets parameter-object display-object pointer-x pointer-y) (goto-base-state parameter-object) (loop for target in targets
for weighting=(computer-weighting target pointer-x pointer-y) do (add-displacement parameter-object (get-displacement target) weighting))
;; update the DISPLAY-OBJECT from the PARAMETER-OBJECT (if they are the same, this is no-op) (apply-update parameter-object display-object) (redisplay window display-object parameter-object)) (defun ADD-DISPLACEMENT (object displacement weighting) (loop for parameter in (get-parameters object)
do (set-parameter-value object parameter
(+ (get-parameter-value object parameter) (* weighting (get-displacement-values displacement))))))
The OBJECT (or “PARAMETER OBJECT”) is anything that may be represented or encoded by a sequence of properties and their associated numeric values. It is this object which is directly changed by the interface in the manner described in the algorithm.
A STATE is a given set of parameters and values associated with a particular object. So, for example, the state of a television set might be defined by the values for the current channel, contrast, brightness, color and tint. Or the state of a human body, for animation purposes, might be defined by the state of bone rotations around their respective joints. One set of angles may define a “throw” pose and another may define a “crouch” pose.
The DISPLAY OBJECT is the object that the user sees in the display window. The DISPLAY OBJECT potentially may be different from the parameter object. The transition from the parameter object to the display object may be arbitrarily complex. For example, if the parameter object represents various parameters used in a physical simulation (gravity, wind velocity, friction, etc.), those parameters will be applied in the simulated environment, and the simulated environment will be redisplayed. On the other hand, often the parameter object may be displayed directly itself. For example, a human animation skeleton may serve both as a displayable structure and as a container for the various parameters and values that define the different body pose states.
The BASE STATE of an object is a default state that is used as a reference to save displacements (see below).
A DISPLACEMENT is the difference between two states of an object. Typically, a DISPLACEMENT is the difference between a desired target state and the base state.
The WEIGHTING CALCULATION is the function used to computer how much influence a given target has. One simple weighting calculation uses a radial falloff where each target represents the center of a circle. When the mouse is directly over the target (in the center of the circle), the full weight of that target's displacement is applied to the object. When the mouse is outside of the circle, the target has no effect on the object's state, and the weighting inside the circle is a number from 0.0 to 1.0, reflecting the pointer's distance from the center.
It is clear that not all possible states may be reached by this interface given a particular set and arrangement of targets. Thus, only those states that result from the linear combination of the defined target displacements, wherein the weightings are derived from the mouse position, may be achieved. The present invention provides a new user interface technique, system or method that may be applied to various domains.
The present invention provides a real-time interface for performer animation that enables a user to create various classes of targets with different behaviors, internal structure, and graphical representations wherein the animation includes some of the expressive power of scripted systems with natural input gestures and real-time control of interactive systems. In addition, target poses for performer animation may be combined into compound target poses and treated as one unit. Thus, the present invention provides the advantages of real-time animation with less complexity in providing development f expression and movement for target poses.
The present invention may be used to control body movement, dancing and facial expressions of a three dimensional character in an on-line shared music environment, chat room, interactive game or the like. The invention may also be applied to dynamically control sound synthesis.
FIG. 1 is a graphical representation of a 4-way split screen depiction of one embodiment of an implementation scheme on a computer screen in accordance with the present invention. In the upper left portion of FIG. 1 , a wire-frame depiction of a head 102 is shown as a basic unit to be animated. The basic unit to be animated is selected by using a cursor directed by a mouse, a mouse-directing post, touchpad or the like, to click on the desired geometry selection selected from the plurality of geometry selections shown on the geometry selection screen 104 indicated in the lower left portion of FIG. 1 . Where desired, the user may select to have the wire frame covered with “skin” that may be shaded in various sections. However, it should be noted that selection of the skin-covered version of the head requires more memory than the wire-frame version of the head, so that, depending on the computer's computational capacity, the skin-covered version of the head may move at a slower rate than the wire-frame version of the head. Typically, for example, a 450 MHz computer with a Pentium processor may implement the present invention.
After selecting the basic unit to be animated, at least one target screen is selected for the upper right portion. In the example shown in FIG. 1 , target facial expression of Fear 106 , Surprise 108 , Anger 110 , Surprise Smile 112 , Smile II 114 and Disgust 116 have been selected by clicking on the + button to show a pull-down screen with available facial expressions, thus providing a dot target or anchor on the screen for each selected facial expression, and then moving the dot target or anchor by mouse-clicking on the dot target or anchor and dragging the dot target or anchor to the desired position on the screen. The software programs listed on the pull-down screen for the facial expressions have been prepared previously. Typically, the cursor is placed on a dot target or anchor for a desired facial expression, and then the cursor is moved to a dot target or anchor for a next desired facial expression. The software for the selected facial expression interpolates the facial expression as the cursor is moved, animating the head to change from the facial expression for the first dot target or anchor to a next facial expression for the next dot target or anchor. Double-clicking and dragging the dot targets or anchors closer together, as shown in FIG. 1 when the dot target or anchor for Anger 110 is dragged to a position 118 close to the Surprise 108 , provides for faster change in facial expression to the next facial expression when the cursor is moved from Anger 18 to Surprise 108 or, when the dot targets or anchors are superimposed, provides for combining the selected facial expressions. As shown in the lower right portion of FIG. 1 , a layer may be added with camera poses. For example, camera pose 1 132 may represent viewing the character from a close-up perspective, and camera pose 2 134 may represent viewing the character from a distance.
In addition, other layers may be added, as, for example, when the facial expression is to be combined with motion. For example, where a wire-frame figure or skin-covered figure is used for a body to be animated, the geometry may be selected by mouse-clicking in the geometry selection area at the lower left of FIG. 1 . A head may be added in the same manner, providing, for example, a character shown in FIG. 2A .
FIG. 2A is an illustration of a character 202 in a dance pose based on clicking a mouse for a cursor 204 very close to the sway-right 206 target pose selection shown on the skeleton controller in FIG. 2B . Two windows are utilized: a performer window and a target pose window, wherein the target pose window may have a plurality of layers. Each layer of the pose window shows available characteristics for a skeletal action, facial expression, or the like. For example, in the lower right portion of FIG. 1 , target poses Arms Up 120 , Arms Raised Halfway 122 , Sway Left 124 , Sway Right 126 are selected in a manner similar to the selection of facial expressions. Where desired, the target screen on the lower right portion of FIG. 1 may be selected and added to the target screen on the upper right portion of FIG. 1 . When the cursor is dragged over the overlaid layers, the facial expression of the character, as well as his target pose, change in accordance with the position of the cursor relative to the target facial expressions and the target poses.
In addition, customized poses may be made, for example, by placing the cursor on each desired limb and dragging the limb to the desired position. The customized pose is then saved. FIG. 3A is an illustration of a character 302 in a dance pose based on clicking a mouse for a cursor 308 approximately equidistant from the sway-right 304 target pose selection and the sway-left 306 target pose selection shown on the skeleton controller in FIG. 3B . As the cursor is dragged from one target pose to a next target pose, geometrical x,y values representing the pose in the underlying software program are interpolated, and the screen shot illustrated shows a change in the pose from a swing-right pose twoard a swing-left pose.
FIG. 4A is an illustration of a character 402 in a dance pose based on clicking a mouse for a cursor 408 vary close to sway-left 406 target pose selection shown on the skeleton controller in FIG. 4B . FIG. 5A is an illustration of a character 502 in a dance pose based on clicking a mouse for a cursor 504 approximately equidistant from the sway-right 508 target pose selection, the in-between 506 pose selection and the sway-left 510 target pose selection shown on the skeleton controller in FIG. 5B .
FIG. 6A is an illustration of a character 602 in a dance pose based on clicking a mouse for a cursor 604 very close to the in-between 606 target pose selection shown on the skeleton controller in FIG. 6B . Where desired, the cursor may be clicked on each limb of the character in the poses when the limb is to be moved, and the limb is dragged to the desired position.
FIG. 7A is an illustration of a facial configuration 702 based on clicking a mouse for a cursor 704 in an area apart from the target selection shown on the facial controller in FIG. 7B . FIG. 8A is an illustration of a facial configuration 802 based on clicking a mouse for a cursor 804 in an area substantially on the surprise target selection shown on the facial controller in FIG. 8B . FIG. 9A is an illustration of a facial configuration 902 based on clicking a mouse for a cursor 906 in an area substantially halfway between the surprise target 904 selection and the anger target 908 selection shown on the facial controller in FIG. FIG. 9B. 10A is an illustration of a facial configuration 1002 based on clicking a mouse for a cursor 1004 in an area substantially on the anger target selection shown on the facial controller in FIG. 10B . FIG. 11A is an illustration of a facial configuration 1102 based on clicking a mouse for a cursor 1106 in an area substantially halfway between the anger target 1104 selection and the smile-big target 1108 selection shown on the facial controller in FIG. 11B . FIG. 12A is an illustration of a facial configuration 1202 based on clicking a mouse for a cursor 1204 in an area substantially on the smile-big target selection shown on the facial controller in FIG. 12B . FIG. 13A is an illustration of a facial configuration 1302 based on clicking a mouse for a cursor 1310 in an area substantially equidistant between the anger target 1306 selection, the surprise target 1304 selection and the smile-big target 1308 selection shown on the facial controller in FIG. 13B . Clearly, other facial expression selections may be utilized.
Sequential changes may be made to an arrangement of a plurality of boxes in accordance with the present invention. The boxes may, for example, be arranged in a circle, a line, a spiral, every third one located inward, every fifth one located inward, randomly, or as a vertical circle inside a horizontal circle. By dragging the cursor to the different dot targets or anchors, the arrangements are transformed from a first configuration to a second configuration. By adding a camera pose layer, the user may zoom in and out for the configurations.
FIG. 14A is an illustration of a configuration of a series of blocks 1402 based on clicking a mouse for a cursor 1404 in an area apart from the target selection shown on the block controller in FIG. 14B . FIG. 15A is an illustration of a configuration of a series of blocks 1502 based on clicking a mouse for a cursor 1504 in an area approaching the line target 1506 selection shown on the block controller in FIG. 15B . FIG. 16A is an illustration of a configuration of a series of blocks 1602 based on clicking a mouse for a cursor 1604 in an area substantially on the line target 1606 selection shown on the block controller in FIG. 16B . FIG. 17A is an illustration of a configuration of a series of blocks 1702 based on clicking a mouse for a cursor 1706 lying intermediate between the line target 1708 selection and the spiral target 1704 selection shown on the block controller in FIG. 17B . FIG. 18A is an illustration of a configuration of a series of blocks 1802 based on clicking a mouse for a cursor 184 in an area substantially on the spiral target 1806 selection shown on the block controller in FIG. 18B . FIG. 19A is an illustration of a configuration of a series of blocks 1902 based on clicking a mouse for a cursor 1904 in an area substantially on the star 3 target 1906 selection shown on the block controller in FIG. 19B . FIG. 20A is an illustration of a configuration of a series of blocks 2002 based on clicking a mouse for a cursor 2006 lying intermediate between the line target 2008 selection and the star 3 target 2004 selection shown on the block controller in FIG. 20B . FIG. 21A is an illustration of a configuration of a series of blocks 2102 based on clicking a mouse for a cursor 2104 lying closer to the line target 2106 selection than to the star 3 target 2108 selection shown on the block controller in FIG. 21B .
The user may insert facial and skeletal target poses in a performer window by dragging and dropping a selected pose from a palette of pre-defined target poses in the target pose window. To animate the character, the user drags the mouse over the target pose window. The target poses are additively applied to the character based on proximity to the cursor. Thus, for example, a smile may dynamically morph into a frown as the cursor moves between a smile target and a frown target, or one dance step may transition to another dance step. The exact layout of targets defines a graphical lexicon of input gestures with corresponding character motions. Various classes of targets may be created with different behaviors, internal structure, and graphical representations. In addition to the target poses on the palette, there may be other choices such as “Begin Recording”, “End Recording”, and “Play Recording”. By selecting “Begin Recording”, the cursor path is recorded, and is shown as a marked path on the computer screen. This recording may be viewed as a video clip by selecting “Play Recording” on the palette and clicking on the marked path. FIG. 22 is an illustration of a recording 2202 of a series of facial expressions utilized wherein the recording may be used to re-implement the series.
The present invention may be implemented as an electronic display system, shown in one embodiment in block diagram form in FIG. 23 , operative to facilitate interactive, expressive, three dimensional animation by a user. The electronic display system includes a central processing unit 2302 , coupled to a system bus 808 ; a memory unit 2304 coupled to the system bus 2308 and having loaded therein an operating system 2312 , application programs 2314 and computer-executable instructions for interactive graphic user-interface animation or searching 2316 ; a display unit 2310 coupled to the system bus 2308 ; a cursor control unit 2306 coupled to the system bus 2308 ; and the system bus 2308 , for linking the central processing unit, the display unit, the memory unit, and the cursor control unit. In one embodiment, the computer-executable instructions for interactive graphic user-interface animation or searching 2316 may include: inserting a desired character, image, or query term onto a first window, which may be accomplished, for example, by selection from a palette in another window; inserting dot targets, anchors, or node terms onto a second window by, for each dot target, anchor, or node term, selecting a desired pose or selection from a plurality of predetermined poses, selections, or terms; and upon a cursor being dragged over the second window to a desired dot target, anchor, or node term, additively applying characteristics for the desired dot target, anchor, or node term to the desired character, image, or query term based on a proximity of the cursor to the desired dot target, anchor, or node term. The cursor control unit 806 may be a mouse, a moveable control peg in a keyboard, a touch-sensitive pad, or the like. The characteristics for the dot targets, anchors, or node terms are selectable for the use employed by the user. For example, for animation, characteristics may include facial expressions, character poses, or camera positions (for zooming in and out with respect to the view). The electronic display system may be implemented by a computer display system. Dot targets, anchors, or node terms may be combined by dragging a desired dot target, anchor, or node term onto at least one other dot target, anchor, or node term to form a compound dot target, anchor, or node term that has the characteristics of the combined dot targets, anchors or node terms. A palette may be generated by the computer-executable instructions and shown in a third window on the display unit. The palette may be used for selecting a desired character, image or query term to be inserted onto the first window.
FIG. 24 shows one embodiment of steps for a method or computer-executable instructions 2408 for facilitating interactive, expressive, three dimensional animation or searching on an electronic display system by a user in accordance with the present invention. The steps include: inserting 2402 a desired character, image, or query term onto a first window; inserting 2404 dot targets, anchors, node terms onto a second window by, for each dot target, anchor, or node term, selecting a desired pose, selection, or query term from a plurality of preselected poses, selections, or query terms; and dragging 2406 a cursor over the second window to a desired dot target, anchor, or query term wherein characteristics for the desired dot target, anchor, or node term are additively applied to the desired character, image, or query term based on a proximity of the cursor to the desired dot target, anchor, or node term. The characteristics are as described above. The electronic display system is typically a computer display system. Combinations of dot targets, anchors, or node terms are made by dragging one dot target, anchor, or node term onto at least one other dot target, anchor, or node term to get combined characteristics (interpolated). A palette may be used to select characters, images or query terms as described above.
Clearly, a computer-readable medium having computer-readable instructions 2408 may be used for implementing the present invention. The instructions provide for executing the steps of the method of the invention and are implemented in the fashion described above.
As shown in FIG. 25 , the present invention may be implemented as a method or computer-readable medium 2502 having computer-executable instructions for facilitating animation or searching using a graphical user interface. The method or computer-readable medium include steps or computer-executable instructions that include: dragging 2504 a pointer over a two/three dimensional arrangement of a plurality of target points, anchors, or node terms in a target or controller window wherein each target, anchor or node term represents a displacement of a state of an object from a base state; and redrawing or updating 2506 the base state of the object in a display window in accordance with the proximity of the pointer to the target points, anchors or node terms as the pointer is dragged over the target window. Where desired, positions of the plurality of target points, anchors, or node terms in the target or controller window may be set by the user.
For example, the user may use the pointer to position the plurality of target points, anchors, or node terms, either individually or as a group. Typically, each target has a predetermined area of influence that is used to determine, based on a position of the pointer, the displacement to be applied to the object. The state of the object is generally redrawn or updated by putting an object into a default base state when a position of the pointer changes, then applying targets, anchors, or node terms to the object based on a weighting of each target, anchor, or node term, wherein the weighting is calculated based on the displacement of the pointer from the target, anchor, or node term. Each redrawing or updating of the base state of the object may be recorded to provide an animation path or search path which may be used to reproduce the series of redrawings or updatings. The animation path or search path is typically editable.
For example, pointing and clicking may be used to select and change or delete any portion of the animation or search path. Where desired, multiple targets, anchors or node terms with individual weightings may be applied simultaneously.
Current search engines use a variety of measures to algorithmically determine whether or not a document (or more generally an object) is relevant to a query. Common examples include statistical measures such as term frequency and the inverse document frequency of the term and its distribution across all documents in the database. Documents that are longer, more recent, more popular, more frequently linked to by other documents, and whose title or meta-tags contain some of the query terms are typically judged more relevant than documents lacking these characteristics. Various algorithms (often proprietary) are used to expand the query terms and weight and combine the relevance ranking factors. The present invention is independent of the particular factors. What is important is that a set of factors and normative weights for each factor are defined.
TABLE 1
Example 1 (33% 33% 33%): trust psychology web
1. Bulkley Book Rvw.html Relevance: 100%
2. High Trust ® Thinking/Leadership/Teaching & Trust
Psychology ® Relevance: 100%
3. Why Christians Can't Trust Psychology Relevance: 100%
4. Why Christians Can't Trust Psychology Relevance: 100%
5. Recommended Reading: Psychology Relevance: 84%
Example 2 (50% 33% 17%): trust trust trust psychology psychology web
1. DEEP-ECOLOGY mar97 discussion:: Eco-Psychology & Activism:
2. GIVING TO THE AMERICAN PSYCHOLOGICAL FOUNDATION
Relevance: 100%
3. Healthcare Psychology Research Group Relevance: 100%
4. PSYCHOHERESY ABOUNDING Relevance: 100%
5. The Trust Advocate 800 Risk Management Program Relevance: 100%
Example 3 (50% 17% 33%): trust trust trust psychology web web
1. Moving WebWord: Gaining Users' Trust Relevance: 100%
2. CPA R. A. Burrell's Accounting Resource Guide Relevance: 100%
3. Legal Notices about This Web site Relevance: 100%
4. Web Security: A Matter of Trust, WWW Journal: Relevance: 100%
5. Awesome Web Solutions for Small Business - THaNet
Relevance: 100%
Example 4 (17% 50% 33%):
trust psychology psychology psychology web web
1. WEB Site for Psychology 101 Relevance: 100%
2. Psych Web list of Psychology Megalists Relevance: 100%
3. Community Psychology Awards Given to Web Sites Relevance: 100%
4. Selected Internet Resources for Psychology Relevance: 100%
5. Social Psychology Network Relevance: 100%
Example 5 (17% 33% 50%): trust psychology psychology web web web
1. Community Psychology Awards Given to Web Sites Relevance: 100%
2. Psychology Resources on the World Wide Web Relevance: 100%
3. WEB Site for Psychology 101 Relevance: 100%
4. Psych Web list of Psychology Megalists Relevance: 100%
5. About the Web Site Relevance: 100%
Current search engines allow limited control over the weights and factors used to determine relevance rankings. Search engines such as ‘http://www.altavista.com’ and many other popular engines allow terms to be prefixed with a “+” indicating that relevant documents must contain the term, and “−” indicating that relevant documents must not contain the query term. A few search engines such as ‘http://www.infoseek.com’ weigh repeated query term more heavily than term used only once in a query. For example, a shown in Table 1 above, where listings were generated by infoseek by varying the occurrences of “trust”, “psychology”, and “web” in a query, it is clear that the query terms “trust”, “psychology” and “web” retrieve different sets of document references depending upon how often each term is repeated. The query was intended to retrieve documents on the psychology underlying attributed trustworthiness of websites. As may be seen from examining Table 1, many of the retrieved references were not relevant to the search goal. Notably, in the examples shown in Table 1, the same number of document references was retrieved for each query. What differs is the relative rank assigned to each.
FIGS. 26A-26C illustrate one embodiment of a graphic user interface in accordance with the present invention. FIG. 26A shows a selection of anchor terms: “trust”, “psychology” and “web”. The numbered arrows indicate different cursor positions. The numbers of the arrows refer to the examples shown in Table 1. FIG. 26B shows a control screen for selecting or deleting anchor terms. FIG. 26C shows a display of a list of documents references and summaries generated for cursor position “2” in FIG. 26A . As shown in FIGS. 26A-26C , in the current invention the query terms, any terms in the expanded query (i.e., semantic cohorts of the original query), and other relevancy factors may be chosen as anchors in a visual display in accordance with the display properties described earlier for the animation system. The relative position of the anchors may be modified via drag-and-drop manipulations. The existence of an anchor may be manipulated by choosing the factor from a list of factors. Positioning the cursor within the display will determine how the anchors are weighted, which in turn will determine the relevance ranking of the documents. Notably, the anchors may be the type of relevance ranking factors mentioned above, or in a mega search engine, e.g., ‘http;//www.dogpile.com’, the anchors may be various constituent search engines that are used by the mega search engine. The weight given to a particular domain or the inclusion of an audio or graphic image may also be used. The present invention is not limited to the preceding lists of factors but may accommodate any well-defined factor.
TABLE 2
Number of
Last
Number of links
hyperlink
Document link
Doc. title
Doc. Summary
modified
referencing doc
in doc.
http://www.ap . . .
GIVING TO THE
Description of the
Apr. 15, 1999
240
6
AMERICAN
types of giving
PSYCHOLOGICAL
to the
FOUNDATION
American
Psychological
Foundation.
Table 2, shown above, is an illustration of a database generated in client memory to permit fast regeneration of a list of document references and summaries. Double-boxed cells are table column headers defining the content of each column. The second row of the table is an example of a row entry taken from the second entry of the web search results shown in FIG. 26C . The number of links in the last two columns represent arbitrary values selected for this example. As shown in Table 2 above, in the preferred arrangement, the search engine returns to the client not only the ten or so most relevant document references and summaries (where relevance is determined algorithmically) as is typically done, but also a database containing a much larger list of references (e.g., the top 1000 documents), summaries, and the unweighted vector of factors. This allows vary fast recompilation and display of the “most relevant” document references.
The examples shown in Table 1 could be generated by moving a cursor appropriately between the anchors, “trust”, “psychology” and “web”. The other factors, e.g., document, recency, and popularity, would continue to affect the relevancy rankings as before. The cursor's movements would only affect the weights associated with the chosen anchors. In the preferred arrangement, the list of relevant document references and summaries is re-generated whenever the mouse button is released in a drag and drop manipulation.
By including or excluding various anchors and moving the anchors and the position of the cursor relative to these anchors, a user may explore the list of retrieved document references far more efficiently than moving to each ‘next’ screen of 10 references, or resubmitting the query with repetitions of some of the query terms.
Although the present invention has been described in relation to particular preferred embodiments thereof, many variations, equivalents, modifications and other uses will become apparent to those skilled in the art. It is preferred, therefore, that the present invention be limited not by the specific disclosure herein, but only by the appended claims.
|
An arrangement provides for displaying an object, such as a drawn object, or a database search result, based on a graphical user interface. A first display window is provided for specifying attributes of an object. A second window is provided for spatially inserting anchors for the object, where each anchor specifies a desired characteristic of the object, such as a pose of a face. A third window is provided for the desired object display. The anchors are placed in the second window with the aid of a controlled cursor. Placement of the cursor in the second window also controls the displayed object in the third window, which is developed based on the placement of the cursor in the second window relative to the anchors.
| 6
|
BACKGROUND OF THE INVENTION
[0001] This invention relates to a process for producing chitin derivatives and/or chitosan derivatives with a crosslinked structure by adding purified water to chitin derivatives and/or chitosan derivatives, kneading the mixture well and applying an ionizing radiation to the kneaded mixture. The chitin derivatives having a crosslinked structure are hydrogels and the chitosan derivatives having a crosslinked structure are hydrogels having antimicrobial activity.
[0002] Hydrogels can hold a large amount of water within the three-dimensional network structure generated by crosslinking with radiation. The retained water will not seep out under slight pressure. Such hydrogels are already in use as disposable diapers and as humectants in cosmetics.
[0003] Carboxymethyl-chitin (CM-chitin) and carboxymethyl-chitosan (CM-chitosan), if they are irradiated in either a solid form or as a dilute (≦5%) aqueous solution, preferentially undergo decomposition and no hydrogels will form. If they are irradiated in a concentrated paste form (that will not flow out if the container is tilted), a crosslinked structure can be introduced and the resulting gel will absorb water upon immersion in it to become a hydrogel. In the case of a CM-chitosan hydrogel, it has been found to have a new feature, antimicrobial activity, in spite of it being a hydrogel.
[0004] Hydrogels can be easily obtained by applying an ionizing radiation to aqueous solutions of polyethylene oxides, poly(vinyl alcohol), polyacrylamides, polyvinylpyrrolidone, etc. Being capable of absorbing and holding a large amount of water, hydrogels are used in medical and cosmetics fields as sanitary products (e.g. disposable diapers) and humectants. These hydrogels are primarily made of poly(sodium acrylate) based materials. Used hydrogels are disposed of by incineration, so if they are treated massively, the temperature in the incinerator will drop to cause a potential problem of producing dioxins. Attempts are therefore being made to use hydrogels that decompose in the soil to exert no environmental impact, as exemplified by poly(sodium glutamate) and poly(sodium aspartate) having irradiation-generated crosslinks.
[0005] Formaldehyde and glutaraldehyde are conventionally used to create chemical crosslinks in chitin and chitosan. However, since the aldehydes contaminate the working environment or the residual aldehydes may irritate the skin, a safer method of crosslinking is desired.
[0006] Hydrogels produced by crosslinking water-soluble polymers absorb a large amount of water, so they are used in sanitary products such as disposable diapers. Typically, zeolite incorporating antimicrobes such as silver are added as an antimicrobial agent. However, accumulation of silver is not preferred from the viewpoint of health. It is therefore required to develop high-molecular weight polymers that themselves have antimicrobial activity.
[0007] Chitosan has positive electric charges, so they bind to negatively charged microorganisms and exhibit antimicrobial activity to inhibit microbial growth. Thus, the applicable scope of chitin and chitosan which are currently discarded will expand and their added value will further increase if a safer method of their crosslinking is found and if hydrogels that themselves have antimicrobial activity are developed. However, chitin and chitosan have no compatible solvents and if they are irradiated in a solid state, marked decomposition will occur. Therefore, chitin and chitosan are difficult to process into films or fibers and it is also difficult to crosslink them by radiation.
[0008] If the hydrogen in hydroxyl groups in chitin and chitosan is replaced by a hydroxyl or carboxyl group, intermolecular hydrogen bonds sufficiently weaken that chitin and chitosan willcome to dissolve in water. As a result of their intensive studies, the present inventors found that carboxymethylated chitin and chitosan (chitin and chitosan derivatives) could be crosslinked when irradiated in a thick paste form. The present invention has been accomplished on the basis of this finding. It was also revealed that CM-chitosan was a hydrogel having a unique feature of presenting antimicrobial activity.
SUMMARY OF THE INVENTION
[0009] Water-soluble chitin and chitosan derivatives, when exposed to radiation either in a solid state or as a dilute (≦5%) aqueous solution, preferentially undergo decomposition, so it has been difficult to process them by radiation-induced crosslinking. The present inventors added purified water to chitin and chitosan derivatives and kneaded them well to prepare a thick paste and successfully crosslinked the paste by applying an ionizing radiation. Interestingly, the hydrogel of CM-chitosan derivative obtained by crosslinking has antimicrobial activity.
BRIEF DESCRIPTION OF THE DRAWING
[0010] [0010]FIG. 1A is a photo showing that a PVA hydrogel has no antimicrobial activity against E. coli;
[0011] [0011]FIG. 1B is a photo showing the antimicrobial activity of a CM-chitosan hydrogel with a gel fraction of 40% against E. coli; and
[0012] [0012]FIG. 1C is a photo showing the antimicrobial activity of a CM-chitosan hydrogel with a gel fraction of 25% against E. coli.
DETAILED DESCRIPTION OF THE INVENTION
[0013] The hydrogels of chitin and chitosan derivatives according to the invention are synthesized by the following method. Chitin and chitosan derivatives having different degrees of substitution are kneaded well with purified water to make a concentrated paste that is thick enough not to flow out if the container is tilted. The paste is put into a poly(vinylidene chloride) bag, evacuated, heat sealed and exposed to electron beams. Before irradiation, the paste was soft but upon irradiation, it turned to a rubbery and elastic gel. In order to perform radiation-induced crosslinking, the paste must have a concentration of at least 10%, preferably between 30% and 50%. In a solid state or at concentrations lower than 10%, decomposition occurs preferentially and there is no visible gel formation by crosslinking. Solubility in water varies with the degree of substitution and the higher the substitution, the thicker the paste that can be prepared and the faster its preparation.
[0014] The ionizing radiation can be γ-rays, electron beams or X-rays. The crosslinking dose is 0.5˜1,000 kGy, preferably 5˜300 kGy.
[0015] Any chitin and chitosan derivatives that are soluble in water can be used in the invention. Higher degrees of substitution are preferred since they increase the affinity for water and, hence, provide thicker pastes. The most preferred degree of substitution is 0.3˜0.9. Chitin is extracted from the outer covering of crustaceans such as shrimps and crabs by deproteinization and chitosan is obtained from chitin by deacetylation. Since chitin and chitosan are comparatively cheap materials, they are preferred as materials for the synthesis of derivatives.
[0016] Examples of the chitin derivatives of the invention include CM-chitin, carboxyethyl-chitin, methyl-chitin, ethyl-chitin, hydroxyethyl-chitin, hydroxypropyl-chitin, oxidized chitin, acetyl-chitin, aminoalkyl-chitin and allyl-chitin. Examples of the chitosan derivatives of the invention include CM-chitosan, carboxyethyl-chitosan, methyl-chitosan, ethyl-chitosan, hydroxyethyl-chitosan, hydroxypropyl-chitosan, oxidized chitosan, acetyl-chitosan, aminoalkyl-chitosan and allyl-chitosan.
[0017] For the purpose of industrial production, two preferred examples of the ionizing radiation are γ-rays from cobalt-60 and electron beams from an accelerator. The most preferred electron accelerator is one of medium to high energy types that have acceleration voltages of at least 1 MeV and can irradiate thick sheets. If a yet-to-be irradiated sample is pressurized to form a film, even the electron beams from a low-energy electron accelerator having an acceleration voltage of less than 1 MeV can penetrate the sample and the intended gel can be formed by radiation-induced crosslinking. During irradiation, oxygen has little effect on crosslinking; however, in order to ensure that water will not evaporate and the density of crosslinks will not decrease during irradiation, the top surface of the sample is desirably covered with a film of plastics such as polyester.
[0018] Gel fraction is determined as follows. The gel formed by irradiation is freeze-dried and put into a vacuum dryer where it is dried at 50° C. until its weight becomes constant. The dried sample is put into a cage of stainless steel wire having a fineness of 200 mesh and immersed in a large volume of water for 48 hours. The uncrosslinked soluble component of the sample has moved into the aqueous phase, leaving only the gelled component in the cage. The stainless steel cage holding the gel is immersed in methanol for 1 hour, recovered and then dried at 50° C. for 24 hours. Gel fraction is calculated by the following equation:
Gel fraction (%)=(gel weight without soluble component/initial dry weight)×100
[0019] To determine the degree of swell, an irradiated paste of sample is immersed in a large volume of water for 48 hours and the obtained gel is freeze-dried and immersed in purified water; the degree of swell is expressed in grams of the purified water absorbed by one gram of the dry gel.
[0020] The antimicrobial activity of the hydrogel is determined as follows. An irradiated paste of sample is immersed in purified water for 48 hours in order to remove the uncrosslinked sol. The remaining gel is cut to a specified size and put into a Petri dish containing an agar medium plated with E. coli . As time passes, E. coli grows. A clear zone forming around the hydrogel indicates an inhibition of E. coli growth and one may conclude that the hydrogel has antimicrobial activity.
[0021] Chitosan has antimicrobial activity whose intensity increases if the molecular weight of chitosan is decreased by irradiation. However, chitosan dissolves only in dilute acids and cannot be easily processed into hydrogel or sheet. According to the invention, a hydrogel having antimicrobial activity could successfully be produced from chitosan derivatives by crosslinking them with radiation. By radiation-induced crosslinking, the hydrogel can be obtained in blocks, sheets or various other shapes and may find use in the following applications.
[0022] In the medical field, the hydrogel of chitosan derivatives or their blends with other hydrogels may be used as wound dressings that are applied to cover wounds due to injury or burn and promote their healing. Wound dressings of wet type have recently been put on the market since burn and wounds such as bedsores of the elderly can heal rapidly in a wet environment and the healed wound has a smooth surface. The wound dressing using the hydrogel of chitosan derivatives according to the invention is different from the conventional wet type wound dressing since the hydrogel itself has antimicrobial activity and there is no need to add any antimicrobes.
[0023] The antimicrobial hydrogel of the invention can be gel spun into fibers having antimicrobial activity. The hydrogel may be deprived of water by evaporation and can subsequently be shaped into a film, which is attached to the surfaces of various substrates to thereby make antimicrobial articles that can prevent the growth of molds and other deleterious microorganisms. Thus, the antimicrobial hydrogel of the invention has potential application in various fields.
[0024] The following examples and comparative examples are provided for further illustrating the present invention.
EXAMPLE 1
[0025] CM-chitin was used; it had a degree of substitution of 0.49, a molecular weight of 2.82×10 4 and a degree of deacetylation of 17.7%. It was kneaded well with varying volumes of purified water to make samples in paste (grease) form at concentrations of 10, 20, 30, 40 and 50%, which were irradiated with electron beams to a dose of 50 kGy. The results are shown in Table 1, from which it is clear that by irradiating the paste, a water-insoluble gel formed and crosslinking occurred. Upon immersion in a large volume of water, the crosslinked CM-chitin swelled to form a hydrogel. For crosslinking, the CM-chitin preferably has a concentration of 20-40%.
TABLE 1 Gel fractions and the degrees of swell in the case of exposing 50 kGy of electron beams to CM-chitin (degree of substitution: 0.49) at varying concentrations Concentration (%) 10 20 30 40 50 of CM-chitin Gel fraction (%) 31 48 50 52 28 Degree of swell 111 56 34 21 93 (g H 2 O/1 g dry gel
EXAMPLE 2
[0026] CM-chitin was used; it had a degree of substitution of 0.83, a molecular weight of 2.93×10 4 and a degree of deacetylation of 31.4%. It was kneaded well with varying volumes of purified water to make samples in paste (grease) form at concentrations of 10, 20, 30, 40 and 50%, which were irradiated with electron beams to a dose of 50 kGy. The results are shown in Table 2, from which it is clear that by irradiating the paste, a water-insoluble gel formed and crosslinking occurred. Upon immersion in a large volume of water, the crosslinked CM-chitin swelled to form a hydrogel. For crosslinking, the CM-chitin preferably has a concentration of 20˜40%.
TABLE 2 Gel fractions and the degrees of swell in the case of exposing 50 kGy of electron beams to CM-chitin (degree of substitution: 0.83) at varying concentrations Concentration (%) 10 20 30 40 50 of CM-chitin Gel fraction (%) 41 52 59 61 46 Degree of swell 148 58 20 14 120 (g H 2 O/1 g dry gel
COMPARATIVE EXAMPLE 1
[0027] Two kinds of CM-chitin were used; one of them had a degree of substitution of 0.49, a molecular weight of 2.82×10 4 and a degree of deacetylation of 17.7%; the other had a degree of substitution of 0.83, a molecular weight of 2.93×10 4 and a degree of deacetylation of 31.4%. Each sample was exposed to electron beams from an accelerator in two states, solid at room temperature and as a dilute (≦5%) aqueous solution, until the dose was 200 kGy. In either case, the molecular weights of the samples decreased to such an extent that they were readily soluble in water; however, no water-insoluble gel component formed and no crosslinking occurred under the conditions employed.
EXAMPLE 3
[0028] CM-chitosan was used; it had a degree of substitution of 0.91, a molecular weight of 3.1×10 4 and a degree of deacetylation of 84.0%. It was kneaded well with varying volumes of purified water to make samples in paste (grease) form at concentrations of 20, 25, 35 and 50%, which were irradiated with electron beams to a dose of 100 kGy. The results are shown in Table 3, from which it is clear that by irradiating the paste, a water-insoluble gel formed and crosslinking occurred. Upon immersion in a large volume of water, the crosslinked CM-chitin swelled to form a hydrogel. For crosslinking, the CM-chitosan preferably has a concentration of 25-35%.
[0029] A test was conducted to evaluate the antimicrobial activity of a CM-chitosan hydrogel that was prepared by exposing electron beams to a paste of 35% CM-chitosan to a dose of 150 kGy. The sample was immersed in purified water for 48 hours to remove the sol which was a soluble component. The thus prepared CM-chitosan hydrogel had a gel fraction of 40%.
[0030] The hydrogel was cut to a disk with a diameter of 10 mm and placed on an agar medium plated with 1×10 6 E. coli cells/mL which were cultured at 37° C. As FIG. 1B shows, a clear zone about 5 mm wide formed around the hydrogel by inhibiting the growth of E. coli ; the CM-chitosan hydrogel obviously had antimicrobial activity.
TABLE 3 Gel fractions and the degrees of swell in the case of exposing 100 kGy of electron beams to CM-chitosanat varying concentrations Concentration (%) 20 25 35 50 of CM-chitosan Gel fraction (%) 36 40 41 43 Degree of swell 126 86 58 117 (g H 2 O/1 g dry gel
EXAMPLE 4
[0031] CM-chitosan was used; it had a degree of deacetylation of 84.0%, a degree of substitution (degree of carboxymethylation) of 0.91 and a viscosity average molecular weight of 3.1×10 4 . A CM-chitosan hydrogel was prepared by exposing electron beams to a paste of 35% CM-chitosan to a dose of 80 kGy. The sample was immersed in purified water for 48 hours to remove the sol which was a soluble component. The thus prepared CM-chitosan hydrogel had a gel fraction of 25%.
[0032] As in Example 3, the hydrogel was cut to a disk with a diameter of 10 mm and placed on an agar medium plated with 1×10 6 E. coli cells/mL which were cultured at 37° C. As FIG. 1C shows, a clear zone about 5 mm wide formed around the hydrogel by inhibiting the growth of E. coli . Growth of E. coli occurred in areas of the medium other than around the hydrogel disk.
COMPARATIVE EXAMPLE 2
[0033] CM-chitosan was used; it had a degree of substitution of 0.91, a molecular weight of 3.1×10 4 and a degree of deacetylation of 84.0%. The sample was exposed to electron beams from an accelerator in two states, solid at room temperature and as a dilute (≦10%) aqueous solution, until the dose was 300 kGy. In either case, the molecular weight of the sample decreased to such an extent that it was readily soluble in water; however, no water-insoluble gel component formed and no crosslinking occurred under the conditions employed.
COMPARATIVE EXAMPLE 3
[0034] A hydrogel prepared by irradiating an aqueous solution of 10% poly(vinyl alcohol) was tested for its antimicrobial activity. A disk of the PVA hydrogel with a diameter of 10 mm was placed on an agar medium plated with 1×10 6 E. coli cells/mL which were cultured at 37° C. As FIG. 1A shows, E. coli grew uniformly around the hydrogel with the lapse of time. No clear zone formed around the hydrogel, clearly demonstrating the absence of its antimicrobial activity. The white bands in the center of FIG. 1A are due to the reflection of light from the clear hydrogel that occurred when the picture was taken.
[0035] Speaking of potential applications of the invention, the CM-chitin has acetyl groups, so after being crosslinked, it can be reacted with such acetyl groups to create a hydrogel having a new property. The CM-chitosan hydrogel is a unique gel which itself has antimicrobial activity. In the medical field, the CM-chitosan hydrogel can be used as a wound dressing which, when applied to a wound, can prevent the ingress of germs to promote the healing of the wound. The CM-chitosan can also be employed in preventing the putrefaction of water and in the production of antimicrobial fibers.
|
A process for producing a chitin derivative and/or a chitosan derivative that have a crosslinked structure, which comprises irradiating a paste of a mixture consisting of 100 parts by weight of a chitin derivative and/or a chitosan derivative and 3˜1,000 parts by weight of purified water.
| 2
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention concerns toothbrushes, and more particularly relates to a toothbrush having a set of bristles for cleaning the teeth and a second set of bristles for cleaning the spaces between the teeth, and under the gumline.
2. Description of the Prior Art
The fundamental purpose of toothbrushes is to remove plaque and debris from the tooth surfaces, both along their outer surfaces and in the interproximal areas as well as provide gum and interdental stimulation. There is a continuing need to improve the interproximal cleaning effectiveness of toothbrushes, particularly because many consumers do not floss.
Currently marketed toothbrushes are classified into three categories: soft, medium and firm according to the degree of hardness or stiffness of the bristles. Firm toothbrushes, having stiff bristles, clean plaque well but irritate the gums. Soft toothbrushes are unable to provide adequate cleaning in the interproximal areas between the teeth. Medium toothbrushes cannot meet all three needs because some teeth need harder cleaning, others need minor cleaning, while the gums need just a massaging.
U.S. Pat. No. 6,021,541 to Mori et. al. describes a toothbrush intended to provide improved cleaning of interdental regions, and comprised of sheath/core bristles wherein the sheath is made from a polyester resin and the core is made from a polyamide resin. Bristles having tapered distal tip extremities are also disclosed.
U.S. Pat. No. 5,732,433 to Gocking et. al. discloses an interproximal brush for an electric toothbrush. The brush has bristles of two different heights, the longer length bristles providing interproximal cleaning function.
U.S. Pat. No. 5,398,367 to Lu concerns a toothbrush having both soft and hard bristles. The soft bristles are longer than the hard bristles, and provide a gum massaging effect. The variation in hardness of the bristles is accomplished by varying the diameter of the bristles.
U.S. Pat. No. 5,392,483 to Henizelman et. al. discloses a toothbrush for improved cleaning, gum stimulation and mouth feel, having varying bristle tuft heights, angling of the tufts, and critical positional arrangement of the tufts.
U.S. Pat. No. 5,511,275 to Volpenhein et. al. describes a toothbrush for achieving improved interproximal cleaning without increasing gum irritation. The ends of the bristles are rounded and have a critically selected stiffness.
U.S. Pat. No. 5,535,474 to Salazar concerns a toothbrush for cleaning teeth while simulating the gums, said toothbrush having polishing rods and stimulator rods that extend above surrounding bristles.
U.S. Pat. No. 5,926,897 to Volpenhein discloses a toothbrush for interdental stimulation comprised of a plurality of tufts having a multiplicity of primary and secondary bristles, said secondary bristles being stiffer than said primary bristles and extending above said primary bristles.
However, despite considerable prior effort, there still exists a need for a toothbrush having the ability to clean the teeth while providing the benefits of flossing. Some of the aforesaid prior toothbrushes, although having technical merit, would be expensive to manufacture.
It is accordingly a primary object of the present invention to provide a toothbrush which serves well in cleaning teeth and also provides the benefits of flossing.
It is another object of this invention to provide a toothbrush as in the foregoing object which will not irritate the gums.
It is a further object of the present invention to provide a toothbrush of the aforesaid nature which is easy to manipulate during the brushing activity.
It is a still further object of this invention to provide a toothbrush of the aforesaid nature of durable construction and amenable to low cost manufacture.
These objects and other objects and advantages of the invention will be apparent from the following description.
SUMMARY OF THE INVENTION
The above and other beneficial objects and advantages are accomplished in accordance with the present invention by a toothbrush comprising an elongated resilient handle extending between two ends and a brush head disposed at one of said ends, said brush head having a flat support surface and a plurality of tufts of bristles fabricated of polybutylene terephthalate, each tuft comprised of:
a) a multiplicity of primary bristles of uniform cross-sectional configuration having proximal ends embedded in said head and distal ends extending orthogonally outward from said support surface, and
b) a multiplicity of secondary bristles having proximal extremities embedded in said head and pointed distal extremities extending orthogonally outward from said support surface to an action zone beyond the distal ends of said primary bristles, said secondary bristles having a tapered cross-sectional configuration in said action zone that terminates in said pointed distal extremity.
BRIEF DESCRIPTION OF THE DRAWING
For a fuller understanding of the nature and objects of the invention, reference should be had to the following detailed description taken in connection with the accompanying drawing forming a part of this specification and in which similar numerals of reference indicate corresponding parts in all the figures of the drawing:
FIG. 1 is a side view of a preferred embodiment of the toothbrush of the present invention.
FIG. 2 is an enlarged fragmentary side view showing the head extremity of the toothbrush of FIG. 1 .
FIG. 3 is a top view of the head extremity shown in FIG. 2 .
FIG. 4 is a further enlarged fragmentary side view of tufts of the toothbrush shown in FIG. 2 .
FIG. 5 is an enlarged sectional view of a single tuft of bristles of the toothbrush of FIG. 4 taken in the direction of the arrows upon the line 5 — 5 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIGS. 1-5, an embodiment of the toothbrush 10 of the present invention is shown comprised of an elongated handle 11 extending between a brushing end 12 and holding end 13 , and a brush head 14 disposed upon said brushing end 12 .
Handle 11 is comprised of a contoured rigid gripping portion 15 extending upwardly from holding end 13 toward brush head 14 , and a narrowed resilient neck portion 18 extending between said gripping portion 15 and brush head 14 . Handle 11 is preferably a monolithic structure molded from a flexible thermoplastic polymer such as polyurethane, plasticized polyvinyl chloride, and product SM1300 available from the Dow Plastics Co., of Midland, Mich. Gripping portion 15 may be provided with protruding features 16 which prevent slipping in the user's hand, and further provided with a recess 17 for thumb placement.
Gripping portion 15 may have a thickness of 13 to 18 millimeters at its site of greatest thickness. Neck portion 18 has a contour which tapers to gradually diminished thickness in proceeding from gripping portion 15 toward brush head 14 . At its site of minimal thickness, adjacent said brush head, the thickness of the neck portion is preferably between about 4 and 6 millimeters. The resiliency of the neck portion may be characterized in terms of bending modulus. The preferred bending modulus is such that a force of one pound applied to brushing end 12 produces a deflection of said brush head between 3 and 8 millimeters, said deflection being produced by flexural movement in said neck portion.
Brush head 14 is comprised of a flat support surface 20 that secures bristles arranged in a plurality of tufts 21 . The number of tufts may range between about 35 and 40. The tufts are preferably symmetrically located with respect to a vertical plane of symmetry 22 that longitudinally bisects the toothbrush. The separation between contiguous tufts is preferably between about 0.5 and 2 millimeters.
Each tuft is comprised of a multiplicity of primary bristles 23 of equal length and uniform cross-sectional configuration, as having been produced by an extrusion operation. Said primary 15 bristles have proximal ends 24 which are embedded in said brush head, and distal ends 25 extending orthogonally outward from support surface 20 and terminating in a plane 30 parallel to support surface 20 . The length of said primary bristles extending above surface 20 may range from about 8 to 12 millimeters, and their distal ends are preferably rounded.
Also included within each tuft 21 is a multiplicity of secondary bristles 26 having proximal extremities 27 embedded in said brush head, and pointed distal extremities 28 extending orthogonally outward from said support surface to an action zone 29 located beyond the distal ends of said primary bristles. Said action zone extends between 2 and 4 millimeters above plane 30 . Within said action zone, said secondary bristles have a tapered cross-sectional configuration that terminates in said pointed distal extremity.
Within each tuft there may be, for example, about 21 primary bristles and 17 secondary bristles. The general ratio of primary to secondary bristles is preferably in the range of 1.1 to 1.4. If too many secondary bristles are employed, their penetrative ability will be diminished, and they will function more like the primary bristles. It has been found that, in order to achieve acceptable stiffness of the bristles without causing gum irritation, all bristles should be fabricated of polybutylene terephthalate. It has also been found preferable that the secondary bristles be of thinner cross-sectional contour than the cross-sectional contour of the primary bristles.
In the operation of the toothbrush of this invention, the secondary bristles in the action zone enter crevices between the teeth and thereby function in the manner of a flossing treatment. With somewhat greater pressure applied by the user, the distal ends of the primary bristles contact the outer surfaces of the teeth to provide a polishing action.
While particular examples of the present invention have been shown and described, it is apparent that changes and modifications may be made therein without departing from the invention in its broadest aspects. The aim of the appended claims, therefore, is to cover all such changes and modifications as fall within the true spirit and scope of the invention.
|
A toothbrush having an elongated resilient handle has a brush head containing a plurality of tufts of bristles fabricated of polybutylene terephthalate. Each tuft has a multiplicity of short primary bristles and longer secondary bristles having tapered and pointed distal extremities. The effect of the secondary bristles is to function in a manner similar to dental floss to clean the spaces between the teeth.
| 8
|
FIELD OF THE INVENTION
The invention relates to purification of organic compounds using surrogate stationary phases on reversed phase columns. Specifically, the invention provides a preparative HPLC method for purification of organic compounds employing reagents selected from hydrophobic quaternary ammonium salt or quaternary phosphonium salt as a surrogate stationary phase.
BACKGROUND OF THE INVENTION
Reversed phase high performance liquid chromatography (RP-HPLC) is used ubiquitously in academic institutions, forensic laboratories, fine chemicals, and pharmaceutical industries etc. for the analysis, characterization, separation, purification and/or isolation of small organic molecules, natural products, and biologically active molecules such as polypeptides, proteins, and nucleotides. In the pharmaceutical industry, analytical RP-HPLC is used for the release and characterization of raw materials, intermediates, and active pharmaceutical ingredients (APIs). Preparative reversed phase high performance liquid chromatography (Prep-RP-HPLC) is used for the commercial production of Peptide APIs, and most other complex APIs that are not amenable to crystallization.
Preparative RP-HPLC in the elution mode is limited by the loading capacity of the analyte. In the elution preparative RP-HPLC mode, the typical loading capacity of synthetic peptides is in the range of 1 to 2 mgs per ml of packed column volume (viz., 0.1% to 0.2% with respect to total column volume).
The patent application US20120322976 discloses a preparative HPLC of a GLP-1 analog. The loading was 0.225% with respect to total column volume {(about 45 mgs on to a 20 ml C-18 substituted (Octadecyldimethylsilyl) silica resin (particle size: 15 microns)}.
The patent application US20110313131 discloses a preparative HPLC of (Aib 8, 35) GLP-1(7-36)-NH2 at loadings up to 20 g/L (2% with respect to total column volume).
Recent advances in RP-HPLC have focussed on producing spherical silica and development of new bonding chemistries to furnish stationary supports that have improved stability and selectivity. The earlier supports were irregular silica particles that were derivatized with C-18 or C-8 chains, and they suffered from high back pressure. The high back pressure limited their use with respect to quantity that could be purified in a single run, and to relatively smaller diameter columns.
The commercial manufacture of spherical silica that has been derivatized by C-18, C-8, and other ligands has overcome these challenges and has extended the utility of preparative HPLC vastly. These technological advances in the bonded silica supports and process HPLC instrumentation have made possible commercial production of complex peptides such as Fuzeon®, a 36-amino acid peptide, in ton quantities. Unfortunately, these large scale HPLC instruments and the associated column hardware are very costly and restrict the affordability of the methods.
Further, RP-HPLC in the displacement mode has better loading capacity than RP-HPLC in the elution mode but it is arduous to develop. The displacement chromatography is best suited for ion exchange mode, and has found numerous recent applications.
Displacement chromatography utilizes as mobile phase a displacer solution which has higher affinity for the stationary phase material than do the sample components. The key operational feature which distinguishes displacement chromatography from elution chromatography is the use of a displacer molecule.
The U.S. Pat. No. 6,239,262 discloses low molecular weight displacers for protein purification in hydrophobic interaction and reverse phase chromatographic systems.
In displacement chromatography separations, the sample components are introduced in the form of homogeneous sample solution, so that individual components are each delivered at a constant concentration throughout the sample application step. The driving force for separation is that weak binders are displaced from the limited number of binding sites on the stationary phase material by more strongly binding components of the product mixture. This proceeds in a continuous manner until the product and other stronger binders are fully retarded in the earlier part of the chromatography bed, thus permitting the more weakly binding impurities to stay bound to the stationary phase material further along the chromatography bed. Once all sample molecules are bound to the stationary phase, no further movement of these molecules will be observed. A problem which may occur because of such use of homogeneous sample solutions, however, is that molecules of strongly binding components introduced during an early part of sample application may inadvertently be displaced by weaker binders introduced during a later stage of sample application.
Therefore there is a need for a simple, cost effective and scalable Prep-RP-HPLC process for peptides.
OBJECTS OF THE INVENTION
The primary object of the invention is to provide a novel method of purification of organic compounds including peptides using Preparative Reversed Phase High Performance Liquid Chromatography (Prep-RP-HPLC) technique.
Another object of the invention is to provide a method for purification of organic compounds including peptides which has 7 to 10 times greater sample loading capacity, and output compared to the traditional Prep-RP-HPLC technique.
A further object of the invention is to provide such method using surfactants as surrogate stationary phases (SSPs)/additional stationary phases (ASPs).
SUMMARY OF THE INVENTION
In one aspect, the invention provides a method for purifying a multicomponent sample by reverse phase chromatography comprising:
(a) configuring a chromatographic system having a hydrophobic stationary phase; (b) saturating the chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt; (c) optionally washing the column after the step (b) with a buffer; and (d) applying a multicomponent sample to one end of the chromatographic bed comprising of stationary phase saturated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt; and (e) eluting the multicomponent sample in a buffer; (f) recovering the desired component of the sample.
In another aspect the invention provides a method for purifying a multicomponent sample by reverse phase chromatography comprising:
(a) configuring a chromatographic system having a hydrophobic stationary phase; (b) saturating the chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt; (c) optionally washing the column after the step (b) with a buffer; (d) applying a multicomponent sample to one end of the chromatographic bed comprising of stationary phase saturated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt; and (e) eluting the multicomponent sample in a buffer containing quaternary ammonium salt or quaternary phosphonium salt; and (f) recovering the desired component of the sample.
In yet another aspect, the invention provides a method for purifying a multicomponent sample by reverse phase chromatography comprising:
(a) configuring a chromatographic system having a hydrophobic stationary phase; (b) saturating the chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt; (c) optionally washing the column after the step (b) with a buffer; (d) applying a multicomponent sample to one end of the chromatographic bed comprising of stationary phase saturated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt; and (e) eluting the multicomponent sample in a buffer; (f) recovering the desired component of the sample; (g) treating the equilibrated chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt with sodium tetrafluoroborate; and (h) washing the treated chromatographic stationary phase after step (g) with a solvent to recover the chromatographic stationary phase from the quaternary ammonium salt or quaternary phosphonium salt.
Still another aspect of the invention is to provide a preparative HPLC method for purification of organic compounds wherein the method has following advantages (1) increased loading (2) limited use of solvents (3) reduced waste disposal (4) ease of operation, and (5) reduced scale of the equipment utilized to chromatograph, elute, concentrate and recover the desired components.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 : Analytical RP-HPLC profile of Leuprolide acetate obtained using the present invention. A Discovery Bio Wide Pore (10 mm×250 mm, C18, 5 u, and 300{acute over (Å)} pore diameter) column was used for the Prep-RP-HPLC process.
FIG. 2 : Analytical RP-HPLC profile of Leuprolide acetate obtained using the present invention. A Waters Symmetry (19 mm×50 mm, C8, 5 u, 120 {acute over (Å)}pore diameter) column was used for the Prep-RP-HPLC process.
FIG. 3 : Analytical RP-HPLC profile of Leuprolide acetate by obtained using standard (conventional) preparative RP-HPLC technique. A YMC, ODS-AQ (50 mm×250 mM, C18, 10μ, 120° A pore diameter [see comparative example] was used for the Prep-RP-HPLC process.
FIG. 4 : Analytical RP-HPLC profile of Leuprolide acetate (pooled preparative HPLC fractions that were greater than 95% pure) obtained using tetra-n-butylammonium bromide (TBA-Br) and a Grace Vydac C18 column (40 micron particles).
FIG. 5 : Analytical RP-HPLC profile of Leuprolide acetate (pooled preparative HPLC fractions that were greater than 95% pure) obtained using tetra-n-butylammonium hydrogen sulfate (TBA-HS) and a Grace Vydac C18 column (40 micron particles).
FIG. 6 : Analytical RP-HPLC profile of Leuprolide acetate (pooled preparative HPLC fractions that were greater than 95% pure) obtained using cetyltrimethylammonium bromide (CTA-Br) and a Grace Vydac C-18 column (40 micron particles).
FIG. 7 : Analytical RP-HPLC profile of Leuprolide acetate (pooled preparative HPLC fractions that were greater than 95% pure) obtained using tetra-n-butylphosphonium chloride (TBP-Cl) and a Grace Vydac C-18 column (40 micron particles).
FIG. 8 : Analytical RP-HPLC profile of Leuprolide acetate (pooled preparative HPLC fractions that were greater than 95% pure) obtained using tetra-n-butylammonium chloride (TBA-Cl) and a Grace Vydac C-18 column (40 micron particles).
DETAILED DESCRIPTION OF THE INVENTION
First embodiment of the present invention provides a preparative HPLC method for purification of organic compounds employing quaternary ammonium salt as a surrogate stationary phase, wherein the chromatographic stationary phase is hydrophobic.
The quaternary ammonium salt of the present invention has the structure as mentioned below:
wherein R, R 1 , R 2 , R 3 is selected independently from the group comprising straight or branched alkyl, cyclic hydrocarbons, aromatic group, alkyl substituted aromatic group, aryl substituted alkyl groups; the anion denoted as B herein in the compound represented by the formula (1) includes bis(trifluoromethylsulfonyl)imide, bis(fluorosulfonyl)imide, dicyanamide, halogens, tetrafluoroborate, hexafluorophosphate, trifluoromethanesulfonate, methanesulfonate, trifluoroacetate, thiocyanate, dimethylphosphate, diethylphosphorodithioate, amino acids, etc. Preferably quaternary ammonium salts are tetra-n-butylammonium bromide, tetra-n-butylammonium hydrogen sulfate, tetra-n-butyl-ammonium hydroxide, tetra-n-octylammonium bromide, methyltrioctylammonium chloride, myristyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride. Most preferably tetra-n-octylammonium bromide
Second embodiment of the present invention provides a preparative HPLC method for purification process of organic compounds employing quaternary phosphonium salt as a surrogate stationary phase in hydrophobic stationary phases, preferably C-18, C-4 and C-8 hydrophobic stationary phase.
The quaternary phosphonium salt of the present invention has the structure as mentioned below,
wherein R, R 1 , R 2 , R 3 is selected independently from the group comprising straight or branched alkyl, cyclic hydrocarbons, aromatic group, alkyl substituted aromatic group, aryl substituted alkyl groups; the anion denoted as B herein in the compound represented by the formula (II) includes bis(trifluoromethylsulfonyl)imide, bis(fluorosulfonyl)imide, dicyanamide, halogens, tetrafluoroborate, hexafluorophosphate, trifluoromethanesulfonate, methanesulfonate, trifluoroacetate, thiocyanate, dimethylphosphate, diethylphosphorodithioate, ethyltriphenylphosphonium bromide, ethyltriphenylphosphoniumiodide, butyltriphenylphosphonium bromide, methyltriphenylphosphonium bromide, triphenylphosphonium bromide, butyltriphenylphosphonium chloride.
According to the process of the invention, the concentration of the organic modifier is held at a sufficiently low concentration to ensure/enforce strong binding of the analytes to the stationary phase (s).
The surrogate stationary phase in the present invention refers to a modified hydrophobic stationary phase that is formed after equilibrating the chromatographic hydrophobic stationary phase with quaternary ammonium salt or quaternary phosphonium salt.
The method of the present invention is distinguished from the prior art displacement chromatography in the following way: the method of the present invention for purifying a peptide by reverse phase chromatography involves the step of applying to the hydrophobic stationary phase a mixture comprising organic compounds to be separated after the addition of the additional (surrogate) stationary phase with or without the organic modifier, whereas the reverse phase displacement chromatography as disclosed in the U.S. Pat. No. 6,239,262, PCT publications WO2013052539 and WO2013052087, for separating organic compounds from a mixture involves the step of applying to the hydrophobic stationary phase a mixture comprising organic compounds to be separated before the addition of the displacer with or without the organic modifier.
In various embodiments, the gradient elution can be accomplished, for example, stepwise, linearly, with multi segmented linear or stepwise changes in composition, or with a combination thereof. In one aspect, gradient elution is performed with increasing amounts of an organic modifier and elution is completed in greater than about 10%, greater than about 20%, greater than about 30%, greater than about 90%, or up to and including about 100% of the organic modifier. In certain aspects, elution is completed with decreasing amount of organic modifier, e.g., less than about 20%, less than about 15%, less than about 10%, less than about 5%, less than about 2%, less than about 1% or about 0% of organic modifier.
The organic modifier in the present invention refers to a solvent or a compound which can be used in chromatographic procedures and like separation methods, to alter the properties of the mobile phase to controllably effect serial elution of desired materials. In one aspect, an organic modifier decreases ionic interactions between molecules in the mobile phase and the stationary phase. For example, in one aspect, an organic modifier comprises a solvent added to a mobile phase to decrease its polarity. Suitable organic modifiers include, but are not limited to, acetonitrile, ethanol, methanol, ethanol, n-propanol or isopropanol. The separating can be accomplished with any suitable solvent or solvent combination.
The nature of the library comprising the multicomponent mixture useful to be separated in the present invention system essentially is unlimited. Thus, mixtures of organic compounds may be used. Digests of biopolymers, either natural or synthetic, are particularly attractive. Such digests may comprise mixtures of peptides, polysaccharides, polynucleotides, various derivatized forms thereof, and variously sized fragments thereof. The biopolymers may be extracted from plant or animal tissues, diseased or healthy, digested if necessary, or used as is. Such libraries are available in abundance, easy to prepare, may be of lower toxicity and more stable than synthetic peptides, and may be varied and screened systematically.
In an embodiment, the concentration of the quaternary ammonium salt or hydrophobic quaternary phosphonium salt in the organic modifier is increased to effect elution of the analytes. The organic modifier may be used with or without the quaternary ammonium salt or the hydrophobic quaternary phosphonium salt.
Third embodiment of the present invention is to provide a process for the removal of the reagents such as hydrophobic quaternary ammonium salt or quaternary phosphonium from the C-18 or C-8 column by employing sodium tetrafluoroborate or potassium hexafluorophosphate with organic modifier.
The fourth embodiment of the present invention is to provide a method for purifying a multicomponent sample by reverse phase chromatography comprising:
(a) configuring a chromatographic system having a hydrophobic stationary phase; (b) saturating the chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt; (c) optionally washing the column after the step (b) with a buffer to remove any unbound quaternary salt; (d) applying a multicomponent sample to one end of the chromatographic bed comprising of stationary phase saturated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt; and (e) eluting the multicomponent sample in a buffer; and (f) recovering the desired component of the sample.
In another aspect, the invention provides a method for purifying a multicomponent sample by reverse phase chromatography comprising:
(a) configuring a chromatographic system having a hydrophobic stationary phase; (b) saturating the chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt; (c) optionally washing the column after the step (b) with a buffer to remove any unbound quaternary salt; (d) applying a multicomponent sample to one end of the chromatographic bed comprising of stationary phase saturated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt; and (e) eluting the multicomponent sample in a buffer containing quaternary ammonium salt or quaternary phosphonium salt; and (f) recovering the desired component of the sample.
In yet another aspect, the invention provides a method for purifying a multicomponent sample by reverse phase chromatography comprising:
(a) configuring a chromatographic system having a hydrophobic stationary phase; (b) saturating the chromatographic stationary phase with quaternary ammonium salt or quaternary phosphonium salt; (c) optionally washing the column after the step (b) with a buffer to remove any unbound quaternary salt; (d) applying a multicomponent sample to one end of the chromatographic bed comprising of stationary phase saturated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt; and (e) eluting the multicomponent sample in a buffer; (f) recovering the desired component of the sample; (g) treating the chromatography stationary phase saturated/coated with quaternary ammonium salt or quaternary phosphonium salt with sodium tetrafluoroborate; and (h) washing the treated chromatographic stationary phase after step g with a solvent to recover the chromatographic stationary phase from the quaternary ammonium salt or quaternary phosphonium salt.
Conventional RPLC hardware systems may be used for the separation, and the term “configuring a chromatographic system” refers to setting up a column or system of column, pump and detector as is well known in the art.
The term “saturating the chromatographic stationary phase” refers to passing the quaternary ammonium salt or quaternary phosphonium salt in a solution over the stationary phase in a particular concentration, thereby preparing the surrogate stationary phase.
In a preferred embodiment of the invention, wherein preparative HPLC method for purification of organic compounds maintains a low concentration of the organic modifier to retain the surrogate stationary phase on the column. The said conditions are required for the interaction of surrogate stationary phase with solute along with interaction with C-18, C-4 and C-8 ligands.
Some aspects and embodiments of this disclosure are described in the examples below, which are provided only for the purpose of illustration and are not intended to limit the scope of the disclosure in any manner.
Illustrative Example of the Present Invention
The C-18/C-8 reversed phase column is equilibrated with 5 to 10 column volumes (V c s) of 5 to 10% aqueous acetonitrile containing 10 mM tetra-n-butylammonium hydrogen sulphate (TBAHS, Buffer A). The pH of the starting buffer was not adjusted, and was about 1.95 (It is important to keep the concentration of acetonitrile lower than the concentration needed to elute the product on an analytical HPLC column). The crude compound to be purified was dissolved in starting buffer A or aqueous TFA or aqueous HOAc and loaded on to the column. After the loading is complete, the column is equilibrated with 2 Column V c s of Buffer A. Next, the gradient elution process is started. The buffer B is usually 300 mM to 500 mM TBAHS in 5 to 10% aqueous acetonitrile. A linear gradient of 0% B to 100% Buffer B over 10 V c s is applied. When the product of interest (API) is about to elute, a gradient hold may be applied until all the API has eluted from the column. Alternately if it is desired to elute the product in a concentrated form the gradient may be allowed to run its course. The fractions containing the pure API product are combined after confirming that the pooled fraction meets the purification criteria. The approximate quantity of the associated TBAHS is calculated. This is then treated with 1.5 to 2 equivalents of sodium tetrafluoroborate (NaBF 4 ) and extracted 3 times with chloroform to remove the TBA cation as its tetrafluoroborate salt. The aqueous residue is then loaded on to a C-18/C-8 column from which all the TBAHS (quaternary ammonium/phosphonium salt) has been removed. Removal of TBAHS from the C-18/C-8 column is accomplished by the following steps: The column is first washed with at least 3 V c s of 80% Acetonitrile-20% Water. Next, the column is washed with 3V c s of 100 mM NaBF 4 in 80% Acetonitrile-20% water. The column is equilibrated with 1M Acetic Acid in 1% Aqueous Acetonitrile (10 V c s). The aqueous phase containing “pure API” and excess NaBF 4 is diluted with water (5× its volume) and loaded on to the C-18/C-8 column on to the column. The column is washed with 5 to 10 V c s of 1% phosphoric acid-1% Acetonitrile-98% Water to exchange the BF 4 anions for phosphate anions. The column is then washed with 5 to 10 V c s of 100 mM aqueous Guanidine. HCl to remove the phosphate anions and to exchange the phosphate anions to chloride anions. Finally the chloride anions are exchanged for acetate anions. The fractions containing the “pure product acetate salt” are combined, and the organic volatiles are removed under reduced pressure. The aqueous residue is lyophilized or precipitated after removal of water. The final API is analysed according to the USP/EP Methods of Analysis.
TABLE 1
Purification of Leuprolide: Comparison of the Surrogate Stationary
Phase aided Prep-RP-HPLC with the Standard Prep-RP-HPLC
Total
%
Column
Column
Input:
Output:
Purity by
Relative
Entry
Prep RP-
dimensions;
volume
Crude
Pure
%
HPLC (USP
Loading
#
HPLC method
(ID × L)
(mL)
API (g)
API (g)
Yield
method)
Capacity
1.
Standard RP-
YMC, ODS-AQ
490.0
4.0 g
1.2 g
30.0%
99.86
1
HPLC
(50 mm × 250 mm,
[Comparative
C18, 10 u, 120 Å
example]
pore diameter)
2.
SSP-
Waters Symmetry
14.2
1.4 g
0.42 g
30.0%
99.79
12.1
Purification
(19 mm × 50 mm,
method
C8, 5 u, 120 Å
[TBAHS-SSP]
pore diameter)
3.
SSP-
Discovery Bio
19.6
1.2 g
0.32 g
26.7%
99.73
6.7
Purification
Wide Pore
method
(10 mm × 250 mm,
[TBAHS-SSP]
C18, 5 u, 300 Å
pore diameter)
The purified product (Leuprolide) output of the standard Prep-RP-HPLC is 2.45 mg/mL of column volume: In contrast the purified product output of the surrogate stationary phase aided Prep-RP-HPLC is 29.6 mg/mL of column volume (table 1, entry 2) and 16.3 mg/mL of column volume (table 1, entry 3). These results suggest that loadings of 7 to 12 times capacity of conventional prep-RP-HPLC are achievable with the processes described in the present invention.
EXAMPLES
Example-1: Preparative RP-HPLC of Leuprolide Acetate
Two different columns were evaluated for the purification of Leuprolide: A Discovery Bio Wide Pore column {column parameters: 10 mm (ID)×250 mm (L), C18, 5 u particles, 300{acute over (Å)} pore diameter, Amount loaded was 1.2 g of crude Leuprolide (prepared by solution phase synthesis) and a Waters Symmetry Column {column parameters: 19 mm (Internal Diameter, ID)×50 mm (Length, L), C8, 5 u particles, 120 {acute over (Å)}pore diameter, Amount loaded was 1.4 g of crude Leuprolide (prepared by solution phase synthesis) were used. The column was pre-equilibrated with 5 to 10 column volumes (V c s) of 10 mM TBAHS in 10% aqueous acetonitrile (Buffer A). After the loading was complete, the column was washed with 2 V c s of Buffer A. Next, the gradient elution process was started. The buffer B was 300 mM TBAHS in 10% aqueous acetonitrile. A linear gradient of 0% B to 100% Buffer B over 60 min. was used for elution. A gradient hold was applied until all the API has eluted from the column. The fractions containing the pure API product were combined and treated with 1.5 to 2 equivalents of sodium tetrafluoroborate (NaBF 4 ) and extracted 3 times with chloroform. The entire purification process was repeated 3 times to demonstrate and confirm the consistent performance. Fractions containing “pure Leuprolide” were combined and loaded on to a C-18 column from which all the TBAHS had been removed as described before.
The conversion of phosphate/hydrogen sulphate anions to acetate anions was done as described earlier. Fractions containing pure Leuprolide Acetate API were lyophilized. The purification yield was about 30%. (TBA-HS herein denotes tetra-n-butyl-ammonium hydrogen sulphate)
Example-2: Preparative RP-HPLC of Triptorelin Acetate
The C-18/C-8 reversed phase column was pre-equilibrated with 5 to 10 V c s of 5 to 10% aqueous acetonitrile containing 10 mM TBAHS (Buffer A). A Discovery Bio Wide Pore column {column parameters: 10 mm (ID)×250 mm (L), C18, 5 u particles, 300{acute over (Å)} pore diameter, Amount loaded was 1.0 g of crude Triptorelin} was used. After the loading was complete, the column was washed with 2 V c s of Buffer A. Next, the gradient elution process was started. The buffer B was 300 mM TBAHS in 10% aqueous acetonitrile. A linear gradient of 0% B to 100% Buffer B over 60 min. was used for elution. A gradient hold was applied until all the API has eluted from the column. The fractions containing the pure API product were combined and treated with 1.5 to 2 equivalents of sodium tetrafluoroborate (NaBF 4 ) and extracted 3 times with chloroform. The entire purification process was repeated 3 times to demonstrate and confirm the consistent performance. Fractions containing “pure Triptorelin” were combined and loaded on to a C-18 column from which all the TBA-HS had been removed as described before.
The conversion of phosphate/hydrogen sulphate anions to acetate anions was done as described earlier. Fractions containing pure Triptorelin API were lyophilized. The purification yield was about 25%. (TBAHS herein denotes tetra-n-butyl-ammonium hydrogen sulphate)
Example-3: Preparative RP-HPLC of Leuprolide Acetate Employing Tetra-n-Butylammonium Bromide (TBA-Br)
The C-18 reverse phased column [Grace Vydac Column parameters 12 g of C-18, 40 microns particles, 60 Å pore diameter] was saturated with 36 g of TBA-Br in 360 mL of water at the flow rate of 8.0 ml/min. The column was then equilibrated 10 V c s with Buffer A (25 mM TBA-Br in water) at a flow rate of 8.0 ml/min. The crude leuprolide trifluoroacetate salt was dissolved in Buffer A and loaded on to the column. After the loading is complete, the gradient elution process was started. The Buffer B is 25 mM of TBA-Br in 50% aqueous acetonitrile. A linear gradient of 0% of Buffer B to 100% of Buffer B over 10 V c s was applied. When Leuprolide is about to elute, a gradient hold may be applied until all the API has eluted from the column. The fraction containing the pure Leuprolide is combined after confirming the purity on an analytical HPLC. Yield: 66.4%. Herein TBA-Br is tetra-n-butylammonium bromide.
Removal of TBA-Br from the C-18 column: The column was first washed with at least 5 V c s of 0.1 M sodium tetrafluoroborate in acetonitrile and water (8:2) followed by aqueous acetonitrile.
Example-4: Preparative RP-HPLC of Leuprolide Acetate Employing Tetra-n-Butylammonium Hydrogen Sulfate (TBA-HS)
The C-18 reverse phased column [Grace Vydac Column parameters 12 g of C-18, 40 microns particles, 60 Å pore diameter] was saturated with a solution of 36 g of TBA-HS in 360 mL of water at a flow rate of 8.0 ml/min. The column was then equilibrated with Buffer A (25 mM TBA-HS in water) about 10 V c s at a flow rate of 8.0 ml/min. The crude leuprolide trifluoroacetate salt was dissolved in Buffer A and loaded on to the column. After the loading is complete, the gradient elution process was started. The Buffer B is 25 mM of TBA-HS in 50% aqueous acetonitrile. A linear gradient of 0% of Buffer B to 100% of Buffer B over 10 V c s was applied. When Leuprolide is about to elute, a gradient hold may be applied until all the API has eluted from the column. The fractions containing the pure Leuprolide are combined after confirming the purity on an analytical HPLC. Yield: 64.4%. Herein TBAHS is tetra-n-butylammonium hydrogen sulfate.
Removal of TBA-HS from the C-18 column: The column was first washed with at least 5 column volumes of 0.1M sodium tetrafluoroborate in acetonitrile and water (8:2) followed by aqueous acetonitrile.
Example-5: Preparative RP-HPLC of Leuprolide Acetate Employing Cetyltrimethylammonium Bromide (CTA-Br)
The C-18 reverse phased column [Grace Vydac Column parameters 12 g of C-18, 40 microns particles, 60 Å pore diameter] was saturated with solution of 1 mM CTA-Br in water at a flow rate of 8.0 ml/min. The column was then equilibrated with Buffer A (5 mM CTA-Br in water) about 10 V c s at a flow rate of 8.0 ml/min. The crude leuprolide trifluoroacetate salt was dissolved in Buffer A and loaded on to the column. After the loading is complete, the gradient elution process was started. The Buffer B is 5 mM of CTA-Br in 50% aqueous acetonitrile. A linear gradient of 0% of Buffer B to 100% of Buffer B over 10 V c s was applied. When Leuprolide is about to elute, a gradient hold may be applied until all the API has eluted from the column. The fractions containing the pure Leuprolide are combined after confirming the purity on an analytical HPLC. Yield: 61.4%. Herein CTA-Br is cetyltrimethylammonium bromide.
Removal of CTA-Br from the C-18 column: The column was first washed with at least 5 V c s of 0.1M sodium tetrafluoroborate in acetonitrile and water (8:2) followed by aqueous acetonitrile.
Example-6: Preparative RP-HPLC of Leuprolide Acetate Employing Tetra-n-Butylphosphonium Chloride (TBP-Cl)
The C-18 reverse phased column [Grace Vydac Column parameters 12 g of C-18, 40 microns particles, 60 Å pore diameter] was saturated with solution of 36 g of TBP-Cl in 360 ml of water at a flow rate of 8.0 ml/min. The column was then equilibrated with Buffer A (25 mM TBP-Cl in water) about 10 V c s at a flow rate of 8.0 ml/min. The crude leuprolide trifluoroacetate salt was dissolved in Buffer A and loaded on to the column. After the loading is complete, the gradient elution process was started. The Buffer B is 25 mM of TBP-Cl in 50% aqueous acetonitrile. A linear gradient of 0% of Buffer B to 100% of Buffer B over 10 Column volumes was applied. When Leuprolide is about to elute, a gradient hold may be applied until all the API has eluted from the column. The fractions containing the pure Leuprolide are combined after confirming the purity on an analytical HPLC. Yield: 60.3%. Herein TBP-Cl is tetra-n-butylphosphonium chloride.
Removal of TBP-Cl from the C-18 column: The column was first washed with at least 5 V c s of 0.1M sodium tetrafluoroborate in acetonitrile and water (8:2) followed by aqueous acetonitrile.
Example-7: Preparative RP-HPLC of Leuprolide Acetate Employing Tetra-n-Butylammonium Chloride (TBA-Cl)
The C-18 reverse phased column [Grace Vydac Column parameters 12 g of C-18, 40 microns particles, 60 Å pore diameter] was saturated with 36 gm of TBA-Cl in 360 ml of water at a flow rate of 8.0 ml/min. The column was then equilibrated with Buffer A (25 mM TBA-Cl in water) about 10 V c s at a flow rate of 8.0 ml/min. The crude leuprolide trifluoroacetate salt was dissolved in Buffer A and loaded on to the column. After the loading is complete, the gradient elution process was started. The Buffer B is 25 mM of TBA-Cl in 50% aqueous acetonitrile. A linear gradient of 0% of Buffer B to 100% of Buffer B over 10 V c s was applied. When Leuprolide is about to elute, a gradient hold may be applied until all the API has eluted from the column. The fractions containing the pure Leuprolide are combined after confirming the purity on an analytical HPLC. Yield: 53.5%. Herein TBA-Cl is tetra-n-butylammonium chloride.
Removal of TBA-Cl from the C-18 column: The column was first washed with at least 5 V c s of 0.1M sodium tetrafluoroborate in acetonitrile and water (8:2) followed by aqueous acetonitrile.
|
There are only two ways to increase the amount of sample that can be purified by preparative reversed phase high performance liquid chromatography (Prep-RP-HPLC) in a single run: (1) The traditional approach is to use a bigger column (greater amount of stationary phase); and (2) Use displacement chromatography which uses the stationary phase more effectively. This invention describes a unique Prep-RP-HPLC technique that uses a C-18/C-8 derivatized silica coated with a hydrophobic quaternary ammonium salt or quaternary phosphonium salt to result in 7 to 12 fold increase in sample loading (of the crude mixture of organic compounds including synthetic crude peptides) in contrast to the conventional Prep-RP-HPLC technique. This increase in sample loading capacity and output is due to the additional surrogate stationary phase characteristic of the C-18/C8 bound quaternary salt. The quaternary surfactant is bound to the C-18/C-8 chains and silanols of the stationary phase.
| 1
|
The invention relates to game playing devices and more particularly to a game playing apparatus that includes a number of display sectors that are labeled with any one of a number of characteristics, of which any one can be randomly selected to display a selected characteristic.
BACKGROUND OF THE INVENTION AND PRIOR ART
With the advent of electronic technology, a number of game devices have become known, which operate to amuse users thereof and to test various skills such as related to speed of reflexes and/or the memory of players or other skills.
Typical of such game devices is U.S. Pat. No. 4,169,592, which discloses an electronic reflex game, and U.S. Pat. No. 4,358,118, which discloses an electronic game that senses physiological responses of players.
The instant invention is a game apparatus that seeks to entertain a group of players by randomly or directedly selecting and displaying any one of a number of personal characteristics that can be labeled and arranged advantageously on a graded scale. Typical of such gradeable characteristics are personal looks, intelligence, knowledge, wit and so forth.
SUMMARY OF THE INVENTION
The invention is accordingly a game device typically in the form of a small hand-held unit, approximately the size of a pocket calculator. It is intended for entertainment and amusement in a social setting.
The device typically has a front face plate that includes: a display with a plurality of display sectors, each having a label in the form of a statement, legend, color or symbol representing a characteristic or sentiment that can be arranged, for example, on a random or graded scale from a high to a low value; a start button and a mode switch with at least four positions, namely OFF, LOW, MIDDLE, HIGH, and electronic circuitry connecting together the display sectors, the start button and the slide switch.
In operation, with the mode switch set to middle position, the start button is depressed for a moment; the electronic circuit starts a timer which enables a clock generator to run while the timer runs; the clock generator drives a recirculating counter having at most as many counts as the number of display sectors. When the timer runs out, the clock generator stops running and the counter stays on the last count reached, when the clock generator stopped. The counter will stop randomly in any sector, since the running time includes the time the start button is depressed plus the time lapse set by the counter.
In accordance with the inventive concept, there is provided a game apparatus which includes a plurality of display sectors each having a label expressing a gradeable characteristic, illuminating elements for illuminating one of the display sectors, and display sector selecting elements connected to the illuminating element for randomly selecting one of the display sectors to be illuminated.
According to a further feature, there is provided a game apparatus wherein the illuminating means include at least one of a liquid crystal display, a light-emitting diode display and an incandescent bulb display.
In accordance with still a further feature, there is provided a game apparatus wherein the display sectors are disposed along a rectangular perimeter, or alternatively wherein the display sectors are disposed along a circular, triangular, curved or arcuate perimeter.
The game apparatus according to the invention may be arranged such that the display sectors are divided into a high group of sectors, a low group of sectors and a middle group of sectors according to a grade assigned to the respective display sector.
The game apparatus according to the invention may further include a start button connected to the selecting elements, and a mode selecting switch connected to the selecting elements, wherein the mode selecting switch may have a high mode position, a low mode position and a middle mode position for respectively selecting a display sector in the high group, the low group or in the middle group for display upon release of the start button.
There may further be provided a game apparatus wherein the selecting elements include pulse generating elements connected to the start button, a counter which has an input connected to the pulse generating elements, and inputs to the display sectors connected to the counter for displaying a sector corresponding to a count stored in the counter upon release of said start button, and wherein the pulse generating elements include a fast pulse generator having an input connected to the start button, a slow pulse generator having an input, a timer having an input connected to the start button and an output connected to the input of the slow pulse generator, and a mode selecting circuit connected between the pulse generating elements and the display sectors, having inputs connected to the mode selecting switch for randomly selecting a display sector in the middle group upon release of the start button elapse of a time interval determined by the timer.
According to again a further feature, there may be provided a game apparatus which includes a transparent overlay for overlaying the game apparatus, and which overlay has imprinted thereon labels for the display sectors.
Other features which are considered as characteristic for the invention are set forth in the appended claims.
Although the invention is illustrated and described herein as embodied in a game apparatus for randomly displaying gradeable characteristics, it is nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the invention and within the scope and range of equivalents of the claims.
The construction and method of operation of the invention, however, together with additional objects and advantages thereof will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a front view of the face of the game device, showing the display sectors, a start button and a mode selecting switch;
FIG. 2 is a side view of the game device;
FIG. 3 is an exemplary view of the display sectors with labels arranged in a graded order;
FIG. 4 is another front view of the game device, showing the display sectors arranged along a circle sector; and
FIG. 5 is a schematic circuit diagram of the electronic circuit of the game device.
FIG. 6 is another view of the game device, showing the display sectors arranged along a triangular perimeter.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The device is shown in one of its preferred embodiments in FIGS. 1 and 2, wherein FIG. 1 is a front view showing the device 1 having a display 2 with a number of display sectors 3 labeled a-j; a start button 4 and a four position mode selection switch 5. FIG. 2 is a side view of the device.
FIG. 3 shows as an example the display sectors each given a legend on a graded scale from "AWFUL" at the low end of the scale to "TERRIFIC" at the high end.
It follows that the number of display sectors can be arbitrarily chosen, as well as the size and shape of the display, and the actual wording of the legends on the sectors.
For example, in addition to locating the display sectors along a rectangular perimeter, as is illustrated in FIGS. 1 and 3, the display sectors can be disposed along a curved perimeter (e.g., FIG. 4) or a triangular perimeter (e.g., FIG. 6).
It is contemplated that an optional replaceable transparent overlay with printed legends and symbols and the like can be provided and placed over the display sectors.
With the mode selector switch 5, having a high, middle and low position, in its LOW position, the final display will always stop on the lowest graded sector in the example according to FIG. 3 shown as "AWFUL", and with the mode selector switch 5 in HIGH position, it will always stop on the highest graded sector shown as "TERRIFIC". With the mode selector switch 5 in MIDDLE position, it will stop randomly on any of the sectors between b and i, and not on display sectors a or j.
The display sectors 3 can be realized as liquid crystal (LCD) displays, light-emitting diode (LED) displays or incandescent bulb displays. With the latter two displays, an LED or bulb may be placed within or near the respective sector, as shown in FIG. 4 wherein an LED or bulb 7 is associated with each sectors a-j. Use of LED's (FIG. 4) allows a choice in the shape of the display, but requires more battery current. An LCD display offers very low current drain, but will advantageously be rectangular in shape, and is somewhat more expensive.
FIG. 5 is an example of a schematic circuit diagram of the electronic circuit for the invention. First, the mode switch 5 is set to one of the modes (LOW), Middle (MID) or High (HI), and simultaneously via switch S battery power is connected to the power pins of the circuit elements and selects the proper mode. Alternatively, switch S is coupled to start button 4 for connecting battery power on, and coupled to mode selector switch 5 for turning power off. Assuming the middle mode MI is selected, and the start button 4 is depressed, a fast pulse generator 8 is started by a logic 1 in the form of plus battery on input EN of the fast pulse generator 8, which starts to run at high speed, e.g. 1 Mega Herz and keeps running while the start button 4 is depressed. During this period a counter 10 is kept running driven by output 9 of pulse generator 8 via OR-gate 11 to a certain count depending upon how long the start button 4 is held. After release of the start button 4, a timer 12, e.g. in the form of an 555-type timer having timing elements C and R, is started as its trigger input T goes from high to low. The timer 12 may be set for e.g. 1 second and enables a slow pulse generator 13 that runs at e.g. 15 Herz, which drives the counter 10 at a low speed which is visible on the display 14 with display sectors 3 labeled a-j. After the elapse of the time determined by the timer 12, the display will illuminate one of the sectors 3 which will be randomly selected as determined by the length of time the start button was operated.
If, however, the mode selection switch 5 is set to LOW (or HI), the display will be seen running while the timer and the slow pulse generator run, but at the end of timing all display sectors will be extinguished except only sector a (or j) will be illuminated, as determined by a number of logic elements which typically include AND-gates, OR-gates, NAND-gates, inverters and amplifiers, as described in more detail in the following paragraph.
All outputs b-i of counter 10 are connected via an upper input of AND-gates 15 to respective display sectors b-i. Assuming that the mode selector switch is in its middle position MID, the lower input of AND-gate 16 is enabled, while its upper input is also enabled by the output of the timer 12, while the timer is active. While AND-gate 16 is active, its output enables the lower input of those AND-gates 15 that control display sectors b-i, which will be seen as flashing while the counter 10 is running, driven by the slow pulse generator 13. When the timer returns to normal, one of the display sectors b-i will remain on, depending on where the counter stops. If, however, the selector switch 5 is in either LOW or HI position, the respective high sector a or low sector j will come on when the upper input of AND-gates 15, which control upper and lower sector a or j, is enabled via inverter 17, when the timer 12 resets to normal.
|
A game apparatus comprising a plurality of display sectors each having a label expressing a characteristic, an illuminating device for illuminating a selected one of the display sectors, and a display selector selecting device connected to the illuminating device for randomly selecting one of the display sectors to be illuminated.
| 0
|
This invention was made in part with government support under grant number DEFG02-91-ER61228 awarded by the Department of Energy. The United States government has certain rights in the invention.
This application claims priority from U.S. Provisional application Ser. No. 60/028,198, filed on Oct. 10, 1996, which is incorporated herein by reference in its entirety.
BACKGROUND OF THE INVENTION
The invention relates to photodynamic therapy.
Photodynamic therapy (PDT) was first developed as an experimental treatment for cancer. The treatment was based on the observation that cancer cells could retain photoactivatable compounds and could be selectively killed when these compounds subsequently interacted with absorbed light (see e.g., Bottiroli et al., Photochem. Photobiol. 47:209-214, 1988; Salet et al., Photochem. Photobiol. 53:391-393, 1991; Gross, In Photobiological Techniques, Valenzeno et al. Eds., Plenum Press, New York, 1991; and Jori et al., In Photodynamic Therapy of Neoplastic Disease, Kessel Ed., CRC Press, Boca Raton, Fla., 1989). A photodynamic compound that is widely used is marketed as Photofrin®. Photofrin®/HPD (hematoporphyrin derivative) was the first FDA approved photosensitizing agent available for PDT trials. Photofrin® has subsequently been tested extensively for the destruction of multiple tumors in numerous medical disciplines (Dougherty et al., In Photodynamic Therapy of Neoplastic Disease, Kessel Ed., supra).
The mechanism of action for hematoporphyrin derivatives such as Photofrin® in the treatment of neoplastic disease is well delineated. Large molecular aggregates of the porphyrins accumulate around tumor neovasculature. This accumulation is caused by poor lymphatic drainage from the neoplastic tissues. Once sequestered in the tissue, the molecular aggregates dissociate, and the hydrophobic components of the porphyrin cause it to partition into cell membranes, primarily into the cellular and mitochondrial membranes.
Initiation of photodynamic activity is caused by excitation of the photodynamic compound by light that falls within its absorption band. The wavelength specificity depends on the molecular structure of the photodynamic compound; a greater degree of conjugation within a molecule leads to greater absorbance at longer wavelengths. Activation of photodynamic compounds occurs with subablative light fluences. Toxicity is achieved by O 2 radical toxicity. The singlet O 2 reacts with, for example, double bonds to produce reactive species, for example, organoperoxides. These, in turn, initiate free radical chain reactions which degrade and disorganize membranes, uncouple oxidative phosphorylation, and lead to cellular disruption (Jori et al., supra; Weishaupt et al., Cancer Res 36:2326-2329, 1976). Nucleic acids and proteins are also damaged by photooxidation (Henderson et al., In Porphyrin Localization and Treatment of Tumors, Doiron et al. Eds., Liss, N.Y., 1984).
Studies demonstrating destruction of synovium without significant side effects indicate that photochemical synovectomy is an effective treatment for rheumatoid arthritis (U.S. Pat. No. 5,368,841).
SUMMARY OF THE INVENTION
The invention features a method of treating a patient who has an osteoarthritic joint by administering a photoactivatable compound, or a precursor thereof, and administering light of a wave-length that activates the compound. The method of the invention may be used to treat a human patient or another mammal, such as a dog, cat, rabbit, horse, cow, sheep or non-human primate.
Another embodiment of the invention is the use of a photoactivatable compound, or a precusor thereof, for the manufacture of a medicament for treating a patient who has an osteoarthritic joint. This treatment involves administering the medicament containing the photoactivatable compound, or a precursor thereof, and administering light of a wave-length that activates the compound.
Photoactivatable compounds can be administered to a patient according to established guidelines, so that the concentration of the compound in the target tissue (i.e., in the joint) will be greater than the concentration of the compound in the surrounding tissue. The ratio of the compound in the affected tissue to the compound in the surrounding tissue is preferably 2:1 or greater. Furthermore, the compound may be administered so that an adequate level of the compound will be maintained in the target tissue. In general, this objective, i.e., an adequate level of a differentially localized compound, can be achieved using standard techniques known to skilled pharmacologists in which the clearance time course for the compound is considered.
Compounds may be administered either systemically or locally to the area of the joint. Systemically or locally administered compounds that are useful in the invention include those that are preferentially taken up by the target tissue or those that are retained substantially longer by the target tissues than by the surrounding tissues of a patient. Furthermore, photoactivatable compounds may be administered alone, or in mixtures containing two or more such compounds. If compounds are combined, light of an effective wavelength for each compound in the mixture must be used to photoactivate the compounds.
Generally, the photoactivatable compound used must have a sufficiently low toxicity to permit administration to a patient with a medically acceptable level of safety. Various photoactivatable compounds are known and can be used in the practice of the invention. These compounds typically have chemical structures that include multiple conjugated rings that allow for light absorption and photoactivation. They differ in the properties of light absorption and fluorescence, biodistribution, temporal uptake, and clearance. Classes of photoactivatable compounds include hematoporphyrins (Kessel, Cancer Lett. 39:193-198, 1988), uroporphyrins, phthalocyanines (Kreimer-Birnbaum, Sem. in Hematol. 26:157-173, 1989), purpurins (Morgan et al., Photochem. Photobiol. 51:589-592, 1990; Kessel, Photochem. Photobiol. 50:169-174, 1989), acridine dyes, bacteriochlorophylls (Beems et al., Photochem. Photobiol. 46:639-643, 1987; Kessel et al., Photochem. Photobiol. 49:157-160, 1989), and bacteriochlorins (Gurinovich et al., J. Photochem. Photobiol. B-Biol. 13:51-57, 1992). Specific photoactivatable compounds which may be used to treat osteoarthritis are summarized, in part, in Table 1. Any photoactivating compound which displays no systemic toxicity and which is useful for photodynamic therapy of neoplasias may generally be useful in the methods of the invention. Preferably, Photofrin® (which is semi-purified hematoporphyrin derivative), benzoporphyrin derivatives, or aminolevulinic acid is administered in accordance with the invention.
TABLE 1
Compounds for Photodynamic Therapy of Osteoarthritis
1. Photofrin®
2. Synthetic diporphyrins and dichlorins
3. Hydroporphyrins such as chlorins and bacteriochlorins of the tetra(hydroxyphenyl) porphyrin series
4. phthalocyanines (PC)
with or without metal substituents,
e.g., chloroaluminum phthalocyanine (CASP)
with or without varying substituents
5. O-substituted tetraphenyl porphyrins
(picket fence porphyrins)
6. 3,1-meso tetrakis (o-propionamido phenyl) porphyrin
7. Verdins
8. Purpurins
tin and zinc derivatives of octaethylpurpurin (NT2)
etiopurpurin (ET2)
9. Chlorins
chlorin e6
mono-l-aspartyl derivative of chlorin e6
di-l-aspartyl derivative of chlorin e6
10. Benzoporphyrin derivatives (BPD)
benzoporphyrin monoacid derivatives
tetracyanoethylene adducts of benzoporphyrin
dimethyl acetylenedicarboxylate adducts of benzoporphyrin
Diels-Adler adducts
monoacid ring "a" derivative of benzoporphyrin
11. sulfonated aluminum PC
sulfonated AlPc
disulfonated (AlPcS 2 )
tetrasulfonated derivative
sulfonated aluminum naphthalocyanines
12. naphthalocyanines
with or without metal substituents
with or without varying substituents
13. anthracenediones
14. anthrapyrazoles
15. aminoanthraquinone
16. phenoxazine dyes
17. phenothiazine derivatives
18. chalcogenapyrylium dyes
cationic selena and tellurapyrylium derivatives
19. ring-substituted cationic PC
20. pheophorbide derivative
21. hematoporphyrin (HP)
22. other naturally occurring porphyrins
23. 5-aminolevulinic acid and other endogenous metabolic precursors
24. benzonaphthoporphyrazines
25. cationic imminium salts
26. tetracyclines
In addition to free photactivatable compounds, photoactivatable compounds may be delivered in various formulations, including liposomal, peptide/polymer-bound, or detergent-containing formulations.
An alternative to administration of the photoactivatable compound itself, is administration of a precursor of that compound. This approach is illustrated by the use of 5-aminolevulinic acid, which causes endogenous production of the photoactivatable compound protoporphyrin IX (Morgan et al., J. Med. Chem. 32:904-908, 1989).
Light of the appropriate wavelength for a given compound may be administered by a variety of methods known to one skilled in the art. These methods may involve laser, nonlaser, or broad band light and may result in either extracorporeal or intraarticular generation of the light of the appropriate wavelengths. Light used in the invention may be administered using any device which generates the appropriate wave form including, but not limited to, fiber optic instruments, arthroscopic instruments, or instruments which provide transillumination, as is known to one of ordinary skill in the art.
The therapeutic method described herein can provide effective treatment for osteoarthritic joints and the inflammation that may accompany any mechanical injury of a joint. As described herein, photoactivatable chemicals are administered, and the local joint region is then exposed to light via optical fibers threaded through small gauge hypodermic needles. Alternatively, the light source may be provided extracorporeally by transillumination. Thus, photodynamic therapy offers an effective, novel, and minimally invasive treatment which may benefit a large number of patients; 60-80% of the population develop some degree of osteoarthritis during their lifetime.
The invention also features an in vitro method for screening for a photoactivatable compound useful in PDT of osteoarthritis. The method involves contacting chondrocytes with the test photoactivatable compound, administering light of an appropriate wave length and determining whether this treatment has decreased the number of viable chondrocytes. Compounds that decrease the number of viable chondrocytes after treatment with light can be useful for PDT of osteoarthritis.
The term "osteoarthritic disease" as used herein is meant to encompass primary osteoarthritis, which may be of unknown etiology, and secondary osteoarthritis, which may occur as the result of a degenerative arthrosis. A patient that has osteoarthritis and, accordingly, an "osteoarthritic joint," may or may not have apparent focal damage, such as lesions, on the articular surfaces of an affected joint. It is expected that most patients availing themselves of the method of treatment described herein will be symptomatic, but the treatment may be also be applied as a prophylactic measure.
As used herein, "precursor" means a compound that is metabolically converted to a photoactivatable compound after administration to a patient.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. In case of conflict, the present document, including definitions, will control. Preferred methods and materials are described below, although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. Unless otherwise indicated, these materials and methods are illustrative only and are not intended to be limiting. All publications, patent applications, patents and other references mentioned herein are illustratiive only and not intended to be limiting.
Other features and advantages of the invention, e.g., treatment of human osteoarthritis, will be apparent from the following description, from the drawings and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A-1D are line graphs depicting the effect of PDT on chondrocyte viability using BPD-MA (FIG. 1A), Ce6 (FIG. 1B), PF (FIG. 1C) or CASP (FIG. 1D) as the photosensitizer.
FIG. 2 is a line graph depicting the effect of PDT on chondrocyte proliferation.
DETAILED DESCRIPTION
Photoactivatable chemicals localize selectively to the synovium or joint fluid and can be used to treat osteoarthritic disease. The anti-inflammatory effects of PDT and its ability to modulate enzymatic activity in chondrocytes can diminish the pathology seen in osteoarthritis. Decreased production, release, or activation of, for example, metalloproteinase enzymes, may allow for prolonged preservation of articular surfaces in oteoarthritis. Photofrin® is one of many examples of a photoactivatable therapeutic agent which may be used in the method of the invention. Its relevant characteristics, which include localization to the synovial tissue and particular clearance characteristics, are typical of many other photoactivatable compounds.
Osteoarthritis is a disease characterized by mechanically or biologically induced breakdown of articular cartilage. The degeneration of the cartilage due to biologic or mechanical effects changes load transmission through the joints and produces painful symptoms. Pain may also be due to inflammation of the joint lining tissue (synovium) which reacts to the free floating particles of cartilage (meniscal or articular). The degenerative cartilage does two things: (a) it produces enzymes which digest the extracellular matrix; and (b) it produces inflammatory mediators which spread throughout the joint and lead to inflammation of the synovium. The synovial inflammation in osteoarthritis is a response to irritating cartilage particles and is not due to an autoimmune response. PDT of osteoarthritis may slow the production of degradative enzymes, destroy inflammatory mediators in joint fluid and modulate inflammation in synovial tissue.
Numerous possibilities exist for delivery of both photosensitizing agents and light energy to the joints. Determining the most appropriate parameters for any photodynamic compound to be used for the treatment of osteoarthritis can be done using the experimental techniques provided herein.
I. Delivery of Photoactivatable Compounds
Therapeutic photoactivatable compounds may be either injected into the joints, or administered systemically according to the methods of the invention. The choice of localized versus systemic administration is determined, in part, by the number of joints to be treated during a given therapeutic regime. If a small number of joints require treatment, the therapeutic compounds may be administered locally. Conversely, if many joints require treatment, the therapeutic compounds may be administered systemically.
The therapeutic compounds to be administered for use in photodynamic therapy can be formulated for pharmaceutical or veterinary use by combination with an acceptable diluent, carrier, or excipient and/or in unit dosage form. In using therapeutic compounds in the methods of the invention, conventional pharmaceutical or veterinary practice may be employed to provide suitable formulations or compositions.
Thus, the formulations of the invention can be administered parenterally by, for example, intravenous, intraarticular, subcutaneous, intramuscular, intraventricular, intracapsular, intraspinal, intraperitoneal, topical, intranasal, or intrapulmonary administration. Patients may also be treated by oral, buccal, rectal, or vaginal administration.
Parenteral formulations may be in the form of liquid solutions or suspensions; oral formulations may be in the form of tablets, liquids, powders or capsules; and intranasal formulations may be in the form of powders, nasal drops, or aerosols.
Methods well known in the art for making formulations can to be found in, for example, Remington's Pharmaceutical Sciences, Mack Publishing Co., Easton, Pa., latest edition. Formulations for parenteral administration may, for example, contain as excipients sterile water or saline, polyalkylene glycols such as polyethylene glycol, oils of vegetable origin, or hydrogenated naphthalenes. Biocompatible, biodegradable lactide polymers or polyoxyethylene-polyoxypropylene copolymers in the form of microspheres may be used to control the in vivo release of the present compounds. Other potentially useful parenteral delivery systems for the compounds include ethylene-vinyl acetate copolymer particles, osmotic pumps, implantable infusion systems, liposomes, and antibody conjugates including, for example, liposomes into which joint tissue-specific antibodies have been incorporated. Formulations for inhalation may contain an excipient, for example, lactose; or may be aqueous solutions containing, for example, polyoxyethylene-9-lauryl ether, glycocholate and/or deoxycholate; or may be oily solutions for administration in the form of nasal drops; or a gel to be applied intranasally. Formulations for parenteral administration may also include glycocholate for buccal administration, methoxysalicylate for rectal administration, or citric acid for vaginal administration.
The present factors can be used as the sole active agents or can be used in combination with other active ingredients.
The concentration of the present factors in the formulations of the invention will vary depending upon a number of issues, including the dosage to be administered, and the route of administration.
In general terms, the compounds of the invention may be provided in an aqueous physiological buffer solution containing about 0.1 to 10% w/v compound for parenteral administration. General dose ranges for systemic administration are from about 0.01 mg/kg to about 20 mg/kg of body weight; a preferred dose range is from about 0.2 mg/kg to 2 mg/kg of body weight. When administered directly to the joint, the compounds may given at 0.01 to 10 mg per joint. The preferred dosage to be administered is likely to depend upon the type and extent of progression of the joint condition being addressed, the overall health of the patient, the patient's size, body surface area, age and sex, the formulation, and the route of administration.
II. Delivery of Photoactivating Light
Newer photosensitizing compounds, which do not cause systemic skin photosensitivity, allow for activation in the near infrared and longer wavelengths of the visible light spectrum. This allows for joint transillumination, which may be performed using a variety of devices involving laser or non-laser sources, i.e., lightboxes or convergent light beams. Alternatively, optical fibers may be passed either through arthroscopes, which will allow direct visual targeting and activation of the compounds, or directly through hypodermic needles which, preferably, have a small gauge. Light may also be passed via percutaneous instrumentation using optical fibers or cannulated waveguides. Activation may also be performed by open arthrotomy.
III. Method of Screening Therapeutic Agents for Use in Photodynamic Therapy for Osteoarthritis
A. Models of Osteoarthritic Joints
The following protocols may be used to generate a model of an osteoarthritic joint in a mammal. The mammal may be, for example but not restricted to, a rat, mouse, guinea pig, rabbit, dog, cat, or non-human primate. Mammals prepared in the manner described below can be used to screen various photoactivatable compounds for their application to the treatment of mechanically injured joints.
i. Section of the Medial Collateral and Both Cruciate Ligaments Combined with Resection of the Medial Meniscus
The following procedure is performed with New Zealand white rabbits, but other species of rabbits and any mammals with analogous joint structures may also be used.
Adult New Zealand white rabbits ranging in weight from three to six kilograms and judged to be mature by roentgenographic demonstration of epiphyseal closure may be used. Each animal is anesthetized (for example with diabutal supplemented with Xylocaine™), and the right knee joint is entered through a median parapatellar incision. The medial collateral ligament, both cruciate ligaments, and the flexor digitorum longus tendon (the muscle has an intraarticular origin in the rabbit) are divided, and the medial meniscus is excised. The capsule is then loosely approximated and the skin is closed, for example, with a continuous nylon suture (Ehrlich et al., J. Bone and Joint Surg.--American Vol. 57:392-396, 1975).
ii. Section of the Fibular Collateral and Sesamoid Ligament and Removal of the Anterior Horn of the Lateral Meniscus
Osteoarthritis may also be induced, for example in adult Dutch Belted rabbits, as described by O'Byrne et al. (Agents and Actions 39:C157-159, 1993) by sectioning the fibular collateral and sesamoid ligaments and removing the anterior horn of the lateral meniscus. This procedure has been shown to result in severe focal lesions of the cartilage on opposing surfaces of the tibia and femur (O'Byrne et al., supra).
B. Gross Pathology
Upon awakening, the animals may be permitted full weightbearing activity. Severe degenerative arthritis secondary to instability will develop over the ensuing three to six months, with visible changes apparent after one month. The knee joint may exhibit gross instability characterized by tibiofemoral and patellofemoral subluxation and occasionally by dislocation. In the early months, the articular surface of the femoral condyles, particularly that of the medial condyle, may appear dulled. In later months, fibrous tissue may cover portions of the articular surface of the tibial condyles. If the animals are allowed to survive for one year, the cartilage on the femoral surface may be thinned and exhibit focal erosion. Osteophytes may be seen on both the patella and the patellar surface of the femoral condyles.
C. Histological Analysis of the Osteoarthritic Joint
Histological studies employed to examine an osteoarthritic joint are well known to skilled artisans and include routine hematoxylin and eosin staining, and staining with safranin O, fast green, and iron hematoxylin. Hydroxyproline can be quantified by the method of Woessner; hexosamine can be quantified by the method of Rondle and Morgan; and acid phosphatase can be quantified by the method of Lowry (Lowry, J. Histochem. 1:420-428, 1953; Lowry et al., J. Biol. Chem. 207:19-37, 1954). Metabolic determinations may be performed using liquid scintillation spectrometric assays of incorporated isotopes after in vitro exposure, as described by Mankin et al. (J. Bone and Joint Surg. 51:1591-1600, 1969).
D. Animal Studies of Photodynamic Compounds Using Animals with Osteoarthritic Joints
In order to determine whether a particular photoactivatable compound is suitable for use in the method of the invention, New Zealand white rabbits weighing 3-4 kg each are divided into 3 groups: a control group consisting of normal, healthy animals (control group 1), a control group consisting of animals that have undergone surgical sectioning of the anterior cruciform ligament but do not receive PDT (control group 2) and an experimental group consisting of animals that have undergone this surgery and do receive PDT. Once instability of the joint is apparent, 24 animals in the experimental group will receive a systemic injection of 2 mg/kg of the compound to be tested via a 25 gauge needle into an ear vein. Additional, localized injections may also be given 48 hours later, or at any other time indicated by drug clearance studies. A comparable number of animals in control group 1 will also receive injections of the therapeutic agent. The animals will be sedated with rompen and ketamine, according to standard protocols, and given light activation treatments. Both knees of all animals in the experimental group and one knee, preferably the right knee, of animals in control group 1 will receive light activation treatments. 400 nm-690 nm wavelength light energy, or any wavelength which is activating for the chosen therapeutic, will be transmitted via a 400 micron optical fiber through a 23 gauge needle into the knee joint cavities. Alternatively, light may be applied extracorporeally. A total light energy of 100 J/cm 2 , or that energy range deemed appropriate for a given compound, will be applied to each joint over 20 minutes with an average laser power setting of 3-5 watts, or that wattage and time which is effective for a given compound.
Six animals from the experimental group and from control group 2, and 4 animals from control group 1 will be sacrificed one-, two-, four-, and 10 weeks after the photodynamic compound was injected into the experimental group and control group 1. After the animals have been killed, samples of synovium, articular cartilage, meniscus, and tendon will be harvested and fixed in formalin. Specimens are then embedded in paraffin, sectioned, stained with hematoxylin and eosin, and then examined microscopically for signs of inflammation, scarring, and necrosis.
It will be understood that specific modifications in dosage, timing, light wavelength, and duration may be necessary for each therapeutic compound tested. These general parameters are known to those skilled in the art and are summarized, in part, in the following papers and references cited therein which are incorporated by reference in their entirety: Gomer, J. Photochem. Photobiol. 54:1093-1107, 1991; Maziere et al., J. Photochem. Photobiol. 8:351-360, 1991; Allison et al., Photochem. Photobiol. 54:709-715, 1991; Allison et al., Photochem. Photobiol. 52:501-507, 1990; Poon et al., J. Neurosurg. 76:679-686, 1992; Reddi et al., Br. J. Cancer 61:407-411, 1990; Richter et al., Br. J. Cancer 63:87-93, 1990.
This protocol allows the practitioner to document, with pathology: (1) the ability of a photoactivatable compound to affect, e.g., inflammation at the joint, and (2) the non-deleterious effects of an activated photodynamic compound on articular cartilage, meniscus, and other periarticular tissues.
In order to document (1), samples of synovium from animals terminated at various times after treatment are fixed, embedded in paraffin, stained with a histological stain, and examined microscopically. In order to document (2), the same procedure is followed with samples of articular cartilage, meniscus, tendon, and muscle. Gross observations at the time of harvest should also be noted. Knee inflammation at the time of light application will be examined clinically and recorded. A test compound that ablates or diminishes, for example, inflammation of the joint or production of proteolytic enzymes by chondrocytes, without concomitant deleterious effects on articular cartilage, meniscus and other periarticular tissues, could be a useful compound for PDT of osteoarthritis.
The following examples are meant to illustrate, not limit, the invention.
IV. EXAMPLES
Materials and Methods
Chondrocyte Isolation
Chondrocytes were harvested by established collagenase digestion techniques. Articular cartilage was aseptically dissected from the femoral condyles and patellas of calf knee joints. Condyle surface shavings were finely minced and digested overnight at 37° C. with collagenase 1 mg/ml (Type II; 355 U/mg dry weight (dw)) and hyaluronidase 0.1 mg/ml (1060 USP/NF units/mg dw) (Worthington Biochemicals, Inc., Freehold, N.J.) in Dulbecco's Modified Eagle's Medium (DMEM; Mediatech, Herndon, Va.) supplemented with 20 mM HEPES, 100 U/ml penicillin G, 100 μg/ml ascorbic acid (serum free TCM). The resulting cell suspensions were filtered through a cell sieve and washed twice with serum free TCM. The cells were resuspended in the same medium containing 5% heat inactivated fetal calf serum (BioWhittaker, Walkerville, Md.) (FCS-TCM) for seeding. Cell number was determined using a hemocytometer. Cell viability, which was determined by trypan blue exclusion, was greater than 99% for all preparations. Cells were plated at a density of 1.5×10 6 cells/ml into Falcon 96 well cell culture plates (Becton Dickinson Labware, Franklin Lakes, N.J.) for the cytotoxicity and cell proliferation experiments and into Falcon 6 well cell culture plates for the Photosensitizer uptake studies. Chondrocyte cultures were maintained at 37° C. in a 5% CO 2 incubator for 1 week prior to initiation of the photosensitization studies.
Photosensitization Studies
Photofrin® (PF) and Benzoporphyrin Derivative (BPD-MA) were obtained from Quadralogic Technologies (Vancouver, Canada). Chlorin e6 (Ce6) and chloroaluminum phthalocyanine (CASP) were obtained from Ciba Geigy (Basel, Switzerland) and Porphyrin Products (Logan, Utah), respectively. All photosensitizers were added to the chondrocytes in the dark 3 hours prior to light exposure. Photosensitizer stock solutions were prepared immediately prior to each experiment; serial dilutions were prepared using FCS-TCM. All irradiations were done at the appropriate excitation wavelengths for each photosensitizer (BPD-MA 690 nm; Ce6 658 nm; CASP 680 nm; PF 624 nm) using light provided by an argon ion pumped dye laser (Coherent, Palo Alto, Calif.). Following light exposure, control and irradiated cells were maintained for 72 hours prior to the assessment of cellular viability and proliferation rates. Cells were examined daily by light microscopy for morphologic changes.
Screening studies of toxicity determined the range of doses and light response for each photosensitizer. These predetermined ranges were used for all of the studies described. For CASP, no dose response was seen. Dosages greater than 50 μg/ml were considered not clinically relevant and a dose range extending to 50 μg/ml was chosen for these studies.
Cytotoxicity Assays
PDT-induced cytotoxicity was determined 72 hours after irradiation. 3-(4,5-dimethylthiazol-2yl)-2-5-diphenyltetrazolium bromide (MTT) (Sigma Chemical Co., St. Louis, Mo.) was used for the determination of cellular viability (Mosmann, J. Immunol. Methods 65:55-63, 1983). MTT is metabolized via mitochondrial dehydrogenase enzymes to a formazan dye which can be measured spectrophotometrically. Cytotoxicity is expressed as the percentage of formazan produced in cells treated with visible light of different wavelengths and intensities relative to control cells (% control). The data are expressed as the mean ±S.E.M. from triplicate experiments.
Cell Proliferation Assays
Cell proliferation was determined by 3 H!-thymidine incorporation for all chondrocyte cultures 72 hours after drug and/or light exposure. The cell cultures were labeled with 5 μCi/ml 3 H!-thymidine (35 Ci/mmol) (ICN, Irvine, Calif.) in FCS-TCM. After incubation for 20 hours, the radioactive medium was removed and the cells were rinsed three times with phosphate buffered saline (PBS) to remove unincorporated label. The cells were then lysed with buffer containing 150 mM Tris pH 8.0, 200 mM sodium chloride, 10% triton X-100 and 1% SDS. 3 H!-thymidine incorporation was determined by liquid scintillation methods and the data are expressed as mean % control ±S.E.M. of samples irradiated without photosensitizer addition.
Cellular Imaging: Direct Immunofluorescence (Confocal Microscopy)
Glass coverslips were coated with 20 μg/ml fibronectin (Collaborative Biomedical Research Corp., Bedford, Mass.) at 4° C. overnight. 1.5-3×10 6 chondrocytes were seeded onto the fibronectin-coated coverslips, which were maintained at 37° C. for 2 hours prior to incubation with 10 μM rhodamine for 15 minutes. The cells were fixed with 2% formalin for 5 minutes and mounted onto histological slides. Rhodamine fluorescence was examined using an epifluorescence illumination microscope under 40× and 100× magnifications (Axiophot, Zeiss, Oberkochen, Germany). Fluorescent images resulted from rhodamine excitation using a 545 nm band pass filter for excitation and a 625 nm band pass filter for emission.
Light Microscopy
The cells were examined daily by light microscopy. Morphologic changes recorded were cellular differentiation, membrane blebbing and cellular exclusion of trypan blue.
Photosensitizer Uptake Studies
Articular chondrocytes were maintained in primary culture for five days after plating. Photosensitizer stocks were serially diluted in FCS-TCM and added to triplicate wells. The cells were incubated in the dark for 3 hours. The photosensitizer-containing FCS-TCM was then removed and the cells were rinsed with 1 ml PBS. To digest the extracellular matrix, the cells were then immersed in 1 ml of a solution of 1 mg/ml collagenase and 0.1 mg/ml hyaluronidase in serum-free TCM. The resulting single cell suspensions were transferred to microfuge tubes and were centrifuged at 3.3×g for 5 minutes. The collagenase solution was removed and the cells were rinsed three times with calcium/magnesium-free PBS. Aliquots were taken for cell counting prior to cell lysis with 1 ml 0.1 N NaOH containing 1% SDS. Cell counting was performed by hemocytometer and Coulter counter. Fluorescent spectra of the cell lysates were obtained using a Spex FluoroMax spectrofluorometer (ISA Instruments, Edison, N.J.) at the appropriate excitation/emission wavelengths for each of the four photosensitizers studied. Fluorescence spectra were corrected for background fluorescence. Relative uptake values were obtained by regression analysis of standard curves of known photosensitizer concentrations. The concentration in the cultures at which each photosensitizer inhibited chondrocyte proliferation (i.e., 3 H!-thymidine incorporation) by 50% (IC 50 ) was calculated from plots of relative proliferation (expressed as a percentage of control) versus the concentration of the photosensitizer in the culture. Values of uptake at the IC 50 are shown in fg/cell. Average protein per cell was calculated from the cell counts and protein concentration determined by the Lowry protein assay.
Gelatin Zymography
Aliquots of conditioned medium were mixed with 1 ml of acetone and maintained at -20° C. for 16-20 hours. The aliquots were microcentrifuged at 14,000×g for 15 minutes, the supernatant was removed and the precipitated protein was dried in a vacuum concentrator (Savant, Farmingdale, N.Y.) to remove residual acetone. Conditioned medium samples were mixed with sample buffer (0.4 M Tris pH 6.8, 5% SDS, 20% glycerol, 0.003% bromophenol blue) and applied directly, without boiling or reduction, to 10% acrylamide gels containing 1% gelatin. After removal of SDS from the gel by incubation in 2.5% Triton X-100 for 1 hour at room temperature, the gels were incubated for 16-18 hours at 37° C. in buffer containing 50 mM Tris pH 7.6, 0.2 M NaCl, 5 mM CaCl 2 and 0.02% Brij 35. The gels were stained for 1 hour at room temperature in 30% methanol/10% acetic acid containing 0.5% coomassie blue R-250 and destained in the same solution without dye. The gelatinolytic activity of the proteins was evidenced by clear bands against the blue background of the stained gelatin.
Example 1
Studies of PDT Efficiency Using Several Clinically Relevant Photosensitizers
Photosensitizer Effects on Chondrocyte Morphology
In the bright field and corresponding rhodamine fluorescence images of articular chondrocytes plated onto fibronectin-coated coverslips, the cells exhibited an overall polygonal to spheroid morphology and formed confluent monolayers in primary culture. Cell density was 70-80% confluence. At plating, staining of the cells with 10 μM rhodamine indicated that >99% of the cells were metabolically active. Subcellular distribution of rhodamine as bright, discrete, punctate regions of fluorescence outside of nuclei was suggestive of mitochondrial localization. Dedifferentiation occurred in 5-10% of control cells over the seven day protocol period.
Fluorescence of Photosensitizers in Chondrocytes
Cellular and subcellular fluorescence patterns as determined by confocal microscopy varied among the photosensitizers evaluated. The strongest fluorescence signals were observed with BPD-MA, which demonstrated diffuse cytoplasmic fluorescence for all drug concentrations studied. No nuclear or membrane staining was observed. Fluorescence occurred uniformly in both differentiated and dedifferentiated chondrocytes. For Ce6, cells exhibited elevated levels of cytoplasmic fluorescence comparable in intensity and distribution to BPD-MA. Cells treated with PF demonstrated a similar cytoplasmic distribution but lower levels of fluorescence than BPD-MA. Photosensitizer uptake was observed only in differentiated chondrocytes. Minimal CASP fluorescence was observed at the drug concentrations studied; fluorescence at the highest drug concentration was difficult to visualize above baseline levels of cytoplasmic autofluorescence.
Photosensitizer Effects on Cellular Viability and Proliferation
Irradiation of chondrocyte cultures with light dosages up to 10 J/cm 2 in the absence of photosensitizer at all wavelengths caused no decrease in cellular viability. In the presence of photosensitizer, treatment of chondrocyte cultures with 1, 5 or 10 J/cm 2 of light elicited general dose-dependent decreases in cellular viability (FIGS. 1A-1D). For BPD-MA (FIG. 1A) and Ce6 (FIG. 1B), saturation of toxicity effects occurred in the light dose range of 5 to 10 J/cm 2 and for PF (FIG. 1C) at 10 J/cm 2 . No saturation effects were observed for CASP in the range studied (FIG. 1D). BPD-MA produced the most toxic responses in chondrocyte cultures. At BPD-MA concentrations exceeding 0.1 μg/ml, cellular viability decreased 80% for irradiations of 5 or 10 J/cm 2 light, and decreased by 60% for 1 J/cm 2 light. CASP was minimally toxic to articular chondrocytes. Irradiation of cells with 1, 5 or 10 J/cm 2 light in the presence of 5 μg/ml CASP attenuated cell viability by less than 20%. Cellular exposure to more than 6 μg/ml Ce6 and 5 or 10 J/cm 2 light decreased viability by approximately 50%. For PF concentrations greater than 12.5 μg/ml, irradiation of cell cultures with 1 J/cm 2 light produced less than a 10% decrease in cellular viability while irradiations at the higher fluences decreased cellular viability by nearly 70%.
All photosensitizers elicited a dose-dependent inhibitory response on cellular proliferation rates determined by 3 H!-thymidine incorporation (FIG. 2). BPD-MA produced the most toxic effects (IC 50 =50.3 ng/ml) relative to Ce6 (IC 50 =4.4 μg/ml) and PF (IC 50 =9.3 μg/ml). CASP was found to be the least toxic. At the highest concentration of CASP investigated, 50 μg/ml, 3 H!-thymidine incorporation was reduced only 25%. The photosensitizing potentials determined by 3 H!-thymidine incorporation correlated with the MTT assay results.
Photosensitizer Uptake Studies
Photosensitizer uptake increased linearly across the dose range studied for all photosensitizers following a three hour incubation period. At the IC 50 concentrations, BPD-MA exhibited the lowest relative uptake. Higher uptake was observed for Ce6 which was markedly less than for CASP and PF (Table 2).
TABLE 2______________________________________In Vitro Uptake of Photosensitizers by Chondrocytes. IC.sub.50 Uptake Photons Absorbed atDrug IC.sub.50 (μg/ml) (fg/cell) IC.sub.50 (photons/cell)______________________________________BPD-MA 0.05 1.02 5.86 × 10.sup.6CASP >50 64.77 1.86 × 10.sup.6Ce6 4.4 2.32 1.44 × 10.sup.8PF 9.3 57.61 9.13 × 10.sup.6______________________________________
Zymography Studies
PDT effects on modulation of metalloproteinase (MMP2 and MMP9) activity, as determined by zymography, varied with the photosensitizer used, light dose applied and drug concentration. For BPD-MA and PF, MMP2 production decreased as a function of cell killing. At the IC 50 doses, MMP2 production was reduced by approximately 50% and at a highly toxic dose, production was non-detectable.
For Ce6, MMP2 production and MMP9 production were reduced at PDT parameter levels non-toxic to chondrocytes. At high drug doses, correspondingly greater decreases in MMP production occured. At the IC 50 dose, MMP2 production decreased by >95%. Total protein concentration did not vary with MMP values.
For the CASP parameters tested, no decrease in cellular viability was observed by MTT production and 3 H!-thymidine incorporation. However, significant reductions in MMP2 levels were recorded by zymography. At drug concentrations greater than 0.2 μg/ml and a light dose of 10 J/cm 2 , MMP2 levels decreased by 25%. At a drug concentration of 3.12 μg/ml with a light dose of 10 J/cm 2 (conditions under which no decrease in cell viability was observed), complete reduction in MMP2 levels was observed.
In summary, the findings of decreased MMP production and 3 H!-thymidine incorporation after photodynamic treatment of the cells indicate the potential to photochemically modulate the disease process in osteoarthritis. In addition to anti-inflammatory effects on inflamed synovium, photochemical treatments may be used to retard the biologic progression of the disease, as mediated by, for example, metalloproteinase enzymes. The method described in this Example can be applied to testing a wide variety of photoactivatable compounds, such as those shown in Table 1, for utility in treatment of osteoarthritis.
Although the invention has been described with reference to the presently preferred embodiment, it should be understood that various modifications can be made without departing from the spirit of the invention. Accordingly, the invention is limited only by the following claims.
|
A method of treating a patient who has osteoarthritic disease by administering a therapeutic composition containing a photoactivatable compound, or a precursor thereof, and administering light of a photoactivating wavelength that activates the compound.
| 8
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a gate for a hook. More particularly, the present invention relates to a hoisting hook provided with a locking gate which closes the mouth of the hook.
2. Description of the Prior Art
Reference is made to the following U.S. patents as typifying the structure of gates for hooks: Ratcliff U.S. Pat. No. 2,796,651, Geraghty U.S. Pat. No. 3,003,214, and Crook U.S. Pat. No. 3,575,458. The Ratcliff patent shows and describes a lockable gate which is pivotally movable about the stem (shank) of the hook for movement out of the mouth of the hook. The gate is attached to the stem by a sleeve and is pivotal about the central axis of the stem. The gate is provided with a cap which engages the tip of the hook automatically when the gate is closed and has a lock (in the second embodiment) which is automatically locked when the cap engages the tip. The Geraghty patent shows another gate having a lock and a sleeve, which is rotatable about the central axis of the stem. In the Crook patent, a gate is shown and described which is pivotally movable about a horizontal pin through the stem of the hook. The gate rotates from the tip toward the stem. A part of the gate will remain in the mouth of the hook. All three patents show the sides of the tip engaged by appendages extending from the arm of the gate to prevent the gate from moving laterally.
The prior constructions, which are laterally movable out of the mouth of the hook, pivot for movement out of the mouth about the sleeve which attaches the gate to the stem. Because of this sleeve, the prior gate constructions have proved practical only for smaller hooks.
SUMMARY OF THE INVENTION
The present invention involves a hook, for example, an eye or shank hoisting hook, which has a gate to close the mouth of the hook. The gate is mounted on the stem of the hook and is pivotal about an axis which is substantially parallel with the vertical axis of the stem and spaced from the stem.
The gate is comprised of a mounting structure which attaches the gate to the stem as described above, an arm pivotally mounted on the mounting structure, a spring biasing the arm in relation to the mounting structure, for example, to the open position across the mouth, a latch attached to the free end of the arm, and a lock also located at the free end of the arm.
The latch is provided with appendages (one on either side of the latch perpendicular to the gate's rotation with respect to the tip of the hook) which, when in contact with the tip, restrain the gate from opening.
The lock has a lever for manually moving the lock to the unlocked position when it is desirable to disengage the latch and a locking spring which biases the lock towards the locked position. When the latch is moved to engage the tip, the latch is automatically locked into the engaged position. While the latch is engaged with the tip, the gate forms a smooth continuous bridge which allows slack load lines to traverse without snagging.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a view in perspective of a hook which includes a latch mechanism constructed according to the present invention;
FIG. 2 is a cross-sectional view, on a slightly enlarged scale, taken along section line 2--2 of FIG. 1;
FIG. 3 is a cross-sectional view similar to FIG. 2 showing a modified means of attachment of the gate arm to the stem of the hook;
FIG. 4 is a cross-sectional view similar to FIG. 2 showing a further modification of the attachment of the gate arm to the stem of the hook;
FIG. 5 is a partial cross-sectional view, on an enlarged scale, taken along section line 5--5 of FIG. 1 showing the latch in the closed position against the tip of the hook;
FIG. 6 is a top view of the latch and lock shown in FIG. 5 with portions broken away to reveal internal details;
FIG. 7 is a cross-sectional view similar to FIG. 5 but showing the latch in the open position with respect to the tip of the hook;
FIG. 8 is a cross-sectional view similar to FIG. 5 but showing the latch in the open position; and
FIG. 9 is a fragmentary view of the mounting structure with portions broken away to reveal internal details.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a typical threaded shank hoisting hook 20 on which is mounted a gate generally designated by the reference numeral 24. The hoisting hook 20 has a C-shaped body 25 with a tip 26, a mouth 30, and a stem 34. A mounting structure 36 is attached to the stem 34 offset from the line between the stem 34 and the tip 26 so that gate 24 may be moved out of the mouth 30 (shown by dotted lines in FIG. 1). The mounting structure 36 is provided with an alignment hole 38 (FIG. 2). The gate includes an arm 44 which has an alignment hole 40 (FIG. 1) slightly larger than the hole 38. A threaded bolt 46 (FIG. 9) having an enlarged upper portion 48 extends through arm 44. The upper portion of the threaded bolt 46 can be secured to the arm 44 by welding, for example. The lower threaded portion 49 of bolt 46 passes through mounting structure 36 so that the lower end or shoulder or the enlarged portion 48 rests against the top of the mounting structure 36 to maintain the arm 44 in spaced relation above themounting structure 36. A nut 50 is received on the lower portion 49 of the bolt 46. A drive pin or locking pin 51 passes through the nut 50 and bolt 46 for preventing the nut from rotating on the bolt. Thus, a pivotal bearing is formed whose axis is parallel to the axis of the stem 34. A helical spring 52 (FIG. 9) is coiled around enlarged portion 48 of the bolt 46 between the mounting structure and the arm 44. One end 53 of spring 52 is received in the opening 54 in mounting structure 36, and the opposite end 55 of spring 52 is received in an opening 56 in arm 44. The spring 52 axially biases the arm 44 to the open position.
As shown in FIG. 2, the mounting structure 36 is formed as an integral part of the stem 34 by welding the same to a rib 58 protruding from the stem 34.
FIG. 3 shows a second embodiment of the mounting structure 36 provided with an integral threaded bolt 62. The stem 34 has a boss 64 with a suitable hole 68 in which the bolt 62 is received. A suitable nut 70 is provided for tightening the mounting structure 36 to the boss 64. Drive pin 63 passes through the boss 64 and bolt 62 and holds bolt 62 from rotating in the boss 64.
In FIG. 4, which shows a third embodiment of the mounting structure 36, the mounting structure 36 is provided with a clamp 76. The clamp 76 has a pair of apertured ears 78. The ears 78 are in a juxtaposed relationship around the stem 34. An alignment hole 79 is provided in each ear 78 so that a suitable bolt 80 and nut 82 may tighten the clamp 76 around the stem 34.
The arm 44 has a dogleg shape formed by a long member 85 (FIG. 1) which is essentially coextensive with the line between the stem 34 and the tip 26 (when the gate 24 is closed) and a short member 87 which is arcuate and which is attached to the mounting structure 36 (as discussed above). The long member of arm 44 slopes toward the tip 26. A latch 90 is located at the free end of the arm 44.
The arm 44 has a rectangular shaped notch 91 (FIG. 6) at its free end. One end of latch 90 has a rectangular shaped projecting part 92 which fits into the rectangular shaped notch 91. The rear surface 93 (FIG. 7) of rectangular shaped part 92 and the top 94 of latch 90 converge to form a rounded, generally V-shaped nib or latch tip 95. The latch 90 is hollowed to form two parallel and vertical ears 96 or appendages (FIGS. 1 and 7) which are parallel to the sides of the arm 44 and which engage the sides 97 (FIG. 5) of the tip 26. The hollowed underneath portion 101 (FIG. 5, 7, and 8) of latch 90 has an arcuate shape generally conforming to the shape of the tip 26. The appendages 96, and the rear underneath portion 101 of the latch 90 form a cap for tip 26.
The latch 90 is pivotal about pin 102 (FIG. 6) which extends through the arm 44 and projecting part 92. The pin 102 supports the latch 90 in realtion to the tip 26 so that the latch and its appendages 96 may be brought in close contact with the tip 26.
The latch 90 is locked into engagement with the tip 26 by a rotatable cam pin 104 (FIGS. 5 to 8) which is received in the arm 44. A lever 108 is attached to one end of the cam pin. The top surface of the lever 108 is flush with the top surface of the arm 44 and latch 90 when in the locked position (FIG. 5). A helical locking spring 110 (FIG. 6) coiled around pin 104 axially biases the cam pin 104 in the locked position. One end 111 of the locking spring 110 is received in an opening 112 in arm 44 while the other end 113 of the spring 110 is received in an opening 114 in the lever 108.
The cam pin 104 has a cut out portion 116 (FIG. 5) which provides a flat surface 117 and a resulting D-shaped cam portion 118 in that portion of the cam pin which crosses the rectangular notch 91. As indicated heretofore, the tip 26 of the hook is covered by the latch 90 in the locked position (FIG. 5). The latch is locked because, if one were to attempt to lift the latch 90 from the FIG. 5 position, the tip 95 would engage the solid portion 118 of the cam pin 104 to prevent rotation of the latch 90 around the latch pin 102. Thus, the gate 24 is restrained from opening laterally bacause the appendages 96 engage the tip sides 97 preventing arm 44 from rotating about mounting structure 36. The latch 90, lever 108, and arm 44 form a smooth bridge which allows a slack load line to traverse without snagging.
To disengage the latch from the locked position (FIG. 5), lever 108 is first rotated until the flat surface 117 is perpendicular to the latch 90. Now, the latch 90 can be rotated about pin 102 to the fully open position (FIG. 7), because the tip 95 can now clear the cam pin 104 in a downward direction. The gate 24 can then be rotated out of the mouth 30 about mounting structure 36 to the gate open position (FIG. 1, dotted lines) by spring 52.
When the lever 108 is released from the fully open position of the latch (FIG. 7), the lever will rotate downwardly until the cam 104 engages the latch 90. If the latch 90 is also released, it will drop by gravity until the latch tip 95 engages the flat surface 117, resulting in the partly open position of the latch as shown in FIG. 8.
Assuming that the latch is in the condition shown in FIG. 8, if it is desired to employ the gate latch 24 to close the mouth of the hook, as shown in FIGS. 1 and 5, the gate 24, or arm 44, is rotated until the arm 44 is disposed over the mouth 30. Thereafter, the latch 90 is rotated manually about the pin 102 by pressing down on the latch. As the latch 90 is forced downwardly, the latch tip 95 will be urged against the flat surface, forcing the cam pin 104 to rotate in a counter-clockwise direction (with respect to FIG. 8) to lift the locking lever 108 upwardly until the flat surface 117 approaches the position shown in FIG. 7 (but not quite that far) at which time the lever tip 95 can pass beyond, or clear of, the cam pin 104. Now the latch 90 can engage or cover the tip 26. However, the locking spring 110 will immediately thereafter rotate the cam pin 104 and the lever 108 to the locked position (FIG. 5).
Although spring 52 is described as biasing the arm 44 toward the gate open position, spring 52 can easily be reversed so that the arm 44 is biased to the closed position.
SUMMARY OF OPERATION
The gate is opened by manually moving a cam to an unlocking position. The latch is then moved at the same time to its position, disengaging the latch from the tip of the hook. The gate may then be swung out of the mouth of the hook.
When it is desired to lock the gate closing the mouth, the gate is moved over the mouth and the latch manually engaged with the tip. The latch will be automatically locked into the engaged position.
Whereas the present invention has been described in particular relation to the drawings attached hereto, it should be understood that other and further modifications, apart from those shown or suggested herein, may be made within the spirit and scope of this invention.
|
A gate latching mechanism comprising a gate for closing the mouth of a hoist hook. The gate is attached to the hook and pivotally movable out of the mouth of the hook about a substantially vertical pivot axis spaced from the central axis of the stem of the hook. A spring which is located at the pivot axis biases the gate to swing to an open position. The free end of the gate is provided with a latch which, when closed, covers the tip of the hook, a lock which holds the latch engaged with the tip until the lock is manually released, and a locking spring for moving the lock to the locked position when the latch is moved to engage the tip.
| 8
|
BACKGROUND OF THE INVENTION
[0001] This invention relates generally to rapid prototyping processes, and more particularly to an infiltrant system to be used for a part made by a rapid prototyping process, and a method for applying the infiltrant system to a part.
[0002] The conventional machining of prototype parts or production of cast or molded parts by hard or soft tooling techniques can take weeks and even months depending on the complexity of the part. It is an expensive and time-consuming process, and if changes need to be made, the mold may be useless.
[0003] Rapid prototyping was developed so that prototype parts could be made quickly, easily, and less expensively. There are two basic methods of rapid prototyping: a selective laser sintering process and liquid binder three dimensional printing process. Both use a layering technique to build a three-dimensional article. Thin cross-sections of the article are formed in successive layers. The particles in the layer are bonded together at the same time the cross-sectional layers are bonded together. Both processes allow parts to be made directly from computer-generated design data, and the parts can have complex cross-sections.
[0004] In selective laser sintering, a thin layer of powdered material is spread on a flat surface with a counter-roller. A laser is applied to the layer of powdered material in a predetermined pattern. The laser fuses the powder together. Additional layers of powdered material are applied and fused with the laser.
[0005] In the liquid binder three dimensional printing process, a layer of powdered material is applied to a surface with a counter-roller. A liquid or colloidal binder is applied to the layer of powder with an ink-jet printhead. The binder coats the powder and hardens, bonding the powder in that layer together and bonding the layers together. The process is repeated until the desired shape is obtained. When the part is taken out of the printer, it is fragile, and it does not have much cohesive strength. The part has to be reinforced and strengthened with an infiltrant system in order to make it functional. The infiltrant may fill in any pores in the part, improving the surface finish, and making it more impervious to water and other solvents. Known infiltrant materials include wax, varnish, lacquer, cyanoacrylate, polyurethane, and epoxy. The infiltrated part can then be used to assess the performance of the design.
[0006] Still, there is a need for improved infiltrant systems for rapid prototyping processes.
SUMMARY OF THE INVENTION
[0007] The present invention meets this need by providing an improved infiltrant system and method for applying the infiltrant system to a part. The infiltrant system generally includes a resin component and a hardener component. The resin component typically includes an epoxy resin, and a diluent. The hardener component typically includes an amine, optionally an amide, and optionally a catalyst.
[0008] In one embodiment, the infiltrant system is a high strength infiltrant system. The high strength infiltrant system generally includes a resin component and a hardener component. The resin component typically includes an epoxy resin, and a diluent. The hardener component typically includes an amine, an amide, and optionally a catalyst.
[0009] In another embodiment, the infiltrant system is a flexible infiltrant system. The flexible infiltrant system generally includes a resin component and a hardener component. The resin component typically includes an epoxy resin, and a diluent. The hardener component typically includes an amine, and optionally an amide.
DETAILED DESCRIPTION OF THE INVENTION
[0010] The infiltrant system generally includes a resin component and a hardener component. The resin component typically includes an epoxy resin, and a diluent. The hardener component typically includes an amine, optionall an amide, and optionally a catalyst.
[0011] In the resin component, suitable epoxy resins include, but are not limited to, bisphenol A, bisphenol F, or combinations thereof. Suitable diluents include, but are not limited to, reactive diluents, nonreactive diluents, or combinations thereof. Suitable reactive diluents include, but are not limited to, difunctional reactive diluents, monofunctional reactive diluents, or combinations thereof. Suitable reactive diluents include, but are not limited to, diglycidyl ether, glycidyl ether, or combinations thereof. A suitable diglycidyl ether is neopentyl glycol diglycidyl ether.
[0012] For the hardener component, suitable amines include, but are not limited to, unmodified aliphatic amines, modified aliphatic amines, unmodified cycloaliphatic amines, modified cycloaliphatic amines, unmodified amidoamines, modified amidoamines, or combinations thereof. One suitable amine is an unmodified aliphatic amine, such as aminoethyl-piperazine. Another suitable amine is a polyamine, such as polyoxypropyleneamine base polyamine. Another suitable amine is an unmodified aliphatic amine such as a diethylene glycol di(aminopropyl) ether base unmodified aliphatic amine. Combinations of amines are also suitable, such as a mixture of a polyoxypropyleneamine base polyamine and a diethylene glycol di(aminopropyl) ether base unmodified aliphatic amine.
[0013] Suitable amides for the hardener component include, but are not limited to, modified amidoamines, or unmodified amidoamines. One suitable amide is an unmodified amide/imidazoline. Mixtures of polyamides are also suitable.
[0014] Suitable catalysts include, but are not limited to, tertiary amines and benzyl alcohol.
[0015] The infiltrant system is made by mixing the materials in the resin component together. The materials in the hardener component are mixed together. The resin component and the hardener component are stored separately. They are mixed together before being applied to the part. The components react and the infiltrant system cures, providing a part with the desired characteristics.
[0016] One desirable infiltrant system is a high strength infiltrant system. The high strength infiltrant is designed to provide superior wicking and penetration properties. It has high tensile strength and durability. The high strength infiltrant generally has a low viscosity, typically less than about 150 cps mixed viscosity. Desirably, it should have a pot life of at least 30 minutes.
[0017] The high strength infiltrant system generally includes a resin component and a hardener component. The resin component for the high strength infiltrant system typically includes about 50% to about 90% by weight of resin component of an epoxy resin, typically about 70% to about 85%.
[0018] Suitable epoxy resins include, but are not limited to, bisphenol A, bisphenol F, or combinations thereof. A low viscosity epoxy resin is a desirable. The use of a low viscosity epoxy resin allows the use of less diluent. High levels of diluent can have an adverse effect on the mechanical properties of the cured material. In addition, lower viscosity allows the infiltrant to penetrate faster and deeper into the printed material. One suitable epoxy resin is a bisphenol F resin with a viscosity of about 2,500 to about 4,500 cps. It is available from Resolution Polymers, Houston, Tex., under the designation Epon 862. Higher viscosity resins can also be used, such as bisphenol A resin with a viscosity of about 11,000 to about 13,000 cps. It is available under the designation Epon 828. Equivalent epoxy resins can be obtained from other manufacturers. Prediluted resins can also be used, such as Epon 815, which is a mixure of Epon 828 (bisphenol A) and Epodil 841 (glycidyl ether).
[0019] The resin component for the high strength infiltrant system also includes a diluent. Diluents are used to reduce the viscosity of the compounded product. However, they can adversely affect the properties of the cured and uncured material. Suitable diluents include, but are not limited to, reactive diluents, nonreactive diluents, or combinations thereof. Suitable reactive diluents include, but are not limited to, difunctional reactive diluents, monofunctional reactive diluents, or combinations thereof. Difunctional diluents minimize the adverse effects of having large amounts of diluents in the system because they do not terminate the polymerization reaction due to the difunctional reactivity. Monofunctional diluents have a larger adverse effect on physical properties than difunctional diluents because they terminate the polymerization reaction. Therefore, it is desirable to keep the use of monofunctional diluents as low as possible to minimize the negative effects.
[0020] One suitable difunctional diluent is a diglycidyl ether, such as neopentyl glycol diglycidyl ether. Diglycidyl ether is a desirable diluent because it has a minimal negative effect on the reactivity of the uncured material and the physical properties of the cured material. Neopentyl glycol diglycidyl ether is available from Air Products, Allentown, Pa. under the designation Epodil 749. A suitable monofunctional diluent is a glycidyl ether. Glycidyl ether provides good viscosity reduction with good retention of overall properties. Glycidyl ether is available from Air Products under the designation Epodil 741.
[0021] Any glycidyl or diglycidyl ether type diluents can be used, although the performance may not be as good as with Epodil 741 and Epodil 749. Equivalent diluents, including but not limited to, diglycidyl ethers and glycidyl ethers, can be obtained from other manufacturers.
[0022] Nonreactive diluents can also be used, including, but not limited to benzyl alcohol.
[0023] The diluent is generally present in an amount of about 10% to about 50% by weight of resin component, typically about 15% to about 30%. Desirably, a combination of diluents is used. A difunctional diluent may be included in an amount of about 5% to about 30% by weight of resin component, typically about 10% to about 20%. A monofunctional diluent may be used in an amount of about 5% to about 20% by weight of resin component, typically about 5% to about 10%.
[0024] The hardener component for the high strength infiltrant system includes an amine. Suitable amines include, but are not limited to, unmodified and modified aliphatic amines, unmodified and modified cycloaliphatic amines, unmodified and modified amidoamines, or combinations thereof. One suitable unmodified aliphatic amine is aminoethyl-piperazine. It provides rapid cure at room temperature, as well as high strength and impact resistance, especially after post-cure at elevated temperatures. Some unmodified aliphatic amines are very brittle and stiff after curing, which is undesirable. Some unmodified and modified aliphatic amines, unmodified and modified cycloaliphatic amines, or unmodified and modified amidoamines may result in lower physical properties, higher viscosity, and lower wetting and penetration by the resulting infiltrant composition. The amine should be selected to provide adequate strength and impact resistance, and good wetting and penetration.
[0025] The amine is generally present in an amount of about 20% to about 80% by weight of hardener component, typically about 30% to about 60%.
[0026] The hardener component for the high strength infiltrant system also includes an amide. Desirably, the amide is free of plasticizers, has a low viscosity, and has good wetting and penetration properties. Using an amide without a plasticizer helps to obtain maximum physical properties in the cured material. Suitable amides include, but are not limited to, modified and unmodified amidoamines. One suitable modified amidoamine is a modified amide/imidazoline. Ancamide 2443 available from Air Products, Allentown, Pa., is a suitable amide. It is a modified amide/imidazoline which is plasticizer free, has a viscosity of about 30 cps, and has excellent wetting and penetrating properties.
[0027] The amide is generally present in an amount of about 20% to about 70% by weight of hardener component, typically about 40% to about 60%.
[0028] The hardener component for the high strength infiltrant system optionally contains a catalyst. Suitable catalysts include, but are not limited to, tertiary amines and benzyl alcohol. The catalyst is a performance promoter, but is not necessary. It helps to cure the system faster, as well as enhancing the wetting and penetration capability of the product. Suitable tertiary amines include, but are not limited to, Ancamine K-54, available from Air Products, Allentown, Pa., and dimethylaminomethylphenol, such as DMP-10 available from Rohm & Haas, Philadelphia, Pa.
[0029] The catalyst is generally present in an amount of 0 to about 10% by weight of hardener component, typically about 3% to about 7%.
[0030] Typical formulations for the high strength infiltrant of the present invention are as follows.
Range (wt %) Range (wt %) Resin Component Epoxy Resin 50-90 70-85 Reactive Diluent (diglycidyl ether) 5-30 10-20 Reactive Diluent (glycidyl ether) 5-20 5-10 Hardener Component Amine 20-80 30-60 Amide 20-70 40-60 Catalyst 0-10 3-7
EXAMPLE 1
[0031] A high strength infiltrant was made according to the following formulation:
Tradename Ingredient Weight % Resin Component Epon 862 Bisphenol F Epoxy resin 79.3 Epodil 749 Neopentyl Glycol 15 Diglycidyl Ether Epodil 741 Butyl Glycidyl Ether 5.7 Hardener Component Aminoethyl-piperazine Unmodified Aliphatic 45 Amine Ancamide 2443 Amidoamine 50 Ancamine K-54 Accelerator/Catalyst 5
[0032] Parts made using the high strength infiltrant system of the present invention were tested and compared to parts made using an existing epoxy infiltrant system (both cured on Z Corp.'s zp100 powder system). The results are shown in Table 1.
TABLE 1 Physical Property Comparison Between High Strength Infiltrant and Existing Infiltrant System High Strength Existing Epoxy Property Infiltrant Infiltrant Tensile Strength (psi) 1,797 1,332 Tensile Modulus (psi) 255,077 114,000 Flexural Strength (psi) 5,055 2,888 Flexural Modulus (psi) 930,005 531,800
[0033] The high strength infiltrant of the present invention can improve one or more of the physical properties of a part (tensile strength, tensile modulus, flexural strength, flexural modulus) by at least about 30% as compared to the existing epoxy infiltrant. One or more properties can be improved by at least about 50%, or at least about 75%, or at least about 100%. High tensile strength and tensile modulus are important for a high strength infiltrant.
[0034] Another desirable infiltrant system is a flexible infiltrant system. The flexible infiltrant will allow flexible parts to be made using the three dimensional printing technology. One advantage of being able to make a flexible prototype is that parts can be made with a snap fit, just as the actual plastic parts would have. Having parts with identical properties to the actual parts to be made will allow the customers to assemble and disassemble the final parts. The flexible infiltrant system can be used to make prototype buckles and snap fit parts like phone housings.
[0035] The flexible infiltrant system should have low viscosity, good wicking and penetration, and flexibility to allow snap fit connections.
[0036] The flexible infiltrant system generally includes a resin component and a hardener component. The resin component generally includes an epoxy resin and a diluent. The hardener component generally includes an amine and optionally an amide.
[0037] The resin component for the flexible infiltrant system generally includes about 50% to about 90% by weight of resin component of an epoxy resin, typically about 70% to about 85%. The diluent is generally present in an amount of about 10% to about 50% by weight of resin component, typically about 15% to about 30%. Desirably, a combination of diluents is used. A difunctional diluent may be included in an amount of about 5% to about 30% by weight of resin component, typically about 10% to about 20%. A monofunctional diluent may be used in an amount of about 5% to about 20% by weight of resin component, typically about 5% to about 10%.
[0038] The resin component for the flexible infiltrant system can use the same types of epoxy resins and diluents as the resin component for the high strength infiltrant system.
[0039] The hardener component for the flexible infiltrant system includes an amine. Desirably, the amine should have flexibility, resiliency, toughness, and impact resistance. It should desirably have a low viscosity, and good wetting and penetration. Suitable amines include, but are not limited to, unmodified and modified aliphatic amines, unmodified and modified cycloaliphatic amines, unmodified and modified amidoamines, or combinations thereof.
[0040] The amine is generally present in an amount of about 30% to about 90% by weight of hardener component, typically about 65% to about 80%.
[0041] One suitable aliphatic amine is a polyoxypropyleneamine base polyamine. The compound has flexibility, toughness, and impact resistance. It also has a low viscosity of about 9 cps which allows it to wet the surface and penetrate through the pores of the printed part. Jeffamine D-230, available from Huntsman, Salt Lake City, Utah, is an example of a suitable polyamine. Other suitable polyamines having similar properties are other amines in the Jeffamine family, such as Jeffamine 400 and EDR-148.
[0042] Another suitable aliphatic amine is a diethylene glycol di(aminopropyl) ether base unmodified aliphatic amine. This unmodified amine has good toughness, resiliency, and impact resistance. It has a viscosity of about 10 cps, so it has good wetting and penetration. Diethylene glycol di(aminopropyl) ether base unmodified aliphatic amine is available from Air Products under the designation Ancamine 1922A.
[0043] Typically, a combination of amines is used, such as a polyamine and an aliphatic amine. For example, a combination of polyoxypropyleneamine base polyamine and diethylene glycol di(aminopropyl) ether base unmodified aliphatic amine can be used. One amine can be present in an amount of about 20% to about 80% by weight of hardener component, typically about 35% to about 60%. The other amine can present in an amount of about 10% to about 40% by weight of hardener component, typically about 20% to about 30%.
[0044] The hardener component for the flexible infiltrant system includes an amide. Suitable amides include, but are not limited to, mixture of polyamides. The amide should provide an elongation of at least about 50%, and typically at least about 75%, or at least about 100%. A suitable polyamide mixture is available from Air Products under the designation Ancamide 910.
[0045] The amide is generally present in an amount of about 10% to about 40% by weight of hardener component, typically about 20% to about 35%.
[0046] In some cases, rather than an amide, a reactive component, such as a modified aliphatic amine could be used. In this case, the hardener component would include a combination of a polyamine and an aliphatic amine, such as polyoxypropyleneamine and diethylene glycol di(aminopropyl) ether base unmodified aliphatic amine. The polyamine would typically be present in an amount of about 20 percent to about 80 percent by weight of hardener component and the aliphatic amine would be present in an amount of about 20 percent to about 40 percent by weight of hardener component.
[0047] A non-reactive flexibilizer could be used, but it will result in decreased strength in the cured product.
[0048] A flexible infiltrant of the present invention can be made using the following typical formulations.
Range (wt %) Range (wt %) Resin Component Epoxy Resin 50-90 70-85 Reactive Diluent (diglycidyl ether) 5-30 10-20 Reactive Diluent (glycidyl ether) 5-20 5-10 Hardener Component Aliphatic Amine 20-80 35-60 Aliphatic Amine 10-40 20-30 Polyamide 10-40 20-35
EXAMPLE 2
[0049] A flexible infiltrant was made according to the following formulation:
Tradename Ingredient Weight % Resin Component Epon 862 Bisphenol F Epoxy resin 79.3 Epodil 749 Neopentyl Glycol 15 Diglycidyl Ether Epodil 741 Butyl Glycidyl Ether 5.7 Hardener Component Jeffamine D-230 Polyoxypropyleneamine 42.9 base polyamine Ancamine 1922A Diethylene glycol 28.55 di(aminopropyl) ether base unmodified aliphatic amine Ancamide 910 Polyamide Mixture 28.55
[0050] Parts were made using the flexible infiltrant system of the present invention with Z Corp.'s zp250 powder system. The cured system provides a flexible and toughened product, allowing the parts to snap in and out hundreds of times without breaking. Table 2 shows representative properties for parts made using the flexible infiltrant system.
TABLE 2 Properties for Flexible Infiltrant System Property Flexible Infiltrant System Tensile Strength (psi) 1,531 Tensile Modulus (psi) 178,151 Flexural Strength (psi) 3,889 Flexural Modulus (psi) 195,688
[0051] The important properties for the flexible infiltrant are the flexural strength and the flexural modulus. These provide the flexibility necessary for snap fit type connections.
[0052] While certain representative embodiments and details have been shown for purposes of illustrating the invention, it will be apparent to those skilled in the art that various changes in the compositions and methods disclosed herein may be made without departing from the scope of the invention, which is defined in the appended claims.
|
An infiltrant system for rapid prototyping processes. The infiltrant system generally includes a resin component and a hardener component. The resin component typically includes an epoxy resin, and a diluent. The hardener component typically includes an amine, optionally an amide, and optionally a catalyst. High strength infiltrant systems, flexible infiltrant systems, and a method for infiltrating a part are also described.
| 1
|
FIELD OF INVENTION
[0001] The present invention relates to a system and method for governing the delivery of electronic mail messages over a communications network such as the Internet.
COPYRIGHT NOTICE
[0002] A portion of the disclosure of this patent document contains material that is subject to copyright protection. The copyright owner has no objection to the. facsimile reproduction by anyone of the patent document or the patent disclosure as it appears in the Patent and Trademark Office patent file or records, but otherwise reserves all copyright rights whatsoever.
BACKGROUND OF INVENTION
[0003] Electronic mail messaging is ubiquitous; it's popularity due in part to speed, convenience, and low cost. The low cost of sending electronic mail messages has become the catalyst for abusing mail messaging systems with e-mail viruses and unsolicited bulk mail, commonly known as spam.
[0004] Spam is most often sent to advertise products or services and frequently used to send computer viruses and objectionable material. Because the cost of sending electronic mail is very low, bulk mailers will send millions of mail messages every day. Recipient addresses for the mails are harvested in a variety of indiscriminate ways and added to mail lists which get shared, sold, and rented by, for, and to bulk mailers without regard to subscriptions or otherwise, the wishes of recipients. The spam and virus problems have reached epidemic proportions, degrading the performance and threatening the viability of the Internet and endangering national security. In April 2003 AOL reported that they alone expect to be blocking over two billion unsolicited bulk mail messages per day. Spam e-mail is currently estimated to account for over 50% of all Internet e-mail traffic.
[0005] With current electronic mail processes, the major cost of providing mail service falls to the ISP (Internet Service Provider), which receives mail for intended recipients. The ISP maintains the computer and infrastructure on which resides a mail server application for outgoing and incoming mail transactions and for maintaining mailboxes and delivering to these mailboxes, messages for intended recipients. Large amounts of monies have been spent by ISPs creating and installing application software to block or at best reduce the influx of spam mail.
[0006] However, that software frequently falls short of the intended purpose because it relies on a variety of filtering, blocking, and identification techniques to distinguish between spam and legitimate mail. McCormick, et al, in U.S. Pat. No. 6,023,723, Feb. 8, 2000 describes filtering mechanisms based on keywords and key phrases. Paul, in U.S. Pat. No. 5,999,932, Dec. 7, 1999 describes heuristic processing to filter received mail. Spammers are quick to catch on to the latest filtering techniques and modify their outgoing mail to defeat these methods.
[0007] Blocking techniques rely on identifying the sending mail server and maintaining large databases listing undesirable servers. One such blocking technique is described by Paul in U.S. Pat. No. 6,052,709, Apr. 18, 2000 and uses spam probe e-mail addresses planted at various Internet sites. If one of these e-mail addresses is received at an incoming mail server, the reverse path information is recorded to a database and any subsequent-mails from that address are blocked. Spammers are quick to subvert blocking methods by masking the originating server and by using previously unidentified relay servers. Frequently,.blocking prevents the delivery of legitimate mail.
[0008] Yet another method of limiting spam mail is based on methods of authenticating the sender. One such method is to auto reply to an incoming message using the reverse path information provided by the sender. The sender must respond to the auto reply or else it is concluded that the sender is not the party indicated by the reverse path and the mail is refused. In theory this method allows recipients of mail that is received to verify the sender and report the sender of spam mail to controlling authorities. This enforcement method fails in the short term, however, because spammers are highly mobile and elusive, frequently changing servers used to send the spam. Additionally, the Spammers location is usually outside the legal jurisdiction of enforcement authorities. U.S. Pat. No. 6,256,739 by Scopp, et al, Jul. 3, 2001 describes such a method.
[0009] Electronic mail viruses are distributed by the common SMTP process through message transfer agents and through the more insidious process of infecting a computer with an e-mail virus that includes an outgoing mail sending application that uses e-mail addresses from the target computer's address book for sending copies of itself directly to a recipients receiving message transfer agent for subsequent delivery to the recipient mailbox. These self-replicating viruses have seriously effected the viability of the Internet. Filtering and blocking software does little to prevent the spread of these viruses because they originate from legitimate sources. Firewalls help but are not installed on a majority of home computers. Other attempts to prevent the spread of self-replicating viruses have seriously degraded mail services. ISPs have had to throttle the amount of mail that can originate-from a sender in any one session. All of the above attempts to block spam have the unintended consequence of increasing the amount of electronic mail traffic. Spammers, knowing mail gets blocked, will send multiple copies of messages with header and content variations in the expectation that one or more of the messages will get through to the intended recipient mailbox. They will also redundantly send messages from different servers. Accordingly the current art is inefficient in the task of blocking spam mail messages and not only does little to reduce the amount of spam traffic but, unfortunately promotes an increase in the traffic, degrading the networks providing mail services.
[0000] Definitions
[0010] Mail: Any electronically, optically, electro-magnetically, or the like transmission over a network of a message intended for use by a human recipient.
[0011] SMTP: Simple Mail Transaction Protocol, SMTP protocols are defined in RFCs of Internet Engineering Task Force, Internet Mail Consortium
[0012] Keywords: SMTP service extensions
[0013] UA: User Agent, A User Interface for generating and reading mail messages
[0014] MTA: Message Transfer Agent, A mail application embodied on a computing device comprising at least one of outgoing and incoming mail functions
[0015] OMTA: Outgoing Message Transfer Agent, The functional portion of an MTA that sends mail.
[0016] IMTA: Incoming Message Transfer Agent, The functional portion of an MTA that receives mail.
[0017] Mailbox: The location where an IMTA delivers messages to an intended recipient. The mailbox may comprise a memory location, a printer, a voice mailbox, or combinations thereof and the like.
[0018] Mail Transaction: The process of negotiating the sending of a batch of one or more messages to one or more recipients at the same MTA.
[0019] Message Transaction: The process of negotiating the sending of a message to a specified recipient.
[0000] Conventions
[0020] Angle brackets (<>) are used to denote the value of the element named within the angle brackets.
[0021] The SMTP convention is used herein as illustrative of an e-mail transaction. The inventor does not intend to limit the scope of the invention to only SMTP transactions where other electronic mail protocols may make use of the same invention. To this end, a general electronic mail transaction will be referred to as “mail” and an SMTP specific transaction will be referred to as “SMTP mail”.
[0000] Cryptography
[0022] Cryptographic systems, including ones implementing public key cryptography, are described in the technical, trade, and patent literature. For a general description, see for instance, Schneier, Bruce, Applied Cryptography, Second Edition, John Wiley & Sons, Inc., 1996. For a description focusing on the PGP.™. implementation of public key cryptography, see for instance, Garfinkel, Simon, PGP: Pretty Good Privacy, O'Reilly & Associates, Inc., 1995. The disclosures of each of the foregoing are hereby incorporated by reference.
[0023] Cryptographic methods for protecting software applications are described in the paper, White - Box Cryptography and an AES Implementation, from Cloakware at http://206.191.60.52. The paper is available in PDF format.
SUMMARY OF INVENTION
[0024] MTAs (Message Transfer Agents) are software applications embodied on pluralities of computing devices in a network for the purpose of transferring electronic mail messages from one location to another. For illustration purposes, the MTAs described herein communicate via electronic means over the Internet, LAN (Local Area Network), WAN (Wide Area Network), or the like using a connection interface which establishes an initial communication protocol and buffers and routes incoming and outgoing signals. MTAs embodied on different computing devices may not be identical; however, they perform similar functions.
[0025] Typically in an SMTP (Simple Message Transfer Protocol) mail process, an electronic mail object is created on a UA (User Agent) GUI (Graphic User Interface) software application in response to input from a person originating the message. The mail object comprises an envelope and the message. The envelope comprises an originator address and one or more recipient addresses. The message comprises headers in the form of field name/value pairs and a message body. The mail object is submitted by the UA to an outgoing mail server, known as an MTA (Message Transfer Agent), in response to a send command from the originating person. The outgoing MTA examines the mail object for recipient information and establishes a two-way communication channel with the MTA of the intended recipient.
[0026] FIG. 1 is exemplary of a mail transaction sequence of communication steps in a successful message transfer process, consistent with SMTP standards RFC2821. The use of the terms OMTA (Outgoing Message Transfer Agent) and IMTA (Incoming Message Transfer Agent) here represent functional distinctions used to identify the operations of the outgoing, MTA- 1 , and incoming MTA- 2 , agents. Typically, in SMTP mail and other mail applications, the mail server comprises both OMTA and IMTA functions in a single software application embodied on a computing device. The combined functions comprise an MTA (Message Transfer Agent). The sequence and description of steps is:
[0027] Step 1 . A communication channel between MTAs is opened, the OMTA sends the command, EHLO in compliance with RFC2821 followed by a space and the fully-qualified domain name of the OMTA. The EHLO command tells the IMTA that the OMTA can process SMTP service extensions and requests a list of extensions supported by the IMTA.
[0028] Step 2 . The IMTA responds with “250” followed by a space, a domain identifier, a greeting, and on separate lines, a plurality of keywords used to identify supported SMTP service extensions.
[0029] Step 3 . The OMTA initiates a mail transaction with a one line command, “MAIL FROM:<reverse path>”. The reverse path is typically the sender's e-mail address as provided in the envelope.
[0030] Step 4 The IMTA responds with “250” to indicate that it is ready to communicate with the OMTA.
[0031] Step 5 . The OMTA sends “RCPT TO:<forward path>”. The forward path is typically the e-mail address of the recipient as provided in the envelope.
[0032] Step 6 . The IMTA responds with “250” to indicate that it has received the recipient information. It stores the forward path information.
[0033] Step 7 . The OMTA sends the command, “DATA”.
[0034] Step 8 . The IMTA responds with an interim reply, “354” to indicate that it is ready to receive data.
[0035] Step 9 . The OMTA sends the message and on a separate line a period (.) to indicate the end of the data transmission.
[0036] Step 10 . The IMTA responds with “250” to indicate successful receipt of data and stores the message.
[0037] Step 11 . The OMTA sends a “QUIT” command.
[0038] Step 12 . The IMTA responds with “250” and closes its connection.
[0039] Step 13 . The OMTA closes its connection upon receipt of the “250” response.
[0040] This process, in itself, does not provide any direct method of determining the acceptability of a mail transaction other than verifying that a valid recipient mailbox does reside with the IMTA. Accordingly, it is the object of this invention, to provide an improved method and means for governing the sending and delivery of electronic mail messages by incorporating a data token of monetary value in an electronic mail transaction. The token comprises a syntactically arranged set of data elements. A token, comprising a number of credits, is sent to an IMTA from an OMTA as part of a mail transaction. The data elements of an incoming token are processed at the IMTA to evaluate and authenticate the token and apply rules of mail delivery that may allow or disallow the delivery of a mail message to the intended recipient's mailbox. Delivery of messages causes to be applied to an IMTA account, the credits comprising the token with an equal number of token credits deducted from the OMTA account. The monetary value of the token is related to the number of credits imbedded in the token. Therefore, it is-a further object of the invention to demonstrate a method and means for issuing and redeeming token credits for MTAs and for establishing the monetary value of a credit and there-by, the monetary value of the token. The token will here-in-after be referred to as an eMstamp (Electronic Mail Stamp pronounced em-stamp).
[0041] An eMstamp derives monetary value by imbedding credits purchased from an issuing,agency. Upon being paid for a given number of eMstamp credits by the administrator of an MTA, the issuing agency electronically communicates via the Internet or the like with the MTA application. The issuing agency increments an eMstamp bank memory count of that MTA by an amount numerically equivalent to the number of eMstamp credits purchased. This is a process similar to “charging” an ordinary postal service stamp machine. Each time an outgoing message is sent, the MTA generates an eMstamp and increments the count of an outgoing memory count by the number of credits imbedded in the outgoing eMstamp. This is a process similar to depleting an ordinary postal service stamp machine. Each time an incoming message with a validated eMstamp is received by an MTA, the count of a received memory count is incremented by the number of credits imbedded in the eMstamp. Administrators of MTAs can contact the issuing agency for redemption of eMstamp credits when the received count plus the bank count exceeds the sent count. The issuing agency electronically communicates via the Internet or the like to the relevant MTA, reduces the number of the bank count by the number of credits being redeemed and pays the administrator an amount equivalent to the number of credits redeemed times a set value related to the purchase cost of an eMstamp credit.
[0042] It is a further object of the invention to demonstrate a method and means for establishing recipient mailbox privacy levels by using a numerical value associated with a mailbox in a rule for determining the number of eMstamp credits required of an incoming mail transaction before message delivery is accepted. Setting high privacy numbers for mailboxes will impose on the outgoing MTA a requirement for an equivalent or greater number of eMstamp credits to cause delivery of a message and consequently a higher cost of sending a message to that particular mailbox.
[0043] Privacy rules not withstanding, this invention provides a method and means where-by mail transactions are governed in a manner that is transparent to the end user, avoiding the need for every day users of electronic mail to learn new techniques. The intended consequence of the invention is to reduce the overall volume of electronic mail currently saturating networks and to discourage the indiscriminate dissemination of unsolicited bulk mail by imposing charges on administrators of MTAs that send more mail than received. Distribution and use of the invention is encouraged by transferring a portion of eMstamp credit charges to administrators of MTAs that receive more mail than is sent. It is yet a further object of the invention to prevent the spread of self-replicating e-mail viruses by refusing mail transactions at incoming MTAs where there is no eMstamp incorporated with the transaction.
[0044] Typically in a trusted environment where fees are imposed, it can be expected that attempts will be made by certain MTA administrators or their agents to subvert the intended purpose of the current invention by altering the software embodiment enabling eMstamp mail transactions. Therefore, in an alternate embodiment of the current invention, security layers, protecting an eMstamp transaction and preventing unauthorized manipulation of eMstamp software and credits are described.
[0045] These and other advantages and features of the present invention will become readily apparent to those skilled in the art of electronic mail systems and software after reading the following detailed description of the invention and studying the accompanying drawings.
BRIEF DESCRIPTION OF DRAWINGS
[0046] FIG. 1 . A basic SMTP message transfer process.
[0047] FIG. 2A A block diagram of eMstamp elements
[0048] FIG. 2B . Illustration of a possible eMstamp string using programming tokens
[0049] FIG. 3 . A block diagram of two MTAs from a network of MTAs with sender UA rules and mailbox rules
[0050] FIG. 4 . A flow chart showing basic steps in the process of sending and receiving mail using an eMstamp
[0051] FIG. 5 . Block diagram of the main elements in an eMstamp enabled system
[0052] FIG. 6 . A basic SMTP message transfer process using an eMstamp.
[0053] FIG. 7A . A block diagram of program functions comprising the incoming module of an eMstamp enabled MTA.
[0054] FIG. 7B . A flow chart of the operation of the incoming eMstamp module
[0055] FIG. 8A . A block diagram of program functions comprising the outgoing module of an eMstamp enabled MTA.
[0056] FIG. 8B . A flow chart of the operation of the outgoing eMstamp module
DETAILED DESCRIPTION OF THE INVENTION
[0057] MTAs embodied on different computing devices may not be identical; however, for purposes of illustration, MTAs 1 and 2 of FIGS. 7A and 8A are shown as having the same memory storage operations as exemplified by using the same numbers to identify each operation. FIGS. 7A and 8A focus on the operations pertinent to the software functions, comprising the eMstamp utility of an MTA.
[0058] FIG. 2A is a block diagram of eMstamp elements. The eMstamp is a data token comprised of data elements assembled into a syntactically consistent string. Each data element has a specific value serving a specific purpose and conforming to specific rules of syntax. For illustrative purposes the data elements are shown separately. However, two or more elements may be combined to make one element serving multiple purposes. Identifier Element 1 is a finite length string of randomly generated allowed characters. Timestamp Element 2 is a series of numbers representing the time in milliseconds from 1970 or the like. Credit Element 3 is a number representing multiples of eMstamp credits and is used to reflect monetary value for the eMstamp. Authorization Element 4 comprises data used to authenticate eMstamp enabled MTAs. Referring here to Identifier Element 1 and Timestamp Element 2 of FIG. 2A , these two elements in practice, may be combined into a single identifier element by appending Timestamp Element 2 to a plurality of randomly generated characters of Identifier Element 1 into a single element having both identification and timestamp information. This possible combination is illustrated in FIG. 2A as TimeID 6 . The two essential data elements needed to constitute an eMstamp data token are an identifier element and a number of credits which can include the zero value. An eMstamp data token may have fewer or more data elements as required specific to a mail transaction and two or more elements may be combined to form one element as long as essential information is not lost.
[0059] FIG. 2B illustrates an example of an eMstamp String 7 using programming tokens in a comma-delimited string. There is no a-priori reason for constructing the eMstamp with this syntactical format since there are currently no engineering standards governing the generation of eMstamps and there is no standard for parsing an eMstamp for the purpose of retrieving the value of the data elements. However this format is suggested to illustrate one possible syntactical construct using name/value pairs to allow parsing without prior knowledge of the sequence of data elements. In this example, three fields are employed; although, it will be appreciated that additional fields with other information, or fewer fields, may also be employed.
[0060] FIG. 3 illustrates two MTAs in a network of MTAs, having established a two-way communication channel each to the other over the Internet or the like for the purpose of conducting a mail transaction. MTA- 1 8 is serving as the outgoing message transfer agent, OMTA 30 . MTA- 2 9 is serving as the incoming message transfer agent, IMTA 50 . An OMTA initiates a mail transaction with an IMTA of the intended recipient using a SMTP or a like protocol. It is understood that MTAs often, but not necessarily, support both incoming and outgoing mail transactions. In a preferred embodiment of the invention, MTAs support the ability to-read-rules associated-with the mail client of the person originating a message, the UA (User Agent), and rules associated with the mailbox of the intended recipient of a message. These rules are illustrated herein as Mailbox Rules 20 established by an intended recipient and Sender UA Rules 21 established by a message sender. The rules can be used independently or in concert to govern the deliverability of mail messages. It is understood that where a specific rule does not exist for a particular mail transaction, the administrators of MTAs can establish policy for substituting default values or, in the case of inappropriate rule values, override the values. In one embodiment of the invention, a rule is established by Sender UA Rules 21 governing the maximum number of credits that can be allowed for a message transaction to a specified intended recipient. In a corresponding rule, an intended recipient can establish a Mailbox Rule 20 governing the minimum number of credits required of a sender before allowing delivery to the mailbox. This Mailbox Rule 20 is called a privacy level rule. In the first instance, MTA- 1 8 requests a message transaction with MTA- 2 9 by sending a mail command with forward path information. The forward path information identifies the intended recipient mailbox. In the second instance, MTA- 2 9 responds with information comprising the requested forward path and a privacy value derived from Mailbox Rule 20 representing a number of credits required to allow delivery to the intended recipient mailbox. In the third instance, MTA- 1 8 insures that the received privacy rule value does not exceed the maximum number of credits allowed by Sender UA Rules 21 for sending mail to the intended recipient. MTA- 1 8 may also apply rules governing the maximum number of credits that can accompany any mail transaction. MTA- 1 8 then continues or quits the message transaction according to an application of the credit rules. In one preferred embodiment of the invention the credits referred to herein are eMstamp Credits 3 of FIG. 2A .
[0061] FIG. 4 illustrates the flow of information for a basic eMstamp transaction between MTAs during an electronic mail transaction. In the first instance, Step 1 , the Outgoing Message Transfer agent Module 30 of an originating MTA sends information comprising. a request for an eMstamp identity data string from the MTA serving the intended recipient of a mail message. In the second instance, Step 2 , the Incoming Message Transfer agent Module 50 of the receiving MTA responds with information comprising an eMstamp identity data string and a privacy rule number. The eMstamp identity may be the TimeID 6 illustrated in FIG. 2A . The privacy rule number is a default value or the value set in a privacy rule governing the number of eMstamp credits required to deliver a message to the mailbox of the intended recipient. In Step 3 , the Outgoing Message Transfer agent Module 30 generates an eMstamp by combining the received eMstamp identity data, an authorization code derived from a confirmation of the authenticity of Outgoing Message Transfer agent Module 30 described as Authorization Element 4 of FIG. 2A , and a default number or the privacy rule number received from Outgoing Message Transfer Module 50 described as eMstamp Credit Element 3 of FIG. 2A . Information comprising the complete eMstamp is returned to the Outgoing Message Transfer agent Module 50 , Step 4 where it is processed according to governing rules, determining the correctness of all eMstamp elements in relation to any other information received, Step 5 . In Step 6 , based on the outcome of the processing in Step 5 , the Incoming Message Transfer Agent Module 50 returns a command to the Outgoing Message Transfer Agent Module 30 to either continue or quit the transaction. The Outgoing Message Transfer Agent Module 30 either continues or quits the transaction, Step 7 .
[0062] FIG. 5 illustrates the main functional elements comprising an eMstamp enabled system for sending and receiving electronic mail. MTA 11 is an eMstamp enabled message transfer agent connected via the Internet or the like to other message transfer agents. Incoming Mail 10 , having an eMstamp, is received by the IMTA 12 function of an eMstamp enabled MTA 11 . Upon validation of the received eMstamp and deemed deliverability to the intended recipient mailbox, IMTA 12 causes the eMstamp Credits 3 of FIG. 2A to be added to the Received Count 83 of MTA 11 Memory 80 . Outgoing Mail 14 comprising an eMstamp is sent by OMTA 13 function of eMstamp enabled MTA 11 . Upon sending, OMTA 13 causes to be added to Sent Count 82 of MTA 11 Memory 80 the number of eMstamp Credits 3 of FIG. 2A , comprising the sent eMstamp. The OMTA of an eMstamp enabled MTA cannot send mail unless Received Count 83 plus credits in eMstamp Bank 86 exceeds Sent Count 82 by an amount equal to or greater than the number of credits comprising a sent eMstamp. MTA Administrator 18 can read MTA 11 Memory 80 via Agent Interface 87 to determine if the total of Received Count 83 plus the eMstamp Bank 86 credits is sufficient for the MTA 11 to continue eMstamp mail sending operations. If the count is not sufficient, MTA Administrator 18 can contact Issuing Agent 15 , over the Internet or the like, via Agent Interface 87 , with a Request to issue Credits 19 . Upon receipt of payment for a requested number of credits, Issuing Agent 15 connects via the Internet of the like with MTA 11 via Agent Interface 87 to Add credits to bank 20 . Agent Interface 87 supports secure communication protocols and read/write access to MTA 11 memory along with general access to elements of the MTA as might be required by the Issuing Agent. Issuing Agent 15 causes to be added to eMstamp Bank 86 memory a credit count equivalent the number of credits purchased. Similarly, eMstamp credits can be redeemed. MTA Administrator 18 can contact Issuing Agent 15 via Agent Interface 87 with a Request to redeem credits 16 . Issuing Agent 15 connects to MTA 11 via Agent Interface 87 and confirms that Received Count 83 plus the count in eMstamp Bank 86 equals or exceeds Sent Count 82 by the requested redemption number. Issuing Agent 15 then causes to be subtracted from eMstamp Bank 86 a count equivalent to the number of credits being redeemed. Issuing Agent 15 then pays MTA Administrator 18 for the redeemed credits.
[0063] It is understood that MTA Administrator 18 may be a person that reads MTA 11 Memory 80 values from the administered MTA to determine when to purchase or redeem eMstamp credits or MTA Administrator 18 may be a software application running on the MTA that automatically connects to Issuing Agent 15 based on MTA count value rules. In the case of an automatic administrator application, payments for purchased or redeemed eMstamp credits would be made to or from pre arranged currency accounts.
[0064] FIG. 6 is exemplary of communication steps in a successful message transfer process using an eMstamp in a process consistent with SMTP standards. This invention is not predisposed toward interjecting eMstamp communications in the sequence at any specific step but, rather toward insuring that the eMstamp is passed and acted upon at some point in the mail transaction or during a subsequent transaction related to the initial transaction. For instance, the eMstamp could be sent after Step 6 and acted upon during a current SMTP transaction or sent in Step 9 as a component comprising the header of a message and acted upon in a subsequent transaction. To that end, the steps of FIG. 6 are exemplary of an eMstamp transaction as it might take place in an SMTP transaction. For clarity, a single recipient is indicated. It is understood that in certain mail transactions, a batch of forward path information may be sent by an OMTA. Subsequent descriptions of software embodiments will show provisions for batch processing multiple recipients. The sequence and description of steps follows:
[0065] Step 1 . Upon establishing a communication channel, the OMTA sends the command, EHLO in compliance with RFC2821 followed by a space and the fully-qualified domain name of the OMTA. The EHLO command tells the IMTA that the OMTA can process SMTP service extensions and requests a list of extensions supported by the IMTA.
[0066] Step 2 . The IMTA responds with “250” followed by a space, a domain identifier, a greeting, and on separate lines, a plurality of keywords used to identify supported SMTP service extensions.
[0067] Step 3 . The OMTA initiates a mail transaction with a one line command, “MAIL FROM:<reverse path>”. The reverse path is typically the sender's e-mail address as provided in the envelope.
[0068] Step 4 . The IMTA responds with “250” to indicate that it is ready to communicate with the OMTA.
[0069] Step 5 . The OMTA sends “RCPT TO:<forward path>”. The forward path is typically the e-mail address of the recipient as provided in the envelope.
[0070] Step 6 . The IMTA responds with “250” to indicate that it has received the intended recipient (forward path) information. It stores the forward path and appends TimeID 6 of FIG. 2A and optionally a number, n 22 as illustrated in FIG. 5 , representing a delivery rule of the intended recipients mailbox, to the 250 reply.
[0071] Step 7 . The OMTA assembles the eMstamp data and returns the command, STAMP:<stamp-data>. Stamp-data is a concatenated string of information making up an eMstamp.
[0072] Step 8 . The IMTA checks the eMstamp for validity and monetary value expressed in units and applies a rule set of the IMTA and optionally the recipient mailbox to accept or reject the eMstamp. Upon acceptance the IMTA returns a “250” reply.
[0073] Step 9 . The OMTA sends the command, “DATA”.
[0074] Step 10 . The IMTA responds with an interim reply, “354” to indicate that it is ready to receive data.
[0075] Step 11 . The OMTA sends the message and on a separate line a period (.) to indicate the end of the data transmission.
[0076] Step 12 . The IMTA responds with “250” to indicate successful receipt of data and stores the message.
[0077] Step 13 . The OMTA sends a “QUIT” command.
[0078] Step 14 . The IMTA responds with “250” and closes its connection.
[0079] Step 15 . The OMTA closes its connection upon receipt of the “250” response.
[0080] FIG. 7A , IMTA eMstamp Module 50 , is exemplary of an architecture for the block of-application software functions serving emstamp operations relating to the incoming mail operations of an MTA. In the first instance, as exemplified by SMTP transaction, Step 5 of FIG. 6 , incoming data from an outgoing eMstamp MTA, FIG. 6 , MTA- 1 , is received at MTA- 2 Connection Interface 66 . Data comprising Batch:<forward path> 60 , identifying intended recipients, is caused to be stored by MTA- 2 Connection Interface 66 in Incoming Storage 84 of MTA- 2 Memory 80 , and causes the activation of Batch Assembler 51 a. Batch Assembler 51 a and 51 b is a software means for assembling strings of information into a computer readable format, typically one string of data per line. Batch Assembler 51 assembles a TimeID comprised of Character Generator 52 output and Timestamp Engine 53 output in accordance with the elements for an eMstamp described and illustrated as FIG. 2A . For each forward path received, Batch Assembler 51 assembles a TimeID, a numerical value (n) 22 derived from the intended recipient's Mailbox Rules 20 governing the mailbox privacy level, and the forward path of the intended recipient in a string format such that each value can be easily identified for parsing on MTA- 1 . If (n) 22 is null or otherwise unavailable, Batch Assembler 51 sets the value of (n) to 1. Batch Assembler 51 loops through the assembly process, creating a data set of TimeID, (n) values, and forward paths for each of the intended recipients into a batch and passes the assembled batch 61 to MTA- 2 Connection Interface 66 for sending to MTA- 1 . A batch may comprise just one data set of intended recipient values. Batch Assembler 51 also causes to be stored in Outgoing Storage 81 the assembled batch. Forward paths unacceptable to IMTA- 2 may be dealt with in the batch by substituting an error code in place of the TIMEID in the string containing that forward path or by negotiating with MTA- 1 over each individual forward path. For purposes of discussion, Batch Assembler 51 , verifies the forward path and substitutes the error code for unacceptable forward paths. Incoming Storage 84 , Incoming eMstamp Storage 85 , Sent Count 82 , Received Count 83 , and eMstamp Bank 86 are memory functions to indicate, in terms of the purpose served, computer memory available to MTA operations and may be hard disk, floppy disk, volatile memory, or any other storage media. These constructs are illustrated as belonging to MTA- 1 Memory 80 and MTA- 2 Memory 88 .
[0081] In the second instance, MTA- 1 returns a batch of eMstamps 62 , assembled with their corresponding forward paths. MTA- 2 Connection Interface causes to be stored the returned batch in Incoming eMstamp Storage 85 . Receipt and storage activates eMstamp Parsing Engine 54 to retrieve and parse one eMstamp data set at a time from Incoming eMstamp Storage 85 and provide the forward path and parsed eMstamp data to eMstamp Rules Engine 55 . eMstamp Rules Engine 55 then retrieves a matching Forward Path 7 set of data from Outgoing Storage 81 . eMstamp Rules Engine 55 then compares TimeID 6 of the parsed eMstamp retrieved from Incoming eMstamp Storage 85 with the TimeID value of the retrieved data set from Outgoing Storage 81 for an exact match. An exact match is required to validate an incoming eMstamp. eMstamp Rules Engine 55 then applies a rule to the parsed Authorization 4 value to determine if the eMstamp has originated from an MTA running authorized eMstamp software. In the basic embodiment described here, without security layers, Authorization 4 has a value representing “true”. eMstamp Rules Engine 55 then compares the parsed eMstamp Credits 3 value with the number (n) 22 of the retrieved data set from Outgoing Storage 81 to determine deliverability of the mail message to the intended recipient's mailbox. The default governing rule is to deliver the mail if the eMstamp Credits 3 value equals or exceeds the value of (n) 22 . A positive validation, authorization, and number of credits constitute an authenticated eMstamp. eMstamp Rules Engine 55 then causes to be added to Received Count 83 the value of eMstamp Credits 3 from an authenticated eMstamp and passes each authenticated eMstamp forward path to batch assembler 51 b. Upon completion of the loop on a batch, Rules Engine 55 causes Batch Assembler 51 to pass the batch of forward paths 63 to MTA- 2 Connection Interface 81 for sending to MTA- 1 .
[0082] FIG. 7B is a flow chart illustrating the sequence of steps in the operation of IMTA eMstamp Module 50 .
[0083] Step 1 . A batch comprising forward path information 60 is received from the outgoing MTA, MTA- 1 , by MTA- 2 Connection Interface 66 and caused to be stored in Incoming Storage 84 . This is the equivalent of Step 5 of FIG. 6 , typifying an SMTP mail transaction.
[0084] Step 2 . Batch Assembler 51 a returns to the outgoing MTA an assembled batch of data sets 61 for each forward path stored in Incoming Storage 84 , comprising a TimeID assembled from Character Generator 52 and Timestamp Engine 53 , an (n) 22 value derived from Mailbox Rules 20 , and the related forward path from Incoming Storage 84 . Batch assembler 51 a also causes to be stored the assembled batch information in Outgoing Storage 81 . Where an invalid forward path is encountered, Batch Assembler 51 a substitutes an error code in place of the TimeID for the related forward path.
[0085] Step 3 . A batch of data sets 62 , comprising an eMstamp and the related forward path information is received back from the outgoing MTA, MTA- 1 and stored in Incoming eMstamp Storage 85 .
[0086] Step 4 . Retrieve eMstamp data and the (n) value from Outgoing Storage 81 , using the parsed Forward Path 7 information to identify the data. If no relevant data is found, the next data set in the batch is parsed and Step 1 repeated for each data set in the batch until a matching data set is found or there are no new data sets to parse. If there is no next Forward Path 7 , proceed to Step 9 . If a forward path matching data set is found, Rules Engine 55 proceeds to Step 5 .
[0087] Step 5 . Require an Authorization 4 value of “true”. If Authorization 4 value is not “true”, Rules Engine 55 causes MTA- 2 to reply to MTA- 1 with a quit message rejecting further transactions and causes the deletion of batches in Outgoing Storage 81 and Incoming eMstamp Storage 85 .
[0088] Step 6 . Compare the retrieved TimeID to the parsed TimeID 6 for an exact match. If there is no exact match, Step 4 is repeated with the next Forward Path 7 . If there is no next Forward Path 7 , proceed to Step 9 . If there is an exact match, Rules Engine 55 proceeds to Step 7 .
[0089] Step 7 . Compare the retrieved value of (n) 22 to the parsed eMstamp Credits 3 . If the parsed credit value does not equal or exceed the value of (n) 22 , Step 4 is repeated with the next Forward Path 7 . If there is no next Forward Path 7 , proceed to Step 9 . If the parsed credit equals or exceeds the value of (n) 22 , Rules Engine 55 proceeds to Step 8 .
[0090] Step 8 . Increment Received Count 83 by the value of eMstamp Credits 3 , and continue to Step 4 , getting next Forward Path 7 from Parsing Engine 54 . If there is no next Forward Path 7 , proceed to Step 9 .
[0091] Step 9 . Cause to be assembled forward paths into a batch in Batch Assembler 51 and passed to MTA- 2 Connection Interface 66 for sending to MTA- 1 .
[0092] FIG. 8A , OMTA eMstamp Module 30 , is exemplary of an architecture for the block of application software functions serving eMstamp operations relating to the outgoing mail operations of an MTA. In the second instance following a mail transaction request from the outgoing MTA by sending a batch of forward path information, as exemplified by SMTP transaction, Step 3 of FIG. 6 , a batch 61 of data sets comprising TimeID, (n) value, and acceptable forward path information is received back at the outgoing MTA via MTA- 1 Connection Interface 64 and caused to be stored in Incoming Storage 84 . OMTA Parser 32 is activated to select one data set at a time from Incoming Storage 84 , separating the forward path information from the TimeID and (n) value and passing the forward path information to by Batch Assembler 36 . An eMstamp is assembled by eMstamp Assembler 35 from each data set using the TimeID 6 and the (n) value as eMstamp Credits 3 and Authorization 4 information from Authorization Engine 33 . The assembled eMstamp is passed to OMTA Rules Engine 34 . OMTA Rules Engine 34 compares the value of eMstamp Credits 3 to Sender UA Rules 21 to insure that the credits do not exceed the value allowed for an eMstamp mail to the intended recipient. If eMstamp rule of Sender UA Rules 21 is null or otherwise unavailable, a global default value assigned by the MTA administrator is applied. Rules Engine 34 next checks that the sum of credits available from eMstamp Bank 86 plus Received Count 83 minus Sent Count 82 equals or exceeds the value of eMstamp Credits 3 . For each eMstamp that passes the Rules Engine 34 checks, the Sent Count 82 value is incremented by the value of eMstamp Credits 3 for that data set and the eMstamp is passed to Batch Assembler 36 for uniting with the forward path information received from OMTA Parser 32 . Batch Assembler 36 is a software means for assembling strings of information into a computer readable batch format and causing the OMTA eMstamp Module 30 to loop through all data sets in Incoming Storage 84 . When all data sets have been processed, Batch Assembler 36 causes MTA- 1 Connection Interface 64 to send the assembled batch 62 of data sets each comprising an eMstamp and related forward path information to MTA- 2 for processing.
[0093] FIG. 8B is a flow chart illustrating the sequence of steps in the operation of OMTA eMstamp Module 30 .
[0094] Step 1 . Request a mail transaction by sending batched forward path information.
[0095] Step 2 . A batch 61 of data sets comprising TimeID, (n) values, and forward path information is received back from the incoming MTA, MTA- 2 , by MTA- 1 Connection Interface 64 in and caused to be stored in Incoming Storage 84 . This is similar to Step 6 , FIG. 4 .
[0096] Step 3 . Retrieve a data set from stored batch.
[0097] Step 4 . Parse data set and pass forward path information to Batch Assembler 36 and the TimeID and (n) value to eMstamp assembler 35 .
[0098] Step 5 . Assemble TimeID and (n) value along with authorization information as an eMstamp and pass to OMTA Rules Engine 34 .
[0099] Step 6 . Compare the value of eMstamp Credits 3 to a Sender UA Rules 21 value governing eMstamp credits assignable to mail to an intended recipient. If the value is null or otherwise unavailable use the default value set by the MTA administrator. If the value of eMstamp credits exceeds the value according to Rules 21 governing eMstamp credits or alternately the default value set by the MTA administrator, discontinue processing of current data and retrieve the next data set.
[0100] Step 7 . Compare the value of eMstamp Credits 3 to the total of eMstamp Bank 86 credits plus Received Count 83 minus Sent Count 82 . If the value of eMstamp Credits 3 exceeds the total discontinue processing of current data and retrieve the next data set. If the value of eMstamp Credits 3 does not exceed the total, add the data set comprising the eMstamp and related forward path information to a batch for sending to MTA- 2 . Add eMstamp Credits 3 value to Sent Count 82 memory. Steps 3 through Steps 8 are repeated until all data sets in Incoming Storage 84 have been processed, whereupon the completed batch 62 is passed to MTA- 1 Connection Interface 64 for sending to MTA- 2
[0101] An alternate preferred embodiment of the current invention comprises methods for protecting an eMstamp transaction, the eMstamp bank of credits, sent and received credit counts, and the eMstamp enabling software itself from alteration and duplication.
[0102] Referring here to FIG. 7A , data returned to the OMTA comprises a TimeID 61 which is stored in Outgoing storage 81 . From the perspective of the IMTA this data creates a short-term unique identifier when returned to the IMTA as part of an eMstamp transaction. Copies of this data from the OMTA are rendered useless by the action of the IMTA which deletes the sent information from Outgoing storage 81 once one instance of identical data is received back. There-by, eMstamp Rules Engine 55 causes to be rejected any further transactions using the identical data. In the same transaction eMstamp enabling software itself is authenticated by encrypting the Batch 61 data sent to an OMTA from an IMTA employing secret or public key encryption techniques know in the trade. Failure of an OMTA to properly decrypt the received data results in a “false” value being entered into the returned eMstamp Authorization Element 4 of FIG. 8A . There-by, eMstamp Rules Engine 55 of FIG. 7A causes to be rejected any further transactions with that particular MTA. In addition, the assembled eMstamp received in Batch 62 may be encrypted by the OMTA, and decrypted by the IMTA.
[0103] In the instance of encryption and decryption using a secret key, both the IMTA and OMTA must have the secret key which is imbedded in the MTA software itself. It is therefore essential to protect this secret key from disclosure to unauthorized parties. A technique known as white box cryptography is employed which prevents the reverse engineering of the software in order to learn the secret key. A document, White - Box Cryptography and an AES Implementation, describing white box cryptography is available in PDF format from Cloakware at http://206.191.60.52 and is included herein by reference. In the instance of encryption and decryption using public/private key pairs the IMTA must refer to a internal cache of known public keys using the identity of the OMTA to get the public key of the OMTA or alternately refer to an outside source for this information. Encrypted data returned to the OMTA is then decrypted at the OMTA using the private key of the OMTA. In this instance, failure of the OMTA to decrypt the data indicates that the OMTA is not the OMTA it identified itself as when initiating a mail transaction. This technique then provides the advantage of authenticating the sending MTA and again, if proper decryption fails, a “false” authentication results causing the rejection of any further transactions with the OMTA by the IMTA eMstamp Rules Engine 55 of FIG. 7A .
[0104] Referring to FIGS. 5, 7A , and 8 A, Sent Count 82 , Received Count 83 , and eMstamp Bank 86 values are encrypted using secret keys, protecting these values from unauthorized alteration. The secret keys encrypting Sent Count 82 and Received Count 83 values are imbedded in the MTA software to allow access to these values for adding sent and received eMstamp credits. These keys are protected from reverse engineering disclosure using the white box cryptography referenced above and may be the same keys. eMstamp Bank 86 values are encrypted using the same or preferably a different secret key known to an issuing agent. This secret key must also be imbedded and protected in the MTA software to allow access to the eMstamp Bank 86 value by OMTA Rules Engine 34 of FIG. 8A . Referring here to FIG. 5 , Issuing Agent 15 employes a Secure Socket Layer (SSL) protocol or the like to communicate with MTA 11 via Agent Interface 87 thereby-protecting any communications from unauthorized intercept. Issuing Agent 15 , by employing the secret keys is then able to read Sent Count 82 and Received Count 83 values and alter the eMstamp Bank 86 value in accordance with the methods established for FIG. 5 . It is understood that the issuing agent could use a master key to access these values and to perform any other operations on the MTA software and stored values as may be required from time to time.
[0105] It is understood that numerous techniques are available for protecting software and stored values. This invention is not predisposed to the use of any particular technique but cites the above use of encryption keys as exemplary of one method to prevent unauthorized tampering with eMstamp enabled software and the values stored within an MTA. It is also understood that an issuing agent may have access to OMTA and IMTA software modules for the purpose of altering secret keys as may be required from time to time to insure protection.
[0000] References
[0106] Standards for SMTP E-Mail objects are defined by RFCs 2821 and 2822 which are included here-in by reference.
RFC2822, P. Resnick (2001) Internet Message Format http://www.ietf.org/rfc/rfc2822.txt RFC2821, J. Klensin (2001) Simple Message Transfer Protocol http://www.ieff.org/rfc/rfc2821.txt Internet Engineering Task Force, Internet Mail Consortium http://www.imc.org/rfcs.html
Patents
Paul, U.S. Pat. No. 5,999,932, Dec. 7, 1999 Mccormick et al, U.S. Pat. No. 6,023,723, Feb. 8, 2000 Paul, U.S. Pat. No. 6,052,709, Apr. 18, 2000 Scopp et al, U.S. Pat. No. 6,256,739 Jul. 3, 2001
|
A system and method for governing the sending and receiving of electronic mail, especially unsolicited bulk mail, spam, and mail viruses is described. A data token called an eMstamp, having a monetary value related to a number of imbedded eMstamp credits, is made a part of an outgoing electronic mail message transaction by the outgoing mail server. A mail server receiving mail examines the data of a message related eMstamp and makes rule based decisions to deliver or reject a mail message to the intended recipient mailbox based on the eMstamp data. Mail servers retain counts of incoming and outgoing eMstamp credits and use incoming eMstamp credits to offset credits needed to send mail. Administrators of mail servers having a greater number of outgoing eMstamp credits over incoming credits, will need to purchase eMstamp credits from an issuing agent to facilitate message delivery to other eMstamp enabled mail servers. Administrators of mail servers having a greater number of incoming eMstamp credits over outgoing credits can periodically redeem the excess of eMstamp credits for a monetary amount related to the purchase cost of credits. An intended consequence of the invention is to transfer revenue derived from the sale of eMstamp credits to eMstamp mail servers receiving more mail than is sent and to discourage the indiscriminate sending of electronic mail and self replicating e-mail viruses.
| 7
|
This is a continuation, of application Ser. No. 047,988, filed May 7, 1987 abandoned.
BACKGROUND OF THE INVENTION
The present invention relates to a pipe bending machine. More particularly, it relates to such a pipe bending machine which has a bending table turnable about an axis, a bending template, and a clamping jaw displaceable relative to the bending template with displaceable carriage which carries a rotatable clamping sleeve. In such a machine both a bending template and the clamping jaw have straight and curved portions and mutually associated clamping bodies which are provided with clamping surfaces for clamping a pipe to be bent and which are spaced from one another and at the same time can be brought to an operative position.
The German document DE-AS No. 1,297,064 published in 1969 describes a fully automatic pipe bending machine for bending pipes which have interconnected arcs located in different planes. In this machine a bending template which is separable at the end of bending from its rotary drive, and an associated pipe clamping jaw are provided with a pipe groove which lies in the bending plane and are also provided with a laterally branching groove which corresponds to the course of the curved pipe. The machine also has a pressing device acting outwardly and engaging transversely the non-bent pipe directly in front of the bending template. Finally, the machine also has a return rotary device for the template separated from the drive, and an adjusting device for the bending template which is activated during pressing of the pipe by the template.
Since the bending template and the clamping jaw are formed of one-piece with the pipe groove lying in the bending plane and with the pipe groove extending therefrom, the above mentioned branching does not provide an embracing full-surface clamping of the pipe. A knot point of the straight and the branching path or groove is not possible in practice, as long as after first bending the pipe is turned for the subsequent bending pipe approximately 90° in the bending plane. When it is turned by deviating values or smaller bending angle, the clamping surfaces of the grooves are so small that a bending is not practically possible, since a notcontrollable slippage takes place which prevents an accurate bending. The very small clamping surfaces lead in many cases to a damage to the pipe, such as a pressing-in in connection with a cross section reduction and grooving during a slippage.
The above described arrangement operates in the following manner: After the formation of the first curve, the bending template is fixed in its position which corresponds to the respective curve shape. After this, the loose clamping jaw is brought back to its original position. Then the bent end of the pipe is pressed outwardly under force radially to the template out of the pipe groove and turned over simultaneously into the new bending plane. When then the adjusting device releases the template, it is returned by the return turning device to its initial position. When then the pressing device for the pipe is turned off, the pipe turns either itself or under the action of the clamping jaw until it again abuts against the template so that the produced pipe curves are inserted in the branching groove of the template and the loose clamping jaw. The pipe is clamped for the production of the next curve, which is performed in a conventional manner by joint rotation of the template and the loose clamping jaw.
Since the arrangement in accordance with the above discussed German document DE-AS No. 1,297,064 does not give satisfactory results, several proposals have been developed for providing different clamping surfaces during bending of pipes. One of such proposals is disclosed in the German patent No. 2,626,202 of the inventor, in which the clamping surfaces are separated spatially from one another and are rotatable relative to the bending table.
The German document DE-AS No. 2,711,340 discloses an arrangement for cold bending of strand material, such as pipes, rods and profiles, which has a bending shaping piece rotatable about an axis and provided with a peripheral groove for receiving a strand material, and a clamping device which core rotates with the bending shaping piece and has a clamping jaw arranged on the bending shaping piece and a counterclamping jaw. The clamping jaw and the counterclamping jaw are provided with a groove which together form a receiving passage for the strand material. Moreover, the bending shaping piece has in some cases further peripheral grooves, the clamping jaws and the counterclamping jaws are provided with further different grooves associated with the peripheral groove of the bending shaping piece, and the clamping jaw with the counter jaw on the one hand and the bending shaping piece on the other hand are adjustable relative to one another for exchanging the receiving passage in direction of the axis of the bending shaping piece.
The German document DE-OS No. 3,407,499 of the Applicant discloses a machine in which the bending template and/or clamping jaw have an abutment surface, particularly a receptacle for exchangeable receipt of a body provided with the clamping surface. This body is arranged in a guide and provided with a drive which drives the body in a vertical movement into the receptacle and out of the same. In this receptacle, at the location of the body provided with a clamping surface, another body is movable in and out and provided with a clamping surface of another shape.
The above discussed three documents disclose the arrangements in which the respective portion of the pipe to be clamped must be engaged or surrounded for clamping over a complete surface, or in other words over its entire periphery. In the event of different spatial shapes which have the portion of the pipe to be clamped, for example when the pipe has an expanded and not expanded end to be clamped or depending on the preceding bending of a pipe portion, this requires completely different clamping bodies with a respective clamping surface associated with each clamping body. The prior art proposes different solutions for provided this clamping body with individually associated clamping surfaces. The above mentioned German patent No. 2,626,202 discloses the clamping bodies which are arranged on the bending template and distributed over its periphery, while they are arranged on the clamping jaw in a rotatable manner and thereby are concentrated locally. In the German document DE-AS No. 2,711,340 the clamping bodies arranged on the clamping jaw and the clamping bodies cooperating with the bending template form a structural unit which is mounted on the clamping jaw support and moved together with it.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a pipe bending machine which is a further improvement of the pipe bending machines known in the art.
More particularly, it is an object of the present invention to provide a pipe bending machine which has a bending template with a clamping jaw mounted thereon and a counter jaw mounted on a clamping jaw support, in which with smaller structural expenses or a number of clamping jaws, a plurality of clamping surfaces of different spatial shapes can be provided.
In keeping with these objects and with others which will become apparent hereinafter, the inventive clamp bending machine has a bending table which is turnable about an axis, a bending template and a clamping jaw displaceable relative to the bending template, and a displaceable carriage which has a rotatable sleeve, wherein the bending template and the clamping jaw have straight and curved portions for clamping associated clamping bodies which correspond to a pipe to be bent and which are provided with clamping surfaces, the clamping bodies are spatially separated from one another and bringable to an operative position, wherein in accordance with the invention one clamping body has one clamping surface which has several different contours of the pipe portions to be clamped, while the associated clamping body has only one clamping surface corresponding to the contour of the pipe portion to be clamped, and thereby the pipe portion to be clamped is engaged over a full surface at the associated portion over an angular distance of 180°.
When the machine is designed in accordance with the present invention, one clamping jaw has a clamping surface designed as a semi-shell which is semi-shell shaped over its entire length, so that the pipe portion abutting against it is engaged over the length of the clamping over an angular distance of 180°, while the opposite clamping jaw has several clamping surfaces over different spatial shapes which surround the inserted portion of the pipe to be clamped in certain regions only partially about 180°, so that in other words there is no there a complete clamping. It was recognized that during bending of the pipes it is sufficient to provide a full-surface clamping only over a half of the pipe cross section over the length of the clamping, while the opposite half can be clamped only in zones in a semi-shell like manner or over 180° so that the clamping surface has gaps which are or can be visible. When the inventive solution is implemented, one clamping jaw with several different clamping surfaces is or can be supported fixedly and does not require any drive.
It was further recognized that this is also true for the semi-shell like complete clamping at the clamping shell mounted on the bending template or at the clamping jaw provided on the clamping jaw support. Therefore in accordance with the further embodiment of the invention it is proposed that the clamping body arranged on the clamping jaw is rotatable and provided with several clamping surfaces distributed over its periphery, while each individual clamping surface has a clamping surface which corresponds to the pipe portion to be clamped, and the bending template has a clamping body with a clamping surface which has several different contours for the pipe portion to be clamped.
This proposal has the advantage that the arrangement of several clamping surfaces of different shapes in one clamping jaw or in some cases clamping jaws arranged over one another and axially displaceable on the bending template results in their local concentration at one point so as to make possible the unobjectionable bending of the pipe by up to 180°. It is especially advantageous in this proposal that in the clamping jaw arranged on the bending template, two or more different clamping surfaces can be provided in one clamping jaw. This inventive solution makes possible arranging of different clamping surfaces on one clamping jaw. This provides for a further advantage in that the clamping jaw arranged on the bending template can be screwed with the bending template, so that in the sense of movement only the counterclamping jaw arranged on the clamping jaw support is to be adjusted.
The inventive solution, particularly in connection with the above described features that the clamping jaw mounted on the bending template has several different clamping surfaces, which mounting means that the clamping jaw can be also axially movable in the bending template and also can be screwed at a certain location, makes possible to perform a method of bending in accordance with which after bending of the pipe by an adjusted bending angle by rotation of the bending template with abutting clamping jaw, the clamping jaw is released from the bending template, and the bending template is further turned in condition of no-supply of pipes by such an amount that the clamped portion of the pipe is removed from the clamping surface and the pipe is rotated about its non-bent longitudinal axis from the clamping surface of the bending template, and then the pipe supply for the next bending and simultaneously the return rotation of the bending plate to its initial position is performed.
In the known arrangements and designs of the clamping jaw and counterclamping jaw, after the end of the bending process and the release of the counterclamping jaw in condition of stopped bending template, the pipe is moved further, so that the bent end is withdrawn from the clamping surface of the clamping jaw of the bending template, then the bending template is returned to its initial position.
In accordance with the present invention, after the bending, the bending template is further turned by a certain amount so that this additional rotation results in that the clamping surface is removed from the bent pipe end. While till now the bent pipe end was removed from the bending template by this feature, the pipe in condition of the stopped bending template is displaced by a special feature, it is proposed now in condition of the stopped pipe to perform the rotation of the bending template over the value required for bending and so that the bent pipe end is no more in the clamping surface and thereby in condition of the stopped pipe of the bending template, is moved further. This has the advantage in that the control is simplified, since after bending of the pipe it retains its position while the bending template is further rotated over the value required for bending. This further rotation is performed in one working step, since with this further rotation no further bending of the pipe is performed, but only the release of the counterclamping jaw.
The inventive proposal leads to an end result in that the movement course is simplified and the accuracy of the bending is increased. In known methods, for releasing the bent pipe portion form the clamping surface the clamping located on the bending template further moved the pipe by an additional movement in its axial direction. This additional movement for releasing from the clamping jaw had to be taken into account in the control program so that the neck bending had to be performed after a respective pipe displacement at a proper location. The displacement for movement of the bent pipe portion from the clamping jaw must, therefore, be considered. It should be mentioned that for determination and execution of the bending program it is respectfully simple that the bending template is moved outside with the clamping jaw mounted thereon, by a value required for the bending.
The novel features which are considered as characteristic for the invention are set forth in particular in the appended claims. The invention itself, however, both as to its construction and its method of operation, together with additional objects and advantages thereof, will be best understood from the following description of specific embodiments when read in connection with the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a pipe bending machine;
FIG. 2 is a perspective view of a bent pipe;
FIG. 3 is a perspective view of a bending template with clamping jaws and counterclamping jaws;
FIG. 4 is a view showing a vertical section of a bending template with a double clamping jaw which is arranged on it and movable in an axial direction;
FIG. 5 is a view showing a bending template with clamping jaws which have several different clamping surfaces;
FIG. 6A-6C are views showing a bending template in FIG. 6B and 6C, with incorporated clamping jaws, which is associated with a couterclamping jaw shown in FIG. 6A; and
FIG. 7 is a view showing a counterclamping jaw which is provided on its surface with several different clamping surfaces.
DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows a conventional pipe bending machine with a displacing carriage 10 which can reciprocatingly slide over the upper side of a machine housing 12 on one or several guiding rails 11. The displacing carriage 10 has a hollow cylinder 13. A clamping sleeve 14 is arranged in the interior of the hollow cylinder 13 and has an end region for clamping a pipe piece or pipe 15 to be bent. The pipe piece 15 is guided around a turnably supported bending template 16. The bending template 16 has a groove 17 provided for the pipe and corresponding to the semidiameter of the pipe. A clamping jaw 19 is pressed against a part of the pipe piece 15 extending around the bending template 16. The pressing is performed by means of a clamping device 18. The clamping jaw 19 also has a groove which corresponds to the semidiameter of the pipe, and clamps the pipe 15 against the bending template 16. For this purpose, the clamping template is provided with a clamping jaw 25 which is arranged on the clamping template and is releasably connected therewith.
A hydraulic cylinder-piston unit is used for example for moving the clamping device 18 of the clamping jaw 19 toward the bending template 16 for fixing the pipe and for withdrawing the same from the bending template. The bending template 16 is fixedly mounted on a bending table 21. The clamping device 18 is reciprocatingly displaceable via the cylinder-piston unit 20 in the shown direction identified by the arrow 22. When the bending template 16 is turned over the bending table 21 together with the clamping jaw 19 in direction of the arrow 23, then the pipe piece 15 obtains a curvature which corresponds to the profile of the bending template 16. During this bending step the end part of the tubular piece 15 remains clamped in the clamping sleeve 14 of the displacing carriage 10, for reliably guiding the pipe piece in all positions. For preventing lateral buckling of the free pipe piece 15 between the clamping piece 14 and the bending template 16, a sliding rail 24 is pressed against this portion of the pipe piece. The sliding rail 24 also has a groove which corresponds to the semidiameter of the pipe. The clamping sleeve 14 of the displacing carriage 10 does not clamp the pipe piece 15 fixedly, but it turns by the angular distance up to 360° when successive bendings of the pipe must be curved in different directions. For turning the clamping sleeve 14, a hydraulic motor turns a screw which cooperates with a not shown screw wheel connected with the clamping sleeve 14.
FIG. 2 shows an exhaust pipe which is produced in the bending machine and has bent portions or pipe bends S 1 and S 2, as well as S 3 and S 4 which follow one another. It also has straight intermediate portion L 1, L 2 and L 3, which however up to the length L 1 cannot be used. The pipe is provided at its front end with an extended part 26.
FIG. 3 shows that the clamping device or a clamping jaw holder 18 is provided at its both sides with beams 27 and 27a which extend in direction toward the bending template 16 and connected at their front end with the counterclamping jaw 19 by means of a pivot axle 28. The counterclamping jaw 19 is formed in this embodiment as a rectangular body having four clamping surfaces. The clamping surfaces of the counterclamping jaw have depressions with a semi-circular cross section so as to form clamping surfaces 29, 30, 31 and 32. These clamping surfaces have different spatial shapes. At the same time, their common feature is that they engage a tubular portion to be clamped over the entire clamping length in a semi-circular manner. The clamping jaw 25 arranged on the bending template 16 has three different peripheral grooves 33, 34 and 35 which are also shown in FIG. 4. The clamping jaw 25 is mounted on the bending template 16 by not shown screws so that it cannot displace relative to the bending template. This solution is especially advantageous since in this construction no movement mechanism is required.
As can be seen from FIG. 3, a further clamping jaw 36 is arranged on the clamping jaw 25 opposite to the bending template 16. The clamping jaw 36 has a clamping surface with different radii of their semi-shells. A part 37 has a greater radius of curvature, while a part 38 has a smaller radius of curvature. Thereby the pipe 15 shown in FIG. 2 is clamped by the semicircular part 37 in its end portion 26, while the remaining part with the smaller radius is clamped in the portion 38.
FIG. 4 shows that the clamping jaw 25 with its depressions 33, 34 and 35 cannot engage the respective clamped pipe portion over half of circular surface. It also engages the same in the regions in which the depressions 34 and 35 intersect one another and also in a non-complete manner.
However, in the present invention the situation is not damaging as long as the counterclamping jaw engages the pipe over the angular distance of 180°, or in other words in a semi-shell manner, over the length of the pipe portion to be clamped in a complete manner.
FIG. 5 shows the bending template 16 on which two clamping bodies 25 and 25a are arranged over one another. The clamping body 25 has three different clamping surfaces, while the clamping body 25a has two different clamping surfaces. The clamping bodies 25 and 25a are adjustable in a vertical direction by a hydraulic cylinder-piston unit. A cylinder 36 of the unit is arranged inside the bending template 16, while a piston rod 37 of the unit extends outwardly and has a transverse support 38 connected with the clamping bodies or jaws 25 and 25a. By means of the cylinder-piston unit, it is possible to make selectively operable either the clamping jaw 25, or the clamping jaw 25a by lowering the jaws.
It should be mentioned that the solution shown in FIG. 5 proposes the bending template on which also the counterclamping jaw holder 18 can be provided. In this construction, in deviation from FIG. 3, the clamping surfaces are arranged not on a body which is rotatable about a horizontal axis, but on a body which is displaceable in a vertical plane. It should also be mentioned here that the clamping surfaces arranged over one another are not so favorable as the clamping surfaces arranged in different planes as shown in FIG. 3 and rotatable about the rotary axle 28. In many cases it is possible to use three surfaces, but also it is possible to use five or six surfaces.
As shown in FIG. 6, the bending template 16 illustrated in FIG. 6B and 6C has a clamping jaw 25 with a unitary formation of their clamping surfaces shown in perspective in FIG. 6A. As a result of this, it has a semi-shell 39 with a greater diameter and a semi-shell 40 with a smaller diameter, for example for clamping the expanded pipe end 26 and the following portion of the pipe with a conventional diameter. The counterclamping jaw 19 in correspondence with FIG. 6A shows a shape with which the pipe portion to be clamped is engaged over the angular distance 180° over the length of the pipe portion to be clamped. The clamping jaw 25 arranged on the bending template 16 and shown in FIG. 6C also provides for a complete clamping extending over an angular distance of 180°. However, FIG. 6B shows a complete clamping only for a selected pipe diameter, and not in the clamping portion 39.
FIG. 7 shows the counterclamping jaw 19 which is provided on its clamping side with several clamping surfaces, namely two clamping surfaces. With respect to their semi-shells, they are formed individually and completely. They cooperate with a counterclamping surface which with respect to the length of the counterclamping surface does not completely engage the pipe or in other words over a distance of 180°, as shown for example in the knot point in FIG. 4. For bringing one clamping surface 30 or the other clamping surface 31 in cooperation with the different radii 40 and 39, the counterclamping jaw is displaceably supported in direction identified by the double arrow 41.
It will be understood that each of the elements described above, or two or more together, may also find a useful application in other types of constructions differing from the types described above.
While the invention has been illustrated and described as embodied in a pipe bending machine, it is not intended to be limited to the details shown, since various modifications and structural changes may be made without departing in any way from the spirit of the present invention.
Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can, by applying current knowledge, readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention.
|
A pipe bending machine having a support, a bending template, a clamping jaw displaceable relative to the bending template, a clamping member for a pipe, and clamping bodies each provided in a respective one of the bending templates and the clamping jaw and movable relative to one another to an operative position, one of the clamping bodies havign a clamping surface which is provided with different contours for portions of a pipe to be clamped, while the other of the clamping bodies being provided with a clamping surface having only one contour corresponding to the portion of the pipe to be clamped so that the portion of the pipe to be clamped is engaged over its whole surface at the respective side over an angular distance of 180°.
| 1
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation-in-part of U.S. patent application Ser. No. 12/276,876, filed on Nov. 24, 2008, and entitled “Oil Condition Sensing Methods and Systems.” The disclosure of the above application is incorporated herein by reference in its entirety.
FIELD
[0002] The present disclosure relates to fluid sensors and more particularly to electro-mechanical fluid sensor systems and methods for controlling electro-mechanical fluid sensor systems.
BACKGROUND
[0003] The background description provided herein is for the purpose of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent it is described in this background section, as well as aspects of the description that may not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the present disclosure.
[0004] Diesel motors combust diesel fuel in combustion chambers to generate torque that can be used to propel a vehicle. If water infiltrates the diesel fuel, the lubricity of the diesel fuel may be reduced, leading to increased wear for components of the engine. For example, a fuel delivery system, which delivers the diesel fuel to the combustion chambers, may include tightly fitting components that rely on the lubricating properties of the diesel fuel. For example only, water intermixed with fuel flowing at high velocity may abrade highly polished valve seats and fine nozzle orifices.
[0005] Further, water may contain biological and chemical impurities, which may cause corrosion of engine components. Water infiltration may also have negative effects in engines using other types of fuel, such as gasoline. Various engines may therefore include a water separator that attempts to remove water from the fuel supply.
[0006] Referring now to FIG. 1 , an exemplary engine system including a water separator is shown. A fuel tank 102 provides fuel to a fuel/water separator 104 . The fuel/water separator 104 separates water from the fuel and directs the fuel to an engine 106 . The fuel/water separator 104 includes a bowl 108 in which the separated water collects.
[0007] The bowl 108 may include a valve 110 that can be opened to drain water from the bowl 108 . The bowl 108 may be clear to allow visual inspection of the water level in the bowl 108 . Traditionally, periodic inspection of the bowl 108 is required to ensure a low water level in the bowl 108 . Once the bowl 108 fills with water, operation of the fuel/water separator 104 may be impaired.
[0008] Some systems may include electrodes in the bowl 108 . A voltage potential is applied to the electrodes, and, because water is more conductive than fuel, the presence of water is indicated by a higher current flow between the electrodes. However, over time, electrodes may corrode in the presence of water and other impurities, which adversely affects their electrical conductivity.
SUMMARY
[0009] A sensor system includes a sensor and a control module. The sensor includes an electrically actuated moving member. The sensor is in fluid communication with a reservoir of a separator that separates a first fluid from a fuel. The control module selectively causes current to be supplied to the sensor to actuate the member. The control module measures the current and determines a parameter of the current. The control module identifies one of presence and absence of the first fluid in the reservoir based on the parameter.
[0010] A method includes selectively causing current to be supplied to a sensor to actuate a movable member of the sensor. The sensor is in fluid communication with a reservoir of a separator that separates a first fluid from a fuel. The method also includes measuring the current supplied to the sensor, determining a parameter of the current, and identifying one of presence and absence of the first fluid in the reservoir based on the parameter.
[0011] Further areas of applicability of the present disclosure will become apparent from the detailed description provided hereinafter. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] The present disclosure will become more fully understood from the detailed description and the accompanying drawings, wherein:
[0013] FIG. 1 is a functional block diagram of an exemplary engine system including a water separator according to the prior art;
[0014] FIG. 2 is a functional block diagram of an exemplary engine system including a water separator according to the principles of the present disclosure;
[0015] FIG. 3 is a partial cross sectional view of a bowl and an exemplary implementation of a sensor according to the principles of the present disclosure;
[0016] FIG. 4 is a graphical depiction of three exemplary traces of current of a solenoid according to the principles of the present disclosure;
[0017] FIG. 5 is a functional block diagram of a sensor system including an exemplary implementation of a sensor control module according to the principles of the present disclosure;
[0018] FIG. 6 is a flowchart depicting exemplary steps performed in analyzing a current signal according to the principles of the present disclosure; and
[0019] FIGS. 7A-7C are functional block diagrams of additional sensor systems according to the principles of the present disclosure.
DETAILED DESCRIPTION
[0020] The following description is merely exemplary in nature and is in no way intended to limit the disclosure, its application, or uses. For purposes of clarity, the same reference numbers will be used in the drawings to identify similar elements. As used herein, the phrase at least one of A, B, and C should be construed to mean a logical (A or B or C), using a non-exclusive logical or. It should be understood that steps within a method may be executed in different order without altering the principles of the present disclosure.
[0021] 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.
[0022] Referring now to FIG. 2 , a functional block diagram of an exemplary engine system is presented. The fuel tank 102 provides fuel, such as gasoline or diesel fuel, to a fuel/water separator 120 . The fuel/water separator 120 separates fuel from water, provides fuel to the engine 106 , and directs water into a bowl 122 . The bowl 122 may include a valve 124 , which allows water to be emptied from the bowl 122 .
[0023] For example only, a water line 126 is shown, indicating that water is present below the water line 126 while fuel is present above the water line 126 (assuming that water is denser than the fuel). A sensor 128 may be installed in the bowl 122 to detect the presence of water. An engine control module 130 controls operation of the engine 106 . For example, the engine control module 130 may control actuators (not shown) within the engine 106 to produce a torque as requested by a driver.
[0024] The engine control module 130 may include a sensor control module 140 that controls and receives signals from the sensor 128 . At various times, a diagnostic module 142 commands the sensor control module 140 to take a reading from the sensor 128 . For example only, the diagnostic module 142 may issue this command on a periodic schedule. For example only, the schedule may be altered based on sensed driving habits, such as average engine run time.
[0025] The sensor control module 140 may interpret readings from the sensor 128 to determine whether water is present in the bowl 122 . The level of water that the sensor 128 detects is determined by where in the bowl 122 the sensor 128 is placed. The diagnostic module 142 may generate a visual/audio indicator 144 when water is detected. For example only, the visual/audio indicator 144 may include a check engine light or a digital instrument panel display.
[0026] The diagnostic module 142 may also set a diagnostic trouble code, which may be stored in a diagnostic interface 146 . The diagnostic interface 146 may be queried by diagnostic tools, such as at a dealership or repair facility. The diagnostic interface 146 may record the times during which water is detected, and provide these to the diagnostic tools.
[0027] User input 148 may instruct the diagnostic module 142 to command a new reading from the sensor 128 . The user input 148 , for example only, may include a button. A user may actuate the user input 148 after water has been drained from the bowl 122 . In various implementations, the valve 124 may be controlled by the diagnostic module 142 , such as with electrical or vacuum signals. Control of the valve 124 may also be performed via the diagnostic interface 146 .
[0028] Referring now to FIG. 3 , a partial cross sectional view is presented of the bowl 122 and an exemplary implementation of the sensor 128 . The sensor 128 may be coupled to the bowl 122 via a gasket 160 . A piston 162 rides within a sleeve 164 to pull liquid through an orifice 166 into a chamber 168 . The liquid may be pulled into the chamber 168 through a channel 170 from the bowl 122 .
[0029] In various implementations, the length of the channel 170 may be reduced, and/or the channel 170 may be removed entirely. For example only, the orifice 166 may be defined at the wall of the bowl 122 . The piston 162 is connected to an armature 172 . The armature 172 is biased to a first position by a coil return spring 174 . When a current is applied to windings 176 , the resulting electromagnetic field actuates the armature 172 to a second position in opposition to the return spring 174 .
[0030] As the armature 172 moves from the first position to the second position, the piston 162 presses the fluid from the chamber 168 through the orifice 166 . For fluids with higher viscosities, the fluid is more difficult to push from the chamber 168 through the orifice 166 . This change in viscosity may be evidenced by a change in the electrical characteristics of the sensor 128 , as described in more detail with respect to FIG. 4 .
[0031] Referring now to FIG. 4 , three exemplary traces 202 , 204 , and 206 of the current of a solenoid are shown. Trace 202 corresponds to a low viscosity, trace 204 corresponds to a higher viscosity, and trace 206 corresponds to an infinite viscosity. An infinite, or extremely high, viscosity has the same effect as if the armature of the solenoid were mechanically stuck. Traces 202 and 204 each include a notch in the current. By contrast, trace 206 lacks the notch. For traces similar to trace 206 , the notch time may be considered to be infinite, or set to a maximum amount of time.
[0032] The location of the notch is an indication of the viscosity of the fluid with which the solenoid is interfacing. Because the solenoid piston displaces fluid in front of the piston, hydraulic resistance is caused by the viscous fluid moving through a restrictive flow passage (such as an orifice). This hydraulic resistance exerts a pressure on the face of the piston, which resists armature movement and changes the current response characteristics of the solenoid.
[0033] At a start point 210 , the solenoid is instructed to actuate. This may be initiated by a trigger signal that arrives at the start point 210 . For purposes of illustration, trace 202 will be analyzed. After the start point 210 , the current of trace 202 begins increasing. At a first point 212 , trace 202 transitions from increasing to decreasing. The first point 212 is therefore a local maximum.
[0034] Trace 202 then decreases until a second point 214 , when trace 202 transitions from decreasing back to increasing. The second point 214 is therefore a local minimum. The armature of the solenoid begins moving at the first point 212 and stops moving at the second point 214 . The measured current decreases between the first and second points 212 and 214 because the moving armature creates a back electromotive force (EMF) that opposes the electrical potential.
[0035] The amount of time elapsed between the start point 210 and the second point 214 is referred to as the notch time. The notch time of trace 204 is greater than the notch time of trace 202 , indicating that the solenoid is interfacing with a higher viscosity fluid in trace 204 . The notch time of trace 206 may be reported as a predetermined maximum value. For example, the notch time for trace 206 may be reported as 45 ms.
[0036] Referring now to FIG. 5 , a functional block diagram of a sensor system including an exemplary implementation of the sensor control module 140 is presented. The sensor 128 includes an electrically-operated element that interfaces with fluid. For example only, the sensor 128 may include a solenoid 302 that interfaces with the fluid. Alternatively, the sensor 128 may include a plate that is moved through the fluid by an electric motor. In various implementations, a rotating or translating plate may be less expensive to implement than a solenoid.
[0037] The solenoid 302 may be connected to a power supply 304 . In various implementations, the power supply 304 may be a vehicle battery, which may also provide power to the sensor control module 140 . Current flow from the power supply 304 through the solenoid 302 is regulated by a switch 306 , such as a transistor. In various implementations, the transistor may include an n-channel metal-oxide semiconductor field-effect transistor (MOSFET) having a source (S) terminal, a drain (D) terminal, and a gate (G) terminal.
[0038] The current flowing through the switch 306 may be routed through a shunt resistor 308 before reaching a reference potential, such as ground. The shunt resistor 308 develops a voltage potential proportional to current flow. An amplifier 310 amplifies the voltage potential across the shunt resistor 308 . Alternatively, other current sensing devices, such as a Hall effect sensor, may be used to determine the current flowing through the solenoid 302 . An output of the amplifier 310 may be converted to a digital value by an analog-to-digital (A/D) converter 312 . The digital value is a representation of the current flowing through the solenoid 302 .
[0039] A notch detection module 314 may evaluate the digital signal from the A/D converter 312 to determine the time at which the notch of the solenoid current occurs with respect to a trigger signal. The trigger signal may be generated when the solenoid is instructed to actuate. The trigger signal may be generated by a solenoid drive module 318 . For example only, the notch detection module 314 may initialize a timer in a timer module 316 when the trigger signal is received. The time elapsed in the timer module 316 between the trigger signal arriving and the current notch being detected is the notch time.
[0040] The solenoid drive module 318 may provide the trigger signal to the gate of the switch 306 , thereby allowing current to flow through the solenoid 302 . A notch analysis module 320 may receive an activation signal, such as from the diagnostic module 142 of FIG. 2 . Based on this activation signal, the notch analysis module 320 may instruct the solenoid drive module 318 to produce the trigger signal. The notch analysis module 320 may instruct the solenoid drive module 318 to actuate the solenoid 302 multiple times to circulate fluid and ensure a representative sample is analyzed. In various implementations, the final notch time may be selected, or an average of selected ones of the notch times may be used.
[0041] A voltage measurement module 322 may measure a voltage of the power supply 304 . The notch analysis module 320 may adjust the notch time based on the measured voltage. For example only, a higher voltage from the power supply 304 may be expected to decrease the notch time. The notch analysis module 320 may therefore increase the indicated notch time when the measured voltage is higher.
[0042] Further, viscosity may vary with temperature. Therefore, a temperature measurement module 324 may be implemented. For example only, fluid temperature may be modeled, measured directly, and/or inferred from other temperature measurements, such as engine coolant temperature. The temperature measurement module 324 may receive data from a temperature sensor (not shown), such as a thermocouple, associated with the solenoid 302 . In various implementations, the temperature sensor may be implemented in the sensor 128 .
[0043] Alternatively, temperature readings from other systems may be used. For example only, the temperature measurement module 324 may receive a temperature used by a fuel injection system for fuel injection control. In various implementations, temperature may be estimated based on resistance of the windings in the solenoid 302 . The notch analysis module 320 may normalize the notch time based on temperature. For example only, if viscosity decreases as temperature increases, the notch analysis module 320 may increase the indicated notch time when the measured temperature is higher.
[0044] The notch analysis module 320 may use the normalized notch time to make determinations about the fluid interfacing with the sensor 128 . For example only, a predetermined value may be stored in a storage module 326 . If the normalized notch time is greater than the predetermined value, indicating that viscosity is relatively high, the notch analysis module 320 may report that fuel, instead of water, is present. Conversely, when the normalized notch time is less than or equal to the predetermined value, the notch analysis module 320 may report that water is present at the sensor 128 .
[0045] In various implementations, the storage module 326 may store multiple values to differentiate between water, air, and/or multiple types of fuel. For example only, different types of diesel fuel, including biodiesel, may have different characteristic notch times. The notch analysis module 320 may report the type of fuel detected as well as the presence of water. The values in the storage module 326 may be stored in a lookup table. These values may be determined empirically and/or estimated based on sensor characteristics, such as solenoid geometries, orifice size, and fluid properties.
[0046] Referring now to FIG. 6 , a flowchart depicts exemplary steps performed in analyzing the signal from the A/D converter 312 of FIG. 5 . Control begins in step 402 , where control determines whether the trigger signal has been activated. If so, control continues in step 404 ; otherwise, control remains in step 402 . In step 404 , a timer is started and control continues in step 406 .
[0047] In step 406 , control begins measuring current flowing through the solenoid. Control continues in step 408 , where control begins calculating a moving average of the current. The moving current average may be calculated in order to decrease the false detection of a local maximum or local minimum. In this way, small disturbances in the current signal, such as those due to noise, will not be incorrectly detected as a change in direction of the current.
[0048] For example only, the moving average may be a two-point moving average. The moving average may be calculated as a prior moving average or as a central moving average, which uses data taken after the point being calculated. In addition, the moving average may be a simple moving average or a weighted moving average, and the weighting may be linear or exponential.
[0049] Control continues in step 410 , where control begins calculating a derivative of the moving average. For example only, control may calculate the derivative as the difference between the current moving average value and the previous moving average value divided by the time between the moving average values. Control continues in step 412 , where control determines whether the derivative has decreased below zero. If so, control transfers to step 414 ; otherwise, control transfers to step 416 . For example only, control may transfer to step 414 only when multiple sequential derivatives remain below zero.
[0050] In step 416 , control determines whether the timer is greater than a predetermined maximum time. If so, control transfers to step 418 ; otherwise, control returns to step 412 . In step 414 , control determines whether the derivative has returned above zero after being below zero in step 412 . If so, control transfers to step 420 ; otherwise, control transfers to step 422 .
[0051] As in step 412 , control may evaluate multiple derivatives in step 414 to ensure that the derivative has reliably increased above zero. In step 422 , control determines whether the timer has exceeded the predetermined maximum time. If so, control transfers to step 418 ; otherwise, control returns to step 414 . In step 420 , control reports the timer value as the notch time and control stops. In step 418 , control reports the predetermined maximum time as the notch time and control stops.
[0052] Referring now to FIGS. 7A-7C , the principles of the present disclosure can be implemented in various vehicle systems. For example only, whenever viscosity can be used to differentiate between different fluids, a sensor system as described in the present application can be implemented to measure viscosity. Viscosity may indicate which variety of a desired fluid is present. Additionally, viscosity may indicate presence of an undesired fluid or the absence of the desired fluid. Further, viscosity may indicate when properties of the desired fluid have been compromised.
[0053] For example only, FIG. 7A depicts a system for detecting water in a fuel tank 502 . A sensor 504 is located in the fuel tank 502 , and a sensor control module 506 analyzes readings from the sensor 504 to determine viscosity of the fluid in the fuel tank 502 . If a viscosity indicative of water is measured, a diagnostic module 508 may alert an operator or a mechanic. In addition, remedial action may be performed, such as operating an engine in a reduced power mode or limiting the speed of the engine.
[0054] For example only, FIG. 7B depicts a system for detecting water or glycol in an oil supply, such as an oil sump 522 . A sensor 524 is located in the oil sump 522 , and a sensor control module 526 analyzes readings from the sensor 524 to determine viscosity of the fluid in the oil sump 522 . If a viscosity indicative of water or glycol is measured, a diagnostic module 528 may alert an operator or a mechanic. In addition, remedial action may be performed, such as operating an engine in a reduced power mode or limiting the speed of the engine.
[0055] For example only, FIG. 7C depicts a system for detecting oil in a cooling system component, such as a radiator 542 . A sensor 544 is located in the radiator 542 , and a sensor control module 546 analyzes readings from the sensor 544 to determine viscosity of the fluid in the radiator 542 . If a viscosity indicative of oil is measured, a diagnostic module 548 may alert an operator or a mechanic. In addition, remedial action may be performed, such as operating an engine in a reduced power mode or limiting the speed of the engine.
[0056] The broad teachings of the disclosure can be implemented in a variety of forms. Therefore, while this disclosure includes particular examples, the true scope of the disclosure should not be so limited since other modifications will become apparent to the skilled practitioner upon a study of the drawings, the specification, and the following claims.
|
A sensor system includes a sensor and a control module. The sensor includes an electrically actuated moving member. The sensor is in fluid communication with a reservoir of a separator that separates a first fluid from a fuel. The control module selectively causes current to be supplied to the sensor to actuate the member. The control module measures the current and determines a parameter of the current. The control module identifies one of presence and absence of the first fluid in the reservoir based on the parameter.
| 6
|
BACKGROUND
The invention refers to a mechanical music box consisting of a set of pieces assembled between two identical frame halves and able to play, using analog techniques, one or more selected melodies in which the musical tone is obtained using a variable number of spring pins, which are alternately lifted and released to produce the desired musical notes.
This invention relates, but is not limited to, the type of mechanical musical box used in clockworks and jewelry, snuffboxes, singing birds, stuffed animals, boxes, display units, and various trinkets.
Traditional music box designs and manufacturing techniques require large complex factories or long and delicate assembly procedures using highly qualified staff and do not permit the mass scale production of a music box capable of playing any kind of repetitive tune, for only a few cents per unit.
A relatively simple to manufacture music box is described in Swiss Patent No. CH-586 441. This music box contains a cylinder (4) equipped with teeth (5) to work vibrating pins (3). In one of its embodiments, a spring (20) is placed inside the cylinder to get it to rotate. The music box pieces are placed in a case (1).
Though it works perfectly well, this music box has a number of problems. One problem is that although the case consists of two parts which make it possible to position and hold the music box components, these two parts are not identical. They therefore have to be made using two different molds, resulting in rather high manufacturing cost. Another problem is that the vibrating pins of the music box are integrally formed as either one or two combs. If, during production, one of the pins breaks or cannot be used for some other reason, the entire comb is unusable. A further problem is that the rewinding mechanism is firmly attached to the cylinder. This means that it cannot be attached in other positions, nor can it have a different shape. This music box, therefore, cannot be adapted and modified to different embodiments. Finally, it is impossible to add a power supply shaft from the music box to drive external components. All of these drawbacks indicate that the music box described in Swiss Patent No. CH-586 441 is largely inflexible and cannot be adapted to different uses.
Swiss Patent No. CH-256 248 describes a music box with individual vibrating tabs in place of the vibrating pins integrally formed as a comb, found in conventional music boxes. However, attaching the tabs in this music box is relatively complicated, making assembly expensive.
For the foregoing reasons, there is a need for a music box that can be easily adapted to a variety of uses, play any type of repetitive tune and be manufactured on a mass scale at a lower cost than known music boxes.
SUMMARY OF THE INVENTION
The invention herein solves these problems by providing a mechanical music box wherein the majority of the components making up the mechanical music box are assembled between two identical frame halves.
A primary object of the present invention is to provided a music box including two identical frame halves, that when placed end to end, enclose and support substantially all of the components of the music box, wherein substantially all of the components are supported by radial open mating half bearings located along the median axis of each of the mating frame halves. These features of the invention make it easier to position the components and assemble the music box, and less expensive to manufacture.
The two identical frame halves can be manufactured at low cost by using a single mold for both halves without the need to use lateral or oblique demolding valves, by injecting plastic containing metallic particles. The two frame halves have integrally molded radially open mating half bearings for locating and holding the music box components. The components are assembled in the bearings on the two frame halves and the two frame halves are then placed end to end. As the frame halves are placed end to end, and are joined together by mating tongues and grooves located all around the outer frame, the components are centered and aligned. These principles enable a substantial reduction in the number of parts and a space saving of about 30% with respect to the state of the art.
One or two music rollers with lifting cams are pushed onto cylinders which drive the rollers. The cylinders are supported by a central axis and driven by a spiral spring.
A speed regulation system gear train is located along the frame's median axis providing a new esthetic appearance and a decrease in the effective force of one or more of the spiral springs due to improved spacing of the transmission gears acting in turn to drive the one or more rollers and to stabilize the tempo of the tune, which must produce even tempo music for as long as possible.
A rewinding mechanism contacts the cylinder's main axis and is equipped with a torque limiter to protect the one or two mainsprings from breaking due to excessive rewinding force. The rewinding mechanism is made so that the force required by the mainsprings can be reduced and the drive period increased.
One or two external power supply shafts can be linked to the cylinder so that the main springs drive the cylinders which in turn drive the one or two external power supply shafts to operate objects outside of the music box. The one or two external power supply shafts may be placed alternately in one or two or, where necessary, three openings provided for that purpose on the two frame halves. In this way it is possible to combine the placement of the rewinding mechanism and the one or two power supply shafts in the positions best adapted to the application.
A regulator, centrifugal stabilizer of the musical tempo, contains a rotating system of heads placed on expanding stretch arms. The regulator on the one hand provides an esthetically pleasing animation and on the other, maintains a linear musical tempo over the entire time the mechanism is in motion.
Spring pins are inserted in and attached to the grooves provided in the frame halves. Each spring pin represents one note which can be struck by a lifting cam of the roller with a minimum of operation and is made without needing major refinishing to produce regular musical notes. Each spring pin may also include a mute when a note requires muting.
One or two cases halves attach to the frame halves to enclose the set of components and to form a resonance chamber for the music.
The sum of the advantages offered by the former principle and components make possible (1) a logical and harmonious division of functions, shapes, and tones, (2) a reduction in the number of effective parts and multifunctionality of a number of components, (3) positioning of the rewinding mechanism in three possible positions, protected by a torque limiter, (4) one or two external power supply shafts which can be built with different drive ratios, (5) the absence of screws, dowels, or other holding devices to align or fix the components, and (6) a decrease in the number of required components by placing the spring pins on one side of the speed regulation system.
These and other features, aspects, and advantages of the present invention will become better understood with regard to the following description, appended claims and accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 represents an enlarged cross-sectional front view of the assembled music box taken on line I--I of FIG. 2.
FIG. 2 represents an enlarged cross-sectional side view of the assembled music box taken on line II--II of FIG. 1.
FIG. 3 represents an enlarged cross-sectional side view of an installed spring pin, roller and spring pin lifting cam taken on line II--II of FIG. 1.
FIG. 4 represents in an approximate scale a representative front view of an eighteen spring pin mechanical music box.
FIG. 5 represents an perspective view of the assembled music box with the case cut away.
FIG. 6 represents an perspective view of the music box components assembled on one frame half.
FIG. 7 represents an perspective view of the music box frame half with the tempo regulator components assembled.
FIG. 8 represents an perspective view of a cylinder without the gear for driving external power supply shafts.
FIG. 9 represents an perspective view of a spiral spring assembled on the core.
FIG. 10 represents an perspective view of the roller.
DETAILED DESCRIPTION
FIGS. 1 through 10, without being unique or limited to other possible types, sizes, and variations, represent a mechanical music box having eighteen spring pins (18 notes) which operate on an analog principle. The mechanical music box includes, in approximate order of assembly, two frame halves 1, which, when placed end to end, support and enclose a central axis 2 supporting two cores 3, two spiral springs 4, two cylinders 5, two rollers 6, a rewinding shaft 7, rewinding ring 8, one or two external power supply shafts 9, a large sprocket 10, a medium sprocket 11, a small sprocket 12, a worm gear 13, two wheels regulating the musical tempo 14, and spring pins 15. This whole assembly is enclosed by two case halves 16.
Referring to FIGS. 1, 2 and 7, frame halves 1 support and hold the components in half bearings, slots and grooves 1e-1n formed in the half frames. Each frame also half has grooves 1a and 1b and tongues 1c and 1d. When the frame halves are placed end to end, the frame half tongues 1c and 1d, and grooves 1a and 1b mate with the tongues 1c and 1d, and grooves 1a and 1b of the opposing frame half to align and center the halves and the components. The joined halves support and enclose all of the components 2 through 13.
Referring to FIGS. 1, 6 and 10, central axis 2 is rotatably supported by bearings 1f of frame halves 1. Central axis 2 supports cores 3, one or more spiral springs 4, cylinders 5, and the rollers 6 having lifting cams 6a. Central axis 2 comprises a cylindrical shaft having a sprocket 2a which is engaged by the rewinding shaft 7, and straight "strillures" 2b which engage and drive cores 3.
Referring to FIG. 9, cores 3 have a tubular shaft which slide over and engage the strillures 2b of central axis 2, a central grooved channel 3a which holds the lower part of spiral spring 4, and a radially extending flange 3b which guides and holds cylinder 5.
Referring to FIG. 8 and 10, cylinders 5, support rollers 6, and have grooves 5e for attaching the spiral springs 4. Cylinders 5 further include ring gears 5d that engages sprocket 10 of the musical tempo regulator and ring gears 5c used to drive the external power supply shafts 9 when an external power supply shaft is used. Cylinder 5 forms a hemispherical housing 5b surrounding ring gear 8. Cylinders 5 are freely supported by and rotatable around cores 3.
Referring to FIGS. 8 and 10, the rollers 6 slide onto cylinders 5. Each cylinder 6 has a notch 6c which engages cylinder 5 to align and drive the rollers 6. The rollers 6 have cams 6a arranged to strike the spring pins 15 in a sequence to produce the desired melody. The cams 6a are press formed from the inside of the roller tube 6b.
Referring to FIGS. 8 and 9, the spiral springs 4 disposed inside the cylinders 5 drive the musical instrument and the adaptable external power supply shafts 9. The spiral springs consist of a wound steel coils with hooked ends to wind it and to drive cylinder 5. One end of the spiral spring 4 is attached to central groove channel 3a of core 3 and the other end of the spiral spring 4 is attached to groove 5e in cylinder 5.
Referring to FIGS. 1 and 2, rewinding stem 7 has a winding key 7a connected to its outer end and a rewinding gear 7c at its inner end which drives ring gear 8. The rewinding gear 7c has slanted notching 7b and spherical part 7d propped against central axis 2 to act as a torque limiter.
The ring gear 8, engages the slanted notching 7b of the rewinding gear 7b, and engages and drives sprocket 2a of central axis 2 to tighten the spiral spring 4. Stop 8c is used to inhibit loss of tension on spiral spring 4 by using groove 5e.
External power supply shafts 9 may be used to drive linking parts outside the music box. The external power supply shafts 9 consist of a cylindrical shaft 9a supported by bearing 1k and a sprocket 9b engaging and driven by ring gear 5c of cylinder 5.
Referring to FIGS. 6 and 7, a musical tempo regulator is comprised of a large sprocket 10, a medium sprocket 11, a small sprocket 12, a worm gear 13 and wheels 14. The musical tempo regulator maintains a substantially constant rotational velocity of rollers 6 to maintain an even tempo of the music.
The large sprocket 10 contains two banks of pinions 10b and 10c. Pinion 10b engages ring gear 5d. The large sprocket 10 has two cylindrical bearing surfaces 10a which rotatably engage supporting bearings 1g of the frame halves 1.
The medium sprocket 11 contains two banks of pinions 11b and 11c. Pinion 11b engages pinion 10c. The medium sprocket 11 has two cylindrical bearing surfaces 11a which rotatably engage supporting bearings 1h of the frame halves 1.
The small sprocket 12 contains two banks of pinions 12b and 12c. Pinion 12b engages pinion 11c and pinion 12c engages worm gear 13. The small sprocket 12 has two cylindrical bearing surfaces 12a which rotatably engage supporting bearings 1i of the frame halves 1.
The worm gear 13 is placed perpendicular to the axis of sprocket 12 and is rotatably supported by bearings 1e.
The wheels 14 are affixed to the ends of the cylindrical shaft 13b of worm gear 13. Two pins 13c align the ends and wheels 14. The wheels 14 have stretch arms 14b having weighted heads 14c. The stretch arms 14b with weighted heads 14c extent radially as a result of increase centrifugal forces with increased rotational velocity.
Spring pins 15, each have a back portion 15a, a middle portion 15b, a front portion 15c and a small mute 15d. The spring pins 15 are placed individually in groove halves 1m in frame half 1. The rear part of the grooves In lock the spring pins 15 to prevent longitudinal movement of the spring pins 15 in grove 1m. The spring pins 15 are inserted axially with respect to I--I. The middle portion 15b, front portion 15c and small mute 15d of the spring pins 15 produce the musical tone when the spring pin 15 is lifted and released by the lifting cams 6a as the rollers 6 rotate. The part in front of 15c is used to give the note the desired pitch and may contain a small mute 15d residual resonance at the top of part 15c.
Referring to FIG. 5, case halves 16 slide on sides 1q of frame halves 1 and are soldered or cemented end to end, forming a case which completely encloses all components 1 through 15, with the exception of rewinding shaft 7 and external power supply shafts 9. These two case halves 16 produce the desired resonance and the means of attachment for the various possible applications.
At the state of the art, the distinction is not sufficiently clear for this type of product to be competitive. Even if the degree of technical sophistication has enabled it to achieve lasting fame, we have to abandon traditional manufacturing techniques in favor of innovations.
A relatively simple to manufacture music box is described in Swiss Patent No. CH-586 441. This music box contains a cylinder (4) equipped with teeth (5) to work vibrating pins (3). In one of its embodiments, a spring (20) is placed inside the cylinder to get it to rotate. The music box pieces are placed in a case (1).
Though it works perfectly well, this music box involves a number of problems. The case consists of two parts which make it possible to position and hold the music box parts. However, these two parts are not identical. They therefore have to be made using two different molds. Manufacturing cost is therefore rather high. The music box contains one or two combs [keyboards]. If, during production, one of the pins breaks or cannot be used for some other reason, the entire comb is unusable. The rewinding mechanism is firmly attached to the cylinder. This means that it cannot be attached in other positions, nor can it have a different shape. This music box, therefore, cannot be adapted and modified to different embodiments. Finally, it impossible to add a power source to this music box. All of these drawbacks indicate that the music box described in this document is largely inflexible and cannot be adapted to different uses.
Swiss Patent No. CH-256 248 describes a music box with individual vibrating tabs in place of the vibrating pins on combs found in conventional music boxes. Attaching the tabs in this music box is relatively complicated, making assembly expensive.
The present invention, characterized by Claims 1 through 10, is aimed at solving all of the above problems.
The salient features described above in presenting the invention are primarily characterized by the fact that the majority of the parts making up this mechanical music box are assembled between two identical frame halves.
Placed end to end, these two frame halves enclose the components, by placing them on radial open bearings located on the median axis of the mating surface. This feature, which makes it easier to assemble and hold the components, represents, as will be demonstrated below, the organization of the new product's concept and general structure.
The sum of the advantages offered by the former principle makes possible a logical and harmonious division of functions, shapes, and tones, a reduction in the number of effective parts, multifunctionality of a number of components, positioning of the rewinding mechanism in three possible position, protected by a torque limiter, one or two external power sources which can be built with different drive ratios, the absence of screws, dowels, or other holding devices to align or fix the components, the possibility of different versions, decreasing
|
A clam housed mechanical music box for stuffed toys and other amusement devices having two identical frame halves containing and supporting all of the components of the music box. The music box has cylinders which drive music rollers equipped with lifting cams. The lifting cams actuate spring pins to produce the notes of a tune. The drive mechanism for the cylinders is provided by at least one spiral spring attached at one end to a core attached to the central axis and at the other to the cylinder. The drive mechanism also includes a speed regulating mechanism to maintain a steady music tempo throughout the tune, a winding shaft to wind the spring and external power supply shafts to supply power to objects external to the music box mechanism.
| 6
|
FIELD OF THE INVENTION
[0001] The present invention relates to farm machinery for shredding bales and, more particularly, to a drive system for a bale processor bale manipulator and a bale processor using said drive system.
BACKGROUND
[0002] In the livestock industry, large round and square bales are shredded to feed and bed livestock. One type of bale processor currently in the market includes a flail drum longitudinally mounted for rotation inside a processing chamber. The flail drum is rotated and flails on the drum engage a bale inside the processing chamber, shred the baled material and discharge the shredded material out of the processor. The processors include at least one manipulator for manipulating the bale within the processing chamber to expose different portions of the bale to the flails. The manipulator may be one or more “feed rollers”. The manipulator is typically driven by a hydraulic motor that allows the user to change the speed and direction of rotation of the manipulator. Typically some kind of flow restrictor is used to limit the speed of the manipulator for proper processing.
[0003] High torque may be required to drive the manipulator when large bales are processed or when baled material becomes wound around the manipulator or wedged between the manipulator and the walls of the processor. High torque is often required when frozen bales are being manipulated.
[0004] Low cost hydraulic motors typically have a peak or maximum intermittent hydraulic oil supply pressure allowance dependant on the design parameters of the motor. Torque capabilities of hydraulic motors vary directly with size (displacement) of the motor. However, as the size of the motor increases, low cost commercial motor design often does not provide for proportional increases in torque or pressure capabilities and the pressure allowance is accordingly decreased.
[0005] If a hydraulic motor is used in an application where its maximum output torque is required and the power source (typically a tractor) can provide a peak pressure higher than the pressure allowance of the motor, then a pressure relief system must be used to protect the hydraulic motor from supply pressures exceeding the pressure allowance. Pressure relief systems are inconvenient, costly and limit the torque output of the motor.
[0006] Problems have been encountered with hydraulic motor reliability or operability in some bale processors of the type described and/or a pressure relief system has been required.
SUMMARY
[0007] A bale processor with a processing chamber includes a bale manipulator driven by a hydraulic motor. The hydraulic motor drives a shaft with an axis of rotation offset from the drive shaft of the manipulator. A drive transmission is used to increase the torque supplied to the manipulator from the hydraulic motor, which is rated to operate within the pressure range of the hydraulic feed from a power source.
[0008] In accordance with an aspect of the present invention there is provided a bale processor bale manipulator drive system in a bale processor of the type having a disintegrator and a bale manipulator rotatably mounted in a processing chamber. The drive system includes a hydraulic motor mounted on the bale processor and adapted for receiving, and rated to operate within the pressure range of, the hydraulic feed from a power source and an offset drive transmission connected between the hydraulic motor and the bale manipulator, the drive transmission including torque multipliers having a ratio adapted to increase available torque to the manipulator.
[0009] In accordance with another aspect of the present invention there is provided a bale processor. The bale processor includes a processing chamber, a disintegrator rotatably mounted in the processing chamber and adapted to disintegrate baled crop material, a bale manipulator rotatably mounted in the processing chamber and adapted to manipulate the baled crop material in the processing chamber to expose different parts thereof to the disintegrator and a bale manipulator drive system. The bale manipulator drive system includes a hydraulic motor mounted on the bale processor and adapted for receiving, and rated to operate within the pressure range of, the hydraulic feed from a power source and an offset drive transmission connected between the hydraulic motor and the bale manipulator, the drive transmission including torque multipliers having a predetermined ratio so as to increase available torque to the manipulator.
[0010] In accordance with a further aspect of the present invention there is provided a bale processor bale manipulator drive system kit for use in a bale processor of the type having a disintegrator and a bale manipulator rotatably mounted in a processing chamber. The drive system kit including a mounting plate adapted for mounting on an end wall of the bale processor and for receiving a shaft connected to the bale manipulator, a hydraulic motor mounted on the mounting plate and adapted for receiving, and rated to operate within the pressure range of, the hydraulic feed from a power source and an offset drive transmission adapted for connecting between the hydraulic motor and the bale manipulator, the drive transmission including torque multipliers having a ratio adapted to increase available torque to the manipulator.
[0011] Other aspects and features of the present invention will become apparent to those of ordinary skill in the art upon review of the following description of specific embodiments of the invention in conjunction with the accompanying figures.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] In the figures which illustrate an embodiment exemplary of the invention:
[0013] [0013]FIG. 1 is a front perspective view of a bale processor according to the invention;
[0014] [0014]FIG. 2 is a front perspective view of a bale processor and drive system according to the invention;
[0015] [0015]FIG. 3 is a detailed perspective view the drive system shown in FIG. 2;
[0016] [0016]FIG. 4 is an exploded view of the front of a bale processor according to the invention;
[0017] [0017]FIG. 5 is an exploded view of the rear of a bale processor according to the invention; and
[0018] [0018]FIG. 6 is an exploded view of the drive system of FIG. 3.
DETAILED DESCRIPTION
[0019] [0019]FIG. 1 illustrates an exemplary bale processor 10 showing one embodiment of the present invention.
[0020] The bale processor 10 has a frame structure 12 that includes a hitch plate 14 and a pair of axle supports 16 . The hitch plate 14 is adapted for installation of a hitch (not shown) for connection of the bale processor 10 to a power source, typically a tractor (not shown). The axle supports 16 allow for support of the frame structure 12 on wheels (not shown). The processor 10 includes a processing chamber 18 having a front end wall 22 , a back end wall 24 , a left side wall 26 and a right side wall 28 . In the embodiment shown, the left side wall 26 includes a discharge opening 30 through which processed crop material is discharged.
[0021] In the illustrated embodiment, a disintegrator comprising a flail drum extending the length of the processing chamber 18 is mounted in the bottom of the processing chamber 18 of the bale processor 10 . The flail drum is rotatable about its longitudinal axis such that, in operation, a series of flails pivotally mounted thereon extend to engage and separate the baled material and discharge it from the processing chamber 18 .
[0022] Mounted between the front end wall 22 and the back end wall 24 of the processing chamber 18 is a manipulator, feed roller 38 , having a driven shaft 36 (see FIG. 4). In operation, rotation of the driven shaft 36 results in rotation of the manipulator, and manipulation of baled material (not shown) in the processing chamber 18 . During operation, a bale is supported above the disintegrator on the feed roller 38 and an opposing support means, which may be either passive or driven. In the illustrated embodiment, the manipulator of the bale processor 10 includes two driven feed rollers 38 , 40 (see FIG. 2) and the bale is supported between said rollers. However, the roller 40 need not be driven, and may be a passive support roller as disclosed in applicants co-pending application PCT/CA02/00926. Generally, the manipulator functions to rotate a bale in the processing chamber 18 such that different portions of the bale are exposed to the disintegrator and the choice of the number of drives and required power will depend on the type of bale processor and the operating parameters thereof.
[0023] As discussed, the illustrated embodiment includes two feed rollers. As the feed rollers and associated drive systems are identical, for simplicity, only one feed roller and drive system is described.
[0024] In the embodiment shown, the feed roller 38 extends the length of the processing chamber 18 . The feed roller 38 is rotatable about its longitudinal axis and has manipulating members comprising teeth 42 and flanges 44 extending therefrom.
[0025] The feed roller 38 is mounted to the front end wall 22 by attachment to a feed roller mounting plate 48 . Specifically, the driven shaft 36 extends through a set of bearings 52 that are attached to the feed roller mounting plate 48 and support the feed roller 38 while permitting rotation thereof. The bearings 52 are housed in a cylindrical flange 68 that extends into the processing chamber 18 from the feed roller mounting plate 48 . The specifications for the bearings 52 are selected depending upon the typical load conditions of the feed roller 38 during operation. As shown in FIG. 5, the feed roller 38 is mounted to the back end wall 24 through a further set of bearings housed in a rear feed roller mounting plate.
[0026] The cylindrical flange 68 (see FIG. 3) extends through an aperture 74 in the front end wall 22 into the processing chamber 18 . The aperture 74 may be obround and sized to allow the feed roller mounting plate 48 including cylindrical flange 68 to slide during operation. Four retainer bars 72 on the front end wall 22 of the processing chamber 18 cooperate with four retainer clips 50 to support and maintain the orientation of the feed roller mounting plate 48 on the front end wall 22 . An adjustable stop plate 56 is rotatably secured to the front end wall 22 of the processing chamber 18 . The adjustable stop plate 56 cooperates with a protrusion 66 outstanding from the feed roller mounting plate 48 to limit the downward travel of the feed roller mounting plate 48 and, consequently, the first feed roller 38 .
[0027] A driven sprocket 54 is detachably connected to the end of the driven shaft 36 of the feed roller 38 . Specifically, the driven shaft 36 of the feed roller 38 has a splined connection to the driven sprocket 54 . As will be apparent to a person skilled in the art, there exist many alternatives for this connection including keyed and cross-holed connections.
[0028] A hydraulic motor 46 is mounted on the feed roller mounting plate 48 such that the axis of rotation of a motor shaft 60 (see FIG. 6) is offset from the axis of rotation of the driven shaft 36 . As shown in FIG. 3, a motor mount 62 on the mounting plate 48 houses a drive sprocket 64 and supports the hydraulic motor 46 . The motor mount 62 supports and retains the hydraulic motor 46 stationary during operation, maintaining the motor shaft 60 engaged with the drive sprocket 64 . The feed roller mounting plate 48 includes a drive bearing set 70 to support the motor shaft 60 and to assist the internal motor bearing set (not shown) in absorbing forces on the motor shaft 60 including those forces transverse to the axis of rotation of the motor shaft 60 .
[0029] The hydraulic motor 46 will typically be powered by the hydraulic feed from a tractor. Appropriate hydraulic hoses, fittings and valves (not shown) are used to connect the hydraulic motor 46 to the hydraulic feed. Where, as illustrated, two feed rollers are used to manipulate a bale in the processing chamber 18 , it should be apparent to a person skilled in the art that the two hydraulic motors driving the two feed rollers may be plumbed either in series or in parallel. Rotation of the motor shaft 60 by the hydraulic motor 46 results in rotation of the drive sprocket 64 . In the illustrated embodiment, a continuous chain (not shown) is used to transfer rotation of the drive sprocket 64 to the driven sprocket 54 and driven shaft 36 and, thus, to the feed roller 38 . Preferably, the hydraulic motor 46 is reversible such that the feed roller 38 can rotate in a clockwise or a counter-clockwise direction.
[0030] As will be apparent to a person skilled in the art, transmission of rotational motion from the drive shaft of the hydraulic motor to the driven shaft of the feed roller is not limited to the exemplary sprocket and chain system. Many known mechanisms may be used to perform this task while acting as a torque multiplier. For instance, a pulley and belt system may use a drive pulley mounted to the drive shaft, a larger diameter driven pulley mounted to the driven shaft and a belt to transfer rotation of the drive pulley to rotation of the driven pulley. As a further alternative, a drive spur gear may be mounted to the drive shaft and a larger diameter driven spur gear mounted to the driven shaft. The driven spur gear meshes with the drive spur gear to transfer rotation of the drive spur gear to rotation of the driven spur gear.
[0031] The gear, chain or belt drive system must be sized to have the proper ratios to increase the available torque to the manipulator to a level where bale processing may be efficiently carried out without excessive stalling under the range of typical operating conditions.
[0032] In operation, as the flail drum is rotated, the flails extend radially to engage the baled crop material positioned between the feed roller 38 and the second feed roller 40 , separating some of the baled crop material from the rest of the baled material and discharging the separated material through the discharge opening 30 . As the feed roller 38 is rotated, the teeth 42 and the flanges 44 engage the bale in the processing chamber 18 to rotate the bale thereby exposing different sections of the bale to the flails for disintegration.
[0033] The selection of an appropriate motor and gear ratio will depend on the application of the processor including the peak hydraulic pressure supplied by the power source and the required torque for efficient processing. For instance, economic, commercially available 22.8 cu. in. motors having a sufficiently high pressure allowance (3,250 psi) to reliably operate with power supplied from the hydraulic feed from most tractors are available. However, the torque available through such a motor is around 9,200 lb.-in. which is insufficient for efficient processing of large bales, particularly if they are frozen. A presently affordable motor that is able to deliver the required torque has a 32.7 cu. in. displacement. However, the pressure allowance on commercially viable motors of that size is generally around 2,500 psi, which is lower than the peak hydraulic pressure supplied by many modern tractors (around 3,000 psi). With a 2:1 ratio between the driven sprocket radius and the drive sprocket radius, the torque available from a given hydraulic motor may be doubled through the use of the disclosed drive system. Doubling the torque available through a 22.8 cu. in. motor provides sufficient torque for efficient processing of bales with the processors of the invention. Accordingly, a 22.8 cu. in. motor, is advantageously used as part of a drive system according to the invention having a 2:1 ratio between the drive sprocket and the driven sprocket.
[0034] As will be apparent to a person skilled in the art, through the use of the drive system disclosed herein, a single hydraulic motor may be arranged to drive two feed rollers. In one example of such an arrangement, the motor shaft 60 supports two drive sprockets. Two chains may then be used to transfer rotation of each of the drive sprockets to rotation of driven sprockets attached to each of the feed rollers.
[0035] Other modifications within the ambit of the following claims will be apparent to those skilled in the art and, the invention is accordingly defined by the claims.
|
A bale processor with a processing chamber includes a manipulator driven by a drive system that includes a hydraulic motor. The hydraulic motor of the drive system drives a drive shaft with an axis of rotation offset from a driven shaft of the manipulator. A rotation transmission mechanism allows a higher torque to be applied to the manipulator than may be applied by the hydraulic motor alone and, thereby, leads to improved performance for the bale processor. Additionally, the hydraulic motor may be sized such that the peak allowable pressure of the hydraulic motor is higher than the peak output pressure of the power source used to drive the hydraulic motor.
| 8
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of and claims the benefit and priority to U.S. patent application Ser. No. 11/908,569, filed on Mar. 14, 2008, which is a U.S. National Phase application of PCT International Application Number PCT/DK2006/000152, filed on Mar. 16, 2006, designating the United States of America and published in the English language, which is an International Application of and claims the benefit of priority to Danish Patent Application No. PA 2005 00383, filed on Mar. 16, 2005. The disclosures of the above-referenced applications are hereby expressly incorporated by reference in their entireties
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a tower foundation system for large, heavy and bulky towers such as wind turbine towers and steel chimneys, said system comprising a foundation and a bottom section of a tower, which bottom section is connected to the upper part of the foundation.
The invention relates to tower foundation systems in general. However, in the following a tower foundation system is described in relation to a wind turbine tower.
2. Description of the Related Art
Modern wind turbines tend to get bigger in order to produce more power. The length of the wings may exceed 60 m and the height of the tower may exceed 100 m, thus increasing the load on the foundation tower holding the wind turbine.
Traditional tower foundations consist of a cast gravity foundation element provided with an embedded steel cylinder with a 300-500 mm flange at the bottom of steel cylinder for transferring the load from the steel cylinder to the concrete. A machined flange is arranged on top of the steel cylinder and is prepared for connection to a bottom section of the wind turbine tower. The steel cylinder is traditionally cast into the cast gravity foundation element with reinforcement elements protruding through the steel cylinder. The embedment depth of casting compared to the diameter of the steel cylinder need to have a certain value in order to ensure proper securing of the steel cylinder to the foundation, i.e. sufficient load transfer from the steel cylinder to the foundation.
To ensure that the tower foundation sustains the load and stress from the tower, the steel cylinder is cast deep into the gravity foundation to transfer the load to the foundation. The curing period of the standard concrete is long, and casting of the entire foundation comprising the embedded steel cylinder is complex and time consuming. Thus the costs of the foundation are relatively high compared to the total assembly costs of the wind turbine.
The steel cylinder having a top flange and a large bottom flange requires transportation to the wind turbine erection site, where it is to be embedded into the concrete gravity base. Logistically this is a challenge increasing the costs of the project.
OBJECT OF THE INVENTION
An object of the invention may be reducing transportation costs by eliminating the need for separate transport of the base cylinder to be embedded into the foundation.
Another object of the invention may be reducing tower assembly costs by eliminating the need for separate casting in the base cylinder to be embedded into the foundation.
Another object may be to eliminate costs of two heavy machined flanges and corresponding bolt assemblies, one from the bottom of the tower section and one form the embedded cylinder.
Furthermore, an object of the invention may be to provide a sufficiently durable and reliable method for providing a tower foundation system for large, heavy and bulky towers such as wind turbine towers and steel chimneys.
SUMMARY OF THE INVENTION
The objects of the invention is achieved by a foundation system comprising a circular, oval or polygonal recess ( 34 ) or plinth ( 55 ) in the upper part, that the foundation ( 32 ) is provided with reinforcement elements ( 44 ), which are protruding from the casting material of the foundation into the recess ( 34 ), and that the recess is intended for accommodating an ultra high performance grout ( 42 ) to be filled into the recess ( 34 ) or around the plinth.
The invention has the advantage that a sufficient load transfer is obtained with only a limited embedment depth compared to the diameter of the bottom section of the tower. As example, the ratio between the diameter D of the tower and the embedded depth h of the bottom section of the tower may be as high as 4 or even more. Other representative cross-sectional dimensions than a diameter may be selected if the bottom section of the tower does not have a circular cross-section.
The bottom section of the tower is directly connected to the foundation, thus there is no need to mount the bottom section onto a flange steel cylinder section or the like. This reduces assembly time and costs considerably, as the number of tower assemblies is reduced compared to prior art. By applying the present invention, the assembly between the steel cylinder and the bottom tower section is avoided.
According to an embodiment of the invention the foundation comprises a preferably circular or polygonal recess in the upper part of the foundation, which is prepared for receiving the bottom section of a tower. The bottom section is arranged into the recess, and cast into the foundation by filling the recess with an ultra high performance grout.
By applying the present invention the bottom section of the tower can be arranged directly into the recess of the foundation and then be cast to the foundation, thus it is no longer necessary to apply a separate steel cylinder that needs separate transportation and other separate handling and separate casting to the foundation. This is a great advantage, where transportation of big diameter steel cylinder is carried out by costly special transportation means. Thus, the present invention reduces transportation and other handling considerably.
Also, a ratio between a representative cross-sectional dimension of the bottom of the tower and the intended depth of embedment of the bottom of the tower into the recess of the foundation may be increased to at least 4, possibly at least 6, or even as high as at least 8. Thus, the length of bottom section of the tower being embedded is limited.
Depending on the cross-sectional geometry of the bottoms section of the tower, the representative cross-sectional dimension of the bottom section of the tower is a diameter of a tower having a circular cross-section, a major axis or a minor axis of a tower having an oval cross-section or a diagonal of a tower having a polygonal cross-section.
The bottom section of the tower is cast to the foundation by filling the recess with an ultra high performance grout. The grout hardening period is very short, thus the rest of the tower can be mounted after 24 hours. Furthermore, the grout is self-leveling and self-compacting, which means that there is no need to vibrate the grout to compact the grout etc. Hence, working hours and installation costs are reduced considerably.
The bottom section of the tower is arranged directly into the foundation recess, and thus there is no need to mount the bottom section onto a flange steel cylinder section or the like by means of bolts and nuts. This reduces assembly time and costs considerably, as the number of assemblies of each tower are reduced.
Each tower assembly consists of a great number of bolts and nuts having to be installed and tightened. By reducing the number of assemblies of each tower a great deal of difficult assembly work is avoided. Furthermore, re-torque and maintenance of the bolts and nuts between the steel cylinder and the bottom section is no longer necessary.
By using the ultra high performance grout there is no need for an embedded steel cylinder or the like to be arranged deep within the foundation in to order absorb and distribute the load and stress of the tower to the foundation. This is achieved as the ultra high performance grout, such as Ducorit®, which is much stronger than standard concrete used in prior art. The bottom flange of the embedded steel cylinder can also be reduced due to the relation between the compressive strength of the normal concrete and the ultra high performance grout. Ducorit® is characterized by extreme strength and stiffness, which makes the ultra high performance grout a strong structural component.
The ultra high performance grout is based on a binder consisting of cement and silicate. Simulations and tests show that the properties of the binder provided under the trademark Densit® by the company Densit A/S of Denmark is very suitable as binder in the ultra high performance grout. Densit® is extremely strong and dense.
The ultra high performance grout comprises of 30%-70% cement-based binder, which is mixed with aggregates such as quartz and/or bauxite and/or fibres. According to a preferred embodiment of the invention the ultra high performance grout is Ducorit®.
The main constituent of Ducorit® is a binder Densit® of the company Densit A/S of Denmark. Ducorit® is characterized by extreme strength and stiffness, which is developed during a very short hardening period, 50% of the final compressive strength being developed in 24 hours at 20° C. Usually, the strength gained after 24 hours is sufficient to continue the installation of the wind turbine. This means that all wind turbine supplies can be delivered and erected without interruption. Standard concrete normally needs 28 days to gain the necessary strength. Furthermore, Ducorit® products are pumpable and very easy to handle and cast.
Ducorit® comprises a binder Densit® of the company Densit A/S of Denmark and aggregates such as quartz or bauxite or fibres or any combination of quartz, bauxite and fibres. The aggregates are added to obtain the desired strength. Different Ducorit® varieties are presented in the table below. The differences between the products are the size and the amount of binder and aggregates—such as quartz or bauxite or fibres or any combination of quartz, bauxite and fibres. For instance, the aggregates in S1W consist of quartz aggregates that are smaller than 1 mm.
D4W
S5W
S1W
Mean
Mean
Mean
Compressive strength
210/30,400
130/18,850
110/16,000
[MPa/Psi]
The values presented in the table are mean values based on 75×75 mm cubes.
The ultra high performance grout applied has a compressive strength of between 75 MPa and 300 MPa, preferably of between 100 MPa and 250 MPa, possibly of between 75 MPa and 150 MPa, or possibly of between 150 MPa and 300 MPa. A compressive strength as stated is many times stronger than the compressive strength of the standard concrete used to connect the steel cylinder and the gravity foundation in prior art. It is important to note that the invention is not limited to the products mentioned above. Other ultra high performance grout products can be applied as well.
According to the invention the foundation is provided with reinforcement elements, which are protruding from the casting material of the foundation and upwards out of the casting material of the foundation. Reinforcing elements ensure that the load and stress from the tower are transferred and distributed from the recess of the foundation to the gravity foundation. Hence there is no need for a deep recess running from the upper part to the lower part of the foundation to transfer the load and stress from the tower.
According to an embodiment of the invention the reinforcement elements are arranged in the circumferential around the bottom section of the tower, and where the reinforcement elements are cast into the foundation and/or are cast into the recess of the foundation by the ultra high performance grout. Thus it is possible to construct a strong foundation designed for a particular load. The reinforcement elements are made of a materiel having the appropriate strength, preferably metal such as steel. Other materials such as fibre reinforced plastic materials or ceramic materials may be employed as well.
The objects of the invention is also achieved by a method for providing a tower foundation system, which method comprises the following steps of casting of the foundation with a circular, oval or polygonal recess or plinth in an upper part of the foundation, arranging reinforcing elements protruding from the casting material of the foundation into the recess or protruding around the plinth, hardening of the casting material of the foundation, arranging a bottom section of the tower in the recess or around the plinth, with the reinforcing elements encircling the bottom section or the bottom section encircling the reinforcement elements, casting the bottom section to the foundation by the ultra high performance grout being filled into the recess or being filled around the plinth, and hardening of the ultra high performance grout.
Firstly, the foundation is cast, which foundation according to a preferred embodiment of the invention consists of standard concrete, thus a hardening period is necessary to obtain the desired strength. A bottom section of the tower is subsequently arranged to the upper part of the foundation by a large crane or the like. The bottom section and the foundation are then cast together with the ultra high performance grout. Then follows a relatively short hardening period, which is necessary to build up the strength of the grout, so that the rest of the tower and the wind turbine can be assembled.
The method disclosed makes installation fast and efficient compared to prior art. Large wind turbines are often installed in a “wind turbine farm”, where a great number of wind turbines are located inside a defined area. When erecting wind turbines of a wind turbine farm, the installation costs and the assembly time must be kept to a minimum. By using the method of the present invention it is possible to cast the foundation and erect the towers in a minimum of time. Furthermore, separate transportation of large steel cylinders for the foundation is no longer necessary.
The towers of modern wind turbines are very tall, thus a crane or perhaps even a helicopter is applied to lift the tower sections in place. When erecting and assembling a great number of wind turbines in a wind turbine farm, it is very important to schedule the use of the crane or helicopter in the most efficient way. Usually, the bottom tower section is relatively short but heavy, thus the crane or helicopter must be rigged for lifting the bottom section, whereas the crane or helicopter for the remaining lifts is rigged for high lifts. Therefore it is ideal to erect all the tower bases and subsequently rig the crane for higher lifts, thus preventing long periods of idleness.
According to an embodiment of the invention the tower foundation system comprises a preferably circular, oval or polygonal recess or plinth, which is implemented by the above mentioned method combined with the following steps of the foundation system being cast with reinforcement elements protruding from the casting material of the foundation into the recess or around the plinth, that a bottom section of the tower is arranged into the recess or around the plinth of the tower foundation system, and that the bottom section of the tower is cast into the foundation by filling the recess with or by filling around the plinth the ultra high performance grout so that the ultra high performance grout is cast in the recess or is cast around the plinth along the bottom of the tower and is cast in the recess or is cast around the plinth and furthermore is cast around the reinforcement elements. Firstly, the foundation is cast with a recess in the upper part. Secondly, the bottom section of the tower is arranged into the recess of the upper part of the foundation by a large crane or the like. Finally, the bottom section and the foundation are cast together by filling the recess with the ultra high performance grout.
The foundation is improved considerably by providing reinforcement elements during the casting of the foundation. The reinforcing elements improve the strength of the foundation and ensure transferring and distributing of the load and stress from the tower to the foundation.
According to the method steps according to the invention the reinforcement elements can be arranged and cast in the recess or around the plinth of the foundation and strengthen the foundation, but primarily assisting in transferring stress and load from the tower to the foundation via the ultra high performance grout.
At the end of the bottom section a small flange is fitted to transfer the load to the surrounding material. Compared to traditional embedded cylinders the flange can be much smaller due to the strength of the ultra high performance grout. The tower bottom section is placed into the recess, and the bottom flange is kept at a distance from the bottom of the recess by adjustable brackets to ensure that the ultra high performance grout serves as a cast support base to the bottom flange thus transferring vertical load to the concrete with normal compressive strength.
According to a preferred embodiment of the invention the recess is shaped as a ring grove, which is prepared for receiving a cylindrical bottom section of a tower.
According to another embodiment of the invention a traditional steel cylinder comprising a mounting flange is arranged in the recess of the foundation and fastened by an ultra high performance grout.
Hence the present invention can be applied for easy installation of a traditional steel cylinder. Furthermore, the time spent on installing the cylinder is reduced compared to prior art, as the hardening time of the ultra high performance grout is much shorter than the hardening time of standard concrete.
The above described method and tower foundation system is particularly efficient when applied in connection with a wind turbine tower. However, the method and tower foundation system also applies for other applications such as fixing of chimneys etc.
BRIEF DESCRIPTION OF THE DRAWINGS
In the following the invention is described with reference to the drawings where
FIG. 1 shows a tower foundation system according to prior art;
FIG. 2 shows a tower foundation system according to the present invention;
FIG. 3 shows an alternative embodiment of the tower foundation system; and
FIG. 4 shows an even alternative embodiment of the tower foundation system.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a tower foundation system 2 according to prior art. The tower foundation system comprises of a cast gravity foundation element 4 with an embedded steel cylinder 8 with a 300-500 mm flange 10 at the bottom in order to transfer the load to the concrete. A machined flange 12 is arranged on top of the steel cylinder 8 and is prepared for connection with a corresponding machined flange 14 of bottom section 16 of a wind turbine tower. The steel cylinder 8 is traditionally cast into the cast gravity foundation element 4 . To ensure that the tower foundation sustains the load and stress from the tower, the steel cylinder 8 must be cast deep into the cast gravity foundation element 4 to absorb the load. The bottom section 16 of a wind turbine tower is fastened to the steel cylinder 8 by a great number of bolts 18 .
FIG. 2 shows a tower foundation system 30 according to the present invention. The tower foundation system 30 comprises a cast gravity foundation 32 with a circular recess 34 . A bottom section 36 of a wind turbine tower is arranged in the circular recess 34 of the cast gravity foundation. The circular recess 34 is filled with an ultra high performance grout 42 , such as Ducorit®. The bottom section 36 has a flange end 38 , which interacts with the ultra high performance grout 42 .
The tower foundation system 30 comprises a reinforcement element 44 , which protrudes into the circular recess 34 of the cast gravity foundation 32 . Furthermore, a number of reinforcement elements 46 are arranged around the bottom section 36 in order to transfer and distribute the load and stress from the bottom section 36 to the bottom of the cast gravity foundation 32 .
A flange (not shown) is mounted on top of the bottom section 36 for connection with another tower section (not shown). According to the present invention a tower assembly is avoided between the bottom section 16 and the steel cylinder 8 shown in FIG. 2 .
According to an alternative embodiment of the invention the bottom section 36 is arranged into the circular recess 34 , which is partly filled with the ultra high performance grout (not shown).
FIG. 3 shows an embodiment of the tower foundation system 50 comprising a foundation element 52 and a bottom section 56 of a tower, which is arranged in a circular recess 54 formed by the circular plinth 55 of the concrete base 52 . The figure shows an outside mould 62 that is circumferentially arranged around the plinth 55 . The ultra high performance grout filled into the circular recess 54 , thereby connecting the tower bottom section 56 to the foundation element 52 .
Reinforcement elements 58 are protruding into the recess 54 filled with ultra high performance grout to transfer and distribute the load and stress from the bottom section 56 to the foundation element 52 . Ring reinforcement 60 is cast into the recess 54 .
FIG. 4 shows an embodiment of the tower foundation system 50 also comprising a foundation element 52 and a bottom section 56 of a tower, which is arranged in a circular recess 54 formed by the circular plinth 55 of the concrete base 52 . The figure shows both an outside mould 62 that is circumferentially arranged, and an inside mounted mould 63 substituting the plinth 55 shown in FIG. 3 . The ultra high performance grout filled into the bottom section of the tower and also into the circular recess 54 , thereby connecting the tower bottom section 56 to the foundation element 52 .
Reinforcement elements 58 are protruding into the recess 54 filled with ultra high performance grout to transfer and distribute the load and stress from the bottom section 56 to the foundation element 52 . Ring reinforcement 60 is cast into the recess 54 .
|
The present invention relates to a tower foundation system ( 30 ) comprising a foundation ( 32 ) for a bottom section ( 36 ) of a tower, which bottom section ( 36 ) is to be connected to the upper part of the foundation ( 32 ), wherein the bottom section ( 36 ) is cast into the foundation ( 32 ) with an ultra high performance grout ( 42 ).
| 4
|
RELATED APPLICATIONS
This application is a continuation of U.S. application Ser. No. 08/767,282, filed Dec. 16, 1996 (U.S. Pat. No. 5,866,389) which is a continuation of Ser. No. 06/889,823, filed Jul. 24, 1986 (now abandoned), the contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
This invention relates to using dioxetanes to detect a substance in a sample.
Dioxetanes are compounds having a 4-membered ring in which 2 of the members are oxygen atoms bonded to each other. Dioxetanes can be thermally or photochemically decomposed to form carbonyl products, i.e., ketones or aldehydes. Release of energy in the form of light (i.e., luminescence) accompanies the decompositions.
SUMMARY OF THE INVENTION
In general, the invention features in a first aspect an improvement in an assay method in which a member of a specific binding pair (i.e., two substances which bind specifically to each other) is detected by means of an optically detectable reaction. The improvement includes the reaction, with an enzyme, of
a dioxetane having the formula ##STR2## where T is a substituted (i.e., containing one or more C 1 -C 7 alkyl groups or heteroatom groups, e.g., carbonyl groups) or unsubstituted cycloalkyl (having between 6 and 12 carbon atoms, inclusive, in the ring) or a polycycloalkyl (having 2 or more fused rings, each ring independently having between 5 and 12 carbon atoms, inclusive) group bonded to the 4-membered ring portion of the dioxetane by a spiro linkage; Y is a fluorescent chromophore, (i.e., Y is capable of absorbing energy to form an excited, i.e., higher energy, state, from which it emits light to return to its original energy state); X is H, a straight or branched chain alkyl group (having between 1 and 7 carbon atoms, inclusive, e.g., methyl), straight chain or branched heteroalkyl (having between 1 and 7 carbon atoms, inclusive e.g., methoxy, hydroxyethyl, or hydroxypropyl), aryl (having at least 1 ring, e.g., phenyl), heteroaryl (having at least 1 ring, e.g., pyrrolyl or pyrazolyl), cycloalkyl (having between 3 and 7 carbon atoms, inclusive, in the ring, e.g., cyclohexyl), cycloheteroalkyl (having between 2 and 7 carbon atoms, inclusive, in the ring, e.g., dioxane), aralkyl (having at least 1 ring, e.g., benzyl), or alkaryl (having at least 1 ring, e.g., tolyl), or an enzyme-cleavable group, i.e., a group having a bond which can be cleaved by an enzyme to yield an electron-rich moiety bonded to the dioxetane, e.g., phosphate, where a phosphorus-oxygen bond can be cleaved by an enzyme, e.g., acid phosphatase or alkaline phosphatase to yield a negatively charged oxygen bonded to the dioxetane; and Z is H, OH, or an enzyme-cleavable group (as defined above), provided that at least one of X or Z must be an enzyme-cleavable group,
so that the enzyme cleaves the enzyme-cleavable group to form a negatively charged substituent (e.g., an oxygen anion) bonded to the dioxetane, the negatively charged substituent causing the dioxetane to decompose to form a luminescent substance (i.e., a substance that emits energy in the form of light) that includes group Y. The luminescent substance is detected as an indication of the presence of the first substance. By measuring the intensity of luminescence, the concentration of the first substance can be determined.
In preferred embodiments, one or more of groups T, X, or Y further include a solubilizing substituent, e.g., carboxylic acid, sulfonic acid, or quaternary amino salt; group T of the dioxetane is a polycycloalkyl group, preferably adamantyl; the enzyme-cleavable group includes phosphate; and the enzyme includes phosphatase.
The invention also features a kit for detecting a first substance in a sample.
In a second aspect, the invention features a method of detecting an enzyme in a sample. The method involves contacting the sample with the above-described dioxetane in which group Z is capable of being cleaved by the enzyme being detected. The enzyme cleaves group Z to form a negatively charged substituent (e.g., an oxygen anion) bonded to the dioxetane. This substituent destabilizes the dioxetane, thereby causing the dioxetane to decompose to form a luminescent substance that includes group Y of the dioxetane. The luminescent substance is detected as an indication of the presence of the enzyme. By measuring the intensity of luminescence, the concentration of the enzyme can also be determined.
The invention provides a simple, very sensitive method for detecting substances in samples, e.g., biological samples, and is particularly useful for substances present in low concentrations. Because dioxetane decomposition serves as the excitation energy source for chromophore Y, an external excitation energy source, e.g., light, is not necessary. In addition, because the dioxetane molecules are already in the proper oxidation state for decomposition, it is not necessary to add external oxidants, e.g., H 2 O 2 or O 2 . Enzyme-triggered decomposition allows for high sensitivity because one enzyme molecule can cause many dioxetane molecules to luminesce, thus creating an amplification effect. Moreover, the wavelength (or energy) of emission and the quantum yields of luminescence can be varied according to the choice of the Y substituent of the dioxetane (as used herein, "quantum yield" refers to the number of photons emitted from the luminescent product per number of moles of dioxetane decomposed). In addition, through appropriate modifications of the T, X, and Y groups of the dioxetane, the solubility of the dioxetane and the kinetics of dioxetane decomposition can be varied. The dioxetanes can also be attached to a variety of molecules, e.g., proteins or haptens, or immobilization substrates, e.g., polymer membranes, or included as a side group in a homopolymer or copolymer.
Other features and advantages of the invention will be apparent from the following description of the preferred embodiments thereof, and from the claims.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
We now describe the structure, synthesis, and use of preferred embodiments of the invention.
Structure
The invention employs dioxetanes having the structure recited in the Summary of the Invention, above. The purpose of group T is to stabilize the dioxetane, i.e., to prevent the dioxetane from decomposing before the enzyme-cleavable group Z is cleaved. Large, bulky, sterically hindered molecules, e.g., fused polycyclic molecules, are the most effective. stabilizers. In addition, T preferably contains only C--C and C--H single bonds. The most preferred molecule is an adamantyl group consisting of 3 fused cyclohexyl rings. The adamantyl group is bonded to the 4-membered ring portion of the dioxetane through a spiro linkage.
Group Y is a fluorescent chromophore bonded to enzyme-cleavable group Z. Y becomes luminescent when an enzyme cleaves group Z, thereby creating an electron-rich moiety which destabilizes the dioxetane, causing the dioxetane to decompose. Decomposition produces 2 individual ketones, one of which contains group T, and the other of which contains groups X, Y, and Z; the energy released from dioxetane decomposition causes the Y group of the latter ketone to luminesce (if group X is H, an aldehyde is produced).
The excited state energy of chromophore Y (i.e., the energy chromophore Y must possess in order to emit light) is preferably less than the excited state energy of the ketone containing group T in order to confine luminescence to group Y. For example, when T is adamantyl, the excited state energy of chromophore Y is preferably less than the excited state energy of spiroadamantanone.
Any chromophore Y can be used according to the invention. In general, it is desirable to use a chromophore which maximizes the quantum yield in order to increase sensitivity.
Examples of suitable chromophores include the following:
1) anthracene and anthracene derivatives, e.g., 9, 10-diphenylanthracene, 9-methylanthracene, 9-anthracene carboxaldehyde, anthrylalcohols and 9-phenylanthracene;
2) rhodamine and rhodamine derivatives, e.g., rhodols, tetramethyl rhodamine, tetraethyl rhodamine, diphenyldimethyl rhodamine, diphenyldiethyl rhodamine, and dinaphthyl rhodamine;
3) fluorescein and fluorescein derivatives, e.g., 5-iodoacetamido fluorescein, 6-iodoacetamido fluorescein, and fluorescein-5-maleimide;
4) eosin and eosin derivatives, e.g., hydroxy eosins, eosin-5-iodoacetamide, and eosin-5-maleimide;
5) coumarin and coumarin derivatives, e.g., 7-dialkylamino-4-methylcoumarin, 4-bromomethyl-7-methoxycoumarin, and 4-bromomethyl-7-hydroxy coumarin;
6) erythrosin and erythrosin derivatives, e.g., hydroxy erythrosins, erythrosin-5-iodoacetamide and erythrosin-5-maleimide;
7) aciridine and aciridine derivatives, e.g., hydroxy aciridines and 9-methyl aciridine;
8) pyrene and pyrene derivatives, e.g., N-(1-pyrene) iodoacetamide, hydroxy pyrenes, and 1-pyrenemethyl iodoacetate;
9) stilbene and stilbene derivatives, e.g., 6,6'-dibromostilbene and hydroxy stilbenes;
10) naphthalene and naphthalene derivatives, e.g., 5-dimethylamino naphthalene-1-sulfonic acid and hydroxy naphthalene;
11) nitrobenzoxadiazoles and nitrobenzoxadiazole derivatives, e.g., hydroxy nitrobenzoxadiazoles, 4-chloro-7-nitrobenz-2-oxa-1,3-diazole, 2-(7-nitrobenz-2-oxa-1,3-diazol-4-yl) methylaminoacetaldehyde, and 6-(7-nitrobenz-2-oxa-1,3-diazol-4-yl-aminohexanoic acid;
12) quinoline and quinoline derivatives, e.g., 6-hydroxyquinoline and 6-aminoquinoline;
13) acridine and acridine derivatives, e.g., N-methylacridine and N-phenylacridine;
14) acidoacridine and acidoacridine derivatives, e.g., 9-methylacidoacridine and hydroxy-9-methylacidoacridine;
15) carbazole and carbazole derivatives, e.g., N-methylcarbazole and hydroxy-N-methylcarbazole;
16) fluorescent cyanines, e.g., DCM (a laser dye), hydroxy cyanines, 1,6-diphenyl-1,3,5-hexatriene, 1-(4-dimethyl aminophenyl)-6-phenylhexatriene, and the corresponding 1,3-butadienes;
17) carbocyanine and carbocyanine derivatives, e.g., phenylcarbocyanine and hydroxy carbocyanines;
18) pyridinium salts, e.g., 4(4-dialkyl diamino styryl) N-methyl pyridinium iodate and hydroxy-substituted pyridinium salts;
19) oxonols; and
20) resorofins and hydroxy resorofins.
The most preferred chromophores are hydroxy derivatives of anthracene or naphthalene; the hydroxy group facilitates bonding to group Z.
Group Z is bonded to chromophore Y through an enzyme-cleavable bond. Contact with the appropriate enzyme cleaves the enzyme-cleavable bond, yielding an electron-rich moiety bonded to chromophore Y; this moiety initiates the decomposition of the dioxetane into 2 individual ketones, or into a ketone and an aldehyde if group X is H. Examples of electron-rich moieties include oxygen, sulfur, and amine or amido anions. The most preferred moiety is an oxygen anion.
Examples of suitable Z groups, and the enzymes specific to these groups, are given below in Table 1; an arrow denotes the enzyme-cleavable bond. The most preferred group is a phosphate ester, which is cleaved by alkaline or acid phosphatase enzymes.
TABLE 1__________________________________________________________________________Group Z Enzyme__________________________________________________________________________1) ##STR3## alkaline and acid phosphatases phosphate ester2) ##STR4## esterases acetate ester3) ##STR5## decarboxylases carboxyl4) ##STR6## phospholipase D 1-phospho-2,3-diacyl glycerides5) ##STR7## β-xylosidase β-D-xyloside6) ##STR8## β-D-fucosidase β-D-fucoside7) ##STR9## thioglucosidase 1-thio-D-glucoside8) ##STR10## ATPase adenosine triphosphate analogs9) ##STR11## ADPase adenosine diphosphate analogs10) ##STR12## 5' nucleotidase AMP analogs11) ##STR13## β-D-galactosidase β-D-galactoside12) ##STR14## α-D-galactosidase α-D-galactoside13) ##STR15## α-D-glucosidase α-D-glucoside14) ##STR16## β-D-glucosidase β-D-glucoside15) ##STR17## α-D-mannosidase α-D-mannoside16) ##STR18## β-D-mannosidase β-D-mannoside17) ##STR19## β-D-fructofuranosidase β-D-fructofuranoside18) ##STR20## β-D-glucosiduronase β-D-glucosiduronate19) ##STR21## trypsin p-toluenesulfonyl-L-arginine dye ester20) ##STR22## trypsin p-toluenesulfonyl-L- arginine dye amide__________________________________________________________________________
Suitable X groups are described in the Summary of the Invention, above. Preferably, X contains one or more solubilizing substituents, i.e., substituents which enhance the solubility of the dioxetane in aqueous solution. Examples of solubilizing substituents include carboxylic acids, e.g., acetic acid; sulfonic acids, e.g., methanesulfonic acid; and quaternary amino salts, e.g., ammonium bromide; the most preferred solubilizing substituent is methane-or ethanesulfonic acid.
Preferably, the enzyme which cleaves group Z is covalently bonded to a substance having a specific affinity for the substance being detected. Examples of specific affinity substances include antibodies, e.g., anti-hCG, where the substance being detected is an antigen, e.g., hCG; antigens, e.g., hCG, where the substance being detected is an antibody, e.g., anti-hCG; or a probe capable of binding to all or a portion of a nucleic acid, e.g., DNA or RNA, being detected. Bonding is preferably through an amide bond.
Synthesis
In general, the dioxetanes of the invention are synthesized in two steps. The first step involves synthesizing an appropriately substituted olefin having the formula ##STR23## where T, X, Y, and Z are as described above. These olefins are preferably synthesized using the Wittig reaction, in which a ketone containing the T group is reacted with a phosphorus ylide (preferably based on triphenylphosphine) containing the X, Y, and Z groups, as follows: ##STR24## The reaction is preferably carried out at -78° C. in an ethereal solvent, e.g., tetrahydrofuran (THF).
The phosphorus ylide is prepared by reacting triphenyl phosphine with a halogenated compound containing the X, Y, and Z groups in the presence of base; examples of preferred bases include n-butyllithium, sodium amide, sodium hydride, and sodium alkoxide; the most preferred base is n-butyllithium. The reaction sequence is as follows: ##STR25##
where Q is a halogen, e.g., Cl, Br, or I. The preferred halogen is Br. The reaction is preferably carried out at -78° C. in THF.
The olefin where T is adamantyl (Ad), X is methoxy (OCH 3 ), Y is anthracene (An), and Z is phosphate (PO 4 ) can be synthesized as follows. ##STR26## is phosphorylated by treating it with the product of phosphorus acid reacted in the presence of HgCl 2 with N-methylimidazole; the net result is to replace the hydroxyl group of An with a phosphate group. The phosphorylated product is then reacted with triphenylphosphine at -78° C. in THF to form the phosphorus ylide having the formula ##STR27## The reaction is conducted in a dry Ar atmosphere. Spiroadamantanone (Ad═O) is then added to the solution containing the ylide, while maintaining the temperature at -78° C., to form the olefin having the formula ##STR28## The olefin is then purified using conventional chromatography methods.
The second step in the synthesis of the dioxetanes involves converting the olefin described above to the dioxetane. Preferably, the conversion is effected photochemically by treating the olefin with singlet oxygen ( 1 O 2 ) in the presence of light. 1 O 2 adds across the double bond to form the dioxetane as follows: ##STR29## The reaction is preferably carried out at -78° C. in a halogenated solvent, e.g., methylene chloride. 1 O 2 is generated using a photosensitizer. Examples of photosensitizers include polymer-bound Rose Bengal (commercially known as Sensitox I and available from Hydron Laboratories, New Brunswick, N.J.) and methylene blue (a well-known dye and pH indicator). The most preferred sensitizer is Rose Bengal.
The synthesis of the dioxetane having the formula follows. ##STR30##
The olefin having the formula ##STR31## is dissolved in methylene chloride, and the solution is placed in a 2-cm 2 pyrex tube equipped with a glass paddle; the paddle is driven from above by an attached, glass enclosed, bar magnet. The solution is cooled to -78° C. and 1 g of polymer-bound Rose Bengal is added with stirring. Oxygen is then passed over the surface of the agitated solution while the reaction tube is exposed to light from a 500 W tungsten-halogen lamp (GE Q500 C1) equipped with a UV-cut off filter (Corning 3060: transmission at 365 nm=0.5%). Thin layer chromatography (tlc) is used to monitor the disappearance of the olefin and the concurrent appearance of the dioxetane. After the reaction is complete (as indicated by tic), the solvent is removed and the dioxetane is isolated.
Use
A wide variety of assays exist which use visually detectable means to determine the presence or concentration of a particular substance in a sample. The above-described dioxetanes can be used in any of these assays. Examples of such assays include immunoassays to detect antibodies or antigens, e.g., a or β-hCG; enzyme assays; chemical assays to detect, e.g., potassium or sodium ions; and nucleic acid assays to detect, e.g., viruses (e.g., HTLV III or cytomegalovirus, or bacteria (e.g., E. Coli)).
When the detectable substance is an antibody, antigen, or nucleic acid, the enzyme capable of cleaving group Z of the dioxetane is preferably bonded to a substance having a specific affinity for the detectable substance (i.e., a substance that binds specifically to the detectable substance), e.g., an antigen, antibody, or nucleic acid probe, respectively. Conventional methods, e.g., carbodiimide coupling, are used to bond the enzyme to the specific affinity substance; bonding is preferably through an amide linkage.
In general, assays are performed as follows. A sample suspected of containing a detectable substance is contacted with a buffered solution containing an enzyme bonded to a substance having a specific affinity for the detectable substance. The resulting solution is incubated to allow the detectable substance to bind to the specific affinity portion of the specific affinity-enzyme compound. Excess specific affinity-enzyme compound is then washed away, and a dioxetane having a group Z that is cleavable by the enzyme portion of the specific affinity-enzyme compound is added. The enzyme cleaves group Z, causing the dioxetane to decompose into 2 ketones (or an aldehyde and a ketone when group X is H); chromophore Y bonded to one of the ketones is thus excited and luminesces. Luminescence is detected using, e.g., a cuvette or camera luminometer, as an indication of the presence of the detectable substance in the sample. Luminescence intensity is measured to determine the concentration of the substance.
When the detectable substance is an enzyme, a specific affinity substance is not necessary. Instead, a dioxetane having a Z group that is cleavable by the enzyme being detected is used. Therefore, an assay for the enzyme involves adding the dioxetane to the enzyme-containing sample, and detecting the resulting luminescence as an indication of the presence and the concentration of the enzyme.
Examples of specific assays follow.
A. Assay for Human IgG
A 96-well microtiter plate is coated with sheep anti-human IgG (F(ab) 2 fragment specific). A serum sample containing human IgG is then added to the wells, and the wells are incubated for 1 hr. at room temperature. Following the incubation period, the serum sample is removed from the wells, and the wells are washed four times with an aqueous buffer solution containing 0.15M NaCl, 0.01M phosphate, and 0.1% bovine serum albumin (pH 7.4).
Alkaline phosphatase bonded to anti-human IgG is added to each well, and the wells are incubated for 1 hr. The wells are then washed four times with the above buffer solution, and a buffer solution of a phosphate-containing dioxetane is added.. The resulting luminescence caused by enzymatic degradation of the dioxetane is detected in a luminometer, or with photographic film in a camera luminometer.
B. Assay for hCG
Rabbit anti-α hCG is adsorbed onto a nylon-mesh membrane. A sample solution containing hCG, e.g., urine from a pregnant woman, is blotted through the membrane, after which the membrane is washed with 1 ml of a buffer solution containing 0.15M NaCl, 0.01M phosphate, and 0.1% bovine serum albumin (pH 7.4).
Alkaline phosphatase-labelled anti-β-hCG is added to the membrane, and the membrane is washed again with 2 ml of the above buffer solution. The membrane is then placed in the cuvette of a luminometer or into a camera luminometer, and contacted with a phosphate-containing dioxetane. The luminescence resulting from enzymatic degradation of the dioxetane is then detected.
C. Assay for Serum Alkaline Phosphatase
2.7 ml of an aqueous buffer solution containing 0.84M 2-methyl-2-aminopropanol is placed in a 12×75 mm pyrex test tube, and 0.1 ml of a serum sample containing alkaline phosphatase added. The solution is then equilibrated to 30° C. 0.2 ml of a phosphate-containing dioxetane is added, and the test tube immediately placed in a luminometer to record the resulting luminescence. The level of light emission will be proportional to the rate of alkaline phosphatase activity.
D. Nucleic Acid Hybridization Assay
A sample of cerebrospinal fluid (CSF) suspected of containing cytomegalovirus is collected and placed on a nitrocellulose membrane. The sample is then chemically treated with urea or guanidinium isothiocyanate to break the cell walls and to degrade all cellular components except the viral DNA. The strands of the viral DNA thus produced are separated and attached to the nitrocellulose filter. A DNA probe specific to the viral DNA and labelled with alkaline phosphatase is then applied to the filter; the probe hybridizes with the complementary viral DNA strands. After hybridization, the filter is washed with an aqueous buffer solution containing 0.2 M NaCl and 0.1 mM Tris-HCl (pH=8.0) to remove excess probe molecules. A phosphate-containing dioxetane is added and the resulting luminescence from the enzymatic degradation of the dioxetane is measured in a luminometer or detected with photographic film.
Other embodiments are within the following claims.
For example, the enzyme-cleavable group Z can be bonded to group X of the dioxetane, instead of group Y. The specific affinity substance can be bonded to the dioxetane through groups X, Y, or T (preferably group X), instead of the enzyme. In this case, the group to which the specific affinity substance is bonded is provided with, e.g., a carboxylic acid, amino, or maleimide substituent to facilitate bonding.
Groups X, Y, or T of the dioxetane can be bonded to a polymerizable group, e.g., a vinyl group, which can be polymerized to form a homopolymer or copolymer.
Groups X, Y, or T of the dioxetane can be bonded to, e.g., membranes, films, beads, or polymers for use in immuno- or nucleic acid assays. The groups are provided with, e.g., carboxylic acid, amino, or maleimide substituents to facilitate bonding.
Groups X, Y, or T of the dioxetane can contain substituents which enhance the kinetics of the dioxetane enzymatic degradation, e.g., electron-rich moieties (e.g., methoxy).
Groups Y and T of the dioxetane, as well as group X, can contain solubilizing substituents.
Appropriately substituted dioxetanes can be synthesized chemically, as well as photochemically. For example, the olefin prepared from the Wittig reaction can be epoxidized using a peracid, e.g., p-nitroperbenzoic acid. The epoxidized olefin can then be converted to the dioxetane by treatment with an ammonium salt, e.g., tetramethylammonium hydroxide.
Another example of a chemical synthesis involves converting the olefin prepared from the Wittig reaction to a 1,2 bromohydroperoxide by reacting the olefin with H 2 O 2 and dibromantin (1,3-dibromo-5,5-dimethyl hydantoin). Treatment of the 1,2-bromohydroperoxide with base, e.g., OH or silver salts, e.g., silver bromide, forms the dioxetane.
Olefin precursors for the dioxetane can be synthesized by reacting a ketone with a perester in the presence of TiCl 3 and lithium aluminum hydride (LAH). For example, to synthesize an olefin where T is adamantyl (Ad), X is methoxy (OCH 3 ), Y is anthracene (An), and Z is phosphate (PO 4 ), the following reaction sequence is used: ##STR32##
To phosphorylate chromophore Y, e.g., anthracene, a hydroxyl derivative of the chromophore, e.g., hydroxy anthracene, can be reacted with a cyclic acyl phosphate having the following formula: ##STR33## The reaction product is then hydrolyzed with water to yield the phosphorylated chromophore. The cyclic acyl phosphate is prepared by reacting 2,2,2-trimethoxy-4,5-dimethyl-1,3-dioxaphospholene with phosgene at 0° C., following by heating at 120° C. for 2 hr.
|
A kit for detecting a first substance in a sample comprising a dioxetane having the formula: ##STR1## wherein T is a cycloalkyl or polycycloalkyl group bonded to the 4-membered ring portion of the dioxetane by a spiro linkage; Y is a fluorescent chromophore; X is H, alkyl, aryl, aralkyl, alkaryl, heteroalkyl, heteroaryl, cycloalkyl, cycloheteroalkyl, or an enzyme-cleavable group; and Z is H or an enzyme-cleavable group, provided that at least one of X or Z must be an enzyme-cleavable group; and an enzyme which cleaves the enzyme-cleavable group of the dioxetane creating an electron-rich moiety which destabilizes the dioxetane, causing it to decompose into two ketones, one ketone comprising the moiety T, and the other ketone comprising moieties X, Y and a portion of Z. The energy released by decomposition causes the moiety Y to luminesce.
| 6
|
REFERENCE DATA
This application is a continuation of international PCT application PCT/CH03/00063 (WO03/065130) filed on Jan. 27, 2003, claiming priority of European patent application EP02405063.5 filed on Feb. 1, 2002, the contents whereof are hereby incorporated.
FIELD OF THE INVENTION
The present invention concerns a device comprising a usual clock movement and a chronograph module according to the preamble of the independent claim 1 .
DESCRIPTION OF RELATED ART
The market of chronograph watches equipped with a device of this kind has developed considerably during the past years, in particular in the up-market segment. However, a very large proportion of such watches comprise a chronograph plate (hereafter called indifferently chronograph part, module or movement) having a quartz oscillator, whilst a certain clientele feels increasingly attracted to mechanical chronograph watches. With the latter, however, and for reasons that will be explained below, the one skilled in the art encounters notably a problem as regards the precision (also called resolution) of reading.
Wrist-watches whose case holds a chronograph module or movement equipped with a quartz oscillator enable the wearer to perform measurements of a precision that depends on the type of display, namely on the order of the tenth or of the hundredth of second, according to whether this display is analog or digital respectively.
CH-667,771 describes a chronograph watch comprising a common central clock movement driving the hour, minute and seconds hands and an autonomous chronograph movement presenting a timekeeper and at least one indicator driven by an electric motor. The organs of the chronograph movement are arranged at the periphery of the usual movement or of the base movement. Each movement comprises its own regulator oscillating at the same frequency as the other. The chronograph movement is provided with an independent case in the shape of a bell covering the basic clock movement and encircling the latter. The two movements are connected by means of a plate interposed between them.
This construction aims at making an electric chronograph watch at low cost. On the other hand, the precision remains very questionable, the chronograph hand beating the fifth of second (which corresponds to an oscillator at 18,000 oscillations per hour). Furthermore, this document does not supply any teachings to the one skilled in the art as to the arrangement of the organs of the chronograph module or movement, supposing this module were mechanical, nor as to the cooperation between a module of this type and the usual basic clock movement.
Yet, this arrangement and cooperation gives rise to complex problems as regards reliability and execution both on the technical and on the aesthetic levels—which are not at all resolved by using a quartz chronograph but merely avoided by being circumvented—to a point where the one skilled in the art has always been dissuaded from contemplating said arrangement and said cooperation and a fortiori from assigning himself the task of realizing them.
In fact, the measurement precision of mechanical chronographs currently available on the market is, for the most part, on the order of 0.125 seconds, the corresponding balance oscillating at 28,000 oscillations per hour, and, more rarely, for certain other, considerably more expensive mechanical chronographs whose balance oscillates at 36,000 oscillations per hour, on the order of 0.1 seconds. This measurement precision cannot be increased with the mechanical chronographs having a common time base for the clock part and the chronograph part, for several reasons. The use for the clock part of a balance oscillating at a greater frequency would modify the unwinding speed of the barrel spring and would diminish the movement's power-reserve time. Furthermore, an ensemble comprising an escape wheel, pallets, an impulse-pin and a balance pivot, that would be subjected continuously to such service conditions, would show after a couple of months already considerable wear that would inevitably cause an irreversible alteration of the good running of the movement. It must also be stressed that at a high frequency, the energy transmission from the barrel to the sprung balance through the wheelwork and the escapement poses, in continuous use, problems whose solutions would most probably imply the use of complex means that would nevertheless still remain chancy. Thus, by way of example, a balance oscillating at a high frequency has a lower amplitude than the same balance oscillating at a lower frequency. Therefore, it will be more sensitive to variations of the barrel spring's driving torque and will offer running stability only during the period where the variation curve of said driving torque of the spring is linear.
Further to these difficulties are those raised by the questions of cost and aesthetics. On the one hand, it is known that a horological piece and in particular a wrist-watch housing a device comprising a basic clock movement and a fully mechanical chronograph movement is in principle classified in the top of the range. Its price is thus high whilst the precision of its chronograph movement is low and does not even achieve that of a low-market digital display quartz chronograph movement. On the other hand, the making of a horological piece housing a double movement, clock and chronograph, both mechanical, conceivably confronts the clockmaker with a delicate problem of space requirement or volume of the piece, a problem that in the absence of a solution will result in wanting aesthetics likely to compromise the commercial success of the watch. One solution that springs to mind would consist in miniaturizing the organs composing the mechanical chronograph. But although it would serve the aesthetic aspect, it would go against the aim of cost-effectiveness and would certainly raise major technical difficulties. Choosing and applying this solution would therefore not be without technical and commercial risks. These risks seem sufficiently dissuasive to invite the one skilled in the art to conceive and investigate other paths in order to realize the device with a quality to price ratio that is as advantageous as possible.
It is one aim of the invention to propose a device that palliates the inconvenience of lack of precision while ensuring furthermore a truly reliable reading whatever the characteristic of the chosen regulator, and thus of the expected precision, and excluding all aforementioned disturbances on the clock part of the device's movements.
BRIEF SUMMARY OF THE INVENTION
This aim is achieved with the means described in the independent claim 1 , the dependent claims relating to means permitting preferred embodiments of the invention, furthermore at low cost, in keeping with the aforementioned quality-price ratio.
Tests performed on inventive prototypes equipped with a chronograph whose balance oscillated at 360,000 oscillations per hour made it possible to ascertain that a precision on the order of the hundredth of second was ensured even in continuous use during at least thirty minutes. In other words, the device according to the invention renders possible the making of a top-of-the-range horological piece that is truly fully mechanical, and whose chronograph precision bears comparison with a high-quality quartz chronograph.
BRIEF DESCRIPTION OF THE DRAWINGS
An embodiment of the device will be described in detail hereafter, by way of a non-limiting example, supporting the attached drawings, in which:
FIG. 1 shows a top view of a horological piece in the form of a wrist-watch incorporating a device according to the invention,
FIG. 2 shows a perspective view of the device in non-assembled state,
FIG. 3 shows a perspective view of only the chronograph module,
FIG. 4 shows a perspective representation of the regulator organ, of the wheelwork and of the barrel of the chronograph module,
FIG. 5 shows a perspective view of a motion-work and small seconds hand gear system of the chronograph module,
FIG. 6 shows a perspective view of a winding system of the chronograph module,
FIG. 7 shows a perspective view of a power reserve of the chronograph module,
FIG. 8 shows a variant embodiment of the example of embodiment represented in FIGS. 1 to 7 ,
FIG. 9 is a cross-section view of the reset and rewind device in several parts,
FIG. 10 is a cross-section view of the date correction transmission device from the base movement towards the auxiliary module, and
FIG. 11 is a diagram indicating the torque of the barrel spring necessary to guarantee a given power-reserve.
DETAILED DESCRIPTION OF THE INVENTION
The device according to the invention will be applied advantageously in a chronograph wrist-watch (not specifically referenced), as represented in FIG. 1 . This watch shows: at two o'clock, a push-piece winding-button (crown) 1 for winding a barrel of the device's chronograph module—hereafter called autonomous chronograph module MCA—and for commanding the starting and stopping functions of the autonomous chronograph module MCA, at three o'clock, a winding-button (crown) 2 of the device's clock movement—hereafter called base movement MB—and at 4 o'clock, a push-piece 3 actuated for the resetting to zero and for the flight returning of the autonomous chronograph module MCA. In a preferred embodiment illustrated further below in relation to FIG. 9 , the watch comprises a single winding-crown allowing to simultaneously reset and rewind, in different axial positions, the base movement MB and the auxiliary chronograph module MCA.
The chronograph watch enables the displaying of the current time by means of an hour hand 4 , of a minutes hand 5 and of a small seconds hand 6 placed at three o'clock. It also allows the displaying of the measurement of an elapsed time by means of a thirty minute counter 7 , placed at nine o'clock at provided with a hand 8 , a chronograph centre seconds hand 9 and a hundredth of second counter 10 placed at six o'clock and provided with a hand 11 . A power-reserve counter 12 of the autonomous chronograph module MCA provided with a hand 13 and placed at twelve o'clock serves to verify said module's autonomy until the next winding. The graduations of these different counters are indicated on a dial 14 ; in particular, the hundredths of second correspond to hundred markings materialized on a circular scale, the hand 11 effecting a 360° rotation per second to ensure a comfortable and accurate reading of the time interval.
FIG. 2 is a perspective view showing the principle of the assembly of the autonomous chronograph module MCA with the base movement MB, centring elements and fastening organs being provided. By way of a non-limitative example, the base movement can for example be constituted by a movement of the type 2892 sold by the company ETA SA. A base plate 76 of the autonomous chronograph module MCA exhibits two holes (not visible and not referenced) in which are driven cylindrical pins 16 , 17 designed to engage in dial pin holes 18 , 19 of a bottom plate 15 of the base movement MB, for the purpose of a correct angular positioning of the MCA module relative to the MB movement. Fastening means connect the base movement MB and the autonomous chronograph module MCA at their periphery. According to the example, screws 20 A, 21 A go through holes (not visible and not referenced) provided in the plate 76 and are screwed in corresponding threaded holes 20 , 21 of the bottom plate 15 . Are further represented in this FIG. 2 : on the one hand, on the autonomous chronograph module MCA and projecting from its flank, a push-piece stem 1 A designed to receive the push-piece winding-crown 1 ( FIG. 1 ) and, emerging from its upper side, a staff 71 of the minutes train, a staff 67 of the seconds train, a staff 61 of the hundredth of second train and a staff 88 of the small seconds hand; on the other hand, on the basic module MB and projecting from its flank, a push-piece stem 2 B designed to receive the winding-crown 2 ( FIG. 1 ) and, emerging from its upper side, in the centre, a wheel 86 of the seconds train and a wheel 77 of the minutes train. As mentioned further above, a single rewind-button (crown) could, by means of the mechanism illustrated in FIG. 9 , be used to actuate axially and rotationally the two stems 1 A and 1 B.
FIG. 3 is a perspective view of the two movements in assembled state, showing essentially the autonomous chronograph module MCA covering the base movement MB (visualized principally by its bottom plate 15 and its winding-crown stem 2 B) and illustrating the remarkable and original arrangement and conformation of the main organs and elements of the autonomous chronograph module MCA on its base plate 76 . This extremely closely packed and compact arrangement results from an optimum exploitation of the available volumes, which avoids a costly miniaturization of said organs and elements without sacrificing the aesthetics, this design and construction enabling the device's dimensions in assembled state to be reduced to extremely low values. According to the described embodiment, these values are on the order of 7.75 mm (height) and 30 mm (overall diameter), whilst the dimensions of the chronograph module MCA itself do not exceed values on the order of 4 mm (height) and 30 mm (diameter). It will be understood that these dimensions afford a wide and extremely varied choice of exteriors for the device and a remarkable and effective aesthetic.
In order to reduce even further the height of the chronograph movement, it is conceivable to place the elements—which will be discussed in more detail further below (notably regulator organs, barrels, respective wheels, power-reserve, levers, winding systems)—on bridges arranged appropriately, from a single bottom plate, with the basic and chronograph movements then overlapping each other, without preventing the chronograph module's good running according to the methods that will be described hereafter, although the manufacturing costs will be increased.
The autonomous chronograph module MCA is equipped with its own barrel 22 and its own regulator organ comprising notably a balance 23 . This characteristic precludes any power take-off on the base movement MB and enables the balance 23 to be stopped without disturbing the sprung balance of the base movement MB.
The chronograph MCA is started and released by a pressing briefly on the push-piece stem 1 A, i.e. on the winding-crown 1 . Each of these pushing actions produces a displacement in the direction of the chronograph MCA's centre of a plate 24 comprising grooves in the shape of oblong openings 25 , 26 , with this displacement, which is guided by screws 27 , 28 working with said grooves, simultaneously actuating a beak 29 . When the pressure is released, the plate 24 and the beak 29 take their initial positions under the action respectively of a wire spring 40 and of a drawback spring 41 .
From an initial position (chronograph stopped, i.e. set at zero), the extremity of the beak 29 , pivoting around a pin 30 , comes into contact with a flank of a central wing of a cam 31 and makes said cam 31 turn around an arbor 32 by an angle defined by a stop 33 . A catch 34 then drives a lever 35 , a catch 39 makes a launcher 36 pivot around its arbor 37 , and a spring-blade 38 projects tangentially from the outer side of the balance 23 . In so doing, the spring 38 supplies to the balance 23 a starting impulse to put it into motion. A new pressing on the winding-crown 1 leads to the stopping of the chronograph at the end of an identical but inverse process (initial position corresponding to that illustrated in FIG. 3 , with the balance in motion), with the spring-blade 38 this time coming tangentially into contact with the outer side of the balance 23 and immobilizing the latter.
A pressure exerted on the push-piece 3 ( FIG. 1 ) causes a resetting to zero of the chronograph module MCA.
Each resetting to zero is effected by actuating a single hammer 48 . The aforementioned pushing action on the push-piece 3 makes a lever 42 and consequently its beak 44 pivot around a pillar staff 43 , which causes a reverser 45 to be driven with its pin 46 , the latter itself commanding a lever 47 that makes the hammer 48 pivot, which causes the hammer's three beaks (not referenced) to drop onto cams (heart-pieces) 49 , 50 , 51 mounted on the mobiles of the minutes counter, of the seconds counter and of the hundredth of second counter (see also FIG. 4 ) and thus causes the resetting to zero of the chronograph module MCA.
When the lever 42 is pushed, the beak 44 remains in contact with the reverser 45 during approximately two thirds of the angular space described by the lever 42 around the pillar staff 43 , then said beak 44 separates tangentially from the extremity of the reverser 45 and the latter returns to its initial position under the action of a drawback spring wound around the pivoting axis of said reverser 45 (in FIG. 3 , neither this drawback spring nor this pivoting axis are referenced, the pivoting axis being moreover hidden by the reverser 45 ).
The hammer 48 is fastened to the wheelwork bridge 52 by a screw 53 and an eccentric washer 54 . The eccentric washer 54 enables the regulation of the hammer 48 to be adjusted so that the three beaks of said hammer 48 press simultaneously on the three heart-pieces 49 , 50 and 51 , the resetting to zero of the chronograph module MCA being thus performed just before the beak 44 leaves the reverser 45 .
The consequences during the resetting to zero of the chronograph module MCA differ according to whether the balance 23 is stopped or moving.
If the balance 23 is stopped, the spring-blade 38 is in contact with the balance 23 and the friction exerted by the staffs 61 , 67 , 71 ( FIGS. 2 and 4 ) on the wheelwork has no influence on the balance 23 .
On the other hand, if the balance is moving, the spring-blade 38 is not in contact with the balance 23 and the friction exerted by the staffs 61 , 67 and 71 on the wheelwork will tend to brake the balance 23 .
When the pressure on the lever 42 is released, the beak 44 , held by a drawback spring 56 , can pivot around a pin 55 to avoid the reverser 45 and enable the lever 42 to take back its initial resting position under the action of a drawback spring 57 .
The operating principle described here above thus serves to prevent said balance to stop because of a prolonged friction of the staffs 61 , 67 and 71 when the autonomous chronograph module MCA is reset at zero with the balance 23 being in motion.
Thus, a same pressure exerted on the push-piece 3 ( FIG. 1 ) causes a resetting to zero of the chronograph module MCA when the balance 23 is stopped, and a resetting to zero of the chronograph module MCA (operation called flight returning) followed by an automatic restarting of a new measurement (without obligation to push again the push-piece stem 1 A) when the balance 23 is in motion.
The sprung balance ensemble of the chronograph's regulator organ is stopped when the latter is not in use.
FIG. 4 is a perspective view illustrating the arrangement of the regulator organ, of the wheelwork and of the barrel mounted on the base plate 76 of the autonomous chronograph module MCA. According to the example, in this configuration, the sprung balance 23 ensemble is dimensioned to oscillate at a frequency of 360,000 oscillations per hour.
In the formula:
f
=
1
2
Π
M
I
It is observed that for a given balance-spring, the frequency is inversely proportional to the square root of the moment of inertia of the balance whose formula can be assimilated to that of a hollow cylinder:
I
=
1
2
m
(
R
2
+
r
2
)
where:
m
=
Π
h
ρ
(
R
2
-
r
2
)
I
=
1
2
Π
h
ρ
(
R
4
-
r
4
)
which leads to:
f
=
1
2
Π
M
1
2
Π
h
ρ
(
R
4
-
r
4
)
f Frequency [Hz]
M Elastic torque of the balance-spring [Nm]
I Moment of inertia of the balance [kg·m 2 ]
R Outer radius of the balance [m]
r Inner radius of the balance [m]
h Thickness of the balance [m]
ρ Specific weight of the balance [kg/m 3 ]
By introducing values for f, R and r in this function, it will be observed that if the frequency is increased for example from 28,000 to 360,000, the diameter of the balance can be divided by approximately five. Experience shows that a balance that is too small does not ensure a good running stability and gives rise to regulating problems. The solution therefore consists in adopting a compromise between a reduction of the balance's outer diameter, which makes it easier to integrate it in the autonomous chronograph module MCA, and an increase of the balance-spring's accelerating power as defined by its CGS number.
In view of these observations, a balance-spring will thus be chosen having technical characteristics allowing a balance to be chosen with dimensions such that the regulator oscillates at the predetermined frequency, that the regulator organ offers good regulating quality and that the balance can be efficiently restarted by the blade-spring 38 .
A pallet 113 and an escape wheel 58 can be seen in FIG. 4 ; these elements can be chosen from existing supplies. According to an embodiment of the device described by way of example, a wheel 59 , driven on the staff of the escape wheel 58 , is chosen so that it turns at a speed of 2.5 turns per second, the balance 23 oscillating according to the example at 50 Hz (i.e. 360,000 oscillations per hour). A wheel 60 of the hundredth of second train turns clockwise at a speed of one turn per second. A wheel (not visible in the figure because it is hidden by the heart-piece 51 ), united with the wheel 60 , is mounted on the staff 61 of the hundredth of second train and meshes with a wheel 62 driven on a pinion 63 , the latter meshing with a wheel 64 . A wheel 65 of the seconds train turns clockwise at a speed of one turn per minute thanks to a reverser 66 that connects it to the wheel 64 . A wheel 84 (represented in FIG. 5 ), hidden by the heart-piece 50 and united with the wheel 65 , is mounted on the staff 67 of the seconds train. This wheel 84 meshes with a wheel 68 driven on a staff united with a wheel 69 that drives a wheel 70 mounted on the staff 71 of the minutes train. The wheel 70 turns clockwise at a speed of one turn in thirty minutes, it meshes with a wheel 72 driven on a staff 73 united with a wheel 74 that meshes with a toothed transmission-wheel 75 of the barrel 22 , with the latter unwinding clockwise under the action of the barrel spring (not represented) at a speed of one turn in 29.7 minutes.
In a mechanical movement, the barrel spring is generally calculated to perform about 7.5 turns. According to the described embodiment, for reasons of limiting the space requirements, the barrel spring is dimensioned to enable the barrel to perform approximately six turns, which equals a power-reserve of 178.2 minutes. But as explained above, use of a regulator organ whose sprung balance ensemble oscillating at high frequency (360,000 oscillations per hour) reduces use of the motor torque of the barrel spring to the period during which the function Δ motor torque/Δ time is linear, means that the useful power-reserve of the autonomous chronograph module MCA is on the order of hundred and twenty minutes (see FIG. 12 ).
During a measurement with a usual mechanical chronograph, the wheelwork of the chronograph part must be uncoupled from the wheelwork of the horological part. In order to prevent the chronograph hands from floating, it is indispensable to immobilize the wheels of the mobiles carrying said hands. With the autonomous mechanical chronograph module MCA according to the invention, this immobilizing operation is not necessary, since—as has emerged from the above description of the wheelwork of the autonomous chronograph module MCA—the gear-train remains permanently constrained by the barrel spring due to the fact that there is no uncoupling system and that on all the mobiles carrying several wheels (for example the wheels 84 and 65 of the seconds train or even the escape wheel 58 and the wheel 59 mounted on the same staff), the latter are united with one another. These characteristics guarantee a permanent rate-resumption of the train-gears.
Furthermore, on a usual chronograph, the operation of uncoupling the wheelwork of the chronograph part from the wheelwork of the horological part (base movement MB or intermediate wheels of the base movement situated in the chronograph module), and/or of uncoupling these wheelworks from one another, causes jumps, in particular during starting up of the chronograph, which can distort the measurement by several tenths of seconds. This defect is avoided by the present invention. To effect the resetting to zero of the counter hands mounted on the staffs 61 , 67 and 71 ( FIG. 4 ), the latter are mounted on their respective trains with a known friction system (for example, by an elastic washer, by indenting, etc.).
As compared with a mechanical chronograph comprising an additional usual chronograph module in which the wheelwork and the arrangement of the counters can be modified, the present invention further gives the possibility of modifying the frequency of oscillation of the balance-spring, the measurement resolution and the power-reserve of the autonomous chronograph module MCA. Generally, the frequency of oscillation supplied by the regulator of the autonomous chronograph module MCA is equal to N times the frequency of oscillation supplied by the regulator organ of the base movement MB; for example, for a base movement of a frequency of 28,000 oscillations per hour, N can be chosen at 12.50, so that the autonomous chronograph module MCA beats the hundredth of second. These characteristics allow the realization of a practically unlimited range of products in all the sectors and commercial niches, from the chronograph watches for the general public to those of top-of-the-range watch-making, up to products reserved for professional use.
FIG. 5 illustrates one of the many ways of transferring the time indications supplied by the base movement MB through the autonomous chronograph module MCA to the time hands 4 , 5 and 6 placed on the dial 14 ( FIG. 1 ).
The wheel 77 mounted on the cannon-pinion of the base movement MB meshes with an intermediate wheel 78 driven on a staff 79 united with the intermediate wheels 80 , 81 . The intermediate wheel 80 drives a cannon-pinion 82 carrying the minutes hand 5 and mounted freely on a tube 85 , with the intermediate wheel 81 driving an hour-wheel 83 carrying the hours hand 4 .
A wheel 86 mounted on the seconds staff of the base movement MB meshes with an intermediate wheel 87 that drives a wheel 89 driven on a staff of the small seconds hand 88 placed at three o'clock. To avoid floating of the small seconds hand 6 , a wire spring (not represented) can press inside a groove 90 of the staff 88 of the small seconds hand.
This design makes it possible to arrange—according to a current practice—the staff 67 of the trotteuse (direct-drive seconds-hand) 9 of the chronograph in the centre of the MCA module (see also FIG. 4 ) and offers the user a display of the time interval measured by the autonomous chronograph module MCA.
It is obvious that other designs can easily be conceived. Thus, FIG. 8 (comparable to FIG. 2 ) represents a variant embodiment according to which a seconds staff 67 B, a cannon-pinion 82 B and an hour-wheel 83 B of the base movement MB have been extended so as to go through a central opening 115 of the autonomous chronograph module MCA and to display the hour, minute and second in the centre of the dial 14 . According to this embodiment, the seconds hand of the autonomous chronograph movement MCA is borne by a staff 88 A placed at three o'clock on a counter.
FIG. 6 is a perspective representation of the winding system of the autonomous chronograph module MCA mounted on the base plate 76 . The manual winding of the barrel 22 is performed by rotating the push-piece stem 1 A, in resting position, in the same clockwise direction than that required for manually winding the basic mechanical movement MB, necessary for restarting the latter when it has not been worn during a sufficiently long period and the barrel spring is totally unwound (automatic movement). The push-piece stem 1 A is guided by a block 91 and held in place by a spring-blade 92 . A pressure exerted from below on the extremity of a catch 93 frees the push-piece stem 1 A and makes it possible to remove the movement from its case represented in FIG. 1 and not referenced, provided that the same operation is effected on the winding-crown stem 2 B (not represented in this Figure).
A bevel-wheel 94 actuated by a driving square 95 of the push-piece stem 1 A drives an intermediate wheel 96 meshing with a coupling wheel 97 . This wheel 97 is engaged with an intermediate wheel 98 if it turns anti-clockwise around its staff 114 , or uncoupled from this intermediate wheel 98 if it turns clockwise, the staff 114 being truncated in amygdaline shape. The intermediate wheel 98 driven by the coupling wheel 97 , when it turns anti-clockwise, meshes with an intermediate wheel 99 actuating a ratchet 100 mounted on a core 101 of the barrel 22 . The winding of the barrel spring is thus effected by rotating the ratchet 100 clockwise (the clicking system required for conserving the energy stored by the barrel spring during winding, known by the one skilled in the art, is not represented).
FIG. 7 represents in perspective an embodiment of a power reserve device of the autonomous chronograph module MCA, the information relating to the power reserve being displayed at noon on the dial 14 by the hand 12 ( FIG. 1 ). According to the embodiment, it is necessary that one turn of the ratchet 100 ( FIG. 6 ) during winding causes an angular displacement of a staff 102 of power reserve around its axis, equal to and in opposite direction to that generated by one turn of the transmission-wheel 75 of the barrel 22 on the same staff 102 during operation of the autonomous chronograph module MCA. During winding, the ratchet 100 and the wheel 98 driven on the staff 106 turn at the same speed and in the same direction (clockwise), one wheel 103 united with a staff 106 meshes with an outer teething of a sun crown 104 , the inner teething of the sun crown 104 drives a planetary wheel 105 , the wheel 105 being united with a planetary wheel 107 pressing on an inner teething of a sun crown 108 for making the staff 102 of the power reserve turn anti-clockwise by an angle of 30.375 degrees per turn of the ratchet 100 .
When the autonomous chronograph MCA is running, the transmission-wheel 75 of the barrel 22 drives a wheel 109 , this wheel 109 being united with a pinion 110 and held by a set-bridge 111 . The pinion 110 meshes with an outer teething of the sun crown 108 , the inner teething of the sun crown 108 drives the planetary wheel 107 united with the planetary wheel 105 pressing on the inner teething of the sun crown 104 for making the staff 102 of the power reserve turn clockwise by an angle of 30,375 degrees per turn of the transmission-wheel 75 of the barrel 22 .
According to this embodiment, the power reserve of the autonomous chronograph module MCA is approximately hundred and twenty minutes, the barrel 22 completes one turn in 29.7 minutes, with one turn of the barrel 22 corresponding to a rotation by 30,375 degrees of the staff 102 of the power reserve. The approximate power reserve of the autonomous chronograph module MCA thus corresponds to an angle of rotation of 127.72 degrees of the power reserve's staff 102 .
In order to guarantee that the winding or running of the autonomous chronograph module MCA does not give rise to an unwinding of the barrel spring beyond the limits defined above, a safety device limiting the rotation of the power reserve staff 102 can be provided; this device (not represented) can consist for example of driving a banking-pin in a hole provided on a planetary disc 112 , this pin working with an oblong opening concentric with the axis of the staff 102 and provided on a mechanism-cover.
FIG. 9 illustrates a preferred embodiment of the invention in which a single winding-crown 1 ′, preferably positioned at 3 o'clock, allows to act both on the base movement MB than on the additional module MCA. For this purpose, the stem 2 B′ of the base module MB is modified by the adjunction of a knob having a teething 201 and a groove 202 . The threading on the stem, which usually allows the external winding-crown 2 to be fastened, is however eliminated.
The stem 1 A′ of the additional module is provided with a threaded blind hole into which the stem 220 of the winding-crown 1 ′ is screwed. A square 213 on the stem 220 allows the winding-crown 1 ′ to be fastened to esp. disunited from the stem 1 A′ by means of an appropriate tool. In a variant embodiment, the winding-crown 1 ′ could be fastened directly on the stem 1 A′. A winding-crown pinion 211 is unitedly mounted on the stem of the auxiliary module MCA. In position (A), i.e. when the winding-crown 1 ′ is completely pushed axially against the watch case, this pinion 211 engages both with an intermediate wheel 96 ′ of the gear-train for rewinding the barrel 22 and with the teething 201 of the assembly 200 on the stem 2 B′.
In the illustrated example, the radius of the pinion 211 is dictated by the distance between the axis of the stem 1 A′ and the plane of the intermediate wheel 96 ′. The engaging ratio between the pinion 211 and the teething 201 is thus imposed by the thickness of the base movement and of the additional module. It can be useful to choose a number of turns and the torque to be applied on the winding-crown to rewind or reset the base module. In practice, it is for example comfortable to use an engaging ratio equal to one, making it possible to rewind and reset the base movement with the optimal number of turns and torque initially devised for this movement. In a variant embodiment not illustrated, the pinion 211 can thus be replaced by two side-by-side pinions of different diameters engaging one with the intermediate wheel 96 ′, the other with the teething 201 .
The intermediate wheel 96 ′ on which the pinion 211 engages is chosen so as to enable to wind the base movement MB by actuating the winding-crown 1 ′ in a first rotational direction, and to rewind the auxiliary module MCA by actuating this winding-crown in the other rotational direction, which allows these two elements to be rewound independently. In a variant embodiment, it could be considered more convenient to engage the rewinding pinion 211 with an intermediate wheel 96 ′ chosen so that the movement MB and the module MCA are both rewound by actuating the winding-crown in the same direction. In such an embodiment, an engaging ratio between the pinion 211 and the teething 201 different from one could be chosen in order to reduce the torque necessary for rewinding the two modules simultaneously.
In a variant embodiment not illustrated, in order to avoid inverting the rotational direction of the winding-crown 1 ′ during rewinding of the base movement MB, a middle intermediate wheel could be provided between the pinion 211 and the teething 201 .
By pulling the winding-crown 1 ′ outwards, the collar 212 drives the stem 2 B′ of the base movement MB outwards through the intermediary of the shoulder 204 . The one skilled in the art will understand that the collar 212 and the assembly 200 can be inverted on the two axes 1 A′ and 2 B′.
In the example illustrated, the reset mechanism of the base movement MB forces the stem 2 B′ to adopt predetermined axial positions, and thus the collar 212 to adopt one of the three indexed axial positions (A), (B) or (C).
In the positions (B) and (C), the pinion 211 does not engage any longer with the intermediate wheel 96 ′ but only with the teething 201 of the assembly 200 which is displaced outwards. In position (B), the winding-crown 1 ′ enables to rapidly correct the indicator 250 ( FIG. 10 ) of the base movement. In position 3 , the winding-crown 1 ′ allows the resetting of the base movement.
An optional pivot, not represented, could be mounted in the prolongation of the stem 2 B′ to reduce the risk of flexion or rupture of this stem. This pivot could pivot in a bearing (not illustrated) worked in the inner face of the watch-case.
FIG. 10 is a cross-sectional view of the date correction transmission device from the indicator disc 250 of the base movement towards the date disc 254 of the auxiliary module. The date disc 254 of the auxiliary module MCA carries the date indications seen by the watch's wearer.
As indicated here above, the winding-crown 1 ′ pulled in position B enables to correct, e.g. to manually advance, the angular position of the disc 250 of the base movement MB through the intermediary of the pinion 211 , of the teething 201 and of the stem 2 B′. According to the invention, the disc 250 , as opposed to the usual date discs, is disengaged from the gear-train of the base movement, for example by removing the day disc; the disc 250 is thus not driven by the base movement, which allows the power necessary to drive it to be saved and thus the power-reserve of the watch to be increased.
The disc 250 is held by a ring 252 connected or screwed to the auxiliary chronograph module MCA. A pinion 2520 mounted on a shaft 253 works with a teething 251 on the outside of the disc 250 , so that the date corrections on the disc 250 are transmitted to the ring 252 and then to the shaft 253 traversing the auxiliary chronograph module MCA. The shaft 253 is held free to pivot in the movement by a jewel or a bearing 255 , a shoulder 2530 preventing the shaft from coming out through the top of the figure.
A pinion 2531 mounted at the upper extremity of the shaft 253 engages with a teething 2540 connected with a second date disc 254 on the upper side of the auxiliary module MCA. This date disc is driven by the auxiliary module MCA, through the intermediary of a day disc not represented. The upper side of the date disk 254 carries date indications visible for the watch bearer through an opening in the face, these known elements having not been represented. Thus, the date disc 254 is driven and regulated by the high-resolution auxiliary module MCA but can be corrected through the base movement MB by acting on the winding-crown 1 ′.
In the variant embodiment illustrated in FIG. 10 , the shaft 253 and the disc 250 of the base module (not visible from outside the watch) are driven in rotation by the date disc 254 . This thus causes an unnecessary movement of parts and an energy loss. In a variant embodiment not represented, the gear constituted by the teething 2540 and the pinion 2532 is replaced by a free coupling, of a type known by the one skilled in the art, permitting only to transmit the correction movements transmitted from the shaft 253 towards the upper date disc 254 , but not the rotations in opposite direction.
It will be understood that it is also possible, within the framework of the invention, to correct the indication of the upper date disc directly by means of the reset stem 1 A′ of the auxiliary module, without using the correction mechanism of the base movement MB. The solution illustrated in FIG. 11 has however the advantage of using the date correction mechanism frequently available on the base movement and thus to avoid duplicating this mechanism in the auxiliary module.
It is obvious that the autonomous chronograph module MCA can be used as such, i.e. not necessarily associated to the base movement MB.
|
A device comprises a basic clock movement MB whose time indicators are driven by a first barrel connected to a first wheelwork and a first regulator organ, and an autonomous chronograph module MCA whose indicators are driven by a second barrel independent from the first, connected to a second wheelwork and a second regulator organ. The chronograph module is exclusively composed of mechanical elements. The frequency of oscillation supplied by its regulator is equal N times the frequency of oscillation supplied by the regulator of the base movement, with the coefficient N being definable according to a specific application of the chronograph, so that any chronograph module thus previously defined can work with the same base movement. The chronograph regulator remains constantly engaged with the corresponding wheelwork. The chronograph module allows a time interval to be read with a minimum precision of a hundredth of second. The organs of the base movement and of the chronograph module are arranged in such a way that in assembled state, the height and overall diameter do not exceed 7.75 mm and 30 mm respectively, the dimensions of the chronograph itself being not greater than 4 mm (height) and 30 mm (diameter) when its elements are mounted on a bottom plate, so that the device can advantageously be integrated in the case of a wrist-watch and affords an aesthetic exterior.
| 6
|
TECHNICAL FIELD
The present invention relates, in general, to a corrosion inhibitor for concrete having steel reinforcing rods (rebar) therein and, more particularly, to an admixture which can be mixed with the concrete when in the plastic state and which prevents corrosion of the steel reinforcing rods over an extended period of time when the concrete is exposed to chloride ion environments.
BACKGROUND ART
Reinforced concrete structures, such as highways, bridges, parking garages, and the like are very susceptible to corrosion from common chloride deicing salts which are applied to their respective surfaces and which cause corrosion of the steel reinforcing rods (rebar) which are an integral part of their structure. Similarly, reinforced concrete structures which are exposed to aggressive marine environments, such as piers, docks and bridge supports, are also susceptible to corrosion of the reinforcing rods therein. In either case, such corrosion is usually caused by chloride ions that penetrate through the surface of the concrete and contact the reinforcing rods. The electrochemical process by which corrosion of the reinforcing rods and rod degradation occurs is well known.
Under highly alkaline conditions, such as that which exists in Portland cement concrete, an oxidized film forms on the steel reinforcing rods inhibiting the corrosion of the rods. (The steel rods are said to have become “passivated.”) However, when chloride ions are allowed to penetrate into the concrete and reach the reinforcing rods, the first phase of the corrosion process (the initiation phase) commences. In this phase, there is no noticeable weakening of the concrete structure, but carbonation and chloride ion penetration occurs. Carbonation reduces the pH of the concrete, thus reducing the corrosion protection usually provided to the reinforcing rods by the alkaline concrete. Eventually, the passivity of the steel reinforcing rods breaks down as the oxidized film on the rods is broken and decays. Such breakage of the film generally occurs locally exposing the steel rods. As the oxidized film decays, the electrical resistance of the steel rods, i.e., the property that prevents the surface of the steel rods from polarizing and forming anodes and cathodes, is compromised. As a result, the small exposed portion of a steel rod acts as an anode, and the larger unexposed portion of the rod, still covered by the oxidized film, acts as a cathode resulting in the creation of a potential difference between the anode and the cathode. When the potential difference between the anode and the cathode is great enough, the steel reinforcing rod begins to corrode, i.e., metal ions are removed from the rod at its anode. As a result, corrosion takes place in spots (pitting) along the surface of the steel reinforcing rod resulting in the commencement of the second phase of the corrosion process (the propagation phase).
During the propagation phase, the effective sectional area of the steel reinforcing rod is progressively reduced by the corrosion causing a significant reduction in the strength of the rod. As the number of corrosion spots (pits) increases, they interconnect with one another spreading over the entire surface of the steel rod. In the initial stages of corrosion, ferrous hydroxide is formed which immediately oxidizes into iron oxides which are the main components of rust. In the course of the rust formation, the corroding rod expands at the point of rust formation. The localized expansion of the steel reinforcing rod caused by the formation of rust results in a high expansion pressure being applied to the concrete surrounding the expanded portion of the rod causing cracks to develop in the concrete along the surface of the rod. As the cracks develop in the concrete, additional chloride ions are permitted to contact the steel reinforcing rods, accelerating the corrosion of same and the spalling of the concrete surface. If corrosion and spalling are permitted to continue, the steel reinforcing rods, as well as the surrounding concrete, deteriorate to the point where the structural integrity of the concrete structure may be jeopardized. In order to remedy this condition, the removal and replacement of a substantially large area of concrete is required which is a very costly process.
Several approaches have been taken to repair concrete structures which have undergone or are susceptible to corrosion deterioration of the steel reinforcing rods therein. For example, severely deteriorated concrete can be removed and an overlay applied to the deteriorated structure. Large areas of chloride contaminated concrete, however, will remain in place, and although the corrosion and deterioration process will be slowed, the corrosion process continues. Alternatively, scarification of the top portion of concrete, e.g. on a bridge deck, can be utilized to remove a major portion of the chloride contaminated concrete permitting the application of a corrosion inhibiting agent to the concrete surrounding the steel reinforcing rods. After a corrosion inhibiting agent has been applied to the surrounding concrete, a new concrete overlay is formed thereon. A preferred rehabilitative technique requires complete removal of the concrete surrounding the steel reinforcing rods prior to the application of a new overlay.
Until now the corrosion inhibiting admixtures that have been developed for mixing with concrete when in the plastic state have been limited in their ability to delay the onset of corrosion in the steel reinforcing rods within the concrete, i.e., the initiation phase of corrosion, or to slow such corrosion after it has started, i.e., the propagation phase of corrosion. In view of the foregoing, it has become desirable to develop an admixture that can be mixed with the concrete when in the plastic state and which significantly delays the onset of corrosion in the steel reinforcing rods within the concrete and slows such corrosion after it has commenced even when the concrete is exposed to chloride ion environments. It is also desirable for such an admixture to protect the reinforcing rods in concrete that has partially or completely carbonated reducing the pH of the concrete and accelerating the onset of the protective oxide film deterioration in a chloride containing environment. Ideally, the admixture would also maintain and preferably increase the pH of the concrete.
SUMMARY OF THE INVENTION
The present invention solves the problems associated with the prior art approaches to minimizing corrosion of steel reinforcing rods in concrete as well as other problems by providing a unique corrosion inhibiting admixture comprising a combination of organic (on the basis of amine) and inorganic (on the basis of nitrite) fractions that provide a synergistic effect when present in a specific ratio. The range of the optimal amine:nitrite ratio (% by weight) is between 1.5 to 2.5. The admixture is introduced into concrete when in the plastic state by placing same in the mix water during the batching process or at the construction site. The admixture is thoroughly distributed throughout the concrete to provide substantially uniform levels of corrosion protection within the concrete. In an alternate embodiment of the present invention, a portion of the nitrite is replaced with lithium nitrite to minimize any undesirable alkali-silica reactions in the concrete. It has been found that the introduction of either embodiment of the aforementioned admixture into concrete when in the plastic state significantly delays the onset of corrosion of the steel reinforcing rods within the concrete and slows such corrosion after it has commenced even when the concrete is exposed to aggressive, salt-bearing environments. In addition, the admixture increases the pH of concrete which has carbonated.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph of the degree (amount) of corrosion in reinforced concrete versus time for the technical service life of reinforced concrete.
FIG. 2 is a graph of corrosion initiation time versus the amount of corrosion inhibiting admixture added to concrete.
FIG. 3 is a graph illustrating performance improvement (increase in corrosion initiation time) versus the amount of corrosion inhibiting admixture added to concrete.
FIG. 4 is a graph comparing the permeability of plain concrete, concrete to which the corrosion inhibiting admixture of the present invention has been added there to, and concrete to which a competitor's corrosion inhibiting admixture has been added thereto.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is directed to a corrosion inhibiting admixture which can be introduced into concrete when in the plastic state by placing the admixture in the mix water during the batching process or at the construction site. Corrosion inhibiting admixtures are presently available, however, their effectiveness in preventing or minimizing corrosion and degradation of reinforcing rods within the concrete is somewhat limited. Through electrochemical testing it has been found that an admixture comprised of organic amines, inorganic nitrites, gluconate and water provides excellent corrosion inhibiting capabilities. Amines that can be utilized include, but are not limited to, primary, secondary and tertiary amines. Examples of such amines include alkylamines, alkanolamines, alkyletheramines, mixtures of amines and alkanolamines, and mixtures of alkanolamines, tertiamines and alkyletheramines. Nitrites that can be utilized include alkali and alkaline earth metals such as sodium nitrite, lithium nitrite, calcium nitrite and potassium nitrite. Similarly, through electrochemical testing, it has been found that the amine:nitrite ratio (percentage by weight) has a synergistic effect on the corrosion inhibiting capabilities of the admixture. In the aforementioned admixture, the range of the optimal amine:nitrite ratio (% by weight) is between 1.5 to 2.5. In this admixture the amines comprise about 20% to 40% by weight of the admixture and the nitrites comprise about 15 to 30% by weight of the admixture.
Tests were conducted comparing concrete containing the aforementioned corrosion inhibiting admixture against concrete without the admixture. For example, a concrete mix comprised of 19.15 pounds of cement, 49.66 pounds of sand, 64.48 pounds of coarse aggregate and 10.95 pounds of water was prepared for control and comparison purposes. Similarly, a second mix comprised of 19.15 pounds of cement, 49.66 pounds of sand, 64.48 pounds of coarse aggregate, 9.12 pounds of water and 420 milliliters of the aforementioned admixture was prepared. The test results for each of the concrete mixes are shown below:
Plain Concrete
Concrete with Admixture
Slump
3.75
4.00
Percentage Air
6.4
7.2
Compressive Strength
1528 psi
2116 psi
(1 day)
Compressive Strength
3251 psi
3919 psi
(4 days)
Compressive Strength
4077 psi
4230 psi
(7 days)
Compressive Strength
4869 psi
5002 psi
(28 days)
In another test, a concrete mix comprised of 517 pounds of concrete, 1330 pounds of sand, 1741 pounds of coarse aggregate and 268 pounds of water was prepared for control and comparison purposes. Similarly, a second mix comprised of 517 pounds of concrete, 1330 pounds of sand, 1741 pounds of coarse aggregate, 232 pounds of water and 3 gallons of the aforementioned admixture was prepared. The test results of the concrete mixes are shown below:
Plain Concrete
Concrete with Admixture
Slump
6.25
5.25
Percentage Air
8.0
7.4
Compressive Strength
1551 psi
2638 psi
(1 day)
Compressive Strength
3179 psi
3653 psi
(3 days)
Compressive Strength
3894 psi
4122 psi
(7 days)
Compressive Strength
4899 psi
5020 psi
(28 days)
As can be seen from the test results, the addition of the aforementioned corrosion inhibiting admixture to concrete when in the plastic state does not adversely affect the physical properties of the resulting “set” concrete since the slump, percentage air entrained and compressive strengths are virtually unaffected by the addition of the admixture.
It has been found that the addition of the aforementioned corrosion inhibiting admixture to concrete significantly increases the amount of time that elapses before the start of corrosion in the concrete, i.e., it significantly delays the onset of the corrosion initiation phase. In addition, the addition of the aforementioned corrosion inhibiting admixture to concrete significantly reduces the rate of corrosion in the concrete after corrosion has commenced, i.e., it significantly increases the time of the corrosion propagation phase. Thus, the addition of the aforementioned corrosion inhibiting admixture to concrete provides a two-fold benefit. The foregoing corrosion process phases are shown graphically in FIG. 1 which is a graph of the degree (amount) of corrosion in reinforced concrete versus time for the technical service life of reinforced concrete and is the accepted model in the industry of the corrosion phenomena in reinforced concrete due to the chloride ion environment and carbonation. During the corrosion initiation phase, which is affected by the amount of atmospheric carbon dioxide and chloride ions to which the concrete is subjected, any corrosion is minimal and there is no noticeable weakening of the concrete structure. When corrosion or rust starts to form, i.e., at point “a” on the graph, the rate of corrosion is affected by the level of oxygen within the surrounding air and the temperature and relative humidity of the surrounding air. The addition of the corrosion inhibiting admixture of the present invention significantly moves point “a” to the right, i.e., it increases the amount of time that elapses before corrosion commences, and also decreases the slope of the line to the right of point “a”, i.e., it reduces the rate of corrosion with respect to time after corrosion commences. It has been found experimentally that the addition of the corrosion inhibiting admixture of the present invention to concrete increases the time of the corrosion initiation phase by a factor of about 1.7 to 2.7 versus the time for same if the admixture was not utilized. It has also been found experimentally that the addition of the corrosion inhibiting admixture of the present invention to concrete decreases the corrosion rate of the steel reinforcing rods within same to about 7×10 −4 mm/year. This extremely low corrosion rate, in effect, places the steel reinforcing rods in a passive state resulting in a technical service life of the reinforced concrete of between 90 to 100 years.
It has also been found that the amount of corrosion inhibiting admixture added to the concrete has a significant effect on the corrosion inhibiting properties of the resulting mix. For example, referring to FIG. 2, if no admixture is added to the concrete, the corrosion initiation time is significantly less than 200 days. If, however, 1.5 gallons of the corrosion inhibiting admixture is added to each cubic yard of concrete, the corrosion initiation time increases to more than 200 days. Similarly, if 3 gallons of the corrosion inhibiting admixture is added to each cubic yard of concrete, the corrosion initiation time increases to almost 300 days, and if 4.5 gallons of the admixture is added to each cubic yard of concrete, the corrosion initiation time increases to almost 400 days. The performance improvement through increasing the amount of admixture to the concrete, i.e., increase in corrosion initiation time, is shown graphically in FIG. 3 .
These significant increases in corrosion initiation time as a result of the addition of the corrosion inhibiting admixture of the present invention to concrete can, in part, be attributed to the fact that the admixture also increases the density of the “set” concrete, thus decreasing its permeability to chloride ion penetration. Such permeability is shown graphically in FIG. 4 which illustrates the permeability of plain concrete, i.e., concrete without any corrosion inhibiting admixture added thereto, after 7 and 28 days versus concrete with the corrosion inhibiting admixture of the present invention added thereto in two concentrations (3 gallons/yd. 3 and 4.5 gallons/yd. 3 ) and after 7 and 28 days and versus concrete having W.R. Grace & Company's DCI corrosion inhibiting admixture added thereto in the same concentrations and for the same time periods. By reviewing the foregoing graphs, it is apparent that the addition of the corrosion inhibiting admixture of the present invention to concrete significantly decreases the permeability of the concrete to chloride ion penetration, thus significantly increasing the technical service life of the concrete. It is also apparent that by increasing the amount of admixture to the concrete, the permeability of the concrete to chloride ion penetration is further decreased thus increasing the corrosion initiation time.
In essence, the corrosion inhibiting admixture of the present invention is a significant improvement over presently available corrosion inhibiting admixtures since it is a complex anodic-cathodic, organic-inorganic inhibitor that can protect the steel reinforcing rods in concrete that has developed cracks or has become carbonated to the depth of the reinforcing rods. Presently available corrosion inhibiting admixtures utilize only inorganic anodic inhibitors based on nitrites. When a crack forms in concrete or the concrete cover over the reinforcing rods carbonates, oxygen is allowed to contact the reinforcing rods and the pH environment is lowered to below that necessary to promote a high polarization resistance of the rod surface and maintain a high passive state. When reinforcing rods in concrete containing only anodic inhibitors are exposed to increased oxygen concentrations by the formation of a crack or the surrounding concrete has become carbonated, a nitrite based anodic inhibitor actually causes the passive oxide layer to decay more rapidly than if the anodic inhibitor was not present. In this environment, the anodic inhibitor can actually accelerate the corrosion process. The complex anodic-cathodic, organic-inorganic inhibitor of the present invention blocks access of oxygen to the surface of the steel reinforcing rods and maintains an elevated pH that is necessary to maintain the stability of the passive oxide layer on the reinforced rods even in carbonated concrete contaminated with chloride ions.
Concrete typically contains alkali materials which may be present in the cement, aggregate, and admixtures. In addition, silica compounds are typically found in the aggregate components of concrete. Silica is subject to attack and dissolution by hydroxide ions present in alkaline materials. Different forms of silica show varying degrees of susceptibility to such dissolution. If there are sufficient alkali metal ions present, the alkali metal ions may react with the reactive forms of silica causing the aggregate particles containing the silica to swell and form an alkali-silica gel which can absorb water and swell. Such swelling can exert internal pressures within the concrete causing the concrete to crack. This process is referred to in the industry as an alkali-silica reaction (ASR). This reaction can decrease the ability of the concrete to withstand other forms of attack, such as from the chloride ions within deicing salts, resulting in increased penetration of the chloride ions into the concrete allowing these ions to contact the reinforcing rods therein. Thus, an alkali-silica reaction can significantly increase the degree of corrosion of the reinforcing rods within the concrete. In order to minimize the effect of this reaction on the reinforcing rods within the concrete, a portion of the nitrite within the aforementioned admixture may be replaced with lithium nitrite.
Certain improvements and modifications will occur to those skilled in the act upon reading the foregoing. It should be understood that all such modifications and improvements have been deleted herein for the sake of conciseness and readability, but are properly within the scope of the following claims.
|
A corrosion inhibiting admixture for concrete is disclosed comprising a combination of organic (amines) and inorganic (nitrites) fractions that provide a synergistic effect when present at a specific ratio. Such a synergistic effect occurs when the amine:nitrite ratio (% by weight) is between 1.5 to 2.5 resulting in the admixture providing excellent corrosion inhibiting capabilities.
| 2
|
FIELD OF THE INVENTION
This invention relates to heating, ventilating and air conditioning (HVAC) systems for motor vehicles and particularly to a control for such a system utilizing infra-red sensing as well as air temperature sensing.
BACKGROUND OF THE INVENTION
It is common practice in automotive climate control to determine the thermal comfort level of a passenger compartment by drawing a stream of air from the compartment across a sensor to measure the air temperature and to estimate the effect of sun load on the occupants by a solar sensor mounted on top of the instrument panel for exposure to the sun. These measurements are combined with measurements of outside air temperature and engine coolant temperature to supply a control algorithm with the data needed to determine the optimum settings for HVAC mode, blower speed, and mixer door settings which together determine outlet air temperature and air speed needed to achieve a target temperature or comfort setting which is chosen by operator input.
The degree of success in achieving the desired comfort level varies according to specific design parameters including the placement of the solar sensor which for aesthetic reasons may be positioned where it is not the most effective. In any event, the measurement of sun load can be misleading in its computed effect on comfort since the sun direction, passenger clothing and other variables are not readily taken into account.
To avoid the drawbacks of solar load control as well as some objections to the conventional method of obtaining the air temperature, it has been proposed to replace both solar sensing and air temperature measurement with infrared (IR) sensing which directly detects the temperature of the occupant seating area and the occupants themselves. Thus irradiation from seat surfaces, occupant skin and occupant clothing, as well as any object in view of an IR sensor becomes the prime control parameter, and the air temperature in the passenger compartment is not considered at all. While this system affords an improvement over the prior systems by providing better correction for solar load and other sources of radiant energy within a vehicle, under many circumstances this correction can be too much, causing the system to overreact to introduction of hot sources. The air temperature has an effect on comfort and the system performance can be improved by including that measurement in the control algorithm.
Dual zone or multiple zone HVAC systems are already known to supply outlet air at different temperatures to different locations in the vehicle in accordance with individual temperature settings at each location. For example, the driver and passenger may have separate controls and separately managed air outlets. In the prior multiple zone systems the same temperature parameters, except for the selected target temperatures, are used to determine each air outlet temperature. The use of IR sensors, however, make it possible to improve those systems by separately measuring the irradiation from each zone.
It has been recognized that a major cause of discomfort during hot sunny days is that when a vehicle is idle, the interior can become extremely hot, so that upon first entering the vehicle the heat seems to be intolerable. The use of IR sensors make it practical to realistically monitor in-car temperatures even when the vehicle is not in operation and to prevent excessive temperatures by turning on ventilation.
SUMMARY OF THE INVENTION
It is therefore an object of the invention to incorporate the advantages of IR sensing in a climate control system while avoiding overreaction to changes in radiant energy in the vehicle. Another object is to enhance multiple zone HVAC systems by detecting and responding to the thermal condition of each zone. A further object is to control vehicle ventilation to prevent very hot conditions in an idle vehicle.
The climate control of an HVAC system uses a microcomputer to receive inputs from sensors and to control the system mode, blower speed and mixer door positions, thereby regulating the air output to the passenger compartment. The sensors comprise an IR sensor, an internal air temperature sensor, an outside air temperature sensor, and an engine coolant sensor. The latter only affects the mixer door position since the coolant temperature determines the hot air temperature in the system.
The IR sensor monitors the radiation level of the front seat and its occupants and includes a thermopile having a sensing junction affected by the radiation level of the scene and a reference junction. The reference junction may be warmer or cooler or the same as the sensing junction, and the thermopile output voltage is dependent on the difference in junction temperatures. A thermistor packaged with the thermopile is responsive to the reference junction temperature. A sensor circuit combines the thermistor and the thermopile outputs to generate a signal which in effect is the combined outputs of those sensors. The signal represents the absolute temperature of the scene and is linear at least in the target temperature range of the climate control.
The internal air sensor is an aspirated thermistor; i.e., a stream of the vehicle compartment air flows across the thermistor so that its output signal represents the internal air temperature. Conventionally, the air flow is produced by a suction arrangement attached to the ventilation blower assembly, but instead it can be produced by a separate motor driven fan.
In the microcomputer an algorithm combines the selected target temperature, IR sensor circuit output information, the internal air temperature information, and outside temperature information to select the HVAC mode (heating, cooling or ventilation) and the blower speed, and further includes engine coolant temperature to select mixer door positions. This combination of information yield an improved comfort level by responding to air temperature and sun load to achieve the selected target temperature without overreacting to the sun load or other radiation source affecting the IR sensor output.
Dual zone control is accomplished by two IR sensors or two thermopiles in the same sensor, each viewing the radiation from one zone, and separate temperature selectors for each zone. The microcomputer separately controls the air outlet to each zone using the same algorithm for each zone. Where the two thermopiles are close together or even in the same package, a single reference junction thermistor and sensor circuit can be used, either one of the two thermopiles being switched into the circuit as needed for each zone control computation.
Automatic ventilation of a vehicle while not in operation is carried out by sensing the in-car temperature by the IR sensor, sensing the outside temperature, and sensing the battery voltage, and turning on the ventilation if the sensed temperature is above a threshold and above outside temperature by a certain increment, and the voltage is above a given value. The ventilation is turned off in dependence on the same variables. Thus when inside temperature reaches a high value and the outside air is cool enough to effectively temper the inside temperature, the HVAC unit will blow in outside air. At all times, the ventilation is subject to available battery voltage since it is not desirable to run down the battery. An additional control may be to actuate the automatic ventilation only just prior to the time the operator expects to return to the vehicle thereby preventing excessive temperatures upon vehicle entry. This may be accomplished by a timer set by the operator according to a known schedule. Still another variable would be opening a sun roof for ventilation instead of or in addition to turning on a blower. In this case it would be desirable to also have a rain sensor to prevent opening the sun roof when it is raining.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other advantages of the invention will become more apparent from the following description taken in conjunction with the accompanying drawings wherein like references refer to like parts and wherein:
FIG. 1 is a diagram of a climate control system according to the invention;
FIG. 2 is a view of a vehicle seat showing the field of view of an IR sensor for the system of FIG. 1;
FIG. 3 is a schematic diagram of an IR sensor assembly for the system of FIG. 1;
FIG. 4 is a circuit diagram for the sensor assembly of FIG. 3;
FIG. 5 is a detailed diagram of the climate control system of FIG. 1;
FIG. 6 is a diagram of a climate control system according to another embodiment of the invention;
FIG. 7 is a view of a vehicle seat showing the fields of view of IR sensors for the system of FIG. 6;
FIG. 8 is a schematic diagram of an IR sensor assembly for the system of FIG. 7; and
FIG. 9 is a flow chart representing a program for system operation to carry out a precool function, according to the invention.
DESCRIPTION OF THE INVENTION
Referring first to FIG. 1, a vehicle climate control 10 is shown comprising a heating, ventilation and air conditioning (HVAC) control 20 comprising a conventionally known microcomputer (not illustrated) having a central processing unit, ROM, RAM, I/O ports and A/D converters which receive various analog input signals from discrete sensors 30-36 and digitize the same for use in automated control of passenger compartment thermal level. Interior air temperature (IAT) sensor 30 and infrared (IR) sensor 32 provide the primary inputs to HVAC control 20 with outside air temperature (OAT) sensor 34 providing further data to HVAC control 20 for climate control. OAT sensor 34 provides in conjunction with IAT sensor 30 a differential measurement between the passenger compartment and the exterior environment which effects the rate of heat transfer therebetween, while the IR sensor 32 provides a measure of the radiation from the vehicle interior and occupants which provides radiant heat resulting from sun load, occupant's skin and clothing and other sources within the passenger compartment. Coolant temperature (COOLANT) sensor 36 provides a signal to HVAC control 20 which is indicative of the heat capacity of the heater core. Another input to the control includes an operator selected temperature setting signal (SET TEMP) 38 corresponding to the desired thermal level. The various inputs are monitored and processed for controlling temperature maintenance functions of the heater, evaporator and blower assembly (HEBA) 40 which, as the name suggests, includes; a heater core for circulating engine coolant for warming air, an evaporator core for circulating refrigerant for cooling air, a blower or fan for circulating air through the heater and evaporator cores in proportion to the position of an air mix door as determined by solenoid operated vacuum switches or electrical motors responsive to the HVAC controller outputs 25. The position of the air mix door determines the temperature of the air circulated by HEBA 40. The HEBA often times further includes control of exiting air to passenger determined modes such as lower, upper, bi-level, defog and defrost and entering air between fresh and recirculated modes. Solenoid controlled vacuum switches responsive to HVAC outputs 25 are the most prevalent actuators used for motive control of air delivery doors effective to establish the modes as described above. Electrical motor control of air delivery doors is also practiced in the art and is equally applicable to the present invention.
FIG. 1 further illustrates the means by which passenger compartment air temperature is measured. In addition to IAT sensor 30 which is normally positioned behind the instrument panel (not illustrated), aspirator tube 50 (functionally illustrated) is utilized to draw passenger compartment air in the vicinity of the front of the instrument panel across IAT sensor 30 for example by connecting the remote end of the tube to a high air flow portion of HEBA 40 through a venturi arrangement to generate a small air flow. A measure of the interior air temperature is thereby obtained.
Turning to FIG. 2, a vehicle seat is designated by the numeral 42 and an occupant by the numeral 44. An infra-red (IR) sensor assembly 32 is positioned within the passenger compartment of the vehicle such that the viewing field, indicated by the ellipse 48 is representative of predetermined portions of the seat 42 and occupant 44. Appropriate locations for the IR sensor assembly 32 include the vehicle instrument panel such that the viewing field is rear facing with respect thereto. This way, a good portion of passenger compartment is within the viewing field of the sensor. In a first embodiment, the IR sensor 32 has a relatively wide field of view as illustrated in two dimensions by the seat and passenger area delimited by the elliptical line 48.
The viewing angle of an IR sensor is determined by design of the sensor and, if inadequate for the desired viewing field, may be modified by lensing. A particularly attractive option for widening the viewing angle and minimizing dimensional penalty is to use a fresnel lens comprised of low loss material such as polyethylene.
Response of the sensor to different wavelengths of electromagnetic radiation can be controlled by the window material. Most of the energy of concern is in the ten micron wavelength range and an electromagnetic radiation sensor designed with windows providing admissibility in that range has been shown to perform adequately for providing a measure of passenger compartment thermal level. Silicon window material has been shown to provide approximately 60 percent admissibility in this range, with polyethylene window material improving this figure to approximately 90 percent. The various window materials therefore provide the means by which selective wavelengths of thermal energy are filtered for inclusion or exclusion depending upon the desired measurement.
FIG. 3 depicts an IR sensor assembly 32 which comprises a can 50 having a window 52 and a target region 54 which receives or transmits IR through the window 50 to approach the temperature of the viewed scene. A thermocouple or thermopile 56 has a sensing junction 58 at the target 54 and a reference junction 60 thermally coupled to the wall of the can 50. The thermopile 56 leads extend to an IR circuit 62. A thermistor 64 on the can senses the temperature of the reference junction and has leads extending to the circuit 62.
In the present embodiment, an IR sensor part number PL-82 available from Armtec/Ragen Incorporated, 10 Ammon Drive, Manchester, NH is utilized. This sensor is a twenty junction thermocouple device with a silicon window 52 and produces a voltage output on the order of 45 microvolts per degree fahrenheit. It is apparent that a change in passenger compartment thermal level of several degrees therefore will only result in voltage changes on the order of tens or perhaps hundreds of microvolts, which small signals pose unique amplification challenges. A cost effective and widely available means for signal amplification meeting the needs of this embodiment is a chopper stabilized amplifier in differential mode which is innately characterized by extremely low input offset voltage thereby being responsive to the small voltage changes provided by the IR sensor chosen. An exemplary circuit 62 is set forth in FIG. 4 for accomplishing a chopper stabilized amplification of the IR sensor signal wherein chopper stabilized amplifier 66 is designated a TL2654 available from Texas Instruments, Dallas, Tex. Exemplary component values are shown but are subject to modification according to required operation.
The present embodiment is configured for non-inverting operation having the non-inverting terminal connected to the positive terminal of the IR sensor. The negative terminal of the thermopile 56 is coupled to one end of a resistor R1 to establish offset node 68, the other end thereof coupled to the inverting input of the amplifier. The output of the amplifier is coupled through resistor R2 to the inverting input in feedback to establish the gain (G) of the circuit in accordance with a ratiometric relationship between R2 and R1[G=(R1+R2)/R1]. Integrating capacitor C1 is preferably coupled across the inverting terminal and the output in order to stabilize the output signal. Each of the capacitors C2,C3 shown coupled to ground provides storage of a potential for nulling the amplifier offset voltage during a respective one of amplifying or nulling phases of the chopper amplifier's operation. The output of amplifier 66 comprises a conditioned IR sensor signal for input into an HVAC control. An offset voltage substantially equal to one-half the operating voltage V of the amplifier is provided at offset node 68 established between thermopile 56 negative terminal and resistor R1 to allow operation through the entire operating voltage range. Output voltage is therefore represented by the equation:
Vo=Voff+G*Vir,
where Vo is the output voltage, Voff is the offset voltage, G is the gain and Vir is the IR sensor voltage.
As with any thermopile device, the voltage produced between two output terminals thereof is a function of the temperature differential between a set of measuring junctions and reference junctions; and, in the present embodiment, the chosen IR sensor produces a voltage signal substantially proportional to the difference in temperature. In the present embodiment using the above exemplary IR sensor, the measuring junctions are exposed through a silicon window to the passenger compartment infra-red radiation content, and the reference junctions are shielded therefrom so as to remain immune to thermal influences attributed thereto. The reference junction temperature will naturally tend toward a temperature in accordance with thermal influences apart from the infra-red radiation content of the passenger compartment from which they are shielded. These influences include convection from passenger compartment and instrument panel air and conduction from mounting means for the IR sensor and resistive heating of the junctions due to current flow therethrough. The sensor output will: 1) approach zero in the case where the reference junctions tend toward the passenger compartment thermal level as "seen" by the measuring junctions, or; 2) approach an offset in the case where the reference junctions tend toward some dominant local thermal influence such as a proximate incandescent light source.
The present embodiment therefore provides a compensation to the offset voltage applied at the offset node by using the thermistor 64 having variable resistance RT connected in series with a resistor R between a supply voltage V and ground, the junction being connected to the node 68 to supply the offset voltage Voff. The thermistor measures the temperature at the reference junctions, its negative coefficient of resistance causing adjustment to offset voltage Voff in proportion to the temperature change at the reference junction to null the effects of varying reference junction temperature from whatever influence. Therefore, the gain G as determined by the resistor pair R2 and R1 is chosen to produce this desired relationship whereby each unit of temperature change at the reference junctions produces a change to the term Voff which is balanced by the change in the term Vir multiplied by the gain G.
Elements of the illustrated preferred climate control architecture of FIG. 1 are further expanded in FIG. 5. IR sensor assembly 32 is shown as an input to an HVAC control. The internal air temperature sensor IAT 30 and outside air temperature sensor OAT 34 are illustrated. Coolant temperature COOLANT 36 is also shown with a signal therefrom as an input to the HVAC control. Operator selected temperature setting signal SET TEMP 38 is similarly shown as an input thereto. Sensors 30-36 and 32 are assumed to produce analog signals, which signals are passed to A/D converter 70 for digitization. The OAT output is converted to OAT -- COR by a look up table 72. SET TEMP signal 38 is assumed a digital input signal commonly obtained from an instrument panel climate control operator interface at the instrument panel. Where SET TEMP signal is analog, A/D conversion can be employed to digitize the signal.
Control processing is advantageously described in terms of establishing a program number PGMno and air mix door number MIXno though other alternatives will be readily apparent to those possessing ordinary skill in the art. PGMno is established according to the following function:
PGMno=IAT+5*(SET TEMP)+IR+OAT.sub.-- COR+K)
where IAT is the internal air temperature signal from sensor 30, SET TEMP is the operator temperature setting, IR is the passenger compartment thermal level as established by the IR sensor assembly 32, OAT -- COR is the outside air temperature correction factor from calibration table 72, and K represents a calibration constant to scale PGMno into a number range compatible with the microcomputer architecture (0<PGMno<255 for 8 bit architecture). PGMno is then utilized to reference blower speed and mode for HEBA 40 operation such as through calibration tables 74 and 76, respectively. The mode is also used for the look-up from calibration table 78 of a corrective value MOD -- COR associated therewith and summed with PGMno at node 80 to establish a mode corrected program number MPGMno.
For control of mixer door position, MIXno is established according to the following general function:
MIXno=f(COOL, ΔT(COOL, Te), MPGMno, K1, K2)
where COOL is the coolant temperature as established by coolant sensor 36, Te is a predetermined evaporator temperature equivalent to a fixed calibrated value when the compressor is cycling and to the ambient temperature as measured by OAT sensor 34 when the compressor is not cycling, MPGMno is the mode adjusted program number, and K1 and K2 represent calibration constants used to scale the function into a number range compatible with the microcomputer architecture (0<MIXno<255 for an 8-bit architecture). MIXno is then utilized to select a temperature door position from the mix door position look-up table 82. This selected door position is used in positioning the air mix door in HEBA 40.
It has been found that this arrangement using the IR signal in conjunction with IAT and the other inputs gives superior control of temperature without the need for solar sensors and in particular improves the correction for radiant energy sources such as sun load.
The same control advantages apply to dual zone or multiple zone systems. As shown in FIG. 6, by using two IR sensors 32 and 33, called IRa and IRb, and separate user controls 38 and 39 to set temperature A and temperature B, two zones, A and B can be individually controlled. Typically the two zones have common mode and common blower speed, and separate mixer doors are set according to individual needs. The HVAC 20 readily calculates the MIXno for each zone using the same algorithm for both zones with the appropriate IR and Set Temp inputs for each zone.
FIG. 7 illustrates the application of two IR sensors 32 and 33 which view local zones 46 and 47 respectively, so that the thermal level of each zone is sensed. It often occurs that sun load affects one side more than the other so that the thermal levels as detected by the IR sensors may differ considerably. If the sensors 32, 33 are physically close to each other, they may use the same IR circuit to generate both IR output signals on a time sharing basis. Referring to FIG. 8, the thermopile 56 of sensor 32 and the thermopile 57 of sensor 33 are connected together at the node 68 at one end and are coupled through a switch 86 to the amplifier 66. The switch is controlled in concert with the HVAC control for employing each IR sensor according to which zone control settings are being calculated.
When a vehicle is left unattended under conditions of high sun load, the interior becomes very hot. To precool the vehicle the blower may be turned on as needed to circulate cooler outside air into the vehicle. The interior temperature as sensed by the IR sensor is used as the primary parameter and is compared to a threshold and the outside temperature for controlling the blower. A program run by the HVAC controller 20 is given in FIG. 9 for a precool control, using particular parameter values which are not necessarily the optimum values for a given application but which illustrate the control method. Using this algorithm the IR temperature is checked every four minutes when the vehicle is off and compared to a 115° F. degree threshold and to outside temperature. When preset conditions are met the system blower is turned on and then every four minutes the temperature is checked to determine when to turn the blower off. In any event the program is interrupted if the vehicle is started.
Referring to FIG. 9, the description of the flow chart contains numerals in angle brackets <nnn> which refer to functions in blocks with corresponding reference numerals. The programmed is entered if the vehicle is off <100> and then a four minute timer is started <102>. If the timer reaches four minutes <104> the IR temperature is compared to a 115° F. threshold <106>. If the IR temperature does exceed the threshold it is determined whether the temperature is at least 10° higher than the outside temperature OAT <108>. If it is, the system voltage is checked to assure that it is above 11.5 volts <110>. Then the precool system is activated to operate the blower <112>. If any condition in blocks 106, 108 and 110 is not met, the timer is restarted <102>. Once the precool system is activated, another four minute timer is started <114> and when it times out <116>, the system voltage is tested <118> and the system is deactivated <120> if the voltage falls below 11.5 volts. If the voltage is above that limit, two temperature conditions are tested <122>: if the IR temperature is below 85° or the IR temperature is within 5° of the outside temperature OAT, the precool system is deactivated <120>; otherwise the timer is restarted <114>.
Since the operation of the precool system is limited by vehicle battery limitations, it is desirable to further enhance it by selectively determining when it may be operative, thereby permitting the ventilating function only when vehicle usage is imminent. For example, a scheduling timer may be set by the operator to indicate the next expected vehicle use or may be programmed with a daily schedule of use which is stored for use each day or on predetermined days. Then the algorithm of FIG. 9 would be entered. Still another scheduling system would employ an adaptive algorithm to learn an operator's schedule by monitoring the vehicle usage over some time period.
|
An air temperature sensor and an infrared sensor are used along with an outside temperature sensor to control an HVAC system. During vehicle operation the IR sensor views an occupant seating area and realistically determines the thermal comfort level and the air temperature adds stability to that determination to control the air output. For dual zone systems two IR sensors separately monitor the two zones for accurate control of each zone air output. When the vehicle is not operating, the internal temperature is monitored and compared to a threshold and to outside temperature to turn on ventilation for limiting the internal temperature, subject to sufficient battery voltage.
| 6
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of Korean Patent Application No. 10-2013-0021491 filed on Feb. 27, 2013, with the Korean Intellectual Property Office, the disclosure of which is incorporated herein by reference.
BACKGROUND
[0002] The present disclosure relates to a semiconductor test device and a semiconductor test method.
[0003] In general, Automatic Test Equipment (ATE) applies a test input signal to a Device Under Test (DUT) and acquires a test output signal corresponding to the test input signal.
[0004] The ATE may determine whether the DUT is faulty or not based on the test input signal and the test output signal.
[0005] Typically, a test input signal has a low clock frequency. Therefore, such a test input signal with a low clock frequency may result in longer testing times for DUTs when using a semiconductor test device.
[0006] Patent Document 1 below discloses a pattern generator to test a DUT, but does not disclose features aimed at improving DUT test speeds.
RELATED ART DOCUMENT
[0007] (Patent Document 1) Korean Patent Laid-Open Publication No. 2000-0004903
SUMMARY
[0008] An aspect of the present disclosure may provide a semiconductor test device and a semiconductor test method capable of testing a semiconductor device faster.
[0009] An aspect of the present disclosure may also provide a semiconductor test device and a semiconductor test method capable of efficiently storing a test input signal.
[0010] According to an aspect of the present disclosure, a semiconductor test device may include: a test information acquisition unit acquiring test information; a test information conversion unit converting the acquired test information into test vector information including a plurality of test vectors; and a test signal generation unit generating a test input signal based on the test vector information.
[0011] The test vector information conversion unit may convert the test information having a first clock rate into test vector information having a second clock rate faster than the first clock rate.
[0012] The test information acquisition unit may acquire a plurality of test information items.
[0013] The semiconductor test device may further include: a test vector information storage unit storing the test vector information.
[0014] The test vector information storage unit may store a pattern of the test vector therein.
[0015] The semiconductor test device may further include: a sense unit acquiring a test output signal in response to the test input signal; and a control unit determining whether a device under test is faulty, based on the test input signal and on the test output signal.
[0016] According to another aspect of the present disclosure, a semiconductor test method may include: acquiring test information; converting the acquired test information into test vector information including a plurality of test vectors; and generating a test input signal based on the test vector information.
[0017] The converting of the test vector information may include converting the test information having a first clock rate into test vector information having a second clock rate faster than the first clock rate.
[0018] The acquiring of the test information may include acquiring a plurality of test information items.
[0019] The semiconductor test method may further include storing the test vector information.
[0020] The storing of the test vector information may include storing a pattern of the test vector.
[0021] The semiconductor test method may further include: acquiring a test output signal in response to the test input signal; and determining whether a device under test is faulty, based on the test input signal and on the test output signal.
BRIEF DESCRIPTION OF DRAWINGS
[0022] The above and other aspects, features and other advantages of the present disclosure will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
[0023] FIG. 1 is a block diagram of a semiconductor test device according to an exemplary embodiment of the present disclosure;
[0024] FIG. 2 is a diagram illustrating examples of test information;
[0025] FIG. 3 is a diagram illustrating an example of converting test information into test vector information;
[0026] FIG. 4 is a diagram illustrating examples of patterns of a test vector; and
[0027] FIG. 5 is a flowchart illustrating a semiconductor test method according to an exemplary embodiment of the present disclosure.
DETAILED DESCRIPTION
[0028] Hereinafter, embodiments of the present disclosure will be described in detail with reference to the accompanying drawings. The disclosure may, however, be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. Throughout the drawings, the same or like reference numerals will be used to designate the same or like elements.
[0029] FIG. 1 is a block diagram of a semiconductor test device according to an exemplary embodiment of the present disclosure.
[0030] The semiconductor test device 100 may determine whether a DUT is faulty or not.
[0031] Referring to FIG. 1 , the semiconductor test device 100 may include a test information acquisition unit 110 , a test information conversion unit 120 , a test vector information storage unit 130 , a control unit 140 , a test signal generation unit 150 , and a sense unit 160 .
[0032] The test information acquisition unit 110 may acquire test information to be applied to a Device Under Test (DUT). By applying the test information to a DUT, the semiconductor test device 100 may determine whether the DUT is faulty or not.
[0033] The test information maybe generated by a Test Pattern Generator (TPG) or a simulator. For example, the TPG or the simulator may provide a file format which can be recognized by the test information acquisition unit 110 of the semiconductor test device 100 . Such a file format may include a Value Change Dump/extended Value Change Dump (VCD/eVCD) file format from a simulator, a waveform generation language (WGL) file format from a TPG, and standard test interface language (STIL), for example.
[0034] FIG. 2 is a diagram illustrating examples of test information.
[0035] As shown in FIG. 2 , first test information may be a predetermined waveform.
[0036] While the first test information is applied to a DUT, the semiconductor test device 100 may determine whether the DUT is faulty at a rate corresponding to the frequency of first clock information.
[0037] That is, the first test information may be applied to the DUT in the form of a digital signal composed of zeros and ones along with the first clock information.
[0038] As shown in FIG. 2 , third test information may be another predetermined waveform.
[0039] While the third test information is applied to a DUT, the semiconductor test device 100 may determine whether the DUT is faulty at a rate corresponding to the frequency of third clock information.
[0040] That is, the third test information may be applied to the DUT in the form of a digital signal composed of zeros and ones along with the third clock information.
[0041] The test information conversion unit 120 may convert the test information acquired by the test information acquisition unit 110 into test vector information including a plurality of test vectors.
[0042] The information contained in the test information may be divided into a predetermined number of vectors. Herein, the vectors each containing the divided information is referred to as test vectors.
[0043] FIG. 3 is a diagram illustrating an example of converting test information into test vector information.
[0044] Referring to FIG. 3 , the first test information may be converted into first test vector information. For example, Section I in the first test information may be represented by three test vectors, i.e., “111” in the first test vector information. In addition, Section II in the first test information may be represented by three test vectors, i.e., “000” in the first test vector information.
[0045] The third test information may be converted into third test vector information. For example, Section III in the third test information may be represented by twenty-four test vectors, i.e., “111 . . . 1” in the third test vector information. For example, Section IV in the third test information may be represented by twenty-four test vectors, i.e., “000 . . . 0” in the third test vector information.
[0046] As described above, sections in the test information may be represented by n test vectors. The number n may be an integer.
[0047] According to an exemplary embodiment of the present disclosure, the first test information may be applied to a DUT at a rate corresponding to the frequency of the first clock information (a first clock rate). The semiconductor test device 100 may determine whether the DUT is faulty or not at a rate corresponding to the frequency of the first clock information (the first clock rate).
[0048] Further, the third test information may be applied to the DUT at a rate corresponding to the frequency of the third clock information (a third clock rate). The semiconductor test device 100 may determine whether the DUT is faulty or not at a rate corresponding to the frequency of the third clock information (the third clock rate).
[0049] The first test vector information and the second test vector information may be applied to the DUT at a rate corresponding to the frequency of second clock information (a second clock rate). Therefore, the semiconductor test device 100 may determine whether the DUT is faulty or not at a rate corresponding to the frequency of the second clock information (the second clock rate).
[0050] The second clock rate may be faster than the first and third clock rates. Accordingly, the semiconductor test device 100 may determine whether the DUT is faulty or not faster by converting the first test information and the third test information into the first test vector information and the third vector information, respectively.
[0051] Therefore, a waveform corresponding to certain test information may be applied to the DUT at a faster clock rate with the same information.
[0052] According to an exemplary embodiment of the present disclosure, the test vector information storage unit 130 may store the test vector information therein.
[0053] For example, the test vector information storage unit 130 may store a pattern of the test vector therein.
[0054] FIG. 4 is a diagram illustrating examples of patterns of a test vector.
[0055] For the third test vector information shown in FIG. 3 , the test vector information storage unit 130 may store a first pattern and a second pattern.
[0056] The storage addresses for the patterns of the test vector maybe set. For example, “a1” maybe set for the storage address representing the first pattern. In addition, “a2” may beset for the storage address representing the second pattern.
[0057] When the third test vector information has a pattern of repeated sections III and sections IV, the test vector information storage unit 130 may require a lot of storage spaces in order to store all of the patterns.
[0058] Accordingly, the test vector information storage unit 130 may save the storage spaces by storing only the repeated first and second patterns.
[0059] When the semiconductor test device 100 retrieves the third test vector information, the semiconductor test device 100 may alternately retrieve the address at which the first pattern is stored (a1) and the address at which the second pattern is stored (a2).
[0060] Further, for the first test vector information shown in FIG. 3 , the test vector information storage unit 130 may store a third pattern and a fourth pattern.
[0061] The storage addresses for the patterns of the test vector may be set. For example, “a3” maybe set for the storage address representing the third pattern. In addition, “a4” may beset for the storage address representing the fourth pattern.
[0062] When the first test vector information has a pattern of repeated section I and section II, the test vector information storage unit 130 may require a lot of storage spaces in order to store all of the patterns.
[0063] Accordingly, the test vector information storage unit 130 may save the storage spaces by storing only the repeated third and fourth patterns.
[0064] When the semiconductor test device 100 retrieves the first test vector information, the semiconductor test device 100 may alternately retrieve the address at which the third pattern is stored (a3) and the address at which the fourth pattern is stored (a4).
[0065] The test signal generation unit 150 may generate a test input signal based on the test vector information.
[0066] Herein, a signal applied to a DUT by the semiconductor test device 100 to determine whether the DUT is faulty or not is referred to as a test input signal.
[0067] The DUT may output a test output signal to the semiconductor test device 100 based on the test input signals.
[0068] The test output signal refers to an output pulse signal output from the DUT in response to the test input signal.
[0069] The sense unit 160 may acquire a test output signal from the DUT.
[0070] The control unit 140 may control the overall operation of the semiconductor test device 100 . In particular, the control unit 140 may determine whether the DUT is faulty or not, based on the test input signal and on the test output signal acquired from the DUT.
[0071] For example, the control unit 140 may determine whether the DUT is normal or not by comparing the waveform of the test vector information with the waveform of the test output signal.
[0072] FIG. 5 is a flowchart illustrating a semiconductor test method according to an exemplary embodiment of the present disclosure.
[0073] According to an exemplary embodiment of the present disclosure, the test information acquisition unit 110 may acquire test information (S 510 ).
[0074] The test information acquisition unit 110 may determine whether the test information is of a format suitable for being used in the semiconductor test device 100 .
[0075] For example, if the test information acquired by the test information acquisition unit 110 is of a VCD format acquired from a simulator, of a WGL format acquired from a TPG, or of a STIL format, the test information acquisition unit 110 may convert the test information into an ATE ASCII format. Further, if the test information acquired by the test information acquisition unit 110 is an ATE binary format, the test information acquisition unit 110 may convert the test information into an ATE ASCII format.
[0076] Further, according to an exemplary embodiment of the present disclosure, the test information conversion unit 120 may convert the test information into test vector information including a plurality of test vectors (S 520 ).
[0077] For example, the test vector information storage unit 130 may store the test vector information therein. Specifically, the test vector information storage unit 130 may store a pattern of the test vector therein.
[0078] Additionally, the test signal generation unit 150 may generate a test input signal based on the test vector information (S 530 ).
[0079] The test input signal may be a binary pattern.
[0080] Further, according to an exemplary embodiment of the present disclosure, the sense unit 160 may acquire a test output signal in response to the test input signal (S 540 ).
[0081] Moreover, according to an exemplary embodiment of the present disclosure, the control unit 140 may determine whether a DUT is faulty or not based on the test input signal and on the test output signals (S 550 ).
[0082] In addition, according to an exemplary embodiment of the present disclosure, the semiconductor test device 100 may acquire a plurality of test information items.
[0083] In this case, the semiconductor test device 100 may apply test vector information on to each of the plurality of test information items to a plurality of pins of the DUT.
[0084] Alternatively, the semiconductor test device 100 may apply test vector information on each of the plurality of test information items to a plurality of DUTs.
[0085] The above-described methods according to the embodiments maybe used separately from or in combination with one another. Further, operations in each of the exemplary embodiments maybe used separately from or in combination with operations in other exemplary embodiments.
[0086] Further, the above-described methods maybe implemented, for example, in a recording medium that is readable by a computer or a similar device by using software, hardware or a combination thereof.
[0087] When implemented as hardware, exemplary embodiments described above may be implemented using at least one of Application Specific Integrated Circuits (ASICs), Digital Signal Processors (DSPs), Digital Signal Processing Devices (DSPDs), Programmable Logic Devices (PLDs), Field Programmable Gate Arrays (FPGAs), processors, controllers, microcontrollers, microprocessors, and electrical units for performing functions.
[0088] When implemented as software, the procedures and functions described herein may be implemented as separate software modules. The software modules maybe implemented with software code written in an appropriate programming language. The software code may be stored in a storage unit and may be executed by a processor.
[0089] As set forth above, according to exemplary embodiments of the present disclosure, a semiconductor test device and a semiconductor test method capable of testing a semiconductor device faster may be provided.
[0090] Further, according to exemplary embodiments of the present disclosure, a semiconductor test device and a semiconductor test method capable of efficiently storing a test input signal may be provided.
[0091] While exemplary embodiments have been shown and described above, it will be apparent to those skilled in the art that modifications and variations could be made without departing from the spirit and scope of the present disclosure as defined by the appended claims.
|
There is provided a semiconductor test device, including: a test information acquisition unit acquiring test information; a test information conversion unit converting the acquired test information into test vector information including a plurality of test vectors; and a test signal generation unit generating a test input signal based on the test vector information.
| 6
|
FIELD OF THE INVENTION
The present invention relates to a twin wire former that is used as a former (i.e. having a formation forming section) in a paper making machine.
DESCRIPTION OF THE RELATED ART
What determines the nature of a paper sheet is mostly the performance of a paper making machine from an initial portion thereof to a former. With respect to the performance required for this former, it is required that retention of raw material is good, that a paper sheet having a large strength can be formed, that only small differences in quality exists such as printability or the like between the front and back surfaces of the paper sheet, that a paper sheet having a large surface strength can be formed, that high speed operation is possible, and that the former can be operated consistently, etc. While various types of formers have been invented in order to fulfill these requirements, any one of them has not fulfilled all the requirements. In the case of the Bel-Baie former in the prior art as shown in FIG. 3, although these requirements were almost fulfilled, there were difficulties in the retention of fine raw material and in the coupling strength in a thicknesswise direction of paper sheets formed thereby.
According to research and investigation, it has been known that after a raw material liquid has been sandwiched between two wires, if dewatering is carried out while scrubbing the wire with a fixed body, then a lot of fine raw material would flow therefrom, that is, retention is lowered. If one employs the construction such that the number of fixed bodies for scrubbing the wire such as shoe blades a, suction boxes b and the like in FIG. 3 are reduced and the number of dewatering means comprising a rotary body such as a suction couch roll c and the like are increased in order to improve the retention, then while the retention is improved, the formation is deteriorated.
With regard to the strength in the thicknesswise direction of a paper sheet, if a paper raw material liquid is sandwiched between two wires d and e and dewatering is effected from the both surfaces to form a fiber mat, then a paper sheet having a structure in which the coupling strength in the thicknesswise direction is low as compared to the case where dewatering is effected from only one surface to form a fiber mat, is formed. In order to reduce differences between the top and bottom surfaces of a paper sheet, it is necessary to dewater at both surfaces to form a mat, and for that purpose, considerably asymmetric both-surface dewatering would suffice. In the case of the asymmetric both-surface dewatering, lowering of the coupling strength in the thicknesswise direction can be also suppressed to a little extent.
In the above-mentioned type of formers, many formers in which a top wire unit is provided at a rear portion of a long wire, are known. One example of the formers is illustrated in FIG. 4. However, in such type of former as shown in FIG. 4, that is, in the former of the type that a long wire f and a twin wire former g in the prior art are joined together (hybrid former), when carrying out high speed operation, a raw material liquid is subjected to an excessive influence by pulse pressure produced by dewatering elements such as foils or the like provided in the portion of the long wire f, resulting in the destruction of the texture of the paper. Therefore, the former was not always suitable for high speed operation. It is to be noted that h in FIGS. 3 and 4 represents a headbox, i in FIG. 3 represents a water deflector, and j represents a vacuum deflector.
SUMMARY OF THE INVENTION
It is therefore one object of the present invention to resolve the difficulties in the prior art twin wire formers with respect to the retention to fine raw material and the coupling strength in the thicknesswise direction of a paper sheet, without an accompanying problem of the texture is being deteriorated or that the former is not suitable for high speed operation being presented.
To that end, according to the present invention, in a twin wire former the top wire is partly provided with a portion in which a water-impermeable belt is made to travel along the inside of the loop, so that dewatering in this portion is effected only on one side, i.e. the bottom wire side, and in this portion a wrapping angle for the wire is varied by adjusting the positions of a plurality of rolls or shoes to improve the formation. Thereafter, dewatering on the side where dewatering has been suppressed by the above-mentioned belt is also effected, and this construction is employed as a measure for resolving the problems.
The present invention will be explained below with reference to its preferred embodiment illustrated in the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side cross-sectional view showing one preferred embodiment of a twin wire former according to the present invention.
FIG. 2 is a perspective view illustrating that fiber distribution is improved by the present invention.
FIG. 3 is a side cross-sectional view of a prior art Bel-Baie former.
FIG. 4 is a side cross-sectional view of a prior art hybrid former.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows the preferred embodiment of the present invention in which raw material ejected from a headbox 36 is sandwiched between a bottom wire 33 and a top wire 34. However, initially, upward dewatering is not effected because a water-impermeable belt 35 is traveling along the top wire 34. In addition, a breast roll 1 is supported in a vertically adjustable manner.
Reference numeral 2 designates forming boards, and numeral 3 designates open rolls which enable adjustment of a wrapping angle of the bottom wire by adjustment of their vertical positions. Reference numeral 4 designates deflectors which prevent white water removed at the portion of the forming boards 2 from striking against the open rolls so as to not be brought again into inlet nips between the bottom wire 33 and the open rolls 3. The deflector 4 can be adjusted with respect to the engagement thereof with the wire in accordance with the vertical position adjustment of the breast roll 1 or the open rolls 3. The forming boards 2 are also adjustable. It is assumed that multiple open rolls 3 and the deflectors 4 are provided. A roll 5 is an open roll similar to the open rolls 3 or a suction roll, but its position is fixed.
Reference numeral 6 designates an optional suction box. In addition, while reference numeral 7 designates a suction box. Its surface is a curved, and it ensures that a fiber mat leaves the top wire 34 and travels on the bottom wire 33. Numeral 8 designates a suction couch roll, numeral 9 designates a turning roll, numeral 10 designates a return wire roll, numeral 11 designates a wire guide roll, and numeral 12 designates a stretch roll.
A wet paper sheet is transferred by a suction roll 37 to a felt 38 and is carried to a press. A top breast roll 13 is vertically adjustable similarly to the breast roll 1, and so it is possible to gradually pinch a jet by reducing a converging angle between the top wire 34 and the bottom wire 33. Reference numeral 15 designates a beam extending in the widthwise direction over the entire width, and it is possible to detachably mount a shoe 14 to the beam 15. The extent to which the top wire 34 is pressed downwards via the belt 35 can be adjusted by employing shoes having different thicknesses or different configurations. Reference numeral 16 designates a shower which feeds lubricant water between the shoes 14 and the belt 35. While the sets of shoes 14 and the shower 16 can be provided respectively behind the rolls 3, the same function performed thereby can be achieved by a roll 17 that is vertically adjustable in position. Or else, as different means, a set of shoes 18 and a pressurizing tube 21 could be employed.
More particularly, the shoe 18 is mounted on a beam 19 extending over the entire width so as to be rotatable about a fulcrum, and the extent to which the top wire 34 is depressed is adjusted by regulating the pressure in the pressurizing tube 21. In order to apply a strong wedge pressure to the raw material sandwiched between both the top and bottom wires, it is also possible to place the shoe 18 above the deflector 4. Or else, as an alternative method, it is also possible that the lower surface of the beam 22 extending over the entire width is used as a shoe and that the amount of depression of the top wire 34 is adjusted by vertically moving this portion.
A roll 23 is supported so as to be vertically adjustable in position, and thereby a wrapping angle of the belt 35 around the roll 5 can be adjusted. Reference numeral 24 designates a stretch roll for the belt 35, numeral 25 designates a guide roll, and numeral 26 designates support rolls for the belt, the rolls being able to simultaneously support the wire 34. Reference numerals 27 and 29, respectively, designate casings for collecting white water extracted on the top wire side, the casings being able to employ a vacuum in combination. Reference numeral 28 designates a wire roll, but it could be an open roll. Numeral 30 designates a stretch roll for the top wire, numeral 31 designates a wire roll, and numeral 32 designates a guide roll.
Now, describing an operation with respect to the preferred embodiment constructed in the above-described manner, based on the adjustment of the positions in the vertical direction of the breast roll 1, the top breast roll 13 and the first open roll 3, a raw material jet ejected from the headbox 36 is gradually sandwiched between two wires 33 and 34 Furthermore, the wrapping angle of the both wires 33 and 34 about the open roll 3 is based upon the position of the adjustable open roll 3. In addition, by adjusting the positions of the shoes 14 and 18, the roll 17, the beam 22 and the like in the direction of the wires, the wrapping angles of the both wires 33 and 34 around these members can be varied, and at the same time the wrapping angles of the both wires 33 and 34 around the open roll 3 and the roll 5 can be adjusted.
At such locations where a wrapping angle exists, due to tension in the wire 33 or in the wire 34 and belt 35 positioned outside of the arc, a pressing pressure acts upon the raw material liquid placed between the two wires, and so, dewatering is effected. In order for the raw material liquid sandwiched between the two wires to pass through the dewatering section in the direction of traveling, it must move from a low pressure side to a high pressure side, and so, it passes while the energy associated with the velocity of the belts is converted to pressure. In other words, the raw material liquid enters the dewatering section while the traveling velocity is reduced and while a dynamic pressure is converted into a static pressure. In the case where the dewatering section is long, the once decelerated raw material liquid is again accelerated by the wires traveling nearly at the same velocity to the same velocity, but in the case where the wrapping angles of the respective dewatering sections are small as shown in FIG. 1, the raw material which has passed a high pressure portion would travel at the wire velocity in a large proportion due to the conversion of a static pressure to dynamic pressure. In any event, each time the raw material passes through the locations of the plurality of rolls 3, the roll 5, the shoes 14 and 18, the roll 17, the beam 22 and the like, dewatering is effected at the respective locations, and acceleration and deceleration in the traveling direction are appropriately applied to the raw material liquid.
The explanation for the fact that if such acceleration and deceleration are applied appropriately, then dispersion of fibers is improved, is set forth in Laid-Open Japanese Patent Specification No. 57-89694 published June 4, 1982 and relating to a headbox, and it can be easily confirmed through a simple experiment as illustrated in FIG. 2. That is, paper making raw material 41 is enclosed in a transparent bag 40 made of plastics and is placed on a table, then a roll-like body 42 such as a rod or the like is pressed against it and moved up and down to move the raw material 41 is to the left and to the right. While this roll-like body 42 is held in the state of lightly pressing the bag 40, the rod-like body 42 is moved to the left and to the right by rolling it along the surface of the bag 40, and thereby the raw material 41 in the bag 40 is moved to the left and the right. If such movement is repeated, dispersion of the raw material 41 in the bag 40 becomes uniform.
In the arrangement as shown in FIG. 1, the movement of the raw material for improving dispersion of fibers is similar to the above-described experiment, and is effected under an adjustable condition. During the period in which the raw material has been ejected from the headbox 36 until it reaches the roll 5, since the raw material is dewatered only on the side of the bottom wire 33, the number of repetitions of acceleration and deceleration for improving dispersion of fibers is increased. In addition, in the interval where the belt 35 is traveling along the top wire 34, since dewatering is effected downwards only, the dewatering is asymmetric although the upward dewatering in which the extracted water is collected in the casings 27 and 29 exists.
Therefore, a reduction in the coupling strength in the thicknesswise direction also can be suppressed. In the initial portion of the former where the amount of dewatering is large, since dewatering is effected on the rollers and the wires are not scrubbed by a fixed body, retention is high (although the shoes 14 and 18 and the beam 22 scrub the belt 35, since the belt 35 is traveling at the same velocity as the wire, the wires are not scrubbed by a fixed body). Dewatering of raw material in a liquid state is not effected on a free surface thereof, but it is effected entirely in the state where the raw material is sandwiched between two wires, the state being adjustable, and so, even upon high speed operation no problem arises.
After the downward dewatering has proceeded, the consistency of the raw material has been raised. In order to improve the dispersion, it becomes necessary to carry out abrupt acceleration and deceleration with a stronger pressure variation. In such a case, the set consisting of the shower 16, the shoe 18 and the tube 21 or consisting of the shower 16 and the beam 22 could be provided above the deflector 4. In this case, since the amount of downward dewatering has been reduced, reduction in the retention is not influenced so much.
As to the open roll 3, if a perforated cell such as a suction roll around which a wire is wound, is used therefor, then the dewatering effected at the portion of the roll 3 on the side of the bottom wire 33 is accompanied by a flow tending to move the raw material between the two wires 33 and 34 towards the holes of the cell. Since multiple open rolls 3 are provided, at the location of the next roll, the raw material is moved in a different direction. Such reciprocating movement of the raw material along a plane is effective for uniformly dispersing fibers similarly to the accelerating and decelerating flow as described previously. In the former having the arrangement shown in FIG. 1, an effect of improving the formation of paper due to such actions is also provided.
As explained above, the present invention can achieve excellent effects in that since formation forming on a free surface is not effected, the former is suitable for high speed operation. Also, since adjustable asymmetric dewatering is effected, only small differences exist between the top and bottom sides of the paper sheet, balance for maintaining the lowering of the coupling strength in the thicknesswise direction minimum can be established and also improvement in the formation can be achieved. Moreover, since dewatering is effected mainly by rotary rolls or a belt, a reduction in retention does not occur, and since both surface dewatering is also effected, a surface strength is also high.
|
The present invention relates to a twin wire former. It aims at resolving the difficulties with respect to the retention of fine raw material and the coupling strength in the thicknesswise direction of a paper sheet without deteriorating the formation and without causing problems associated with high speed operation. A top wire (34) is partly provided with a portion in which a water-impermeable belt (35) travels along the inside of its loop. Dewatering in this portion is effected only on one side, that is, on the side of the bottom wire (33). Also in this portion, wrapping angles for the wires (33) and (34) are varied by adjusting the positions of a plurality of rolls (3), (17) and (23) or shoes (14) and (18) to improve the formation, and thereafter, dewatering on the side where dewatering has been suppressed by the above-mentioned belt (35) is also effected.
| 3
|
FIELD OF THE INVENTION
This invention relates to a novel polymer compound having a fluorene residue in a side chain. In particular, it relates to a novel polymer compound which can form a charge transfer complex with an electron acceptor compound or an electron donor compound, and a charge transfer complex formed by addition of the electron acceptor compound or electron donor compound.
BACKGROUND OF THE INVENTION
As described in Tokkai 2000-319366, a polyester with a fluorene residue is already known. This polyester has excellent heat-resistance and transparency, high refractive index, low birefringence and low water absorptivity, and is therefore suitable as an optical instrument material. However, as there was almost no overlap of fluorene residues, it was difficult to make it express electrical characteristics using the properties of n-conjugated electrons.
It is also known that by adding an electron acceptor compound or an electron donor compound to a polymer material with a π-conjugated group such as polyacethylene or polyfluorene, a material exhibiting charge transport qualities will be obtained. However, as such a material is degraded by water or oxygen, there was a problem as to its stability as a material exhibiting charge transport qualities.
SUMMARY OF THE INVENTION
The inventor made a detailed study of polymer compounds having special electrical qualities due to the properties of π-conjugated electrons. As a result, it was discovered that a polyester having a fluorene residue in a side chain had unique electrical qualities, and forms a charge transfer complex of excellent stability with a suitable electron acceptor compound or electron donor compound, which led to the present invention.
It is therefore a first object of this invention to provide a polyester having π-conjugated electrons, that is a polyester having unique electrical qualities due to the properties of π-conjugated electrons.
It is a second object of this invention to provide a composition which forms a stable charge transfer complex with an electron acceptor compound or an electron donor compound.
The aforesaid objects of this invention are attained by a polyester expressed by the following structural formula 1.
In the formula, m is an integer equal to 2 or more.
Structural Formula 1
In addition, in the aforesaid structural formula, Ar is an aromatic group and this aromatic group may contain a heterocyclic ring.
R 1 is a carbon atom or absent (direct bond), R 2 –R 9 are hydrogen atoms, electron donor groups or electron attracting groups, R 20 , R 21 are hydrogen atoms or organic groups, and X is a hetero atom, hetero atom-containing group, organic group or absent (direct bond).
In this invention, it is preferred that R 1 is absent, i.e., that it is the end of a polymerizing unit.
DETAILED DESCRIPTION OF THE INVENTION
The hetero atom X in the structural formula 1 is —O—, —NR— or —S—. The organic group is preferably —(CH 2 )— or an aromatic group.
The electron donor group in the aforesaid structural formula 1 of this invention is a functional group which, due to the introduction of a substituent, has an increased electron density in the fluorene residue and enhanced electron donor properties in the fluorene residue. This electron donor group may for example be —F, —Cl, —Br, —I, —OH, —OR, —O(C═O)R, —NR 10 R 11 , —SR, —SH or an alkyl group, but among these, —C 6 H 11 , -t-C 4 H 9 and —NR 10 R 11 are preferred. R, R 10 and R 11 may be H or an organic group, but preferably an aromatic group or an alkyl group. R 20 , R 21 may be a hydrogen atom, alkyl group, aromatic group, —CN or ester group.
The electron attracting group is a functional group which, due to the introduction of a substituent, has a decreased electron density in the fluorene residue, and enhanced electron acceptor properties in the fluorene residue. This electron acceptor group may for example be —C≡N, —(C═O)R, —SO 2 —, —NO 2 , phenyl, —COOH or —COOR, but —C≡N and —NO 2 are preferred.
By introducing the aforesaid electron-attracting group and electron donor group into the polymer, a more stable charge-transfer complex is obtained when an electron donor compound and electron acceptor compound, described later, are added.
Preferred combinations of R 2 –R 9 are:
(1) all of R 2 –R 9 are H; (2) R 3 , R 8 are NR 10 R 11 (R 10 , R 11 are respectively H, an alkyl group or an aromatic group), and R 2 , R 4 –R 7 , R 9 are H; (3) R 3 , R 8 are NH 2 , and R 2 , R 4 –R 7 , R 9 are H; (4) R 3 , R 8 are —N(C 6 H 5 ) 2 , and R 2 , R 4 –R 7 , R 9 are H; (5) R 3 , R 8 , R 6 are NO 2 , and R 2 , R 4 , R 5 , R 7 , R 9 are H; (6) R 3 , R 8 are NO 2 , and R 2 , R 4 –R 7 , R 9 are H; (7) R 3 , R 8 , R 6 are CN, and R 2 , R 4 , R 5 , R 7 , R 9 are H; (8) R 3 , R 8 are CN, R 2 , R 4 –R 7 , R 9 are H.
The electron acceptor compound described above is a compound having a stronger electron affinity than the polymer of structural formula 1. Examples are the following halogens, Lewis acids, proton acids and transition metal halogens etc. Halogens: I 2 , Br 2 , Cl 2 , ICl, ICl 3 , IBr, IF Lewis acids: BF 3 , PF 5 , AsF 5 , SbF 5 , SO 3 , BBr 5 , BF 4 − , PF 6 − , AsF 6 − , SbF 6 − , ClO 4 −
Proton acids: HNO 3 , H 2 SO 4 , HClO 4 , HF, HCl, FSO 3 H, CFSO 3 H Transition metal halides: FeCl 3 , MoCl 5 , WCl 5 , SnCl 4 , MoF 5 , FeOCl, RuF 5 , TaBr 5 , SnI 4 , LnCl 3 (Ln is La, Ce, Pr, Nd or Sm). Others: (9-fluorenylidene)acetonitrile, (9-fluorenylidene)malononitrile, (2,4,7-trinitro-9-fluorenylidene)acetonitrile, (2,4,7-trinitro-9-fluorenylidene)malononitrile, o-dinitrobenzene, m-dinitrobenzene, p-dinitrobenzene, 2,4,7-trinitrobenzene, 2,4,7-trinitrotoluene, TCNQ, TCNE, DDQ.
On the other hand, the electron donor compound is a compound having a smaller ionization potential than the polymer of structural formula 1. Examples are hexamethylbenzene, alkali metals, ammonium ion and lanthanoids.
When an electron-attracting functional group is introduced into a fluorene residue, an electron donor compound is preferably added, and when an electron donor functional group is introduced into a fluorene residue, an electron acceptor compound is preferably added. A stable charge-transfer type complex is thus obtained.
(Synthesis Method)
To synthesize the polymer of this invention, for example, the following compounds may be polycondensed using the usual catalyst.
R 1 –R 9 , and R 20 , R 21 are respectively identical to R 1 –R 9 , and R 20 , R 21 in structural formula 1.
The molecular weight of the polymer is preferably 400–1 million but more preferably 800–100,000 in terms of number average molecular weight. If it is less than 400, it is rare for an electron acceptor compound or electron donor compound to enter between fluorene residues, and if it is more than 1 million, the solubility decreases.
The distance between fluorene residues is 4–20 Å, but preferably 5–10 Å. If it is less than 4 Å, the electron acceptor compound or electron donor compound cannot enter between fluorene residues. If it is more than 20 Å, the electron acceptor compound or electron donor compound which entered between fluorene residues cannot easily form an electron donor-acceptor complex.
Tg of the polymer is preferably 30–300° C., but more preferably 80–200° C. When Tg is less than 30° C., formation of the electron donor-acceptor complex is blocked by structural change of the polymer due to temperature change.
If the aforesaid conditions are satisfied, a stable electron donor-acceptor complex can be obtained. Such a stable electron donor-acceptor complex is suitable as a charge transport material, for example as a hole transport layer of an organic EL or a solar cell. Such a charge transport material can be easily manufactured by a known method, such as spin coating.
EXAMPLES
Hereafter, this invention will be described in further detail referring to examples, but this invention is not to be construed as being limited in any way thereby.
Example 1
Polymer Synthesis
Synthesis of 9-hydroxymethyl-9-fluorene carboxylic acid (monomer)
9-fluorene carboxylic acid (4.98 g, 23.7 mmol) and anhydrous THF (300 ml) were introduced into a flame-dried reaction vessel in which the atmosphere had been replaced by nitrogen, the reaction solution was cooled to −78° C., and n-butyl lithium (41.0 ml of 1.6M hexane solution, 71.0 mmol) was added. After stirring the reaction solution at −78° C. for 30 minutes, paraformaldehyde (2.30 g, 75.0 mmol) dissolved in anhydrous THF (100 ml) was added at −78° C., and stirred at room temperature for 13 hours. Distilled water was added, the solution was extracted with ether, and the pH of the aqueous layer was adjusted to 2 using 1N hydrochloric acid. It was then extracted again with chloroform, and the organic layer was dried by anhydrous magnesium sulfate. The low-boiling fraction was distilled under reduced pressure with the rotary evaporator, and 4.21 g of crude product was thus obtained. The methylene chloride-insoluble fraction of this crude product was collected, and the target compound (4.60 g, 19.3 mmol, 80.5%) was thus obtained. 1 H-NMR (500 MHz, CDCl 3 ) d: 7.78 (d, J=7.5, 2H), 7.67 (d, J=7.5, 2H), 7.46 (dd, J=7.0, 2H), 7.54 (dd, J=8.0, 2H), 4.02(s, 4H).
Synthesis of polymer using 9-hydroxymethyl-9-fluorene carboxylic acid as starting material
9-hydroxymethyl-9-fluorene carboxylic acid (50.4 mg, 0.21 mmol) and 0.9 mg of a catalyst (CF 3 SO 3 ) 2 Sn were introduced into a reaction vessel (9 mm Φ×50 mm), and the mixture was shaken to render it uniform. Subsequently, it was heated at 180° C. for 3 hours while blowing in nitrogen (a syringe needle was fixed over about 2 mm of compound). After 3 hours, the obtained compound was separated by decantation into a THF soluble part (47.1 mg) and a THF-insoluble part (2.20 mg). The dried and weighed THF-soluble part was re-dissolved in THF (3 ml), diazomethane (ether solution, 1 ml) was slowly dripped in with stirring, and stirred at room temperature for 5 hours. After 5 hours, the solvent and volatile component were distilled off with the rotary evaporator, the obtained crude product was divided into a methanol-soluble part (8.10 mg) and methanol-insoluble part (34.9 mg), and the methanol-insoluble part was divided into a THF-soluble part (14.19 mg) and a THF-insoluble part (20.64 mg). The part which was insoluble in methanol but soluble in THF had a molecular weight distribution of approx. 1,000 to 10 5 (SEC, polystyrene conversion).
Example 2
Polymer Synthesis
Anhydrous methylene chloride (17 ml) was added to 9-hydroxy-9-fluorene carboxylic acid (1.01 g, 4.42 mmol) in a flame-dried reaction vessel in which the atmosphere had been replaced by nitrogen, and stirred at room temperature for 5 minutes to give a uniform solution. Anhydrous triethylamine (0.62 ml, 4.502 mmol) was then dripped in. The reaction solution was stirred at room temperature for 30 minutes, and an anhydrous methylene chloride (3 ml) solution of p-tosyl chloride (762 mg, 4.42 mmol) was dripped in. The reaction solution was stirred at room temperature for 15 hours and extracted with chloroform, and the organic layer was dried by anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure with the rotary evaporator, and the obtained crude product was classified into a hexane-soluble part (111 mg) and a hexane-insoluble part (777 mg). The hexane-insoluble part was dissolved in THF (20 ml), diazomethane (ether solution, 3 ml) was gradually dripped in with stirring, and the solution stirred at room temperature for 5 hours. The reaction product was a mixture of polymers consisting of 2–10 monomers. This polymer mixture was classified by recycling liquid chromatography, and the pure dimer, trimer and tetramer were thus obtained.
Example 3
D-A Complexing, Spectrometry
Formation of D-A complex from poly(9-hydroxymethyl-9-fluorene carboxylic acid) and m-dinitrobenzene (DNB)
1. Absorption Spectrum Measurement in Solution
The polymer (2.98 mg) and DNB (1.80 mg, 0.01 mmol) were dissolved in THF for ultraviolet absorption spectra to give 10 ml of solution. This was diluted 100 times, and used for absorption spectrum measurements (quartz cell; 10 mm) at room temperature. The absorption intensity of the polymer and DNB mixture was smaller than the absorption intensity of the polymer alone. The intensity which was 0.140 at 242 nm changed to 0.108 after adding DNB. This change depended on the concentration, and when the DNB concentration was changed to 2.5×10 −5 M and 5.0×10 −5 M, the absorption intensity at 242 nm changed to 0.077 and 0.059, respectively. This hypochromic effect proved that the fluorene ring of the polymer and DNB formed a stacked complex.
The absorption at long wavelength extended from 310 nm to 345 nm.
2. D-A Complexing in Solid State
The polymer (100 mg) and m-nitrobenzene (100 mg) were taken up as a CH 2 Cl 2 solution, and the light red solid produced while distilling off the solvent was collected. When this was again dissolved in CH 2 Cl 2 and the solvent was distilled off, thin red acicular crystals were obtained.
Example 4
Formation of D-A complex using poly(9-hydroxy-9-fluorene carboxylic acid) and 2,4,7-trinitrol-9-fluorenylidene malononitrile (TNFMN)
1. Absorption Spectrum Measurement in Solution
TNFMN (363.3 mg, 1.0 mmol) was dissolved in methylene chloride solvent for ultraviolet absorption spectra to give 100 ml of solution. Next, a polymer (10.4 mg of a mixture of polymer consisting of 2–10 monomers, 0.05 mmol in monomer units) was dissolved using this solution. The absorption spectrum was measured at room temperature on 1 ml of solution (quartz cell; 0.1 mm). As a result of this measurement, new peaks due to a D-A complex, 386 nm (λ max =0.038) and 488 nm (λ max =0.009), were observed.
2. D-A Complexing in Solid State
TNFMN (15.1 mg, 0.04 mmol) and a polymer (10.4 mg, 0.05 mmol in monomer units) were put into methylene chloride solution, and the solvent was distilled off to dryness to give an orange-red solid. A composition analysis by 1 HNMR of this solid showed that the proportion of monomer units:TNFMN was 1:1.
Example 5
D-A complexing using trimer of 9-hydroxy-9-fluorene carboxylic acid and TNFMN
1. Absorption Spectrum Measurement in Solution
TNFMN (363.3 mg, 11.0 mmol) was dissolved in methylene chloride solvent for ultraviolet absorption spectra to give 100 ml of solution. Next, the trimer (10.4 mg, 0.05 mmol in monomer units) was dissolved using this solution, and the absorption spectrum was measured at room temperature on 1 ml of solution (quartz cell; 0.1 mm). As a result, new peaks due to the D-A complex, 388 nm (λ max =0.037) and 489 nm (λ max =0.009), were observed. These absorption intensities depended on concentration, and when the concentration of fluorene was changed to 0.03M and 0.04M, the absorption intensity at 388 nm changed to 0.022 and 0.029, respectively.
2. D-A Complexing in Solid State
TNFMN (15.1 mg, 0.04 mmol) and a trimer (10.4 mg, 0.05 mmol in monomer units) were put into methylene chloride solution, and the solvent was distilled off to dryness to give an orange solid. A composition analysis by 1 HNMR of this solid showed the proportion of monomer units:TNFMN was 1:1.
Example 6
Conductivity: Time of Flight Measurement
A mixture having a polymerization degree of approx. 20 (principal components are dimer-tetramer) was taken in CH 2 Cl 2 solution, 1% 2,4,7-trinitrofluorene malononitrile was added to this, and dissolved. The solution was then spread on an ITO glass substrate, and dried to produce a thin film (1 μm thickness). Aluminum was deposited on the obtained film (thickness 1000 Å, area 5 mm×5 mm). A voltage of 5.0V was applied between the ITO and aluminum using TOF301 (Optel, Inc.), a 337 nm pulse laser (nitrogen laser, pulse width, 1 ns, 150 μJ) was simultaneously irradiated from the ITO side, and the time of flight was measured. From the test results at room temperature, the hole mobility was determined as 1.20×10 −4 cm 2 V −1 sec −1 .
INDUSTRIAL APPLICATION
The polyester of this invention has a fluorene residue in a side chain, and it can form a charge transfer complex having excellent stability with an electron acceptor compound or electron donor compound. It is therefore suitable as a charge transport material such as an organic EL material, or the hole transport layer of a solar cell.
|
A polyester expressed by the following structural formula 1, and a charge transport material obtained by adding an electron acceptor compound or an electron donor compound to this polyester.
In the aforesaid structural formula, Ar is an aromatic group and this aromatic group may contain a heterocyclic ring.
R 1 is a carbon atom or absent (direct bond), R 2 –R 9 are hydrogen atoms, electron donor groups or electron attracting groups, R 20 , R 21 are hydrogen atoms or organic groups, X is a hetero atom, hetero atom-containing group, organic group or absent (direct bond), and m is an integer equal to 2 or more.
| 6
|
RELATED APPLICATIONS
This application is a continuation of and claims priority to International Application No. PCT/US00/01788 filed Jan. 25, 2000, which claims priority to U.S. Ser. No. 60/117,169 filed on Jan. 25, 1999 and U.S. Ser. No. 60/143,228 filed Jul. 9, 1999. The entire disclosures of the aforesaid patent applications are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to the use of a ligand, BAFF, a β-cell activating factor belonging to the Tumor Necrosis Family and its blocking agents to either stimulate or inhibit the expression of B-cells and immunoglobulins. This protein and its receptor may have anti-cancer and/or immunoregulatory applications as well as uses for the treatment of immunosuppressive disorders such as HIV. Specifically, the ligand and its blocking agents may play a role in the development of hypertension and its related disorders. Furthermore, cells transfected with the gene for this ligand may be used in gene therapy to treat tumors, autoimmune diseases or inherited genetic disorders involving B-cells. Blocking agents, such as recombinant variants or antibodies specific to the ligand or its receptor, may have immunoregulatory applications as well. Use of BAFF as a B-cell stimulator for immune suppressed diseases including for example uses for patients undergoing organ transplantation (ie bone marrow transplant) as well as recovering from cancer treatments to stimulate production of B-cells are contemplated. Use of BAFF as an adjuvant and or costimulator to boast and or restore B cells levels to approximate normal levels are also contemplated.
BACKGROUND OF THE INVENTION
The tumor-necrosis factor (TNF)-related cytokines are mediators of host defense and immune regulation. Members of this family exist in membrane-anchored forms, acting locally through cell-to-cell contact, or as secreted proteins capable of diffusing to more distant targets. A parallel family of receptors signals the presence of these molecules leading to the initiation of cell death or cellular proliferation and differentiation in the target tissue. Presently, the TNF family of ligands and receptors has at least 11 recognized receptor-ligand pairs, including: TNF:TNF-R; LT-α:TNF-R; LT-α/β:LT-β-R; FasL:Fas; CD40L:CD40; CD30L:CD30; CD27L:CD27; OX40L:OX40 and 4-1BBL:4-1BB. The DNA sequences encoding these ligands have only about 25% to about 30% identity in even the most related cases, although the amino acid relatedness is about 50%.
The defining feature of this family of cytokine receptors is found in the cysteine rich extracellular domain initially revealed by the molecular cloning of two distinct TNF receptors. This family of genes encodes glycoproteins characteristic of Type I transmembrane proteins with an extracellular ligand binding domain, a single membrane spanning region and a cytoplasmic region involved in activating cellular functions. The cysteine-rich ligand binding region exhibits a tightly knit disulfide linked core domain, which, depending upon the particular family member, is repeated multiple times. Most receptors have four domains, although there may be as few as three, or as many as six.
Proteins in the TNF family of ligands are characterized by a short N-terminal stretch of normally short hydrophilic amino acids, often containing several lysine or arginine residues thought to serve as stop transfer sequences. Next follows a transmembrane region and an extracellular region of variable length, that separates the C-terminal receptor binding domain from the membrane. This region is sometimes referred to as the “stalk”. The C-terminal binding region comprises the bulk of the protein, and often, but not always, contains glycosylation sites. These genes lack the classic signal sequences characteristic of type I membrane proteins, type II membrane proteins with the C terminus lying outside the cell, and a short N-terminal domain residing in the cytoplasm. In some cases, e.g., TNF and LT-α, cleavage in the stalk region can occur early during protein processing and the ligand is then found primarily in secreted form. Most ligands, however, exist in a membrane form, mediating localized signaling.
The structure of these ligands has been well-defined by crystallographic analyses of TNF, LT-α, and CD40L. TNF and lymphotoxin-I (LT-I) are both structured into a sandwich of two anti-parallel β-pleated sheets with the “jelly roll” or Greek key topology. The rms deviation between the Cα and β residues is 0.61 C, suggesting a high degree of similarity in their molecular topography. A structural feature emerging from molecular studies of CD40L, TNF and LT-α is the propensity to assemble into oligomeric complexes. Intrinsic to the oligomeric structure is the formation of the receptor binding site at the junction between the neighboring subunits creating a multivalent ligand. The quaternary structures of TNF, CD40L and LTα have been shown to exist as trimers by analysis of their crystal structures. Many of the amino acids conserved between the different ligands are in stretches of the scaffold β-sheet. It is likely that the basic sandwich structure is preserved in all of these molecules, since portions of these scaffold sequences are conserved across the various family members. The quaternary structure may also be maintained since the subunit conformation is likely to remain similar.
TNF family members can best be described as master switches in the immune system controlling both cell survival and differentiation. Only TNF and LTα, are currently recognized as secreted cytokines contrasting with the other predominantly membrane anchored members of the TNF family. While a membrane form of TNF has been well-characterized and is likely to have unique biological roles, secreted TNF functions as a general alarm signaling to cells more distant from the site of the triggering event. Thus TNF secretion can amplify an event leading to the well-described changes in the vasculature lining and the inflammatory state of cells. In contrast, the membrane bound members of the family send signals though the TNF type receptors only to cells in direct contact. For example T cells provide CD40 mediated “help” only to those B cells brought into direct contact via cognate TCR interactions. Similar cell-cell contact limitations on the ability to induce cell death apply to the well-studied Fas system.
It appears that one can segregate the TNF ligands into three groups based on their ability to induce cell death. First, TNF, Fas ligand and TRAIL can efficiently induce cell death in many lines and their receptors mostly likely have good canonical death domains. Presumably the ligand to DR-3 (TRAMP/WSL-1) would also all into this category. Next there are those ligands which trigger a weaker death signal limited to few cell types and TWEAK, CD30 ligand and LTa1b2 are examples of this class. How this group can trigger cell death in the absence of a canonical death domain is an interesting question and suggests that a separate weaker death signaling mechanism exists. Lastly, there are those members that cannot efficiently deliver a death signal. Probably all groups can have antiproliferative effects on some cell types consequent to inducing cell differentiation e.g. CD40. Funakoshi et al. (1994).
The TNF family has grown dramatically in recent years to encompass at least 11 different signaling pathways involving regulation of the immune system. The widespread expression patterns of TWEAK and TRAIL indicate that there is still more functional variety to be uncovered in this family. This aspect has been especially highlighted recently in the discovery of two receptors that affect the ability of rous sacroma and herpes simplex virus to replicate as well as the historical observations that TNF has anti-viral activity and pox viruses encode for decoy TNF receptors. Brojatsch et al. (1996); Montgomery et al. (1996); Smith et al. (1994), 76 Cell 959-962; Vassalli et al. (1992), 10 Immunol. 411-452.
TNF is a mediator of septic shock and cachexia, and is involved in the regulation of hematopoietic cell development. It appears to play a major role as a mediator of inflammation and defense against bacterial, viral and parasitic infections as well as having antitumor activity. TNF is also involved in different autoimmune diseases. TNF may be produced by several types of cells, including macrophages, fibroblasts, T cells and natural killer cells. TNF binds to two different receptors, each acting through specific intracellular signaling molecules, thus resulting in different effects of TNF. TNF can exist either as a membrane bound form or as a soluble secreted cytokine.
LT-I shares many activities with TNF, i.e. binding to the TNF receptors, but unlike TNF, appears to be secreted primarily by activated T cells and some β-lymphoblastoid tumors. The heteromeric complex of LT-α, and LT-β is a membrane bound complex which binds to the LT-βreceptor. The LT system (LTs and LT-R) appears to be involved in the development of peripheral lymphoid organs since genetic disruption of LT-β leads to disorganization of T and B cells in the spleen and an absence of lymph nodes. The LT-β system is also involved in cell death of some adenocarcinoma cell lines.
Fas-L, another member of the TNF family, is expressed predominantly on activated T cells. It induces the death of cells bearing its receptor, including tumor cells and HIV-infected cells, by a mechanism known as programmed cell death or apoptosis. Furthermore, deficiencies in either Fas or Fas-L may lead to lymphoproliferative disorders, confirming the role of the Fas system in the regulation of immune responses. The Fas system is also involved in liver damage resulting from hepatitis chronic infection and in autoimmunity in HIV-infected patients. The Fas system is also involved in T-cell destruction in HIV patients. TRAIL, another member of this family, also seems to be involved in the death of a wide variety of transformed cell lines of diverse origin.
CD40-L, another member of the TNF family, is expressed on T cells and induces the regulation of CD40-bearing B cells. Furthermore, alterations in the CD40-L gene result in a disease known as X-linked hyper-IgM syndrome. The CD40 system is also involved in different autoimmune diseases and CD40-L is known to have antiviral properties. Although the CD40 system is involved in the rescue of apoptotic B cells, in non-immune cells it induces apoptosis. Many additional lymphocyte members of the TNF family are also involved in costimulation.
Generally, the members of the TNF family have fundamental regulatory roles in controlling the immune system and activating acute host defense systems. Given the current progress in manipulating members of the TNF family for therapeutic benefit, it is likely that members of this family may provide unique means to control disease. Some of the ligands of this family can directly induce the apoptotic death of many transformed cells e.g. LT, TNF, Fas ligand and TRAIL. Nagata (1997) 88 Cell 355-365. Fas and possibly TNF and CD30 receptor activation can induce cell death in nontransformed lymphocytes which may play an immunoregulatory function. Amakawa et al. (1996) 84 Cell 551-562; Nagata (1997) 88 Cell 355-365; Sytwu et al. (1996); Zheng et al. (1995) 377 Nature 348-351. In general, death is triggered following the aggregation of death domains which reside on the cytoplasmic side of the TNF receptors. The death domain orchestrates the assembly of various signal transduction components which result in the activation of the caspase cascade. Nagata (1997) 88 Cell 355-365. Some receptors lack canonical death domains, e.g. LTb receptor and CD30 (Browning et al. (1996); Lee et al. (1996)) yet can induce cell death, albeit more weakly. It is likely that these receptors function primarily to induce cell differentiation and the death is an aberrant consequence in some transformed cell lines, although this picture is unclear as studies on the CD30 null mouse suggest a death role in negative selection in the thymus. Amakawa et al. (1996) 84 Cell 551-562. Conversely, signaling through other pathways such as CD40 is required to maintain cell survival. Thus, there is a need to identify and characterize additional molecules which are members of the TNF family thereby providing additional means of controlling disease and manipulating the immune system.
Here we characterize the functional properties of a new ligand of the TNF cytokine family. The new ligand, termed BAFF (B cell activating factor belonging to the TNF family), appears to be expressed by T cells and dendritic cells for the purpose of B-cell co-stimulation and may therefore play an important role in the control of B cell function. In addition, we have generated transgenic mice overexpressing BAFF under the control of a liver-specific promoter. These mice have excessive numbers of mature B cells, spontaneous germinal center reactions, secrete autoantibodies, and have high plasma cell numbers in secondary lymphoid organs and Ig deposition in the kidney.
SUMMARY OF THE INVENTION
Accordingly, the present invention is directed to the use of BAFF-ligands, blocking agents and antibodies for the ligand, to either stimulate or inhibit the growth of B-cells and the secretion of immunoglobulin. The claimed invention may be used for therapeutic applications in numerous diseases and disorders, as discussed in more detail below, as well as to obtain information about, and manipulate, the immune system and its processes. Further, this invention can be used as a method of stimulating or inhibiting the growth of B-cells and the secretion of immunoglobulins. BAFF associated molecules, as described by this invention, may also have utility in the treatment of autoimmune diseases, disorders relating to B-cell proliferation and maturation, BAFF ligand regulation and inflammation. The invention may be involved in the regulation or prevention of hypertension and hypertension-related disorders of the renal and cardiovascular tissue.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be apparent from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the methods particularly pointed out in the written description and claims hereof, as well as in the appended drawings.
Thus, to achieve these and other advantages, and in accordance with the purpose of the invention, as embodied and broadly described herein, the invention includes a method of effecting B-cell growth and secretion of immunoglobulins through the administration of various BAFF ligands and related molecules.
The invention also contemplates stimulating B-cell growth through the use of BAFF ligands or active fragments of the polypeptide. The polypeptide may be use alone or with a CD40 ligand or an anti-murine antibody.
In other embodiments, the invention relates to methods of stimulation of dendritic cell-induced B-cell growth and maturation through the use of BAFF ligands or active fragments of BAFF. Again, the polypeptide may be used alone or with CD40 ligand or anti-μ antibodies.
In other embodiments, blocking agents of BAFF and the BAFF receptor have been used to inhibit B-cell growth and immunoglobulin secretion. These agents can be inoperable, recombinant BAFF, BAFF specific antibodies, BAFF-receptor specific antibodies or an anti-BAFF ligand molecule.
In yet other embodiments, the invention relates to the use of BAFF, BAFF related molecules and BAFF blocking agents to treat hypertension, hypertension related disorders, immune disorders, autoimmune diseases, inflammation and B-cell lympho-proliferate disorders.
The invention encompasses the use of BAFF and BAFF-related molecules as either agonists or antagonists in effecting immune responses by effecting the growth and/or maturation of B-cells and secretion of immunoglobulin.
The invention relates in other embodiments to soluble constructs comprising BAFF which may be used to directly trigger BAFF mediated pharmacological events. Such events may have useful therapeutic benefits in the treatment of cancer, tumors or the manipulation of the immune system to treat immunologic diseases.
Additionally, in other embodiments the claimed invention relates to antibodies directed against BAFF ligand, which can be used, for example, for the treatment of cancers, and manipulation of the immune system to treat immunologic disease.
In yet other embodiments the invention relates to methods of gene therapy using the genes for BAFF.
The pharmaceutical preparations of the invention may, optionally, include pharmaceutically acceptable carriers, adjuvants, fillers, or other pharmaceutical compositions, and may be administered in any of the numerous forms or routes known in the art.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory, and are intended to provide further explanation of the invention as claimed.
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in, and constitute a part of this specification, illustrate several embodiments of the invention, and together with the description serve to explain the principles of the invention.
DESCRIPTION OF THE DRAWINGS
FIG. 1 (A) depicts the predicted amino acid sequence of human [SEQ. ID. NO.: 1] and mouse BAFF [SEQ. ID. NO.:2]. The predicted transmembrane domain (TMD, dashed line), the potential N-linked glycosylation sites (stars) and the natural processing site of human BAFF (arrow) are indicated. The double line above hBAFF indicates the sequence obtained by Edman degradation of the processed form of BAFF. (B) Depicts a comparison of the extracellular protein sequence of BAFF [SEQ. ID. NO.: 3] and some members of the TNF ligand family [SEQ. ID. NO.: 4 (hAPRIL); SEQ. ID. NO.: 5 (hTNF alpha); SEQ. ID. NO.: 6 (hFasL); SEQ. ID. NO.: 7 (hLT alpha); SEQ. ID. NO.: 8 (hRANKL)]. Identical and homologous residues are represented in black and shaded boxes, respectively. (C) Depicts dendrogram of TNF family ligands
FIG. 2 is a schematic characterization of recombinant BAFF (A) Schematic representation of recombinant BAFF constructs. Soluble recombinant BAFFs starting at Leu 83 and Gln 136 are expressed fused to a N-terminal Flag tag and a 6 amino acid linker. The long form is cleaved between Arg 133 and Ala 134 (arrow) in 293 T cells, to yield a processed form of BAFF. Asn 124 and Asn 242 belong to N-glycosylation consensus sites. N-linked glycan present on Asn 124 is shown as a Y. TMD: transmembrane domain. (B) Peptide N-glycanase F (PNGase F) treatment of recombinant BAFF. Concentrated supernatants containing Flag-tagged BAFFs and APRIL were deglycosylated and analyzed by Western blotting using polyclonal anti-BAFF antibodies or anti-Flag M2, as indicated. All bands except processed BAFF also reacted with anti-Flag M2 (data not shown). (C) Full length BAFF is processed to a soluble form. 293T cells were transiently transfected with full length BAFF. Transfected cells and their concentrated supernatants were analyzed by Western blotting using polyclonal anti-BAFF antibodies. Supernatants corresponding to 10× the amount of cells were loaded onto the gel. (D) Size exclusion chromatography of soluble BAFF on Superdex-200. Concentrated supernatants containing soluble BAFF/short were fractionated on a Superdex-200 column and the eluted fractions analyzed by Western blotting using anti-Flag M2 antibody. The migration positions of the molecular mass markers (in kDa) are indicated on the left-hand side for SDS-PAGE and at the top of the figure for size exclusion chromatography.
FIG. 3 depicts expression of BAFF (A) Northern blots (2 μg poly A + RNA per lane) of various human tissues were probed with BAFF antisense mRNA. (B) Reverse transcriptase amplification of BAFF, IL-2 receptor alpha chain and actin from RNA of purified blood T cells at various time points of PHA activation, E-rosetting negative blood cells (B cells and monocytes), in vitro derived immature dendritic cells, 293 cells, and 293 cells sterilely transfected with full length BAFF (293-BAFF). Control amplifications were performed in the absence of added cDNA. IL-2 receptor alpha chain was amplified as a marker of T cell activation.
FIG. 4 depicts BAFF binding to mature B cells. (A) Binding of soluble BAFF to BJAB and Jurkat cell lines, and to purified CD19 + cells of cord blood. Cells were stained with the indicated amount (in ng/50 μl) of Flag-BAFF and analyzed by flow cytometry. (B) Binding of soluble BAFF to PBLs. PBLs were stained with anti-CD8-FITC or with anti-CD19-FITC (horizontal axis) and with Flag-BAFF plus M2-biotin and avidin-PE (vertical axis). Flag-BAFF was omitted in controls.
FIG. 5 depicts BAFF costimulates B cell proliferation. (A) Surface expression of BAFF in stably transfected 293 cells. 293-BAFF and 293 wild-type cells were stained with anti-BAFF mAb 43.9 and analyzed by flow cytometry. (B) Costimulation of PBLs by 293-BAFF cells. PBLs (10 5 /well) were incubated with 15.000 glutaraldehyde-fixed 293 cells (293 wt or 293-BAFF) in the presence or absence of anti-B cell receptor antibody (anti-p). Fixed 293 cells alone incorporated 100 cpm. (C) Dose dependent costimulation of PBL proliferation by soluble BAFF in the presence of anti-μ. Proliferation was determined after 72 h incubation by [ 3 H]-thymidine incorporation. Controls include cells treated with BAFF alone, with heat-denatured BAFF or with an irrelevant isotype matched antibody in place of anti-μ. (D) Comparison of (co)stimulatory effects of sCD40L and sBAFF on PBL proliferation. Experiment was performed as described in panel C. (E) BAFF costimulates Ig secretion of preactivated human B cells. Purified CD19 + B cells were activated by coculture with EL-4 T cells and activated T cell supernatants for 5-6 d, then re-isolated and cultured for another 7 days in the presence of medium only (−) or containing 5% activated T cell supernatants (T-SUP) or a blend of cytokines (IL-2, IL-4, IL-10). The columns represent means of Ig concentrations for cultures with or without 1 μg/ml BAFF. Means± SD in terms of “fold increase” were 1.23±0.11 for medium only, 2.06±0.18 with T cell supernatants (4 experiments) and 1.45±0.06 with IL-2, IL-4 and IL-10 (2 experiments). These were performed with peripheral blood (3 experiments) or cord blood B cells (one experiment; 2.3 fold increase with T cell supernatants, 1.5 fold increase with IL-2, IL-4 and IL-10). (F) Dose-response curve for the effect of BAFF in cultures with T cell supernatants, as shown in panel D. Mean± SD of 3 experiments.
FIG. 6 depicts that BAFF acts as a cofactor for B cell proliferation. The proliferation of human PBL was measured alone (500 cpm), with the presence of BAFF ligand alone, with the presence of goat anti-murine (mu) alone, and with both BAFF ligand and anti-mu. The combination of both anti-mu and BAFF significantly raised proliferation of PBL as the concentration of BAFF increased suggesting BAFF's cofactor characteristics.
FIG. 7 depicts increased B cell numbers in BAFF Tg mice.
(A) Increased lymphocytes counts in BAFF Tg mice. The graph compares 12 control littermates (left panel) with 12 BAFF Tg mice (right panel). Lymphocytes counts are shown with circles and granulocytes (including neutrophils, eosinophils, basophils) with diamonds. (B) Increased proportion of B cells in PBL from BAFF Tg mice. PBL were stained with both anti-B220-FITC and anti-CD4-PE for FACS analysis and gated on live cells using the forward side scatter. Percentages of CD4 and B220 positive cells are indicated. One control mouse (left) and two BAFF Tg mice (right) are shown and the results were representative of 7 animals analysed in each group. (C) FACS analysis of the ratio of B to T cells in PBL. The difference between control animals and BAFF Tg mice in (A) and (C) was statistically significant (P<0.001). (D) Increased MHC class II expression on B cells from BAFF Tg mice PBL.
MHC class II expression was analysed by FACS.
(E) Increased Bcl-2 expression in B cells from BAFF Tg mice PBL.
Bcl-2 expression was measured by intracytoplasmic staining and cells were analysed by FACS. In both (D) and (E) Live cells were gated on the forward side scatter. Four control littermates (white bars) and 4 BAFF Tg mice are shown and are representative of at least 12 animals analysed for each group. MFI: mean of fluorescence intensity. The difference between control animals and BAFF Tg mice was statistically significant (P<0.005).
(F) Increased expression of effector T cells in BAFF Tg mice. PBL were stained with anti-CD4-Cychrome, anti-CD44-FITC and anti-L selectin-PE. Are shown CD4 + -gated cells. Percentages of CD44 hi /L-selectin lo cells are indicated. One control mouse (left) and two BAFF Tg mice (right) are shown and the results were representative of 8 animals analysed in each group.
FIG. 8 depicts ncreased B cell compartments in the spleen but not in the bone marrow of BAFF Tg mice.
(A) FACS staining for mature B cells using both anti-IgM-FITC and anti-B220-PE, in spleen (top panel), bone marrow (medium panel) and MLN (bottom panel). Percentages of B220+/IgM+mature B cells are indicated. (B) FACS staining for preB cells (B220+/CD43−) and proB cells (B220+/CD43+) in the bone marrow using anti-CD43-FITC, anti-B220-Cy-chrome and anti-IgM-PE simultaneously. Are shown cells gated on the IgM negative population. Percentages of preB cells (B220+/CD43−) and proB cells (B220+/CD43+) cells are indicated.
For all figures (A and B) one control mouse (left) and two BAFF Tg mice (right) are shown and results are representative of 7 animals analysed for each group.
FIG. 9 depicts increased Ig, RF and CIC levels in BAFF Tg mice
(A) SDS-PAGE of two control sera (−) and 4 sera from BAFF Tg mice (+) side by side with the indicated amount of a purified mouse IgG for reference. The intensity of the albumin band in similar in all lanes indicating that the material loaded on the gel is equivalent for each sample. ELISA-based analysis of total mouse Ig (B), RF (C) and CIC (D) in the sera of 19 control littermates (white bars) and 21 BAFF Tg mice (Black bars). In the absence of a proper RF control, the titer (log base 2) for RF is defined as the dilution of the sera giving an O.D. 3 times higher than that of background. The quantity of CIC is defined as the quantity of PAP required to generate an O.D. equivalent to that obtained with the tested serum. The difference between control animals and BAFF Tg mice was statistically significant (P<0.001 in (B) and (C), P<0.003 in (D)).
FIG. 10 depicts the presence of anti-ssDNA and anti-dsDNA autoantibodies in some BAFF Tg mice.
(A) Analysis by ELISA of anti-ssDNA autoantibodies in 19 control littermates (gray bars) and 21 BAFF Tg mice (black bars). (B) Analysis by ELISA of anti-ssDNA autoantibodies in 5 control littermates and the 5 animals showing levels of anti-ssDNA autoantibodies from (A). (C) Paraffin sections of kidneys from a control mouse (left) and a BAFF Tg mouse (right), stained with goat anti-mouse Ig-HRP. Ig deposition is shown by a brown staining. These pictures are representative of 6 BAFF Tg mice analysed.
FIG. 11 depicts enlarged Peyer's patches in BAFF Tg mice.
Photography of Peyers patches (indicated with an arrow) on the small intestine of a control mouse (left) and a BAFF Tg mouse (right). This pictures is representative of at least 12 mice sacrificed for each group. Magnification 5×
FIG. 12 depicts disrupted T and B cell organization, intense germinal center reactions, decreased number of dendritic cells and increased number of plasma cells in the spleen of BAFF Tg mice.
A control mouse is shown in A, C, E and G and a BAFF Tg in B, D, F, and H. B cells are blue and T cells brown (A and B). Germinal centers are shown with an arrow (C and D). Only few residual germinal centers are seen in control mice (C). CD11c positive dendritic cells are brown and appear in the T cell zone, bridging channels and the marginal zone (E). Very few are present in BAFF Tg mice (F). Syndecan-1-positive plasma cells were only detectable in the red pulp of BAFF Tg mice (H) but not control mice (G).
These pictures are representative of at least 12 BAFF Tg mice analysed and 12 control mice. The magnification is 100× for all pictures except C and D which are 50×.
B: B cell follicle, T: PALS, WP: white pulp, RP: red pulp.
FIG. 13 depicts disrupted T and B cells organization, intense germinal center reactions and large number of plasma cells in the MLN of BAFF Tg mice.
The control mouse is shown in A, C, E and G and the BAFF Tg mouse is shown in B, D, F, and H. The immunohistochemistry was performed as described in FIG. 6. T and B cell staining is shown in A and B, germinal centers in C and D, dendritic cells E and F and plasma cells in G and H. GC: germinal center. Magnification 100×.
DETAILED DESCRIPTION OF THE INVENTION
Reference will now be made in detail to the present preferred embodiments of the invention. This invention relates to the use of BAFF and BAFF related molecules to effect the growth and maturation of B-cells and the secretion of immunoglobulin. The invention relates to the use of BAFF and BAFF related molecules to effect responses of the immune system, as necessitated by immune-related disorders. Additionally, this invention encompasses the treatment of cancer and immune disorders through the use of a BAFF, or BAFF related gene through gene therapy methods.
The BAFF ligand and homologs thereof produced by hosts transformed with the sequences of the invention, as well as native BAFF purified by the processes known in the art, or produced from known amino acid sequences, are useful in a variety of methods for anticancer, antitumor and immunoregulatory applications. They are also useful in therapy and methods directed to other diseases.
Another aspect of the invention relates to the use of the polypeptide encoded by the isolated nucleic acid encoding the BAFF-ligand in “antisense” therapy. As used herein, “antisense” therapy refers to administration or in situ generation of oligonucleotides or their derivatives which specifically hybridize under cellular conditions with the cellular mRNA and/or DNA encoding the ligand of interest, so as to inhibit expression of the encoded protein, i.e. by inhibiting transcription and/or translation. The binding may be by conventional base pair complementarity, or, for example, in the case of binding to DNA duplexes, through specific interactions in the major groove of the double helix. In general, “antisense” therapy refers to a range of techniques generally employed in the art, and includes any therapy which relies on specific binding to oligonucleotide sequences.
An antisense construct of the present invention can be delivered, for example, as an expression plasmid, which, when transcribed in the cell, produces RNA which is complementary to at least a portion of the cellular mRNA which encodes Kay-ligand. Alternatively, the antisense construct can be an oligonucleotide probe which is generated ex vivo. Such oligonucleotide probes are preferably modified oligonucleotides which are resistant to endogenous nucleases, and are therefor stable in vivo. Exemplary nucleic acids molecules for use as antisense oligonucleotides are phosphoramidates, phosphothioate and methylphosphonate analogs of DNA (See, e.g., U.S. Pat. No. 5,176,996; U.S. Pat. No. 5,264,564; and U.S. Pat. No. 5,256,775). Additionally, general approaches to constructing oligomers useful in antisense therapy have been reviewed, for example, by Van Der Krol et al., (1988) Biotechniques 6:958-976; and Stein et al. (1988) Cancer Res 48: 2659-2668, specifically incorporated herein by reference.
C. BAFF-Ligand
The BAFF-ligand of the invention, as discussed above, is a member of the TNF family and is described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith. The protein, fragments or homologs thereof may have wide therapeutic and diagnostic applications.
The BAFF-ligand is present primarily in the spleen and in peripheral blood lymphocytes, strongly indicating a regulatory role in the immune system. Comparison of the claimed BAFF-ligand sequences with other members of the human TNF family reveals considerable structural similarity. All the proteins share several regions of sequence conservation in the extracellular domain.
Although the precise three-dimensional structure of the claimed ligand is not known, it is predicted that, as a member of the TNF family, it may share certain structural characteristics with other members of the family.
The novel polypeptides of the invention specifically interact with a receptor, which has not yet been identified. However, the peptides and methods disclosed herein enable the identification of receptors which specifically interact with the BAFF-ligand or fragments thereof.
The claimed invention in certain embodiments includes methods of using peptides derived from BAFF-ligand which have the ability to bind to their receptors. Fragments of the BAFF-ligands can be produced in several ways, e.g., recombinantly, by PCR, proteolytic digestion or by chemical synthesis. Internal or terminal fragments of a polypeptide can be generated by removing one or more nucleotides from one end or both ends of a nucleic acid which encodes the polypeptide. Expression of the mutagenized DNA produces polypeptide fragments.
Polypeptide fragments can also be chemically synthesized using techniques known in the art such as conventional Merrifield solid phase f-moc or t-boc chemistry. For example, peptides and DNA sequences of the present invention may be arbitrarily divided into fragments of desired length with no overlap of the fragment, or divided into overlapping fragments of a desired length. Methods such as these are described in more detail below.
Generation of Soluble Forms of BAFF-ligand
Soluble forms of the BAFF-ligand can often signal effectively and hence can be administered as a drug which now mimics the natural membrane form. It is possible that the BAFF-ligand claimed herein are naturally secreted as soluble cytokines, however, if not, one can reengineer the gene to force secretion. To create a soluble secreted form of BAFF-ligand, one would remove at the DNA level the N-terminus transmembrane regions, and some portion of the stalk region, and replace them with a type leader or alternatively a type II leader sequence that will allow efficient proteolytic cleavage in the chosen expression system. A skilled artisan could vary the amount of the stalk region retained in the secretion expression construct to optimize both receptor binding properties and secretion efficiency. For example, the constructs containing all possible stalk lengths, i.e. N-terminal truncations, could be prepared such that proteins starting at amino acids 81 to 139 would result. The optimal length stalk sequence would result from this type of analysis.
E. Generation of Antibodies Reactive with the BAFF-ligand
The invention also includes antibodies specifically reactive with the claimed BAFF-ligand or its receptors. Anti-protein/anti-peptide antisera or monoclonal antibodies can be made by standard protocols (See, for example, Antibodies: A Laboratory Manual ed. by Harlow and Lane (Cold Spring Harbor Press: 1988)). A mammal such as a mouse, a hamster or rabbit can be immunized with an immunogenic form of the peptide. Techniques for conferring immunogenicity on a protein or peptide include conjugation to carriers, or other techniques, well known in the art.
An immunogenic portion of BAFF-ligand or its receptors can be administered in the presence of an adjuvant. The progress of immunization can be monitored by detection of antibody titers in plasma or serum. Standard ELISA or other immunoassays can be used with the immunogen as antigen to assess the levels of antibodies.
In a preferred embodiment, the subject antibodies are immunospecific for antigenic determinants of BAFF-ligand or its receptors, (e.g. antigenic determinants of a polypeptide of SEQ. ID. NO.: 2, said sequence as described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith), or a closely related human or non-human mammalian homolog (e.g. 70, 80 or 90 percent homologous, more preferably at least 95 percent homologous). In yet a further preferred embodiment of the present invention, the anti-BAFF-ligand or anti-BAFF-ligand-receptor antibodies do not substantially cross react (i.e. react specifically) with a protein which is e.g., less than 80 percent homologous to SEQ. ID. NO.: 2 or 6 said sequence as described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith; preferably less than 90 percent homologous with SEQ. ID. NO.: 2 said sequence as described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith; and, most preferably less than 95 percent homologous with SEQ. ID. NO.: 2 said sequence as described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith. By “not substantially cross react”, it is meant that the antibody has a binding affinity for a non-homologous protein which is less than 10 percent, more preferably less than 5 percent, and even more preferably less than 1 percent, of the binding affinity for a protein of SEQ. ID. NO.: 2 said sequence as described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith.
The term antibody as used herein is intended to include fragments thereof which are also specifically reactive with BAFF-ligand, or its receptors. Antibodies can be fragmented using conventional techniques and the fragments screened for utility in the same manner as described above for whole antibodies. For example, F(ab′) 2 fragments can be generated by treating antibody with pepsin. The resulting F(ab′) 2 fragment can be treated to reduce disulfide bridges to produce Fab′ fragments. The antibodies of the present invention are further intended to include biospecific and chimeric molecules having anti-BAFF-ligand or anti-BAFF-ligand-receptor activity. Thus, both monoclonal and polyclonal antibodies (Ab) directed against BAFF-ligand, Tumor-ligand and their receptors, and antibody fragments such as Fab′ and F(ab′) 2 , can be used to block the action of the Ligand and their respective receptor.
Various forms of antibodies can also be made using standard recombinant DNA techniques. Winter and Milstein (1991) Nature 349: 293-299, specifically incorporated by reference herein. For example, chimeric antibodies can be constructed in which the antigen binding domain from an animal antibody is linked to a human constant domain (e.g. Cabilly et al., U.S. Pat. No. 4,816,567, incorporated herein by reference). Chimeric antibodies may reduce the observed immunogenic responses elicited by animal antibodies when used in human clinical treatments.
In addition, recombinant “humanized antibodies” which recognize BAFF-ligand or its receptors can be synthesized. Humanized antibodies are chimeras comprising mostly human IgG sequences into which the regions responsible for specific antigen-binding have been inserted. Animals are immunized with the desired antigen, the corresponding antibodies are isolated, and the portion of the variable region sequences responsible for specific antigen binding are removed. The animal-derived antigen binding regions are then cloned into the appropriate position of human antibody genes in which the antigen binding regions have been deleted. Humanized antibodies minimize the use of heterologous (i.e. inter species) sequences in human antibodies, and thus are less likely to elicit immune responses in the treated subject.
Construction of different classes of recombinant antibodies can also be accomplished by making chimeric or humanized antibodies comprising variable domains and human constant domains (CH1, CH2, CH3) isolated from different classes of immunoglobulins. For example, antibodies with increased antigen binding site valencies can be recombinantly produced by cloning the antigen binding site into vectors carrying the human: chain constant regions. Arulanandam et al. (1993) J. Exp. Med., 177: 1439-1450, incorporated herein by reference.
In addition, standard recombinant DNA techniques can be used to alter the binding affinities of recombinant antibodies with their antigens by altering amino acid residues in the vicinity of the antigen binding sites. The antigen binding affinity of a humanized antibody can be increased by mutagenesis based on molecular modeling. Queen et al., (1989) Proc. Natl. Acad. Sci. 86: 10029-33 incorporated herein by reference.
F. Generation of Analogs: Production of Altered DNA and Peptide Sequences
Analogs of the BAFF-ligand can differ from the naturally occurring BAFF-ligand in amino acid sequence, or in ways that do not involve sequence, or both. Non-sequence modifications include in vivo or in vitro chemical derivatization of the BAFF-ligand. Non-sequence modifications include, but are not limited to, changes in acetylation, methylation, phosphorylation, carboxylation or glycosylation.
Preferred analogs include BAFF-ligand biologically active fragments thereof, whose sequences differ from the sequence given in SEQ. ID NO. 2 said sequence as described in PCT application number PCT/US98/19037 (WO99/12964) and is incorporated in its entirety herewith, by one or more conservative amino acid substitutions, or by one or more non-conservative amino acid substitutions, deletions or insertions which do not abolish the activity of BAFF-ligand. Conservative substitutions typically include the substitution of one amino acid for another with similar characteristics, e.g. substitutions within the following groups: valine, glycine; glycine, alanine; valine, isoleucine, leucine; aspartic acid, glutamic acid; asparagine, glutamine; serine, threonine; lysine, arginine; and, phenylalanine, tyrosine.
G. Materials and Methods of the Invention
The anti-Flag M2 monoclonal antibody, biotinylated anti-Flag M2 antibody and the anti-Flag M2 antibody coupled to agarose were purchased from Sigma. Cell culture reagents were obtained from Life Sciences (Basel, Switzerland) and Biowhittaker (Walkersville, Md.). Flag-tagged soluble human APRIL (residues K 110 -L 250 ) was produced in 293 cells as described (10, 11). FITC-labeled anti-CD4, anti-CD8 and anti-CD19 antibodies were purchased from Pharmingen (San Diego, Calif.). Goat F(ab) 2 specific for the Fc 5 μ fragment of human IgM were purchased from Jackson ImmunoResearch (West Grove, Pa.). Secondary antibodies were obtained from either Pharmingen or from Jackson ImmunoResearch and used at the recommended dilutions.
Human embryonic kidney 293 T (12) cells and fibroblast cell lines (Table 1) were maintained in DMEM containing 10% heat-inactivated fetal calf serum (FCS). Human embryonic kidney 293 cells were maintained in DMEM-nutrient mix F12 (1:1) supplemented with 2% FCS. T cell lines, B cell lines, and macrophage cell lines (Table 1) were grown in RPMI supplemented with 10% FCS. Molt-4 cells were cultivated in Iscove's medium supplemented with 10% FCS. Epithelial cell lines were grown in MEM-alpha medium containing 10% FCS, 0.5 mM non-essential amino acids, 10 mM Na-Hepes and 1 mM Na pyruvate. HUVECs were maintained in M199 medium supplemented with 20% FCS, 100 μg/ml of epithelial cell growth factor (Collaborative Research, Inotech, Dottikon, Switzerland) and 100 μg/ml of heparin sodium salt (Sigma). All media contained penicillin and streptomycin antibiotics. Peripheral blood leukocytes were isolated from heparinized blood of healthy adult volunteers by Ficoll-Paque (Pharmacia, Uppsala, Sweden) gradient centrifugation and cultured in RPMI, 10% FCS.
T cells were obtained from non-adherents PBLs by rosetting with neuraminidase-treated sheep red blood cells and separated from non-rosetting cells (mostly B cells and monocytes) by Ficoll-Paque gradient centrifugation. Purified T cells were activated for 24 h with phytohemagglutinin (Sigma) (1 μg/ml), washed and cultured in RPMI, 10% FCS, 20 U/ml of IL-2. CD14 + monocytes were purified by magnetic cell sorting using anti-CD14 antibodies, goat anti-mouse-coated microbeads and a Minimacs™ device (Miltenyi Biotech), and cultivated in the presence of GM-CSF (800 U/ml, Leucomax®, Essex Chemie, Luzern, Switzerland) and IL-4 (20 ng/ml, Lucerna Chem, Luzern, Switzerland) for 5 d, then with GM-CSF, IL-4 and TNFα(200 U/ml, Bender, Vienna, Austria) for an additional 3 d to obtain a CD83 + , dentritic cell-like population. Human B cells of >97% purity were isolated from peripheral blood or umbilical cord blood using anti-CD 19 magnetic beads (M450, Dynal, Oslo, Norway) as described (13).
Northern Blot Analysis
Northern blot analysis was carried out using Human Multiple Tissue Northern Blots I and II (Clontech #7760-1 and #7759-1). The membranes were incubated in hybridization solution (50% formamide, 2.5× Denhardt's, 0.2% SDS, 10 mM EDTA, 2× SSC, 50 mM NaH 2 PO 4 , pH 6.5, 200 μg/ml sonicated salmon sperm DNA) for 2 h at 60° C. Antisense RNA probe containing the nucleotides corresponding to amino acids 136-285 of hBAFF was heat-denatured and added at 2×10 6 cpn/ml in fresh hybridization solution. The membrane was hybridized 16 h at 62° C., washed once in 2× SSC, 0.05% SDS (30 min at 25° C.), once in 0.1× SSC, 0.1% SDS (20 min at 65° C.) and exposed 70° C. to X-ray films.
Characterization of BAFF cDNA.
A partial sequence of human BAFF cDNA was contained in several EST clones (e.g. GenBank Accession numbers T87299 and AA166695) derived from fetal liver and spleen and ovarian cancer libraries. The 5′ portion of the cDNA was obtained by 5′-RACE-PCR (Marathon-Ready cDNA, Clonetech, Palo Alto, Calif.) amplification with oligonucleotides AP1 and JT1013 (5′-ACTGTTTCTTCTGGACCCTGAACGGC-3′) [SEQ ID. NO.: 9] using the provided cDNA library from a pool of human leukocytes as template, as recommended by the manufacturer. The resulting PCR product was cloned into PCR-0 blunt (Invitrogen, NV Leek, The Netherlands) and subcloned as EcoRI/Pstl fragment into pT7T3 Pac vector (Pharmacia) containing EST clone T87299. Full-length hBAFF cDNA was therefore obtained by combining 5′ and 3′ fragments using the internal PstI site of BAFF. Sequence has been assigned GenBank accession number AF116456.
A partial 617 bp sequence of murine BAFF was contained in two overlapping EST clones (AA422749 and AA254047). A PCR fragment spanning nucleotides 158 to 391 of this sequence was used as a probe to screen a mouse spleen cDNA library (Stratagene, La Jolla, Calif.).
Expression of Recombinant BAFF
Full length hBAFF was amplified using oligos JT1069 (5′-GACAAGCTTGCCACCATGGATGACTCCACA-3′) [SEQ. ID. NO.: 10] and JT637 (5′-ACTAGTCACAGCAGTTTCAATGC-3′) [SEQ. ID. NO.: 11]. The PCR product was cloned into PCR-0 blunt and re-subcloned as HindIII/EcoRI fragment into PCR-3 mammalian expression vector. A short version of soluble BAFF (amino acids Q136-L285) was amplified using oligos JT636 (5′-CTGCAGGGTCCAGAAGAAACAG-3′) [SEQ. ID. NO.: 12] and JT637. A long version of soluble BAFF (aa L83-L285) was obtained from full length BAFF using internal PstI site. Soluble BAFFs were resubcloned as PstI/EcoRI fragments behind the haemaglutinin signal peptide and Flag sequence of a modified PCR-3 vector, and as PstI/SpeI fragments into a modified pQE16 bacterial expression vector in frame with a N-terminal Flag sequence (14). Constructs were sequenced on both strands. The establishment of stable 293 cell lines expressing the short soluble form or full length BAFF, and the expression and purification of recombinant soluble BAFF from bacteria and mammalian 293 cells was performed as described (14, 15).
Reverse Transcriptase PCR
Total RNA extracted from T cells, B cells, in vitro derived immature dendritic cells, 293 wt and 293-BAFF (full length) cells was reverse transcribed using the Ready to Go system (Pharmacia) according to the manufacturer's instructions. BAFF and β-actin cDNAs were detected by PCR amplification with Taq DNA polymerase (steps of 1 min each at 94° C., 55° C. and 72° C. for 30 cycles) using specific oligonucleotides: for BAFF, JT1322 5′-GGAGAAGGCAACTCCAGTCAGAAC-3′ [SEQ. ID. NO.: 13] and JT1323 5′-CAATTCATCCCCAAAGACATGGAC-3′ [SEQ. ID. NO.: 14]; for IL-2 receptor alpha chain, JT1368 5′-TCGGAACACAACGAAACAAGTC-3′ [SEQ. ID. NO.: 15] and JT1369 5′-CTTCTCCTTCACCTGGAAACTGACTG-3′ [SEQ. ID NO.: 16]; for β-actin, 5′-GGCATCGTGATGGACTCCG-3′ [SEQ. ID. NO.: 17] and 5′-GCTGGAAGGTGGACAGCGA-3′ [SEQ. ID. NO.: 18].
Gel Permeation Chromatography
293T cells were transiently transfected with the short form of soluble BAFF and grown in serum-free Optimem medium for 7 d. Conditionned supernatants were concentrated 20×, mixed with internal standards catalase and ovalbumin, and loaded onto a Superdex-200 HR10/30 column. Proteins were eluted in PBS at 0.5 ml/min and fractions (0.25 ml) were precipitated with trichloroacetic acid and analyzed by Western blotting using anti-Flag M2 antibody. The column was calibrated with standard proteins: ferritin (440 kDa), catalase (232 kDa), aldolase (158 kDa), bovine serum albumine (67 kDa), ovalbumine (43 kDa), chymotrypsinogen A (25 kDa) and ribonuclease A (13.7 kDa).
PNGase F Treatment
Samples were heated in 20 μl of 0.5% SDS, 1% 2-mercaptoethanol for 3 min at 95° C., then cooled and supplemented with 10% Nonidet P-40 (2 μl), 0.5 M sodium phosphate, pH 7.5 (2 μl) and Peptide N-glycanase F (125 units/μl, 1 μl, or no enzyme in controls). Samples were incubated for 3 h at 37° C. prior to analysis by Western blotting.
EDMAN Sequencing
293 T cells were transiently transfected with the long form of soluble BAFF and grown in serum-free Optimem medium for 7 d. Conditioned supernatants were concentrated 20×, fractionated by SDS-PAGE and blotted onto polyvinylidene difluoride membrane (BioRad Labs, Hercules, Calif.) as previously described (16), and then sequenced using a gas phase sequencer (ABI 120A, Perkin Elmer, Foster City, Calif.) coupled to an analyzer (ABI 120A, Perkin Elmer) equipped with a phenylthiohydantoin C18 2.1×250 mm column. Data was analyzed using software ABI 610 (Perkin Elmer).
Antibodies
Polyclonal antibodies were generated by immunizing rabbits (Eurogentec, Seraing, Belgium) with recombinant soluble BAFF. Spleen of rats immunized with the same antigen were fused to x63Ag8.653 mouse myeloma cells, and hybridoma were screened for BAFF-specific IgGs. One of these monoclonal antibodies, 43.9, is an IgG2a that specifically recognizes hBAFF.
Cells were stained in 50 μl of FACS buffer (PBS, 10% FCS, 0.02% NaN 3 ) with 50 ng (or the indicated amount) of Flag tagged short soluble hBAFF for 20 min at 4° C., followed by anti-Flag M2 (1 μg) and secondary antibody. Anti-BAFF mAb 43.9 was used at 40 μg/ml. For two color FACS analysis, peripheral blood lymphocytes were stained with Flag tagged soluble BAFF/long (2 μg/ml), followed by biotinylated anti-Flag M2 ({fraction (1/400)}) and PE-labeled streptavidin ({fraction (1/100)}), followed by either FITC-labeled anti-CD4, anti-CD8 or anti-CD19.
PBL Proliferation Assay
Peripheral blood leukocytes were incubated in 96-well plates (10 5 cells/well in 100 μl RPMI supplemented with 10% FCS) for 72 h in the presence or absence of 2 μg/ml of goat anti-human μ chain antibody (Sigma) or control F(ab′) 2 and with the indicated concentration of native or boiled soluble BAFF/long. Cells were pulsed for an additional 6 h with [ 3 H]thymidine (1 μCi/well) and harvested. [ 3 H]thymidine incorporation was monitored by liquid scintillation counting. In some experiments, recombinant soluble BAFF was replaced by 293 cells stably transfected with full length BAFF (or 293 wt as control) that had been fixed for 5 min at 25° C. in 1% paraformaldeyde. Assay was performed as described (17). In further experiments, CD 19 + cells were isolated form PBL with magnetic beads and the remaining CD19 − cells were irradiated (3000 rads) prior to renconstitution with CD19 + cells. Proliferation assay with sBAFF was then performed as described above.
B Cell Activation Assay
Purified B cells were activated in the EL-4 culture system as described (13). Briefly, 10 4 B cells mixed with 5×10 4 irradiated murine EL-4 thymoma cells (clone B5) were cultured for 5-6 d in 200 μl medium containing 5% v/v of culture supernatants from human T cells (10 6 /ml) which had been activated for 48 h with PHA (1 μg/ml) and PMA (1 ng/ml). B cells were then reisolated with anti-CD19 beads and cultured for another 7 d (5×10 4 cells in 200 μl, duplicate or triplicate culture in flat bottomed 96 well plates) in medium alone or in medium supplemented with 5% T cell supernatants, or with 50 ng/ml IL-2 (a kind gift from the former Glaxo Institute for Molecular Biology, Geneva) and 10 ng/ml each IL-4 and IL-10 (Peprotech, London, UK), in the presence or absence of sBAFF. The anti-Flag M2 antibody was added at a concentration of 2 μg/ml and had no effect by itself. IgM, IgG and IgA in culture supernatants were quantitated by ELISA assays as described (13).
Human BAFF was identified by sequence homology as a possible novel member of the TNF ligand family while we screened public databases using an improved profile search (18). A cDNA encoding the complete protein of 285 amino acids (aa) was obtained by combining EST-clones (covering the 3′ region) with a fragment (5′ region) amplified by PCR. The absence of a signal peptide suggested that BAFF was a type II membrane protein that is typical of the members of the TNF-ligand family. The protein has a predicted cytoplasmic domain of 46 aa, a hydrophobic transmembrane region, and an extracellular domain of 218 aa containing two potential N-glycosylation sites (FIG. 1 A). The sequence of the extracellular domain of BAFF shows highest homology with APRIL (33% amino acid identities, 48% homology), whereas the identity with other members of the family such as TNF, FasL, LTα, TRAIL or RANKL is below 20% ( FIGS. 1B , C). The mouse BAFF cDNA clone isolated from a spleen library encoded a slightly longer protein (309 aa) due to an insertion between the transmembrane region and the first of several β-strands which constitute the receptor binding domain in all TNF ligand members (19). This β-strand rich ectodomain is almost identical in mouse and human BAFF (86% identity, 93% homology) suggesting that the BAFF gene has been highly conserved during evolution (FIG. 1 A).
Although TNF family members are synthesized as membrane inserted ligands, cleavage in the stalk region between transmembrane and receptor binding domain is frequently observed. For example, TNF or FasL are readily cleaved from the cell surface by metalloproteinases (20, 21). While producing several forms of recombinant BAFF in 293T cells, we noticed that a recombinant soluble 32 kDa form of BAFF (aa 83-285, sBAFF/long), containing the complete stalk region and a N-terminal Flag-tag in addition to the receptor binding domain, was extensively processed to a smaller 18 kDa fragment ( FIGS. 2A , B). Cleavage occurred in the stalk region since the fragment was detectable only with antibodies raised against the complete receptor interaction domain of BAFF but not with anti-Flag antibodies (data not shown). Also revealed was that only N124 (located in the stalk) but not N242 (located at the entry of the F-□ sheet) was glycosylated, since the molecular mass of the non-processed sBAFF/long was reduced from 32 kDa to 30 kDa upon removal of the N-linked carbohydrates with PNGase F whereas the 18 kDa cleaved form was insensitive to this treatment. Peptide sequence analysis of the 18 kDa fragment indeed showed that cleavage occurred between R133 and A134 (FIG. 1 A). R133 lies at the end of a polybasic region which is conserved between human (R-N-K-R) and mouse (R-N-R-R). To test whether cleavage was not merely an artifact of expressing soluble, non-natural forms of BAFF, membrane-bound full length BAFF was expressed in 293T cells (FIG. 2 C). The 32 kDa complete BAFF and some higher molecular mass species (probably corresponding to non-dissociated dimers and trimers) were readily detectable in cellular extracts, but more than 95% of BAFF recovered from the supernatant corresponded to the processed 18 kDa form, indicating that BAFF was also processed when synthesized as a membrane-bound ligand.
A soluble BAFF was engineered (Q136-L285, sBAFF/short) whose sequence started 2 aa downstream of the processing site (FIG. 1 B). As predicted, the Flag-tag attached to the N-terminus of this recombinant molecule was not removed (data not shown) which allowed its purification by an anti-Flag affinity column. To test its correct folding, the purified sBAFF/short was analyzed by gel filtration where the protein eluted at an apparent molecular mass of 55 kDa (FIG. 2 D). The sBAFF/short correctly assembles into a homotrimer (3×20 kDa) in agreement with the quaternary structure of other TNF family members (19). Finally, unprocessed sBAFF/long was readily expressed in bacteria, indicating that the cleavage event was specific to eukaryotic cells.
Northern blot analysis of BAFF revealed that the 2.5 kb BAFF mRNA was abundant in the spleen and PBLs (FIG. 3 A). Thymus, heart, placenta, small intestine and lung showed weak expression. This restricted distribution suggested that cells present in lymphoid tissues were the main source of BAFF. Through PCR analysis, we found that BAFF mRNA was present in T cells and peripheral blood monocyte-derived dendritic cells but not in B cells (FIG. 3 B). Even naive, non-stimulated T cells appeared to express some BAFF mRNA.
A sequence tagged site (STS, SHGC-36171) was found in the database which included the human BAFF sequence. This site maps to human chromosome 13, in a 9 cM interval between the markers D13S286 und D13S1315. On the cytogenetic map, this interval corresponds to 13q32-34. Of the known TNF ligand family members, only RANKL (Trance) has been localized to this chromosome (22) though quite distant to BAFF (13q14).
In order for the ligand to exert maximal biological effects, it was likely that the BAFF receptor (BAFF-R) would be expressed either on the same cells or on neighboring cells present in lymphoid tissues. Using the recombinant sBAFF as a tool to specifically determine BAFF-R expression by FACS, we indeed found high levels of receptor expression in various B cell lines such as the Burkitt lymphomas Raji and BJAB ( FIG. 4A , Table 1). In contrast, cell lines of T cell, fibroblastic, epithelial and endothelial origin were all negative. Very weak staining was observed with the monocyte line THP-1 which, however, could be due to Fc receptor binding. Thus, BAFF-R expression appears to be restricted to B cell lines. The two mouse B cell lines tested were negative using the human BAFF as a probe, although weak binding was observed on mouse splenocytes (data not shown). The presence of BAFF-R on B cells was corroborated by analysis of umbilical cord and peripheral blood lymphocytes. While CD8 + and CD4 + T cells lacked BAFF-R (FIG. 4 B and data not shown), abundant staining was observed on CD19 + B cells (FIGS. 4 A and 4 B), indicating that BAFF-R is expressed on all blood B cells, including naive and memory ones.
Since BAFF bound to blood-derived B cells, experiments were performed to determine whether the ligand could deliver growth-stimulatory inhibitory signals. Peripheral blood lymphocytes (PBL) were stimulated with anti-IgM (μ) antibodies together with fixed 293 cells stably expressing surface BAFF (FIG. 5 A). The levels of [ 3 H]thymidine incorporation induced by anti-μ alone was not altered by the presence of control cells but was increased two-fold in the presence of BAFF-transfected cells (FIG. 5 B). A dose-dependent proliferation of PBL was also obtained when BAFF-transfected cells were replaced by purified sBAFF (FIG. 5 C), indicating that BAFF does not require membrane attachment to exert its activity. In this experimental setup, proliferation induced by sCD40L required concentrations exceeding 1 μg/ml but was less dependent on the presence of anti-μ than that mediated by BAFF (FIG. 5 D). When purified CD19 + B cells were co-cultured with irradiated autologous CD19 − PBL, costimulation of proliferation by BAFF was unaffected, demonstrating that [ 3 H]thymidine uptake was mainly due to B cell proliferation and not to an indirect stimulation of another cell type (data not shown). The observed B cell proliferation in response to BAFF was entirely dependent on the presence of anti-μ antibodies, indicating that BAFF functioned as costimulator of B cell proliferation.
To investigate a possible effect of BAFF on immunoglobulin secretion, purified peripheral or cord blood B cells were preactivated by coculture with EL-4 T cells in the presence of a cytokine mixture from supernatants of PHA/PMA stimulated T cells (23). These B cells were reisolated to 98% purity and yielded a two-fold increase in Ig secretion during a secondary culture in the presence of BAFF and activated T cell cytokines as compared to cytokines alone. A very modest effect occurred in the absence of exogenous cytokines, and an intermediate (1.5-fold) effect was observed in the presence of the recombinant cytokines IL-2, IL-4 and IL-10 ( FIGS. 5E , F).
The biochemical analysis of BAFF is also consistent with the typical homotrimeric structure of TNF family members. Among this family of ligands, BAFF exhibits the highest level of sequence similarity with APRIL which we have recently characterized as a ligand stimulating growth of various tumor cells (11). Unlike TNF and LT□ which are two family members with equally high homology (33% identity) and whose genes are linked on chromosome 6, APRIL and BAFF are not clustered on the same chromosome. APRIL is located on chromosome 17 (J. L. B., unpublished data) whereas BAFF maps to the distal arm of human chromosome 13 (13q34). Abnormalities in this locus were characterized in Burkitt lymphomas as the second most frequent defect (24) besides the translocation involving the myc gene into the Ig locus (25). Considering the high expression levels of BAFF-R on all Burkitt lymphoma cell lines analyzed (see Table 1), this raises the intriguing possibility that some Burkitt lymphomas may have deregulated BAFF expression, thus stimulating growth in an autocrine manner.
The role of antigen-specific B lymphocytes during the different stages of the immune response is highly dependent on signals and contacts from helper T cells and antigen-presenting cells such as dendritic cells (20). B lymphocytes first receive these signals early on during the immune response when they interact with T cells at the edge of the B cell follicles in lymphoid tissues, leading to their proliferation and differentiation into low affinity antibody forming cells (18). At the same time some antigen-specific B cells also migrate to the B cell follicle and contribute to the formation of germinal centers, another site of B cell proliferation but also affinity maturation and generation of memory B cells and high affinity plasma cells (19).
Signals triggered by another member of the TNF super family CD40L have been shown to be critical for the function of B lymphocytes at multiple steps of the T cell-dependent immune response. However, several studies clearly showed that CD40L/CD40 interaction does not account for all contact-dependent T-cell help for B cells. Indeed, CD40L-deficient T cells isolated from either knock-out mice or patients with X-linked hyper IgM syndrome have been shown to sucessfully induce proliferation of B cells and their differentiation into plasma cells. Studies using blocking antibodies against CD40L showed that a subset of surface IgD positive B cells isolated from human tonsils proliferate and differentiate in response to activated T cells in a CD40-independent manner. Other members of the TNF family such as membrane-bound TNF and CD30L have also been shown to be involved in a CD40- and surface Ig-independent stimulation of B cells. Similar to our results with BAFF, it has been shown that CD40-deficient B cells can be stimulated to proliferate and differentiate into plasma cells by helper T cells as long as the surface Ig receptors are triggered at the same time. BAFF as well as CD30L and CD40L is expressed by T cells but its originality resides in its expression by dendritic cells as well as the highly specific location of its receptor on B cells which is in contrast to CD40, CD30 and the TNF receptor which expression has been descrided on many different cell. This observation suggests independent and specific BAFF-induced functions on B cells.
In support of a role for BAFF in T cell- and dendritic cell-induced B cell growth and potential maturation, we found that BAFF costimulates proliferation of blood-derived B cells concomitantly with cross-linking of the B cell receptors, and, thus, independently of CD40 signalling. Moreover, using CD19 positive B cells differentiated in vitro into a pre-plasma cell/GC-like B cell (14), we observed a costimulatory effect of BAFF on Ig secretion by these B cells in the presence of supernatant from activated T cells or a blend of IL-2, IL-4 and IL-10. Interestingly, the costimulatory effect was stronger in presence of the activated T cell supernatant when compared to the cytokine blend, suggesting additional soluble factors secreted by activated T cells involved in antibody production which can synergize with BAFF or additional BAFF itself. It is, therefore, possible that BAFF actively contributes to the differentiation of these GC-like B cells into plasma.
It is clear that BAFF can signal in both naive B cells as well as GC-commited B cells in vitro. Whether this observation will translate or not during a normal immune response will have to be addressed by proper in vivo experiments.
The biological responses induced in B cells by BAFF are distinct from that of CD40L, since proliferation triggered by CD40L was less dependent on an anti-μ costimulus (17) (and FIG. 5 D). Morever, CD40L can counteract apoptotic signals in B cells following engagement of the B cell receptor (29), whereas BAFF was not able to rescue the B cell line Ramos from anti-μ-mediated apoptosis, despite the fact that Ramos cells do express BAFF-R (Table 1; F. M. and J. L. B., unpublished observations). It is therefore likely that CD40L and BAFF fulfill distinct functions. In this respect, it is noteworthy that BAFF did not interact with any of 16 recombinant receptors of the TNF family tested, including CD40 (P.S and J.T, unpublished observations).
B cell growth was efficiently costimulated with recombinant soluble BAFF lacking the transmembrane domain. This activity is in contrast to several TNF family members which are active only as membrane-bound ligand such as TRAIL, FasL and CD40L. Soluble forms of these ligands have poor biological activity which can be enhanced by their cross-linking, thereby mimicking the membrane-bound ligand (15). In contrast, cross-linking Flag-tagged sBAFF with anti-FLAG antibodies or the use of membrane-bound BAFF expressed on the surface of epithelial cells did not further enhance the mitogenic activity of BAFF, suggesting that it can act systemically as a secreted cytokine, like TNF does. This is in agreement with the observation that a polybasic sequence present in the stalk of BAFF acted as a substrate for a protease. Similar polybasic sequences are also present at corresponding locations in both APRIL and TWEAK and for both of them there is evidence of proteolytic processing (30) (N.H. and J.T, unpublished observation). Although the protease responsible for the cleavage remains to be determined, it is unlikely to be the metalloproteinase responsible for the release of membrane-bound TNF as their sequence preferences differ completely (21). The multibasic motifs in BAFF (R-N-K-R) (SEQ ID NO:23), APRIL (R-K-R-R) (SEQ ID NO:24) and Tweak (R-P-R-R) (SEQ ID NO:25) are reminiscent of the minimal cleavage signal for furin (R-X-K/R-R) (SEQ ID NO:26), the prototype of a proprotein convertase family (31).
Practice of the present invention will employ, unless indicated otherwise, conventional techniques of cell biology, cell culture, molecular biology, microbiology, recombinant DNA, protein chemistry, and immunology, which are within the skill of the art. Such techniques are described in the literature. See, for example, Molecular Cloning: A Laboratory Manual, 2nd edition. (Sambrook, Fritsch and Maniatis, eds.), Cold Spring Harbor Laboratory Press, 1989; DNA Cloning , Volumes I and II (D. N. Glover, ed), 1985; Oligonucleotide Synthesis , (M. J. Gait, ed.), 1984; U.S. Pat. No. 4,683,195 (Mullis et al.,); Nucleic Acid Hybridization (B. D. Hames and S. J. Higgins, eds.), 1984; Transcription and Translation (B. D. Hames and S. J. Higgins, eds.), 1984; Culture of Animal Cells (R. I. Freshney, ed). Alan R. Liss, Inc., 1987; Immobilized Cells and Enzymes , IRL Press, 1986; A Practical Guide to Molecular Cloning (B. Perbal), 1984; Methods in Enzymology , Volumes 154 and 155 (Wu et al., eds), Academic Press, New York; Gene Transfer Vectors for Mammalian Cells (J. H. Miller and M. P. Calos, eds.), 1987, Cold Spring Harbor Laboratory; Immunochemical Methods in Cell and Molecular Biology (Mayer and Walker, eds.), Academic Press, London, 1987; Handbook of Experiment Immunology , Volumes I-IV (D. M. Weir and C. C. Blackwell, eds.), 1986; Manipulating the Mouse Embryo , Cold Spring Harbor Laboratory Press, 1986.
The following Examples are provided to illustrate the present invention, and should not be construed as limiting thereof.
EXAMPLES
The following experimental procedures were utilized in Examples 1-6.
DNA Construct for the Generation of Murine BAFF Tg Mice
Both human and murine cDNA sequences have been described previously (Schneider et al., 1999). A PCR fragment encoding full-length murine BAFF was generated by RT-PCR. First strand cDNA was synthesized from mouse lung polyA+ (Clontech, Palo Alto, Calif.) using oligo dT according to the manufacturer's protocol (GibcoBRL, Grand Island, N.Y.). The PCR reaction contained 1× Pfu buffer (Stratagene, La Jola, Calif.), 0.2 mM dNTPs, 10% DMSO, 12.5 pM primers, 5 units Pfu enzyme (Stratagene) and the following primers with Not1 restriction sites 5′-TAAGAATGCGGCCGCGGAATGGATGAGTCTGCAAA-3′ [SEQ. ID. NO.: 19] and 5′-TAAGAATGCGGCCGCGGGATCACGCACTCCAGCAA-3′ [SEQ. ID. NO.: 20]. The template was amplified for 30 cycles at 94° C. for 1 min, 54° C. for 2 min and 72° C. for 3 min followed by a 10 min extension at 72° C. This sequence corresponds to nucleotides 214 to 1171 of the GenBank file AF119383. The PCR fragment was digested with Not1 and then cloned into a modified pCEP4 vector (Invitrogen, Carlsbad, Calif.). The fragment containing murine BAFF was removed with Xba1 in order to include the SV40 polyA addition site sequence. This fragment was cloned into a pUC based vector where the promoter sequence was added. The promoter, a 1 Kb blunt Bg12-Not1 fragment containing the human ApoE enhancer and AAT (alpha anti-trypsin) promoter was purified from the plasmid clone 540B (a kind gift from Dr. Katherine Parker Ponder, Washington University, St. Louis, Mo.). An EcoRV/Bg12 fragment was purified from the final vector and used for the generation of transgenic mice. The injected offspring of C57BL/6J female×DBA/2J male F1 (BDF1) mice were backcrossed onto C57BL/6 mice. Techniques of microinjection and generation of transgenic mice have been previously described (Mcknights et al., 1983).
Analytical Methods:
Serum samples were subject to reduced SDS-PAGE analysis using a linear 12.5% gel. Total RNA from mouse liver was prepared and processed for Northern Blot analysis using an isolation kit from Promega (Madison, Wis.) according to the manufacturer's guidelines. BAFF transgene-specific mRNA was detected using a probe spanning the SV40 poly A tail of the transgene construct and obtained by digestion of the modified pCEP4 vector with Xba1 and BamH1. The probe recognizes a 1.8-2 Kd band corresponding to mRNA from the BAFF transgene. PCR analysis of tail DNA from BAFF Tg mice was carried using 12.5 pM of the following primers 5′-GCAGTTTCACAGCGATGTCCT-3′ [SEQ. ID. NO.: 21] and 5′-GTCTCCGTTGCGTGAAATCTG-3′ [SEQ. ID. NO.: 22] in a reaction containing 1× Taq polymerase buffer (Stratagene), 0.2 nM dNTPs, 10% DMSO and 5 units of Taq polymerase (Stratagene). A 719 bp of the transgene was amplified for 35 cycles at 94° C. for 30 sec., 54° C. for 1 min. and 72° C. for 1.5 min. followed by a 10 min. extension at 72° C.
The presence of proteins in mouse urine was measured using Multistix 10 SG reagent strips for urinalysis (Bayer Corporation, Diagnostics Division, Elkhart, Ind.).
Cell-dyn and Cytofluorimetric Analysis (FACS).
Differential WBC counts of fresh EDTA anticoagulated whole blood were performed with an Abbott Cell Dyne 3500 apparatus (Chicago, Ill.). For FACS analysis, Fluorescein (FITC)-, Cy-chrome- and Phycoerythrin-(PE)-labeled rat anti-mouse antibodies: anti-B220, anti-CD4, anti-CD8, anti-CD43, anti-IgM, anti-CD5, anti-CD25, anti-CD24, anti-CD38, anti-CD21, anti-CD44, anti-L-selectin and hamster anti-Bcl-2/control hamster Ig kit were purchased from Pharmingen (San Diego, Calif.). Production of recombinant E. coli as well as mammalian cell-derived human and mouse Flag-tagged BAFF were previously described (Schneider et al., 1999). All antibodies were used according to the manufacturer's specifications. PBL were purified from mouse blood as follows: mouse blood was collected in microtubes containing EDTA and was diluted ½ with PBS. Five hundred μl of diluted blood was applied on top of 1 ml of ficoll (Celardane, Hornby, Ontario, Canada) in a 4 ml glass tube, the gradient was performed at 2000 rpm for 30 min at room temperature and the interface containing the lymphocytes was collected and washed twice in PBS prior to FACS staining. Spleen, bone marrow and mesenteric lymph nodes were ground into a single cell suspension in RPMI medium (Life Technologies, Inc., Grand Island, N.Y.) and washed in FACS buffer (PBS supplemented with 2% fetal calf serum (JRH Biosciences, Lenexa, Kans.). Cells were first suspended in FACS buffer supplemented with the following blocking reagents: 10 μg/ml human Ig (Sandoz, Basel, Switzerland) and 10 μg/ml anti-mouse Fc blocking antibody (Pharmingen) and incubated 30 min on ice prior to staining with fluorochrome-labeled antibodies. All antibodies were diluted in FACS buffer with the blocking reagent mentioned above. Samples were analyzed using a FACScan cytofluorometer (Becton Dickinson).
Detection of Total Mouse Ig and Rheumatoid Factors in Mouse Sera by ELISA Assays.
ELISA plates (Corning glass works, Corning, N.Y.) were coated overnight at 4° C. with a solution of 10 μg/ml of goat anti-total mouse Ig (Southern Biotechnology Associates, Inc. Birmingham, Ala.) in 50 mM sodium bicarbonate buffer pH 9.6. Plates were washed 3 times with PBS/0.1% Tween and blocked overnight with 1% gelatin in PBS. One hundred μl/well of serum serial dilutions or standard dilutions was added to the plates for 30 min at 37° C. Mouse Ig were detected using 100 μl/well of a 1 μg/ml solution of an Alkaline Phosphatase (AP)-labeled goat anti-total mouse Ig (Southern Biotechnology Associates) for 30 min at 37° C. After a last wash, 3 times with PBS/0.1% Tween, the enzymatic reaction was developed using a solution of 10 μg/ml of p-nitrophenyl phosphate (Boehringer Mannheim, Indianapolis, Ind.) in 10% diethanolamine. The reaction was stopped by adding 100 μl of 3N NaOH/well. The optical density (O.D.) was measured at 405 nm using a spectrophotometer from Molecular Devices (Sunnyvale, Calif.). Standard curves were obtained using purified mouse Ig purchased from Southern Biotechnology Associates. In the case of detection of rheumatoid factors (RF), the plates were coated with normal goat Ig (Jackson ImmunoResearch laboratories, Inc., West Grove, Pa.) instead of goat anti-mouse Ig and detection of mouse Ig was performed as described above. Detection of mouse isotypes in the RF assay was done using AP-labeled goat anti-mouse IgA, IgM, IgG2a, IgG2b and IgG3, as well as purified mouse IgA, IgM, IgG2a, IgG2b and IgG3 for standard curves (Southern Biotechnology Associates Inc.). All statistical comparisons were performed by analysis of variance.
Detection of Circulating Immune Complexes (CIC) and Precipitation of Cryoglobulins in Mouse Sera.
The assay was performed as previously described (June et al., 1979; Singh and Tingle, 1982) with the following modifications: ELISA plates (Corning glass works) were coated overnight at 4° C. with 5 μg/ml of human C1q (Quidel, San Diego, Calif.) in 50 mM sodium bicarbonate buffer pH 9.6. The plates were washed 3 times with PBS/0.1% Tween. Fifty μl/well of 0.3 M EDTA was added to the plates plus 50 μl/well of serum serial dilutions or solutions of known concentrations of a standard immune complex (peroxidase-mouse anti-peroxidase (PAP) from DAKO (Carpinteria, Calif.). The plates were incubated 30 min at 37° C. The plates were washed 3 times with PBS/0.1% Tween. Mouse Ig in the immune complexes were detected using 100 μl/well of a 1 μg/ml solution of an AP-labeled goat anti-mouse Ig (Southern Biotechnology Associates, Inc.) as described above for the ELISA assays. Cryoglobulins were detected by incubating overnight at 4° C. mouse serum diluted {fraction (1/15)} in water and precipitates were scored visually.
Anti-Double Stranded (ds) and Single Stranded (ss) DNA Assays.
Anti-ssDNA were performed using NUNC-immuno Plate MaxiSorp plates (NUNC A/S, Denmark). Plates were coated overnight at 4° C. first with 100 μg/ml methylated BSA (Calbochem Corp., La Jolla, Calif.), then with 50 μg/ml grade I calf thymus DNA (Sigma, St. Louis, Mo.). The calf thymus DNA was sheared by sonication and then digested with S1 nuclease before use. For the anti-ssDNA assay, the DNA was boiled for 10 min and chilled on ice before use. After blocking, serial dilutions of the serum samples were added and incubated at room temperature for 2 h. Autoantibodies were detected with goat anti-mouse IgG-AP (Sigma) and develop as described above for the ELISA assays. Standard curves were obtained using known quantities of anti-DNA mAb 205, which is specific for both ss- and dsDNA (Datta et al., 1987).
Immunohistochemistry
Spleen and lymph nodes were frozen in O.C.T. embedding medium (Miles, Elkhart, Ind.) and mounted for cryostat sectioning. Sections 7-10 μm thick were dried and fixed in acetone. All Ab incubations (10 μg/ml) were done for 1 hr at room temperature in a humidified box after dilution in Tris-buffered saline A (TBS-A, 0.05M Tris, 0.15M NaCl, 0.05% Tween-20 (v/v), 0.25% BSA), rinsed in TBS-B (0.05M Tris, 0.15M NaCl, 0.05% Tween-20) and fixed 1 min in methanol before initiating the enzymatic reaction. Horseradish peroxidase (HRP) and alkaline phosphatase (AP) activities were developed using the diaminobenzidine (DAB) tablet substrate kit (Sigma) and the 5-bromo-4-chloro-3-indolyl phosphate/nitro blue tetrazolium (BCIP/NBT, Pierce, Rockford, Ill.), respectively. Stained tissue sections were finally fixed 5 min in methanol and counter stained with Giemsa (Fluka, Buchs, Switzerland). Biotin-labeled antibodies rat anti-B220, anti-CD11c, anti-syndecan-1 as well as unlabeled rat anti-CD4, anti-CD8α and anti-CD8β were purchased from Pharmingen. Biotin-labeled peanut agglutinin (PNA) was obtained from Vector laboratories (Burlingame, Calif.). (HRP)-labeled mouse anti-rat Ig and (HRP)-streptavidin were purchased from Jackson ImmunoResearch laboratories, Inc. and AP-labeled streptavidin from Southern Biotechnology Associates, Inc. In the case of immunohistochemistry on kidney tissue to detect Ig deposition, paraffin section were used, dewaxed and blocked using diluted horse serum from Vector (Burlingame, Calif.), followed by staining with HRP-goat anti-mouse Ig from Jackson Immunoresearch. Detection was performed as described above.
Example 1
BAFF Transgenic (BAFF Tg) Founder Mice have an Abnormal Phenotype.
Full length murine BAFF was expressed in transgenic mice using the liver specific alpha-1 antitrypsin promoter with the APO E enhancer. The full length version was chosen with the expectation that BAFF would be either cleaved and act systemically or if retained in a membrane bound form that local liver specific abnormalities would be observed possibly providing functional clues. We obtained 13 founder mice positive for the BAFF transgene (Table 2). Four of these mice died at a young age. Routine pathology was carried out on mice 811 and 816 (Table 2). There was no obvious infection in these mice; however, cardiovascular and renal abnormalities were apparent and similar to those described for severe hypertension (Fu, 1995) (Table 2). Hematoxylin and eosin (H&E)-stained kidney tissue sections of founder 816 showed that the morphology of glomeruli in that mouse was abnormal, whereas the rest of the kidney tissue seemed normal (data not shown). Many BAFF transgenic founder mice had proteinuria (Table 2). Immunohistochemistry on spleen frozen tissue sections from mouse 816, revealed an abnormal and extensive B cell staining and reduced staining for T cells and this observation was confirmed in the progeny (see below, FIG. 12 ).
Using two color FACS analysis, the ratio of % B220 positive B cells over % CD4 positive T cells was calculated. This ratio was two to seven times higher in BAFF Tg founder mice when compared to control negative BDF1 mice (Table 2), suggesting an increase of the B cell population in BAFF Tg mice. We selected nine of these founder mice to generate our different lines of transgenic mice as underlined in Table 2. None of the remaining BAFF Tg founder mice or the derived progeny showed any signs of ill health months after the early death of founders 696, 700, 811 and 816, suggesting that these 4 mice might have expressed higher levels of BAFF which caused their death. BAFF overexpression in the liver of transgenic mice was confirmed by Northern blot analysis (data not shown). In all BAFF-Tg mice examined histologically, the livers showed no abnormalities indicating that local overexpression of BAFF did not induce any immunological or pathological events. An ELISA assay for murine BAFF is not available; however, we showed that 2% serum from BAFF Tg mice, but not from control mice, blocked the binding of mammalian cell-derived mouse soluble Flag-tagged BAFF to BJAB cells. Moreover, 5% serum from BAFF Tg mice but not from control mice increased the proliferation of human B cells from PBL in the presence of anti-μ (data not shown). These data suggest that substantial amounts of soluble BAFF are present in the blood of BAFF Tg.
Example 2
Peripheral Lymphocytosis in BAFF Tg Mice is Due to Elevated B Cell Numbers
The transgenic mice population was found to have more lymphocytes in the blood when compared to control negative littermates, reaching values as high as 13000 lymphocytes/μl of blood (FIG. 7 A). In contrast, the number of granulocytes per μl of blood in both BAFF Tg mice and control mice remained within normal limits (FIG. 7 A). Since FACS analysis, using anti-CD4 and anti-B220 antibodies, of peripheral blood cells (PBL) from 18 BAFF Tg mice issued from six different founder mice showed increased B/T ratios (FIGS. 7 B and 7 C), the elevated lymphocyte levels resulted from an expanded B cell subset. Likewise, using this method, calculation of absolute numbers of CD4 circulating T cells revealed a 50% reduction of this T cell subset in BAFF Tg mice when compared to control mice, and the same observation was made for the CD8 T cell subset (data not shown). All B cells from the PBL of BAFF Tg mice have increased MHC class II and Bcl-2 expression when compared to B cells from control mice ( FIGS. 7D and 7E , respectively), indicating some level of B cell activation in PBL of BAFF Tg mice. T cells in the blood of BAFF Tg mice did not express the early activation markers CD69 or CD25; however, 40 to 56% of CD4 or CD8 T cells were activated effector T cells with a CD44 hi , L-selectin lo phenotype versus only 8% to 12% in control littermates (FIG. 7 F). Thus BAFF Tg mice clearly show signs of B cell lymphocytosis and global B cell activation along with T cell alterations.
Example 3
Expanded B Cell Compartments are Composed of Mature Cells.
To see whether overexpression of BAFF in the transgenic mice was affecting the B cell compartment centrally in the bone marrow and peripherally in secondary lymphoid organs, we examined by FACS the spleen, bone marrow and mesenteric lymph nodes from a total of seven BAFF Tg mice and seven control littermates derived from four different founder mice. The mature B cell compartment was analyzed by staining with both anti-B220 and anti-IgM antibodies. Two representative BAFF Tg mice and one representative control littermate are shown in FIG. 8 . The mature B cell compartment (IgM+. B220+) was increased in both the spleen and the mesenteric lymph nodes ( FIG. 8A , top and bottom panels, respectively). Analysis of B220+/IgM+ B cells ( FIG. 7A , middle panel) or the proB cell (CD43+/B220+) and the preB cell (CD43−/B220+) compartments in the bone marrow ( FIG. 8B ) showed that BAFF Tg mice and control littermates were similar. These data indicate that overexpression of BAFF is affecting the proliferation of mature B cells in the periphery but not progenitor B cells in the bone marrow. Analysis by FACS of the B cell subpopulations in the spleen, revealed an increased proportion of marginal zone (MZ) B cells in BAFF Tg mice when compared to control mice (Table 3). The population of follicular B cells remained proportional in both BAFF Tg and control mice whereas the fraction of newly formed B cells is slightly decreased in BAFF Tg mice (Table 3). This result was also confirmed on B220 + splenic B cells using anti-CD38 versus anti-CD24 antibodies and anti-IgM versus anti-IgD antibodies and analyzing for at the CD38 hi /CD24 + and IgM hi /IgD lo for the MZ B cell population, respectively, as previously described (Oliver et al., 1997)(data not shown). Immunohistochemical analysis using an anti-mouse IgM antibody revealed the expansion of the IgM-bright MZ B cell area in the spleen of BAFF Tg mice when compared to control mice (data not shown). All BAFF Tg B220 + 0 splenic B cells also express higher levels of MHC class II (Table 3) and Bcl-2 (data not shown) compared to splenic B cells from control mice, indicating that splenic B cells as well as B cells from PBL are in an activated state.
Example 4
BAFF Tg Mice have High Levels of Total Immunoglobulins, Rheumatoid Factors and Circulating Immune Complexes in their Serum.
The increased B cell compartment in BAFF Tg mice suggested that the level of total Ig in the blood of these animals might also be increased. SDS-PAGE, analysis of serum from BAFF Tg mice and control littermates showed that the heavy and light chains IgG bands were at least fold more intense in 3 out of 4 BAFF Tg mice compared to the control sera (FIG. 9 A). Likewise, an ELISA determination on the sera from BAFF Tg mice show significantly higher total Ig levels when compared to that of the control mice (FIG. 9 B).
Despite the high levels seen by SDS-PAGE, the excessively high levels of Ig seen by ELISA determination in some mice, e.g., 697-5, 816-8-3 and 823-20, led us to suspect the presence of rheumatoid factors (RF) in the sera, or autoantibodies directed against antigenic determinants on the Fc fragment of IgG (Jefferis, 1995). These antibodies could bind to the goat anti-mouse Ig used to coat the ELISA plates and give erroneously high values. ELISA plates were coated with normal irrelevant goat Ig and the binding of BAFF Tg Ig to normal goat Ig was measured. FIG. 9C shows that sera from most BAFF Tg mice contained Ig reacting with normal goat Ig, whereas only two out of 19 control mice exhibited reactivity in the same assay. These RF were mainly of the IgM, IgA and IgG2a isotypes (data not shown).
Presence of RF can be associated with the presence of high levels of circulating immune complexes (CIC) and cryoglobulin in the blood (Jefferis, 1995). To verify whether or not BAFF Tg mice have abnormal serum levels of CIC, a C1q-based binding assay was used to detect CIC in the 21 BAFF Tg mice analyzed above. Only 5 BAFF Tg showed significantly high levels of CIC when compared to control mice, nonetheless these mice corresponded to the animals having the highest total Ig and rheumatoid factor levels (FIG. 9 D). We also observed precipitate formation when BAFF Tg mice sera were diluted {fraction (1/15)} in water but not control sera indicating the presence of cryoglobulin in these mice (data not shown). Thus, in addition to B cell hyperplasia, BAFF Tg mice display severe hyperglobulinemia associated with RF and CIC.
Example 5
Some BAFF Tg Mice have High Levels of Anti-Single Stranded (ss) and Double-Stranded (ds) DNA Autoantibodies.
Initially, we observed kidney abnormalities reminiscent of a lupus-like disease in two of our founder mice (Table II). The presence of anti-DNA autoantibodies have also been described in SLE patients or the SLE-like (SWR×NZB)F1 (SNF1) mouse (Datta et al., 1987). Anti-ssDNA autoantibody levels were detected in BAFF Tg mice previously shown to have the highest level of total serum Ig (FIG. 10 A). We analyzed the serum of two BAFF Tg mice negative for antibodies against ssDNA (697-5 and 816-1-1) and three transgenic mice secreting anti-ssDNA antibodies (820-14, 816-8-3 and 820-7) for the presence of anti-dsDNA antibodies in parallel with five control littermates. BAFF Tg mice also secreted anti-dsDNA, however, the levels of secretion did not always correlate with that of anti-ssDNA antibodies, as serum from BAFF Tg mouse 697-5 which did not contain detectable levels of anti-ssDNA antibodies, was clearly positive for the presence of anti-dsDNA (FIG. 10 B). Therefore, BAFF Tg mice showing the most severe hyperglobulinemia secrete pathological levels of anti-DNA autoantibodies. Additionally, and also reminiscent of a lupus-like problem in these mice we detected immunoglobulin deposition in the kidney of six BAFF Tg mice analyzed (FIG. 10 C), three of these mice did not secrete detectable levels anti-DNA antibodies (data not shown).
Example 6
BAFF Tg Mice have Enlarged B Cell Follicles, Numerous Germinal Centers, Reduced Dendritic Cell Numbers and Increased Plasma Cell Numbers in both the Spleen and Mesenteric Lymph Nodes (MLN).
BAFF Tg mice had large spleens, MLN (data not shown) and Peyer's patches (FIG. 11 ). Immunohistochemistry showed the presence of enlarged B cell follicles and reduced peripheral arteriolar lymphoid sheets (PALS or T cell area) in BAFF Tg mice (FIG. 12 B). Interestingly, few germinal centers were observed in non-immunized control littermates (and is typical of this colony in general) and those present were small (FIG. 12 C), whereas BAFF Tg mice possessed numerous germinal centers in the absence of immunization (FIG. 12 D). Staining with anti-CD11c for dendritic cells in the T cell zone and the marginal zone of control mice ( FIG. 12E ) was considerably reduced in BAFF Tg mice (FIG. 12 F). Syndecan-1-positive plasma cells were almost undetectable in the spleen from control littermates (FIG. 12 G), yet the red pulp of BAFF Tg mice was strongly positive for syndecan-1 (FIG. 12 H). Very similar observations were made for the MLN (FIG. 13 ). In the MLN of BAFF Tg mice the B cell areas were dramatically expanded ( FIG. 13B ) in contrast to the normal node where B cell follicles were easily recognizable at the periphery of the node under the capsule with a typical paracortical T cell zone (FIG. 13 A). The medulla of MLN from BAFF Tg mice were filled with syndecan-1 positive cells which presumably are plasma cells (FIG. 13 H). In conclusion, analysis of secondary lymphoid organs in BAFF Tg mice was consistent with the expanded B cell phenotype showing multiple cellular abnormalities and intense immune activity.
REFERENCES
1. Smith et al. (1994) Cell 76:959-962.
2. Vassalli (1992) Annu. Rev. Immunol. 10:411-452.
3. De Togni et al. (1994) Science 264:703-707.
4. Koni et al. (1997) Immunity 6:491-500.
5. Amakawa et al. (1996) Cell 84:551-562.
6. Russell et al. (1993) Proc. Natl. Acad. Sci. USA 90:4409-4413.
7. Zheng et al. (1995) Nature 377:348-351.
8. van Kooten and Banchereau (1997) Curr. Opin. Immunol. 9:330-337.
9. Stuber and Strober (1996). J. Exp. Med. 183:979-989.
10. Schneider et al. (1997) J. Biol. Chem. 272:18827-18833.
11. Hahne et al. (1998) J. Exp. Med. 188:1185-1190.
12. Hahne et al. (1996) Science 274:1363-1366.
13. Grimaitre et al. (1997) Eur. J. Immunol. 27:199-205.
14. Thome et al. (1997) Nature 386:517-521.
15. Schneider et al. (1998) J. Exp. Med. 187:1205-1213.
16. Matsudaira, P. (1987) J. Biol. Chem. 262:10035-10038.
17. Armitage et al. (1992) Nature 357:80-82.
18. Bucher et al. (1996) Computer Chem. 20:3-24.
19. Banner et al. (1993) Cell 73:431-445.
20. Nagata (1997) Cell 88:355-365.
21. Black et al. (1997) Nature 385:729-733.
22. Wong et al. (1997) J. Biol. Chem. 272:25190-25194.
23. Kindler and Zubler. (1997) J Immunol. 159:2085-2090.
24. Sonoki et al. (1995) Leukemia 9:2093-2099.
25. Magrath, I. (1990) Adv Cancer Res 55:133-270.
26. Garside et al. (1998) Science 281:96-99.
27. MacLennan et al. (1997) Immunol. Rev. 156:53-66.
28. Dubois et al. (1997). J. Exp. Med. 185:941-951.
29. Tsubata et al. (1993) Nature 364:645-648.
30. Chicheportiche et al. (1997) J. Biol. Chem. 272:32401-32410.
31. Nakayama (1997) Biochem. J. 327:625-635.
32. Jefferis, R. (1995). Rheumatoid factors, B cells and immunoglobulin genes. Br. Med. Bull. 51, 312-331.
33. Schneider et al. (1999) J. Exp. Med. 189, 1747-1756.
34. Mcknights et al. (1983) Cell 34, 335-341.
35. Datta et al. (1987) J. Exp. Med. 165, 1252-1261.
|
The invention provides methods for treating or preventing disorders associated with expression of BAFF comprising BAFF and fragments thereof, antibodies, agonists and antagonists.
| 0
|
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority under 35 U.S.C. Section 119(e) to U.S. Provisional Application 60/791,731, filed on Apr. 13, 2006.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention refers to a process for manufacturing a breathable thermoadhesive transfer, for application onto a fabric or onto other materials, and a breathable thermoadhesive transfer obtained.
[0004] 2. Description of the Prior Art
[0005] In recent years the clothing manufacturing industry has paid particular attention to the use and development of so-called ‘technical’ fibres and/or fabrics.
[0006] In particular in the sportswear sector, fabrics that are capable of ‘helping’ athletes improve their performance in sports activities have been developed.
[0007] Among the various requirements for sportswear, particular attention has been given to developing extremely lightweight and/or breathable fabrics.
[0008] Articles of clothing often feature graphic designs, lettering, logos and decorations in general that help to improve the look of the garment and/or convey an advertising message, represent a logo, a concept, etc.
[0009] Various printing techniques are used to customize garments, depending, for example, on the type of fabric, the desired end result, etc. However, these ‘prints’, whether applied directly or indirectly onto the fabric, basically impede the adequate breathability thereof. In short, they cancel out the breathability of the fabric in the area onto which they are applied.
[0010] With reference to FIGS. 1 a and 1 b , a thermoadhesive transfer for application onto a fabric or onto materials in general is of a type known per se, obtained by means of a silk-screen, lithographic or offset printing process and/or a combination of these or other printing techniques.
[0011] The thermoadhesive transfer basically comprises:
a base sheet 1 made of paper, polyester, or in short any release base that allows the product 2 to be transferred; at least one layer of product 2 , made of polyurethane or flock or other materials, containing graphic designs, lettering, decorations and logos deposited on the base sheet 1 ; at least one thermoadhesive layer over the product layer 2 for application onto the fabric.
[0015] The thermoadhesive transfer is then applied onto a fabric (which may be of various types: natural, synthetic, elastic, etc.) for instance using a hot press transfer process.
[0016] The product 2 is basically transferred from the base sheet 1 to the fabric, or material in general, to which it is ‘fixed’ through the thermoadhesive.
[0017] If the fabric is of the breathable, technical or elastic type, or for use in sportswear applications, etc. it may be important to maintain its ‘breathability’ even on the surface covered by the transfer which, in some cases, may regard a large portion of the fabric, up to a much as 30%.
[0018] According to the current state of the art, the process used to manufacture breathable transfers consists of creating products provided with holes (indicated by number 3 in FIGS. 1 a and 1 b ) on the surface. Said holes are obtained for example by means of a silk-screen printing process in which the printed product is not applied to the whole surface.
[0019] However this process has a number of drawbacks and inevitable limitations:
The diameter of the holes cannot be made as ‘small’ as may be desirable. Thus, depending on the type of transfer product that is used, it is not usually possible to create holes with a diameter of less than a certain size. Holes of a given size increase the overall transparency of the transfer with a subsequent loss of definition of the image, significantly reducing the communicative effect (of an advertisement for instance) of the actual image. Some types of transfers consist of several layers of product. In the final top layer (of the product that has not yet been applied), the thermoadhesive layer is wider or thicker than the underlying layers. During application the adhesive tends to close the area of the holes thus cancelling out and/or obstructing the desired level of breathability.
SUMMARY OF THE INVENTION
[0022] The purpose of the present invention is to overcome all the drawbacks described above with a process for manufacturing a breathable thermoadhesive transfer, for instance for application onto a fabric, or onto materials in general, and the relative breathable thermoadhesive transfer that is obtained, so as to allow holes of any size, any shape, and any geometry, including variable geometry, to be created, and so as to guarantee breathability.
[0023] The present invention relates to a process for manufacturing a breathable thermoadhesive transfer, suitable for application onto a fabric or onto other materials, said thermoadhesive transfer comprising a base sheet, at least a layer of transfer product, and at least a layer of thermoadhesive material, characterized in that a step of processing using laser technology to create holes in said thermoadhesive transfer is carried out, before the application onto the fabric.
[0024] In particular, the present invention relates to a process for manufacturing a breathable thermoadhesive transfer, for instance for application onto a fabric, or onto materials in general, and the relative breathable thermoadhesive transfer that is obtained, as described more fully in the claims, which are an integral part of this description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Further characteristics and advantages of this invention will become clear from the following detailed description of a preferred embodiment thereof, with the help of the drawings attached hereto, which are merely illustrative and not limitative, in which:
[0026] FIGS. 1 a and 1 b are views respectively from the top and of a side cross-section of a preferred embodiment of a thermoadhesive transfer with holes according to the prior art;
[0027] FIGS. 2 a , 2 b are views respectively from the top and of a side cross-section of preferred embodiments of a thermoadhesive transfer with holes obtained by means of the process according to the present invention;
[0028] FIG. 3 shows a side cross-section of an embodiment of a thermoadhesive transfer having a surface of variable depth.
[0029] In the drawings the same numbers are used to indicate the same elements.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0030] According to the main aspect of the present invention, a step of processing using laser technology is introduced in order to create the holes in the thermoadhesive transfer.
[0031] Firstly the thermoadhesive transfer is manufactured using a conventional process, for instance silk-screen printing without holes, so as to obtain the desired image on the transfer.
[0032] A laser is then used to make holes in the thermoadhesive transfer before applying it to the fabric.
[0033] Finally, the thermoadhesive transfer is transferred to the fabric using a process known in the art.
[0034] The use of laser technology makes it possible to create holes of any diameter, even a diameter as small as desirable, and of any shape, even not round, for instance slits, at any distance from one another, even at variable distances on different areas of the thermoadhesive transfer.
[0035] This method overcomes the problem of the readability of the image on the thermoadhesive transfer, in that the smaller the diameter of the holes the more the transparency in the area comprising the holes can be reduced, and the better the definition and communicative effect of the image.
[0036] It is possible to selectively vary the size and distance between the holes on the surface of the thermoadhesive transfer.
[0037] By using the laser technology, the width of the holes is constant throughout the entire depth of the thermoadhesive transfer, optionally including the base sheet layer. The laser creates an initial heat seal effect on the edge of the holes in correspondence with the adhesive, preventing any ‘re-closing’ of the holes; the latter is a phenomenon that occurs when using the methods known in the art, due to the adhesive being transferred onto the fabric during the subsequent step of hot application. By applying the invention the adhesive remains confined to the areas without holes even after application to the fabric.
[0038] With reference to FIG. 2 b , the drawing illustrates the base sheet 4 , the top layer 5 of transfer product, and the holes 6 made using the laser, that pass through the entire thickness of the thermoadhesive transfer, including the base sheet.
[0039] In the variant embodiment of FIG. 2 c the base sheet 4 is not holed.
[0040] Furthermore, the use of laser technology makes it possible to achieve further significant visual effects. The surface of the thermoadhesive transfer can be cut to varying depths (see FIG. 3 ), and/or on different levels, eliminating portions thereof, to create image effects with variable depths.
[0041] A non-limitative example of a conventional laser machine for thermoadhesive transfer processing comprises a CO 2 laser source, with a power of between 100-200 Watt, electronically controlled by means of a computer provided with a monitor and operating software for cutting/marking the thermoadhesive transfer. The machine also comprises a three-axis galvanometric scanner with polar guide of the laser beam, focusing and adjustable cutting depth, and an external graphics station for defining the specific geometry of the holes in the thermoadhesive transfer.
[0042] The programming of the laser machine to obtain the desired hole geometry and cutting depths is performed in an usual way.
[0043] It will be apparent to the person skilled in the art that other alternative and equivalent embodiments of the invention can be conceived and reduced to practice without departing from the true spirit of the invention.
[0044] From the description set forth above it will be possible for the person skilled in the art to embody the invention without introducing any further construction details.
|
A process is described for manufacturing a breathable thermoadhesive transfer, for instance suitable for application onto a fabric, in which a step of processing using laser technology to create holes in said thermoadhesive transfer is carried out before the application step.
| 8
|
RELATED APPLICATIONS
This application claims priority from U.S. Provisional Application having Ser. No. 61/180,621 filed May 22, 2009, the entire content of which is hereby incorporated by reference.
TECHNICAL FIELD
The present subject matter relates to enabling portability of credentials across dual mode devices, for example, across dual mode devices configured to operate in both a CDMA network and an LTE network, while preventing certain type of situation that might permit fraudulent device operation.
BACKGROUND
In recent years, use of mobile communications devices for voice telephone services, email or text messaging services and even multi-media services has become commonplace, among mobile professionals and throughout the more general consumer population. Mobile service provided through public cellular or PCS (personal communication service) type networks, particularly for voice telephone service, has become virtually ubiquitous across much of the world. The rapid expansion of such mobile communication services has resulted in deployment of a variety of different and often incompatible wireless network technologies, in different jurisdictions or regions and in some cases as competing services within the same area. A large carrier may operate its network over a wide geographic area and have roaming agreements with operators of other compatible technology networks in other areas. However, occasions still arise in which a service technology of a home network may not be available in a visited area or region into which a customer roams and intends to use her mobile device. The service provider may utilize a different technology in a different area or country, or more often, networks of other operators in other region utilizing alternative technology. To allow continued operation in regions where the local provider offers service via a different technology, station manufactures have developed dual or multi mode mobile devices, which have the capability of communicating via two or more wireless mobile technologies.
Hence, global devices that use 3GPP2 type CDMA technologies (1XRTT and EVDO) are also required to operate in networks that support 3GPP technologies (GSM/UMTS/LTE). This is necessary because in many countries around the world CDMA is not deployed. One example would be European countries where a CDMA device would have no coverage at all. In addition, there are many countries, e.g., China and India, where both 3GPP2 and 3GPP based networks exist with extensive coverage.
To facilitate customer roaming where a particular operator may not have network coverage, the service provider or operator of one network will have agreements with other operators/service providers. Under such agreements, customers of the other operators may roam-in and use the one provider's network, whereas customers of the one provider may roam-out and use the networks of the other operators/service providers. As a result of the differences in network technologies and the availability of multimode mobile devices, there may be roaming agreements with operators providing the two different technologies.
3GPP variants of the mobile devices utilize a Subscriber Identity Module or “SIM” card (called UICC in the 3GPP standards documents—universal integrated circuit card). Such a case provides secure storage for various data needed for operation of a mobile station, such as data identifying the mobile device to the network (e.g. MDN and/or MN). However, the SIM card is a standardized removable module that can be moved from one mobile device to another, to effectively move the subscriber identity from one device to another.
For a mobile device conforming to CDMA technology standard, the credentials of the subscriber traditionally are stored on the mobile device instead of on the SIM card. The CDMA variant of the mobile devices often use an R-UIM/CSIM which is an internal memory module of the mobile device to store various data needed for operation of the mobile device, such as data identifying the subscriber and the mobile device to the network (e.g. MDN, PRL, MN, secure information). The concept of UICC cards were introduced at the very latest stage in the current development of CDMA technology. As such, many of the CDMA operators are still using models of the mobile devices without a UICC for CDMA.
With these operators moving to 3GPP technology, a UICC card is mandatory to access the network. Hence with dual mode (3GPP-CDMA) devices there are two options for accessing both CDMA and 3GPP technologies: (1) use the device UIM for CDMA access technologies credentials and UICC (e.g., SIM/USIM) for 3GPP access technologies credentials or (2) use removable UICC with R-UIM/CSIM in the device for CDMA and UICC card for 3GPP to access both the technologies. In the first scenario, the CDMA credential of the subscriber is stored in the memory (e.g., UIM) of the mobile device and the 3GPP credential of the subscriber is stored in the UICC card. This scenario may result in having two mobile devices with a single account. For example, a UICC card of a first mobile device may be inserted into a second mobile device. Inserting a UICC card of the first mobile device into the second mobile device will result in transfer of 3GPP credentials, which is stored in the UICC card, to the second mobile device. However, the CDMA credentials of the first mobile device, which is stored in the memory of the first mobile device, continues to remain on the first mobile device. The first mobile device has the otherwise valid credentials and is still operable at least in old CDMA technology networks. The second mobile device has the same credentials and fully operable in all network technologies.
As such, there occurs a fraud condition with the same active credential of a user on two different devices. That is, both the first and second mobile devices may be provisioned and used with the same phone number or the like without informing the network operator. For example, the first mobile device may work in the CDMA network and the second mobile device may work in the 3GPP network with the same number.
In the second scenario, the credentials of the subscriber are stored on two separate chips (e.g., UICC with CSIM in the device and UICC card). The UICC with CSIM stores CDMA credentials of the subscriber; whereas, the UICC card stores 3GPP credentials of the subscriber. As such, transferring both cards from one mobile device to another may result in full transfer of subscriber account from one device to another. That is, since the CDMA credentials are not stored on the device itself, when the SIM cards are transferred, so is the credentials of the subscriber. As such, the fraud situation described above may be avoided.
The problem with second solution, however, is that many CDMA operators are using model devices without a UICC card and, as such, the solution would not cover many mobile devices that do not have a UICC card and/or are not configured to receive a UICC card.
Hence, for mobile devices that store CDMA credential on the device itself, there is a need for additional security infrastructures to counter attack this fraud condition. In particular, there is a need for a method that minimizes the fraud condition and/or enhances user experience when switching from one dual mode CDMA-3GPP device to another.
SUMMARY
In one general aspect, the instant application describes a method for enabling dual-mode mobile devices to access a Code Division Multiple Access (“CDMA”) network. The method includes steps of receiving, from a first mobile device, a request to access a CDMA network, a first mobile device identifier identifying the first mobile device for the CDMA network access and a first integrated circuit card identifier identifying a first integrated circuit card being used by the first mobile device to access a Third Generation Partnership Project (“3GPP”) network; associating the first mobile device identifier with the first integrated circuit card identifier; and storing in a database the association between the first mobile device identifier and the first integrated circuit card identifier.
The method also includes steps of receiving, from a second mobile device, a request to access the CDMA network, a second mobile device identifier identifying the second mobile device for the CDMA network access and a second integrated circuit card identifier identifying a second integrated circuit card being used by the second mobile device to access the 3GPP network; associating the second mobile device identifier with the second integrated circuit card identifier; and storing in the database the association between the second mobile device identifier and the second integrated circuit card identifier. The method also includes steps of authorizing the first mobile device to access the CDMA network only after associating the first mobile device identifier with the first integrated circuit card identifier; and authorizing the second mobile device to access the CDMA network only after associating the second mobile device identifier with the second integrated circuit card identifier.
Implementations of the above general aspect may include one or more of the following features. The method may further include a step of receiving, from a third mobile device, a request to access a CDMA network, a third mobile device identifier identifying the third mobile device for the CDMA network access; referencing the database to determine whether the third mobile device identifier is associated with an integrated circuit card identifier; determining that the third mobile device identifier is not associated with the integrated circuit card identifier; and denying the CDMA network access to the third mobile device.
The first integrated circuit card may include a first Subscriber Identity Module (“SIM”) card. The second integrated circuit card may include a second SIM card. The first mobile device identifier may include a first Mobile Directory Number (“MDN”), a first Mobile Equipment Identifier (“MEID”), or a first Mobile Identifier Number (“MIN”). The second mobile device identifier may include a second MDN, a second MEID, or a second MIN.
The method may further include steps of receiving, from the first mobile device, a new request to access the CDMA network and the second integrated circuit card identifier identifying the second integrated circuit card being used by the first mobile device to access the 3GPP network; associating the first mobile device identifier with the second integrated circuit card identifier; and updating the database to reflect the association between the first mobile device identifier and the second integrated card identifier.
The method may further include steps of determining, via referencing the database, that the first mobile device identifier is associated with the first integrated circuit card identifier and requesting, from the first mobile device, credential information to provision the first mobile device for the second integrated circuit card. In response to the request, receiving the credential information from the first mobile device. Determining whether the credential information is valid; and upon determining that the credential information is valid, provisioning the first mobile device for the second integrated circuit card identifier.
Updating the database may include updating the database after determining that the credential information is valid. Updating the database may include removing from the database the previous association between the first mobile device identifier and the first integrated circuit card identifier; and adding to the database the new association between the first mobile device identifier and the second integrated circuit card identifier. Alternatively, updating the database may include updating the database to include the new association between the first mobile device identifier and the second integrated circuit card identifier in addition to the previous association between the first mobile device identifier and the first integrated circuit card identifier.
The method may further include steps of authorizing the first mobile device to access the CDMA network only after associating the first mobile device identifier with the second integrated circuit card identifier. The method may further include steps of updating the database to remove the association between the second mobile device identifier and the second integrated circuit card identifier; and preventing the second mobile device to access the CDMA network.
The method may further include steps of receiving, from the second mobile device, a new request to access the CDMA network and a third integrated circuit card identifier identifying a third integrated circuit card being used by the second mobile device to access the 3GPP network; associating the second mobile device identifier with the third integrated circuit card identifier; and
updating the database to reflect the association between the second mobile device identifier and the third integrated card identifier. Updating the database may include removing from the database the previous association between the second mobile device identifier and the second integrated circuit card identifier; and adding to the database the new association between the second mobile device identifier and the third integrated circuit card identifier. The method may further include a step of authorizing the second mobile device to access the CDMA network only after associating the second mobile device identifier with the third integrated circuit card identifier.
In one general aspect, the instant application describes an article of manufacture comprising a computer-readable storage medium and a computer program for enabling a dual-mode mobile device to access a CDMA network, the computer program being embodied on the computer-readable storage medium and including instructions that, when executed, cause the mobile device to implement functions comprising: identifying a first integrated circuit card included in the mobile device, the first integrated circuit card being used to access a 3 GPP network; associating the first integrated circuit card identifier with a mobile device identifier assigned to the mobile device; and storing in the mobile device a database the association between the first integrated circuit card identifier and the mobile device identifier. The computer-readable medium further includes instructions to cause the mobile device to implement additional functions comprising: enabling access to a CDMA network only after associating the first integrated circuit card identifier with the mobile device identifier; identifying a second integrated circuit card included in the mobile device, the second integrated circuit card replacing the first integrated circuit card and being used to access the 3GPP network; referencing the database to determine whether the second integrated circuit card is associated with the mobile device identifier. Determining that the second integrated circuit card is not associated with the mobile device identifier and requesting from a user to insert the first integrated circuit card or to provision the mobile device for the second integrated circuit card to enable access to the CDMA network.
Implementations of the above general aspect may include one or more of the following features. The computer-readable medium may further include instructions to cause the mobile device to implement additional functions comprising: receiving, from the user and in response to the request, the first integrated circuit card; and enabling access to the CDMA network upon receiving the first integrated circuit card. The computer-readable medium may further include instructions to cause the mobile device to implement additional functions comprising: receiving, from the user and in response to the request, credentials for provisioning the mobile device for the second integrated circuit card; authenticating the received credentials; and updating the database to reflect the association between the mobile device identifier and an identifier of the second integrated circuit card.
The instructions to cause the mobile device to update the database may include instructions to cause the mobile device to implement additional functions comprising: removing from the database the previous association between the mobile device identifier and the first integrated circuit card identifier; and adding to the database the new association between the mobile device identifier and the second integrated circuit card identifier. The instructions to cause the mobile device to update the database may include instructions to cause the mobile device to implement additional functions comprising updating the database to include the new association between the mobile device identifier and the second integrated circuit card identifier in additional to the previous association between the mobile device identifier and the integrated circuit card identifier.
The computer-readable medium may further include instructions to cause the mobile device to implement additional functions comprising authorizing the mobile device to access the CDMA network only after associating the mobile device identifier with the second integrated circuit card identifier. The mobile device identifier may include a Mobile Directory Number (“MDN”), a Mobile Equipment Identifier (“MEID”), or a Mobile Identifier Number (“MIN”). The computer-readable medium may further include instructions to cause the mobile device to implement additional functions comprising denying the user access to the CDMA network if the user does not provider the first integrated circuit card or provision the mobile device for the second integrated circuit card.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawing figures depict one or more implementations in accord with the present teachings, by way of example only, not by way of limitation. In the figures, like reference numerals refer to the same or similar elements.
FIG. 1 illustrates an exemplary database that stores information about multiple subscriber accounts.
FIG. 2 illustrates the exemplary database shown in FIG. 1 which has been updated to indicate that each subscriber account has been provisioned to access the CDMA network.
FIG. 3 is a high level functional block diagram, useful in explaining mobile devices, network elements and other components that may be involved in mobile device communications and related system selection functions.
FIG. 4 is a high level functional block diagram of a handset type example of a mobile device describes with respect to FIGS. 1-3 .
FIG. 5 is a simplified functional block diagram of a computer that may be configured as a host or server.
FIG. 6 is a simplified functional block diagram of a personal computer or other work station or terminal device.
DETAILED DESCRIPTION
In the following detailed description, numerous specific details are set forth by way of examples in order to provide a thorough understanding of the relevant teachings. However, it should be apparent to those skilled in the art that the present teachings may be practiced without such details. In other instances, well known methods, procedures, components, and/or circuitry have been described at a relatively high-level, without detail, in order to avoid unnecessarily obscuring aspects of the present teachings.
In one aspect, the instant application describes techniques that allow a true portability of credentials across dual-mode devices when dual-mode devices exchange their UICC with each other. That is, the instant application describes techniques that allow the subscriber account to follow the UICC card and stay within one device instead of staying within multiple devices. As such, the instant application can solve the problem associated with the prior art in which two mobile devices may become associated with one subscriber account.
The dual mode mobile devices are configured to operate in both CDMA network and 3GPP network. For the purposes of the description, the 3GPP network in this application is assumed to be an LTE network. However, one of ordinary skill in the art would recognize that the 3GPP network may include other types of network such as GSM/UMTS.
Once the UICC card is inserted in the mobile device, the mobile device and the CDMA network both keep track of the ICCID of the UICC card. To do this end, the mobile device includes a file or a database that keeps an association between the mobile device's ID (e.g., IMEI/MEID) and the ICCID. Once the device dials *228 to be provisioned, the ICCID and the mobile device's ID are forwarded to the CDMA network. As such, the CDMA recognizes the particular UICC card that is being used on the mobile device and stores this association within its database.
Thereafter, when the user changes the UICC card of the mobile device, the mobile device recognizes that the ICCID of the newly inserted UICC card does not match the one stored in its internal database. In this manner, the mobile device realizes that this is a new UICC card, which is associated with new credentials. The mobile device informs the user of the mismatch/new credential condition and requests that the user either inserts a correct UICC card or provision the mobile device for the newly inserted UICC card. If the user chooses to provision the device for the newly inserted UICC card, the mobile device prompts the user to enter a PIN. The PIN may include an account number or a secret password or information that is only known to the owner of the device/account. The PIN can be administered through a web interface (e.g., Verizon Wireless™ webpage) in case the user forgets or accidentally locks the UICC card. To illustrate, in one example, the webpage may solicit identification information from the user who has forgotten his/her PIN to authenticate the user. Upon successful authentication, the user is provided with the new PIN. The new PIN may be downloaded securely to the UICC card. In one example, for better user experience, the PIN entry can be overcome by an internal comparison of the PIN stored in the UICC with the one administered through the web interface, without asking the user to key in the PIN.
In one implementation, the PIN is associated with the credentials previously stored in the mobile device. In this scenario, the user associated with the credentials previously stored in the mobile device can authorize the provisioning of the mobile device for the newly inserted UICC card. In another implementation, the PIN is associated with the account of the newly inserted UICC card. As such, the user associated with the account of the newly inserted UICC card can authorize the provisioning of the mobile device for the newly inserted UICC card. The newly inserted UICC card may include, for example, credential information necessary to authenticate the PIN received from the user. To this end, the mobile device compares the PIN received from the user with the one stored on the newly inserted UICC card and based on the result of the comparison determines whether to provision the device for the newly inserted mobile device. Another approach would be to communicate with the network to implement the challenge and PIN or password authentication as against account data stored in the network, although the account could be that associated with the previously stored credentials or an account associated with the newly inserted UICC.
The comparison such as PIN and ICCID against MEID can either be executed in the device or in the UICC card. If the user-provided PIN matches, then the mobile device forwards the ID of the newly inserted UICC card to the CDMA network and receives from the network the credentials pertaining to the newly inserted UICC card. The network updates its database accordingly, provisions the new device with the right user credentials, and grants access to the mobile device. However, if the PIN does not match the credentials associated with the newly inserted UICC card, then no access is granted on the CDMA network. Of course, if the device moves to the LTE network, the device can continue its operation. In one implementation, the mobile device that previously included the newly inserted UICC card is deactivated until it receives a new UICC card and is properly provisioned for the new UICC card. The device from which the UICC card was removed shall not work on CDMA network until a correct UICC card is inserted into it. This ensures that the device only works in one mode, which has the right UICC card.
In this manner, the scenario in which the subscriber account ends up being associated with both of two otherwise different mobile devices is avoided. With this overview, it is helpful to first describe in detail how a dual mode mobile device can be provisioned while operating in different networks and then describe what happens when the provisioned dual mode mobile device receives a new UICC card.
FIG. 1 illustrates an exemplary database 5 that stores information about first and second dual-mode devices. The two entry table and the data in the table entries are given here by way of a simple example useful in explaining the present concepts. The table may be stored in the CDMA network and may include two accounts, each for a different dual-mode mobile device. An actual database, of course, would include listings or entries for many devices or accounts, and there may be more data stored for each account or device. As shown, the table includes a first account 007 associated with one dual-mode mobile device and a second account 009 associated with another dual-mode mobile device. The first account includes account number 007 and is associated with user Zon. The dual-mode mobile device associated with this account includes a UICC chip ID of ICCID — 007 and a device ID of IMEI — 007.
The second account includes account number 009 and is associated with user Solo. The dual-mode mobile device associated with this account includes a UICC chip ID of ICCID — 009 and a device ID of IMEI — 009. Since both of the mobile devices include a valid UICC chip they can operate in the LTE network. As shown in the table 5, however, neither of the devices can operate in the CDMA network since they have not yet been provisioned for complete access to CDMA network. As such, they do not yet include CDMA provisioning information in table 5.
The methodology to provision a mobile device while it is operating in one network may be different than provisioning the same device while it is operating in another network. To illustrate, in a CDMA only network, upon boot up the device checks to see if there is any previous reference of UICC stored in its memory. It is assumed that the device is new with no credentials. As such, there should be no previous reference to UICC.
Moving forward, the device recognizes the UICC operating on it and in order to keep track of it stores the ICCID of the UICC card in its internal database. In keeping with a previous example, the device associated with account number 007 will store ICCID — 007 in its memory, whereas the device associated with account number 009 will store ICCID — 009 in its memory.
To provision the device in the CDMA network, the device sends its IMEI/MEID to the CDMA network. In one example, the user connects to a computer and selects a connect option on, for example, Verizon Wireless Access Messenger, assuming that the CDMA network is the Verizon CDMA network. As a result, the device sends the IMEI to the network for provisioning the device as usual. The computer also sends the ICCID to the network for registering the device to the IMEI/MEID. As a result, the network associates the ICCID to the IMEI in its database.
In keeping with the previous example, the device associated with account number 007 sends ICCID — 007 and IMEI — 007 to the CDMA network upon connecting thereto via the air interface. The CDMA network receives the ICCID — 007 and IMEI — 007 and associates the ICCID — 007 with the IMEI — 007. Similarly, the device associated with account number 009 sends ICCID — 009 and IMEI — 009 to the CDMA network. The CDMA network receives the ICCID — 009 and IMEI — 009 and associates the ICCID — 009 with the IMEI — 009.
FIG. 2 illustrates the exemplary database 5 which has been updated to reflect that each subscriber account has been provisioned to access the CDMA network. As shown, the set flag column indicates that the mobile device associated with account number 007 is provisioned and the provisioning information column indicates the network in which the mobile device is provisioned in, namely, the CDMA network. Similarly, for account number 009, the set flag column indicates that the dual mobile device is provisioned and the provisioning information column indicates that the mobile device is provisioned in the CDMA network. For each account, the database 5 also illustrates that there is an association between the mobile device ID and the UICC chip operating on the mobile device.
Provisioning the device in CDMA and LTE network is slightly different than provisioning the device in the CDMA only network. Similar to provisioning steps in the CDMA network, on boot up the device checks to see if there is a previous reference of UICC stored in its memory. Since the device is a new device, it likely includes no such reference. The device identifies the ICCID of the UICC card operating on it and stores this ID into its memory. In keeping with a previous example, the device associated with account number 007 stores ICCID — 007 in its memory. The device associated with account number 009 stores ICCID — 009 in its memory.
Since the mobile device receives communication services from the LTE network the user is granted access right away. Since the device also receives communication services from the CDMA network, in the background, the device sends the ICCID and the IMEI to the CDMA network. The CDMA network uses the IMEI to provision the device as usual. The CDMA network also registers that ICCID to the IMEI of the device. In keeping with the previous example, the device associated with account number 007 sends ICCID — 007 and IMEI — 007 to the CDMA network. The CDMA network receives the ICCID — 007 and IMEI — 007 and associates the ICCID — 007 to the IMEI — 007. Similarly, the device associated with account number 009 sends ICCID — 009 and IMEI — 009 to the CDMA network. The CDMA network receives the ICCID — 009 and IMEI — 009 and associates the ICCID — 009 to the IMEI — 009. In this manner, the CDMA network tracks the UICC card that is operating on each mobile device.
Provisioning the device on the LTE only network, is slightly different from provisioning the dual-mode mobile device on the CDMA only network or the LTE and CDMA network. Similar to the provisioning steps in the CDMA network, on boot up the device check to see if there is any previous reference of UICC stored in its memory. Since the device is a new device, it stores the value of the ICCID inserted therein into its memory. In keeping with a previous example, the device associated with account number 007 will store ICCID — 007 in its memory. The device associated with account number 009 will store ICCID — 009 in its memory.
Since the device is in the LTE network, the access is granted right away and the device is ready to go. To be provisioned in the CDMA network, however, the user may have to send its credentials to the CDMA network. Since the device only receives communication services from the LTE network and not in the CDMA network, the device tracking application informs the database to set a flag to provision the device for CDMA when CDMA becomes available. When the CDMA does become available, in the background, the device sends the ICCID and its IMEI to the CDMA network and the network associates the ICCID with the IMEI of the device in a manner described above with respect to FIG. 2 .
As pointed out above, once the UICC card is inserted in the device the device keeps tracks of the ID (e.g., ICCID) associated with the UICC card. In the process of being provisioned the device sends this ID to the CDMA network to inform the network of the UICC card that the device is using or for which it is being provisioned. The CDMA network also updates its database to associate the UICC ID with the device (e.g., with the IMEI of the device). In the CDMA network, when the user changes UICC card of the device, the device references its database and recognizes the mismatch between the new UICC card ID and the previous UICC card ID stored in memory in the device.
The device informs the user of the mismatch and requests the user to either insert the previous UICC card or provision the phone for the newly inserted UICC card. For example, the device may display to the user “for connectivity please insert the correct UICC or would you like to provision this device for your credentials.” If the user chooses to provision the device for the newly inserted UICC card, the device prompts the user to enter a PIN that is known to the subscriber and the network. The PIN may include an account number and/or a secrete password.
In one implementation, the PIN is associated with the credentials previously stored in the mobile device. In this scenario, the user associated with the credentials previously stored in the mobile device can authorize the provisioning of the mobile device for the newly inserted UICC card. In another implementation, the PIN is associated with the account of the newly inserted UICC card. As such, the user associated with the account of the newly inserted UICC card can authorize the provisioning of the mobile device for the newly inserted UICC card. The newly inserted UICC card may include, for example, credential information necessary to authenticate the PIN received from the user. In another implementation, the credential information necessary to authenticate the PIN received from the user may be stored in the network. To this end, the mobile device may communicate with the network to implement the challenge and PIN or password authentication as against account data stored in the network. The account could be that associated with the previously stored credentials or an account associated with the newly inserted UICC.
In either case, the mobile device compares the PIN received from the user with the credentials associated with the newly inserted UICC card and based on the result of the comparison determines whether to provision the device for the newly inserted mobile device. If the password matches, then the device forwards the ID of the newly inserted UICC card to the CDMA network and receives from the network the credentials pertaining to the newly inserted UICC card. The network updates its database accordingly. However, if the PIN does not match the credentials associated with the newly inserted UICC card, then no access is granted on the CDMA network. Of course, if the device moves to a different network (e.g., LTE network), the device will work in that network.
To illustrate further and in keeping with previous examples, assume that the user is in the CDMA network and decides to remove the UICC card including ICCID — 007 from the dual mode mobile device associated with account number 007 and in its place inserts the UICC card having ICCID — 009 associated with account number 009. In this scenario, upon boot up the device compares the ICCID value with the one stored in the device and recognizes the mismatch. The device may recognize the mismatch by referencing an internal table that includes the ICCID of the UICC card for which the device is provisioned.
Upon recognizing the mismatch, the device informs the user of the same and requests the user to either insert the previous UICC card (e.g., UICC having ICCID — 007, hereinafter “UICC card 007”) or provision the device for the newly inserted UICC card (e.g., UICC having ICCID 009, hereinafter “UICC card 009”). If the user chooses to provision the phone for UICC card 009, the user is prompted to enter a PIN. If the PIN matches with the credential stored on the device, then ICCID — 009 is sent to the network and the credentials pertaining to ICCID — 009 is provisioned in this device. The network also updates its database to reflect in account 007 that ICCID — 009 is now associated with IMEI — 007.
Similarly, the network also updates its database to reflect in account entry 009 that no ICCID — 009 is associated with IMEI — 009. As such, account 009 is temporarily deactivated until another device receives a new UICC card associated with the account 009 and can be provisioned in the CDMA network.
In another scenario, when the user is in an area with overlapping CDMA and LTE network coverage, and the user changes the UICC card of the device, on boot up the device compares the ICCID value of the newly inserted UICC card with the one stored in its database and recognizes the mismatch between them. If the device is connecting to the LTE network, however, the access is granted right away even though there is a mismatch between the devices and no further changes may be made to the device. This is because in the LTE network the credentials are transferred from one device to another via the UICC card. The UICC provides the credentials regardless of any other credentials that may be stored on in the device.
If connecting to the CDMA network, however, the device informs the user of the mismatch and requests the user to either insert the previous UICC card or provision the phone for the newly inserted UICC card. For example, the device may display to the user “for connectivity please insert the correct UICC or would you like to provision this device for your credentials.” If the user chooses to provision the device for the newly inserted UICC card, the device prompts the user to enter a PIN. If the user-entered PIN matches with the PIN on the device, then the device forwards the ID of the newly inserted UICC card to the CDMA network and receives from the network the credentials pertaining to the newly inserted UICC card. The network updates its database accordingly. However, if the PIN does not match the credentials associated with the newly inserted UICC card, then no access is granted on the CDMA network.
In yet another scenario, when the user is in only the LTE network and changes the UICC card of the device, on boot up the device compares the ICCID value of the newly inserted UICC card with the one stored in its database and recognizes the mismatch between them. However, since the device is connecting to the LTE network, the access is granted right away and no further changes to the device may be necessary. This is because in the LTE network the credentials are transferred from one device to another via the UICC card, as noted in the CDMA and LTE example.
If the device later on moves to the CDMA network, due to the mismatch between the ICCID of the newly inserted UICC and the ICCID stored in the device's database, the device requests the user to either insert the previous UICC card or provision the device for the newly inserted UICC card in a manner described above. If the user chooses to provision the device for the newly inserted UICC card, the device prompts the user to enter a PIN. Upon successful authentication, the device forwards the ID of the newly inserted UICC card to the CDMA network and receives from the network the credentials pertaining to the newly inserted UICC card. The network updates its database accordingly. However, if the PIN does not match the credentials associated with the newly inserted UICC card, then no access is granted on the CDMA network.
FIG. 3 is a functional block diagram of an exemplary system of wireless networks for providing mobile voice telephone services and various data services. For discussion purposes, the diagram shows two wireless networks 10 and 30 operated in accord with different technology standards. The networks 10 and 30 often (but not always) may be operated by different providers, carriers or operators. The communication networks 10 and 30 implementing the illustrated system provide mobile voice telephone communications as well as other services such as text messaging and various multimedia packet data services, for numerous mobile devices. For purposes of later discussion three mobile devices 12 , 13 and 33 appear in the drawing.
The elements indicated by the reference numerals 10 and 30 generally are elements of the respective operator's network, although the mobile devices 12 , 13 and 33 typically are sold to the carrier's customers. Today, mobile devices typically take the form portable handsets, smart-phones or personal digital assistants, data cards for computers, although they may be implemented in other form factors. Each mobile communication network 10 or 30 provides communications between mobile devices 12 , 13 and 33 as well as communications for the mobile devices with other networks and devices shown generally at 11 outside the mobile communication networks. An inter-carrier or other intermediate network 29 may provide communication connectivity between the mobile communication networks 10 and 30 .
Each network 10 and 30 allows users of the mobile devices operating through the respective network to initiate and receive telephone calls to each other as well as through the public switched telephone network (PSTN) 19 and telephone stations 21 connected thereto. One or both of the networks typically offers a variety of text and other data services, including services via the Internet 23 , such as downloads, web browsing, e-mail, etc. via servers shown generally at 25 as well as message communications with terminal devices represented generally by the personal computer 27 .
The networks 10 and 30 are generally similar, except in our example, they offer respective services via two different wireless communication technologies. For purposes of an example for discussion here, we will assume that the network 10 is a CDMA technology network, whereas the network 30 is an LTE technology network.
The mobile communication network 10 typically is implemented by a number of interconnected networks. Hence, the overall network 10 may include a number of radio access networks (RANs), as well as regional ground networks interconnecting a number of RANs and a wide area network (WAN) interconnecting the regional ground networks to core network elements. A regional portion of the network 10 , such as that serving mobile device 13 will typically include one or more RANs and a regional circuit and/or packet switched network and associated signaling network facilities.
Physical elements of a RAN operated by one of the mobile service providers or carriers, include a number of base stations represented in the example by the base stations (BSs) 17 . Although not separately shown, such a base station 17 typically comprises a base transceiver system (BTS) which communicates via an antennae system at the site of base station and over the airlink with one or more of the mobile devices 13 , when the mobile devices are within range. The BTS is the part of the radio network that sends and receives RF signals to/from the mobile devices that the base station currently serves. Hence, in our example, the BTS would utilize CDMA type transceiver equipment and implement communications in accord with the protocols of the applicable 3GPP2 standard, for signaling, registration, voice communication, data communication, etc. For example, each base station 17 will broadcast certain standardized information to allow a mobile device 12 or 13 in the region to search for, find and lock-onto the base station 17 and acquire information needed to register and initiate communications via the network 10 , all in accord with the standard 3GPP2 protocols.
The radio access networks also include a traffic network represented generally by the cloud at 15 , which carries the user communications for the mobile devices 12 , 13 between the base stations 17 and other elements with or through which the mobile devices communicate. Individual elements such as switches and/or routers forming the traffic network 15 are omitted here for simplicity. Although not separately shown, the network 15 will include or connect with a number of service control elements, for authenticating mobile devices to use the network 10 , for authenticating mobile device users and/or for authorizing users or devices to access various services and service features offered by the particular network 10 , and for usage accounting and billing functions. At least some of the authentication functions and/or authorization functions require credentials information from the mobile devices, from time to time.
The traffic network portion 15 of the mobile communication network 10 connects to a public switched telephone network 19 . This allows the network 10 to provide voice grade call connections between mobile devices and regular telephones connected to the PSTN 19 . The drawing shows one such telephone at 21 . The traffic network portion 15 of the mobile communication network 10 also connects to a public packet switched data communication network, such as the network commonly referred to as the “Internet” shown at 23 . Packet switched communications via the traffic network 15 and the Internet 23 may support a variety of user services through the network 10 , such as mobile device communications of text and multimedia messages, e-mail, web surfing or browsing, programming and media downloading, etc. For example, the mobile devices may be able to receive messages from and send messages to user terminal devices, such as personal computers, either directly (peer-to-peer) or via various servers 25 . The drawing shows one user terminal device as a personal computer (PC) at 27 , by way of example.
The carrier or service provider that operates the network 10 will also operate a number of systems that provide ancillary functions in support of the communications services provided through the network 10 , and those elements communicate with other nodes/elements of the network 10 via one or more private IP type packet data networks or Intranets (not separately shown). Such systems maintain various records used for authentication and authorization functions and provisioning necessary information into the mobile devices to enable the devices to operate via the network 10 . Of note for purposes of the present discussion credential management function, one or more such systems provide the capability to receive and store credential information and download provisioning into the mobile devices of the network operator, in this example, via the networks. These systems may also support downloading of the executable programming for credential management, to initially install such programming in the mobile devices or to fix or update the programming in the mobile devices over time. An example of such a system that may facilitate such operations via the networks is the Over-The-Air service activation/provisioning Function (OTAF) 28 . In the example, the OTAF 28 may be a server connected to the traffic network 15 , to enable the server to communicate with the mobile devices of the network operator's customers.
As noted earlier, many mobile wireless communications networks have been deployed and are available today. For purposes of discussion, the example of FIG. 3 shows a second mobile network 30 . In our example, the network 30 is operated by a different carrier or service provider than the operator of network 10 . In some areas, the second network 30 could utilize the same wireless technology as the network 10 , but in our example, the network 30 utilizes a different wireless network technology. The network 10 is a CDMA technology network, and in the example, the network 30 is a LTE technology network.
Like the network 10 , the physical elements of the radio access network (RAN) 30 include a number of base stations (BSs) 37 , each of which includes a base transceiver system (BTS) and associated antenna system. In our example, each BTS of a base station 37 would utilize LTE type transceiver equipment and implement communications in accord with the protocols of the applicable 3GPP standard, for signaling, registration, voice communication, data communication, etc. For example, each base station 37 will broadcast certain standardized information to allow a mobile device 12 or 33 in the region to search for, find and lock-onto the base station 37 and acquire information needed to register and initiate communications via the network 30 , all in accord with the standard LTE protocols.
The radio access network portions of network 30 also include a traffic network represented generally by the cloud at 35 , which carries the user communications for the mobile devices 12 , 33 between the base stations 37 and other elements with or through which the mobile devices communicate. Individual elements such as switches and/or routers forming the traffic network 35 are omitted here for simplicity. Although not separately shown, the network 35 will include or connect with a number of service control elements, for authenticating mobile devices to use the network 30 , for authenticating mobile device users and/or for authorizing users or devices to access various services and service features offered by the particular network 30 .
Similar to network 10 , the traffic network portion 35 of the mobile communication network 30 connects to a public switched telephone network 19 , to offer voice grade telephone call connections between mobile devices and regular telephones 21 connected to the PSTN 19 . The traffic network portion 35 of the mobile communication network 30 also connects to a public packet switched data communication network, such as the network commonly referred to as the “Internet” shown at 23 , for various mobile device communications with servers 25 and/or user terminal devices 27 . Although omitted for simplicity, the network 30 may also include various systems that provide ancillary functions in support of the communications services provided through the network 30 , such as a system similar to the OTAF 29 provisioning the mobile devices of the network operator's customers.
In keeping with the previous examples, mobile devices 12 , 13 , and 33 have dual mode capability to utilize both CDMA and LTE technology networks. Each mobile device may include a database that associates a particular UICC to the mobile device. The CDMA network also may include a database that associates a particular UICC to the mobile device. As such, the device can recognize when its UICC is changed and limit the access of the user in the CDMA network based on such recognition.
For example and referring also to FIG. 1 , assume that mobile device 13 is associated with account 007 and the mobile device 12 is associated with account 009. As such, mobile device 13 includes a database that associates CCID — 007 with the IMEI — 007 and mobile device 12 includes a database that associates CCIC — 009 with IMEI — 009. The CDMA network may also include a similar database as shown in FIG. 1 . Now, if the user of mobile device 13 changes its UICC card (hereinafter “UICC card 007”) with UICC card of mobile device 12 (hereinafter, “UICC card 009”), mobile device 13 recognizes the mismatch between the CCID — 009 and CCID — 007 stored in its database and informs the user of the same.
The mobile device 13 requests the user to either insert UICC card 007 or provision the phone for the newly inserted UICC card 009. For example, the device may display to the user “for connectivity please insert a cored UICC card or would you like to provision this device for your credentials.” If the user inserts UICC 007, the user is granted access on CDMA network 15 . If, however, the user chooses to provision the device for UICC card 009, the device prompts the user to enter a PIN. The PIN may include an account number or a secrete password. If the password matches, then the device forwards the ICCID — 009 to the CDMA network 15 and receives from the network 15 the credentials pertaining to ICCID — 009.
The CDMA network 15 updates its database accordingly and grant access to mobile device 13 . That is, the CDMA network 15 updates table 5 to reflect that in account 007 ICCID — 009 (instead of ICCID — 007) is now associated with the IMEI — 007. Furthermore, the CDMA network 15 updates table 5 to erase the association between ICCID — 009 and the IMEI — 009. As such, mobile device 12 cannot use the CDMA network 10 or the LTE network 33 since it does not include a valid UICC. To communicate on the LTE and CDMA networks, mobile device 12 will require a valid UICC (e.g., UICC card 007).
In one implementation the CDMA table 5 may be stored in database 200 . The database 200 generally stores credentials (e.g., MIN, MDN, PRL) associated with mobile devices 12 , 13 , and 33 and may be used/modified by various elements of the network, from time to time. For example, the CDMA network may update the table to reflect new association formed for each mobile device when the UICC card of the mobile device is changed. Some or all of the credential information is populated into storage in or associated with various device control elements of the network 15 for use in actual authentication and authentication operations.
If the user inserts the UICC card 007 inside mobile device 12 , then similar to the above scenario, mobile device 12 recognizes the mismatch between its internal ICCID — 009 and the ICCID 007 associated with UICC card 007. Therefore, similar to the above-described scenario, mobile device 12 requests the user to either insert UICC card 009 or provision the phone for the newly inserted UICC card 007. If, however, the user chooses to provision the device for UICC card 007, the device prompts the user to enter a PIN. The PIN may include an account number or a secrete password. If the password matches, then the device forwards the ICCID — 007 to the CDMA network 15 and receives from the network 15 the credentials pertaining to ICCID — 007. At this point, mobile device 12 can use either CDMA network 15 or LTE network 33 to make a call.
The CDMA network 15 updates its database accordingly. That is, the CDMA network updates table 5 to reflect that in account 009 ICCID — 007 (instead of ICCID — 009) is now associated with the IMEI — 009. Of course, if the inserted PIN does not match, the access to CDMA network 15 is denied to mobile device 13 and the table remains unchanged.
FIG. 4 provides a block diagram illustration of an exemplary wireless device 100 , which may be the wireless device 12 , 13 or 33 of a customer of any of the network operators. Although the wireless device 100 may be a smart-phone or may be incorporated into another device, such as a portable personal computer, personal digital assistant (PDA) or the like, for discussion purposes, the illustration shows the wireless device 100 in the form of a handset. The handset embodiment of the wireless device 100 functions as a normal digital wireless telephone station. For that function, the station 100 includes a microphone 102 for audio signal input and a speaker 104 for audio signal output. The microphone 102 and speaker 104 connect to voice coding and decoding circuitry (vocoder) 106 . For a voice telephone call, for example, the vocoder 106 provides two-way conversion between analog audio signals representing speech or other audio and digital samples at a compressed bit rate compatible with the digital protocol of wireless telephone network communications or voice over packet (Internet Protocol) communications.
For digital wireless communications, the handset 100 also includes at least one digital transceiver (XCVR) 108 . The handset 100 is a multimode device capable of operations on various technology type networks, such as the networks 10 and 30 . For example, the handset 100 may utilize either or both of 3GPP2 (1XRTT and EVDO) technologies and 3GPP (LTE/GSM/UMTS) technologies. For that purpose, the transceiver (XCVR) 108 could be a multimode transceiver, or the handset 100 may include two or more transceivers each of which supports a subset of the various technologies or modes. The concepts discussed here encompass embodiments of the station 100 utilizing any digital transceivers that conform to current or future developed digital wireless communication standards.
The transceiver 108 provides two-way wireless communication of information, such as vocoded speech samples and/or digital message information, in a selected one of the technology modes. The transceiver 108 also sends and receives a variety of signaling messages in support of the various voice and data services provided via the station 100 and the communication network (described earlier with regard to FIG. 3 ). Each transceiver 108 connects through RF send and receive amplifiers (not separately shown) to an antenna 110 . In the example, the transceiver 108 is configured for RF communication in accord with a digital wireless protocol, such as the current 3GPP2 and 3GPP protocols. For the network selection function, network communications via the transceiver 108 and antenna 110 detect the available network technology types in any given service area and select an available network accordingly.
The station 100 includes a display 118 for displaying messages, menus or the like, call related information dialed by the user, calling party numbers, etc. A keypad 120 enables dialing digits for voice and/or data calls as well as generating selection inputs, for example, as may be keyed-in by the user based on a displayed menu or as a cursor control and selection of a highlighted item on a displayed screen. The display 118 and keypad 120 are the physical elements providing a textual or graphical user interface. In addition to normal telephone and data communication related input/output, these elements also may be used for display of menus and other information to the user and user input of selections, if needed during a system selection operation or during a selection software download operation. Various combinations of the keypad 120 , display 118 , microphone 102 and speaker 104 may be used as the physical input output elements of the GUI, for multimedia (e.g. audio and/or video) communications. Of course other user interface elements may be used, such as a stylus and touch sensitive display screen, as in a PDA or smart phone.
A microprocessor 112 serves as a programmable controller for the wireless device 100 , in that it controls all operations of the wireless device 100 in accord with programming that it executes, for all normal operations, and for operations involved in tracking the UICC on the mobile device. In the example, the wireless device 100 includes flash type program memory 114 , for storage of various “software” or “firmware” program routines and mobile configuration settings, such as mobile directory number (MDN) and/or mobile identification number (MIN), and ICCID number, etc. The wireless device 100 may also include a non-volatile random access memory (RAM) 116 for a working data processing memory. Of course, other storage devices or configurations may be added to or substituted for those in the example. In a present implementation, the flash type program memory 114 stores firmware such as a boot routine, device driver software, an operating system, call processing software and vocoder control software, and any of a wide variety of other applications, such as client browser software and short message service software. The memories 114 , 116 also store various data, such as telephone numbers and server addresses, downloaded data such as multimedia content, and various data input by the user. Provisioning related programming is part of the basic programming typically stored in the flash type program memory 114 , sometimes referred to as “firmware,” is loaded into and executed by the microprocessor 112 .
The executable provisioning program stored in the flash memory 114 may include a program for controlling credential management functions and for enabling the mobile device to keep track of its UICC card and does not authorize or restrict access to the CDMA network when the UICC card is replaced with a new UICC card. The flash memory 114 may also store CDMA credentials of associated with the subscriber, for example, so that a portion of the memory serves as a R-UIM module.
In a slightly different implementation, some or all of the provisioning program may be stored in UICC 111 instead of flash memory 114 . 3GPP variants of the mobile devices often utilize UICC 111 , which provides secure storage for various data needed for operation of a mobile device, such as data identifying the mobile device to the network (e.g. MDN and/or MIN). As discussed above, if the UICC 111 is changed on the device, the device recognizes this change and informs the user of the same. In particular, the device informs the user to either insert the correct UICC or to provision the device for the new UICC.
As shown by the above discussion, functions relating to enabling the mobile device to track its UICC card may be implemented on a mobile device in the form of programming. An example of the device has been discussed above relative to FIG. 4 . The relevant software (programming and/or list data) may be downloaded and/or updated from a computer platform, for example, from an OTAF server or the like communicating with the mobile device via the network. Although special purpose devices may be used to support the provisioning and/or related download and update functions, such devices also may be implemented using one or more hardware platforms intended to represent a general class of data processing device commonly used to run “server” and/or “client” programming so as to implement the functions discussed above, albeit with an appropriate network connection for data communication.
As known in the data processing and communications arts, a general-purpose computer typically comprises a central processor or other processing device, an internal communication bus, various types of memory or storage media (RAM, ROM, EEPROM, cache memory, disk drives etc.) for code and data storage, and one or more network interface cards or ports for communication purposes. The software functionalities involve programming, including executable code as well as associated stored data, e.g. files used for the various technology and system or network selection lists. The programming code is executable by the microprocessor 112 of the mobile device, e.g. from storage in the flash memory 114 . For downloading and installation, however, the software is stored within the general-purpose computer platform or the like serving as the OTAF system 29 running its own programming.
FIGS. 5 and 6 provide functional block diagram illustrations of general purpose computer hardware platforms. FIG. 5 illustrates a network or host computer platform, as may typically be used to implement a server. FIG. 5 depicts a computer with user interface elements, as may be used to implement a personal computer or other type of work station or terminal device, although the computer of FIG. 6 may also act as a server if appropriately programmed. It is believed that those skilled in the art are familiar with the structure, programming and general operation of such computer equipment and as a result the drawings should be self-explanatory.
A server, for example, includes a data communication interface for packet data communication. The server also includes a central processing unit (CPU), in the form of one or more processors, for executing program instructions. The server platform typically includes an internal communication bus, program storage and data storage for various data files to be processed and/or communicated by the server, although the server often receives programming and data via network communications. The hardware elements, operating systems and programming languages of such servers are conventional in nature, and it is presumed that those skilled in the art are adequately familiar therewith. Of course, the server functions may be implemented in a distributed fashion on a number of similar platforms, to distribute the processing load.
Hence, aspects of the methods of network selection outlined above may be embodied in programming. Program aspects of the technology may be thought of as “products” or “articles of manufacture” typically in the form of executable code and/or associated list data that is carried on or embodied in a type of machine readable medium. “Storage” type media include any or all of the memory of the computers, processors or the like, or associated modules thereof, such as various semiconductor memories, tape drives, disk drives and the like, which may provide storage at any time for the software programming. All or portions of the software may at times be communicated through the Internet or various other telecommunication networks. Such communications, for example, may enable loading of the software from a computer or processor into the mobile station, for example, from the OTAF server or other computer of the network operator into the mobile station(s) of the operator's customer(s). Thus, another type of media that may bear the software elements includes optical, electrical and electromagnetic waves, such as used across physical interfaces between local devices, through wired and optical landline networks and over various air-links. The physical elements that carry such waves, such as wired or wireless links, optical links or the like, also may be considered as media bearing the software. As used herein, unless restricted to tangible “storage” media, terms such as computer or machine “readable medium” refer to any medium that participates in providing instructions to a processor for execution.
Hence, a machine readable medium may take many forms, including but not limited to, a tangible storage medium, a carrier wave medium or a physical transmission medium. Non-volatile storage media include, for example, optical or magnetic disks, such as any of the storage devices in any computer(s) or the like, such as may be used to implement the information flow control, etc. shown in the drawings. Volatile storage media include dynamic memory, such as main memory of such a computer platform. Tangible transmission media include coaxial cables; copper wire and fiber optics, including the wires that comprise a bus within a computer system. Carrier-wave transmission media can take the form of electric or electromagnetic signals, or acoustic or light waves such as those generated during radio frequency (RF) and infrared (IR) data communications. Common forms of computer-readable media therefore include for example: a floppy disk, a flexible disk, hard disk, magnetic tape, any other magnetic medium, a CD-ROM, DVD or DVD-ROM, any other optical medium, punch cards paper tape, any other physical storage medium with patterns of holes, a RAM, a PROM and EPROM, a FLASH-EPROM, any other memory chip or cartridge, a carrier wave transporting data or instructions, cables or links transporting such a carrier wave, or any other medium from which a computer can read programming code and/or data. Many of these forms of computer readable media may be involved in carrying one or more sequences of one or more instructions and/or associated list data to a processor for execution.
While the foregoing has described what are considered to be the best mode and/or other examples, it is understood that various modifications may be made therein and that the subject matter disclosed herein may be implemented in various forms and examples, and that the teachings may be applied in numerous applications, only some of which have been described herein.
Other implementations are contemplated. For example, the attached Appendix A titled “Proposed Solution to Solve Device—UICC Swap” may describe additional implementations and provide additional information about the implementation thus far described. Although the instant application has been described in context of global devices that support 3GPP2 type CDMA technologies (1XRTT and EVDO) and 3GPP technologies (GSM/UMTS/LTE), it should be noted that the instant application can be applied to any dual-mode device that supports technologies other than the 3GPP2 type CDMA technologies as long as the dual-mode device supports the 3GPP technologies. For example, the instant application can by applied to a dual-mode device that is configured to support WiMax technologies and 3GPP technologies.
APPENDIX
Acronym List
The description above has used a large number of acronyms to refer to various services, messages and system components. Although generally known, use of several of these acronyms is not strictly standardized in the art. For the convenience of the reader, the following list correlates terms to acronyms, as used in the detailed description above.
1XRTT—One (1) times (x) Radio Transmission Technology
3GPP—Third (3rd) Generation Partnership Project
3GPP2—Third (3rd) Generation Partnership Project 2
ADPU—Application Protocol Data Unit
BS—Base Station
BTS—Base Transceiver System
CAT—Card Application Toolkit
CCAT—CDMA Card Application toolkit
CD—Compact Disk
CDMA—Code Division Multiple Access
CD-ROM—Compact Disk-Read Only Memory
CPU—Central Processing Unit
CSIM—CDMA Subscriber Identity Module
DVD—Digital Video Disk
DVD-ROM—Digital Video Disk-Read Only Memory
EEPROM—Electrically Erasable Programmable Read Only Memory
EF—Elementary File
EPROM—Erasable Programmable Read Only Memory
EVDO—1x/Evolution—Data Only
GSM—Global System for Mobile Communications
ICCID—Integrated Mobile Equipment Identity
ID—IDentification
IMEI—International Mobile Equipment Identity
IMSI—International Mobile Subscriber Identity
IR—InfraRed
ISIM—IP Multimedia Services Identity Module
LTE—Long Term Evolution
MDN—Mobile Directory Number
MEID—Mobile Equipment Identifier
MF—Master File
MIN—Mobile Identification Number
OTAF—Over-The-Air Functionality
OTAPA—Over the Air Parameter Administration
OTASP—Over the Air Service Programming
PC—Personal Computer
PCS—Personal Communication Service
PDA—Personal Digital Assistant
PIN—Personal Identification Module
PRL—Preferred Roaming List
PROM—Programmable Read Only Memory
PSTN—Public Switched Telephone Network
RAM—Random Access Memory
RAN—Radio Access Network
RF—Radio Frequency
ROM—Read Only Memory
R-UIM—Removable-User Identity Module
SIM—Subscriber Identity Module
SMS—Short Message Service
SMS-PP—Short Message Service-Point to Point
UICC—Universal Integrated Circuit Card
UIM—User Identity Module
UMTS—Universal Mobile Telecommunications Systems
USAT—Universal SIM Application Toolkit
USIM—Universal Subscriber Identity Module
WAN—Wide Area Network
XCVR—Transceiver
|
In one general aspect, the instant application describes a method for enabling dual-mode mobile devices to access a Code Division Multiple Access (“CDMA”) network. The method includes steps of receiving, from a first mobile device, a request to access a CDMA network, a first mobile device identifier identifying the first mobile device for the CDMA network access and a first integrated circuit card identifier identifying a first integrated circuit card being used by the first mobile device to access a Third Generation Partnership Project (“3GPP”) network; associating the first mobile device identifier with the first integrated circuit card identifier; and storing in a database the association between the first mobile device identifier and the first integrated circuit card identifier. The method further includes a step of authorizing the first mobile device to access the CDMA network only after associating the first mobile device identifier with the first integrated circuit card identifier.
| 7
|
CLAIM TO BENEFIT OF EARLIER FILED PATENT APPLICATIONS
This invention claims the benefit under 35 U.S.C. 119(e) of the filing date and disclosure contained in Provisional Patent Application having U.S. Ser. No. 60/844,058, filed, Sep. 11, 2006, entitled “FALLBACK VIDEO COMMUNICATION”, incorporated herein by reference.
BACKGROUND
In a media telecommunications environment, users subscribe to a service provider for telecommunications services. The telecommunications services may include a range of capabilities, including simple voice (telephone), voice mail, audio (i.e. music) downloads, email, text messaging (texting), video calling, video mail, and Internet access, to name several. The user, or subscriber, employs a personal communications device such as a cell phone, PDA or other personal computing device operable to provide the services subscribed to. Often such services entail communications to another subscriber. The other subscriber employs a similar device operable for the service to be employed, such as voice, text or video, for example.
From time to time, the service providers enhance their service offerings with new and/or improved services, to keep pace with technology and marketing trends. As is often the case with new technology, an initial release of functionality may take some time to establish a substantial user base. In the case of interactive operations between subscribers (i.e. services between two or more users), both users employ a device operable according to the service to be employed.
When new communications services are launched, so called “network effects” frequently limit the early adoption of the service. The problem is the new service requires new terminal devices and/or new facilities in the network. Until there is a critical mass of enabled users, i.e. a “network” of users, the early adopters have few people to communicate with and there is little incentive for others to adopt the devices or use the new service. This is particularly a problem with video communications services today, but is a general problem with any new communication service.
SUMMARY
New and/or enhanced telecommunications capability may suffer from the shortcoming that widespread usage may not be achieved until a substantial user base has devices conversant in the new capability. Configurations disclosed herein are based, in part, on the observation that conventional communications attempts to employ new capabilities or services may fail if both devices are not operable according to the new capability or service. For example, conventional video calls (video telephony and/or video sharing) calls will fail if an initiating device makes a call to a receiving device that does not have video capability.
Accordingly, conventional approaches to communication services suffer from the shortcoming that call attempts encountering a device inoperable according to a desired capability (i.e. a video call) will fail if the receiving device is unable to complete the call at the desired service level. In addition to frustrating the communication attempts between users, another issue is that resources consumed in the attempted but failed exchange are not recoverable, since the call never completed. Therefore, configurations herein substantially overcome such shortcomings by providing a fallback mechanism that recognizes a call about to fail, identifies a service level operable by both the initiating device and the receiving device, and completes the call at a lower service level operable by both devices. The disclosed approach allows a call to complete at an alternate service level (i.e. voice instead of video) rather than failing the call completely, resulting in a source of lost revenue to the service provider (operator).
Configurations disclosed herein include a strategy for solving the general problem, solutions for various types of multimedia communications and specific embodiments for typical forms of video communications being offered by mobile operators. Video calling and content-based services such as MobileTV are key applications identified by operators. So called 3G-324M circuit-switched video telephony and packet-based video sharing, by itself or combined with a circuit-switched call, have been deployed or are in trials across operator networks. However, in the absence of mass-market penetration of handsets which are video call enabled or video share enabled, the adoption of video communication may be prolonged. As a result, some operators are promoting content-based video services rather than video communication, and some are offering PC-based video clients to their customers to increase the community of video-enabled users.
Such 3G video telephony is based on the 3G-324M standard, which provides a full-duplex video & audio connection between two parties over a circuit-switched data path. 3G video sharing provides one-way video transmission over an IP data connection, with or without an associated circuit-switched voice call. Video sharing can be one-to-one or one-to-many. In addition to mobile video services, other video telephony systems are available, based on H.320, H.323, MGCP, MEGACO, SIP and other standard and proprietary schemes.
With any new service such as 3G video telephony or 3G video sharing, new subscribers have a problem, as relatively few people have handsets capable of receiving a video call. In addition, it's frequently impossible to know in advance if the called party can receive the call. And, after placing a video call or initiating video sharing, it can take 5-10 seconds or more before the calling party finds out whether the connection is going to complete.
Many of today's video communications services include video mail, but video mail only provides call completion for called parties who already have the appropriate video terminal and video service. In addition, video mail doesn't always work if the called party is roaming on other networks and not all video subscribers also subscribe to video mail. Video store and forward services exist, particularly for content delivery. However, conventional approaches do not address the problem of video call completion when the called party does not have an appropriate terminal or an appropriate service to support video communication.
Both the Fallback Video Telephony and the Fallback Video Sharing operate by automatically recognizing a video session that is not going to be successful. The fallback application intercepts the call attempt, buffers the video if necessary, and then uses alternate means to deliver the caller's video, thus using a mechanism that covers a much larger proportion of the population. Depending upon the receiving party's capabilities, the caller's video is provided in near real-time or is made available for later viewing using one or more of the following techniques: via an SMS message that includes a URL or other link to where the video is available for streaming or download, via streaming video or progressive download over GPRS, EDGE, 3G or other Internet connection; video delivered as an MMS message; video delivered to a 3G-324M handset; video delivered to a Web browser, WAP browser or FTP client (fixed or mobile), or to an instant messaging client, either by streaming, as a file or as a link to a file, video files or links delivered as email, or other suitable method. As a final fallback for multimedia adaptation, it is possible to provide sequences of still images at rates of a few images per second down to one to several seconds per image for those with still image but no video capabilities. These images can be delivered to the called party directly or indirectly by any of the means discussed above. The ultimate fallback for notification is to place a voice call to the called party and have an interactive voice response (IVR) system verbally alert the called party to the existence of a video for them, explain delivery alternatives and solicit their input on how to proceed.
Configurations herein benefit the video subscriber who has signed up for, and is paying for, video services because it greatly increases the likelihood their video will get to the intended party. It also represents an excellent opportunity to sell video products and services to non-subscribers, as the receiving party has received a video from a mobile subscriber and is thus aware of the service and more likely to respond to targeted marketing.
Other feature of the claimed approach include:
1. Service-specific means to recognize a video call or video share that would otherwise fail and re-route it to a Video Telephony Service Node (VTSN).
2. Means to establish called-party capabilities, by lookup (typically for an operator's own subscribers) and by rule for other called parties.
3. Terminating the initial video call or video share at the VTSN, including negotiating video capabilities with the calling party. The negotiation can be arranged to maximize video quality, or to minimize any subsequent video transcoding and/or translating that may be required, based on the called party's video capabilities.
4. Means (within the VTSN) to buffer, transcode and/or rate-adapt the video material between the calling party's negotiated format and the called party's capabilities.
5. Means, either within the VTSN or by linking to a video mail system or other video storage system like the NMS MobilePlace content locker, to store video for later replay in any of the supported formats.
6. Means to extract a sequence of still images from the original video for those clients that can view images but have no video capability of any kind.
7. Means to deliver video and/or a sequence of still images using any of the following technologies: streaming video over GPRS, EDGE or 3G; video delivered as an MMS message; video delivered to a 3G-324 handset; video delivered to a Web or WAP browser, or an instant messaging client, either by streaming or as a file; video files delivered as email; or sequences of still images at rates between one to a few images per second and one to several seconds per image.
8. An interactive voice response (IVR) system arranged to place a voice call to an otherwise video-unreachable called party, which uses IVR to alert the called party to the availability of video content intended for them and to solicit information on how to deliver the content.
9. A database of called parties indicating which alternate delivery means have worked, which didn't, how much time delay was involved in the delivery and other details including dates, times and results of delivery attempts.
10. A direct marketing system that leverages our knowledge of called party capabilities to implement targeted marketing campaigns that promote relevant products and services to people with whom the fallback video communications system has interacted.
For 3G-324M video calls, use IN approaches to recognize a call that will fail or has failed and divert it to the VTSN. For on-net calls, the called party's capabilities can be determined from the HLR or HSS or other operator database during the database dip that determines their current status and location. If the called party does not subscribe to the appropriate video service, the original call is diverted to the VTSN. For off-net 3G-324M calls, 3G-324M-specific ISDN bearer elements are passed in the ISUP IAM message. If the call fails, the distant party release message will include a cause, for example, bearer service not supported. If so, divert the call to the VTSN or other suitable device responsive to the indication of a device mismatch (i.e. non-video supporting device, in the example shown). For 3G video sharing attempts, the network's SIP proxy or 3G CSCF maintains or has access to registration and routing information. For on-net calls, in addition to routing info, the called parties capabilities can also be determined from registration information (i.e. whether video capable) or through capability exchange preceding/during call setup. For off-net calls the SIP session is routed to the Proxy that the called party is anchored to. When an SIP Video Session initiation request is received by the SIP Proxy or CSCF, it performs a database query to determine:
a) whether the session could be routed to the called party b) if (a) is true, whether the called party is video capable
If check on either (a) or (b) returns failure for on-net calls, the SIP Proxy or CSCF diverts the session to the VTSN. Similarly, in the case of off-net calls, if no route exists to the called party, the SIP Proxy or CSCF diverts the session to the VTSN. Even upon successful routing, for both on-net and off-net calls, the session setup could fail due to incompatible video capabilities between the calling and called party—on session setup failure, the SIP Proxy or CSCF diverts the session to the VTSN. Session setup may also fail due to the called party being busy, unreachable, not answering or rejecting the Video Share Session, which would also result in the session being directed to VTSN.
If the called party is off-net, we can use rules to make an educated guess as to their video capabilities. If they are in a country where mobile numbers have distinct prefixes, for example in any country with “calling party pays,” then mobile phones can be assumed to have SMS capability and the system may offer (via SMS) a choice of getting the video content via the Web, WAP or MMS.
In a typical deployment, video will be buffered in whatever format is available from the calling party's handset or video terminal. Video will then be transcoded and/or rate adapted zero, one or more times to provide versions appropriate for each of the alternative delivery methods. This can be done after the video has been recorded or can be done in real time as the video is being recorded. If near real time delivery is an option, then any required transcoding or rate adaptation is done in real time as well.
Many of the features of fallback video communications can be realized by client software on individual handsets or other video terminals or video terminal software for PCs, in cooperation with a relatively few network-based elements. For example, with adequate on-device storage, terminal software can buffer video and, upon failure of the initial call, attempt alternate delivery methods. These could be direct from the terminal and/or could involve transferring the buffered video content to a network-based server for later download after the called party receives an email, SMS, IM or other message from the calling party's terminal software. Similarly, client software can request alternate delivery information from a network element and can post alternate delivery results to a network element that is part of, or is connected with, a network-based targeted marketing system.
Alternate configurations of the invention include a multiprogramming or multiprocessing computerized device such as a workstation, handheld or laptop computer or dedicated computing device or the like configured with software and/or circuitry (e.g., a processor as summarized above) to process any or all of the method operations disclosed herein as embodiments of the invention. Still other embodiments of the invention include software programs such as a Java Virtual Machine and/or an operating system that can operate alone or in conjunction with each other with a multiprocessing computerized device to perform the method embodiment steps and operations summarized above and disclosed in detail below. One such embodiment comprises a computer program product that has a computer-readable medium including computer program logic encoded thereon that, when performed in a multiprocessing computerized device having a coupling of a memory and a processor, programs the processor to perform the operations disclosed herein as embodiments of the invention to carry out data access requests. Such arrangements of the invention are typically provided as software, code and/or other data (e.g., data structures) arranged or encoded on a computer readable medium such as an optical medium (e.g., CD-ROM), floppy or hard disk or other medium such as firmware or microcode in one or more ROM or RAM or PROM chips, field programmable gate arrays (FPGAs) or as an Application Specific Integrated Circuit (ASIC). The software or firmware or other such configurations can be installed onto the computerized device (e.g., during operating system or execution environment installation) to cause the computerized device to perform the techniques explained herein as embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects, features and advantages of the invention will be apparent from the following description of particular embodiments of the invention, as illustrated in the accompanying drawings in which like reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the invention.
FIG. 1 is a context diagram of an exemplary video telephony environment having personal communications devices suitable for use with the present invention;
FIG. 2 is a flowchart of fallback processing in the environment of FIG. 1 ;
FIG. 3 is a block diagram of video call fallback processing in the environment of FIG. 1 ; and
FIGS. 4-7 are a flowchart of video call fallback processing according to the diagram of FIG. 3 .
DETAILED DESCRIPTION
The disclosed method and apparatus for providing fallback video communication completes a video communication that otherwise would have failed. It works for typical forms of video communication and acts to deliver the calling party's video content to the called party, as rapidly as possible, using one or multiple alternate means. In addition, the mechanism accumulates information on called party capabilities, so as to simplify and/or improve delivery of future communications and to target appropriate marketing messages, e.g. messages promoting video equipment and services.
Configurations discussed below therefore identify video communications that have failed or will fail, for example because the called user is not video capable, not reachable, busy or not answering, and divert such communications attempts to a fallback server system that can terminate the call (compete the connection attempt) and buffer the video. The mechanism buffers the video and/or multimedia content as required, and determines an appropriate alternate delivery means, either the one best means or multiple means to be attempted in parallel or in sequentially.
FIG. 1 is a context diagram of an exemplary video telephony environment having personal communications devices suitable for use with the present invention. Referring to FIG. 1 , a video telephony environment 100 includes a network 110 , such as a 3G network operable for multimedia transport. The network 110 supports a multitude of communication devices 102 , such as an initiating communication device 112 and a recipient communication device 114 . In a conventional scenario, the initiating device 112 calls the recipient communication device 114 to allow the devices 102 to complete a call connection and allow the devices to communicate. With the advent of so called 2.5G and 3G networks, however, the initiating communication device 112 and recipient communication device 114 may not be similarly equipped, and thus have different capability features. Thus, a call initiated at an expected service level, such as video telephony, may not be able to complete if the recipient device has only capability features to support a voice service level.
Accordingly, a switch 120 - 1 . . . 120 - 3 ( 120 generally) in the network detects when a call is about to fail due to equipment mismatch, and reroutes the call to a fallback server 130 for resolution. In the example case of a video telephony call or shared video call, the fallback server 130 bifurcates, or separates the audio 142 and video 144 components of the call 140 . The audio component 142 is allowed to continue unhindered between the communication devices 112 , 114 . The video component 144 , however, is intercepted by the fallback server and stored in a video repository 150 for later delivery to the non-video conversant recipient device 114 . The fallback server 130 examines the capability features of the recipient device 114 and determines an optimal mitigating medium by which the intercepted video 144 may be delivered. Subsequent to the call, the fallback server 130 transports the captured video 146 from the video repository 150 to the recipient device 114 , such as by a subsequent video stream, email of a video file (.flv or other), or simply a voice or text indication of an external web server via which the intercepted video component 146 may be viewed, discussed further below.
Therefore, fallback video communications ensures the majority of attempted video calls result in video communication with the intended party. The mechanism intercepts video calls that would not be successful because the called party is not capable, not reachable, busy or not answering. It buffers the video as required and uses alternate means to deliver the video content to the called user. This enables video communication for a larger proportion of the population.
In the case of called party not reachable and busy, the fallback solution doubles as a video mail service with the difference that the called user does not have to sign up for video mail service and does not have to explicitly retrieve the video mail if MMS or email forwarding is enabled.
If an SMS, IM or email, with a RTSP link, is sent to the called party, the video can be streamed to the called party in near-realtime. Potential called parties are not limited to those with 3G video-enabled mobile handsets and could include PCs with instant messaging, email, RTSP or browser clients, for example. Also, fallback video communication ensures that user-to-user video communication is possible with communication endpoints that have only basic capabilities. Fallback Video Telephony and Fallback Video Share are typical example embodiments for the two most common forms of mobile video communications that provide user-to-user video services; configurations herein are operable for other suitable communication device mismatches and for avoiding call failure thereto.
FIG. 2 is a flowchart of fallback processing in the environment of FIG. 1 . Referring to FIG. 1 , the method of fallback processing for avoiding call failure disclosed herein include, at step 200 , determining a set of capability features of communications devices 102 , the communications devices including an initiating device 112 and a receiving device 114 , such that the capability features are indicative of a service level of each of the communications devices. The network 110 receives an incoming call 140 from the initiating device 112 , in which the incoming call has an expected service level, and the call being directed to the receiving device 114 , as depicted at step 201 . The service level is typically based on the capabilities or expectations of the initiating device 112 , thus ripening the possibility of capability mismatch. The network 110 , via an array of switches and routing devices 120 , concludes that an insufficiency exists between the capability features of the calling devices 102 , in which the insufficiency results in an inability to complete the call at the expected service level, as disclosed at step 202 . The network 110 , via a predetermined trigger or proxy at one of the switches 120 (discussed further below), invokes fallback logic 132 in the fallback device operable to complete the call at a service level common to the set of capability features of the communications devices, as disclosed at step 203 . In the example configuration, the fallback logic 132 is operable to complete the call automatically, according to predetermined instructions, without user intervention or manual selection of operation, in a manner consistent with the capability features common to the communications devices, as depicted at step 204 .
FIG. 3 is a block diagram of video call fallback processing in the environment of FIG. 1 . Referring to FIG. 3 , the initiating device 112 includes capability features 112 - 1 for carrying on a call 140 to a recipient device 114 , also including capability features 114 - 1 , at an expected service level. The fallback logic 132 includes an interface 145 to the network 110 for establishing interception of a potentially failed call 140 , such as a so-called trigger or set proxy, as is known in the art. The intercepted call 140 is bifurcated into audio components 142 and video components 144 . The intercepted call 140 is rerouted such that the fallback logic 132 buffers, caches, or otherwise stores the video component 144 in the video repository 150 , and subsequently delivers it to the recipient device 114 by a suitable mitigating option 160 , such as via a separate email or other communication 146 - 1 directly to the device 114 , or indirectly via an IP network 162 to an alternate browser 166 device 164 .
FIGS. 4-7 are a flowchart of video call fallback processing according to the diagram of FIG. 3 . Referring to FIGS. 3 and 4 , in the case of a video-based call such as with a video telephony or shared video enabled phone, the network 110 carrying the call determines a set of capability features of communications devices 102 , in which the communications devices 102 include an initiating device 112 and a receiving device 114 , such that the capability features are indicative of a service level of each of the communications devices, as depicted at step 300 . Similar to the scenario above, the network 110 receives an incoming call from the initiating device 112 , in which the incoming call has an expected service level, and the call is directed to the receiving device 114 , as disclosed at step 301 . The network 110 , upon realizing the eminent call failure, compares the capability features of the initiating device 112 and the receiving device 114 , as depicted at step 302 , by traversing the capability features of each of the communication devices 102 , as shown at step 303 . In the network, the devices 102 are generally supported by specific carriers, or operators, which provide an operation or function to query and identify capabilities 112 - 1 , 114 - 1 of the various devices 102 .
Based on a comparison of the capabilities 112 - 1 , 114 - 1 or other attempts by the network 110 to complete the call, one of the communication devices 102 is identified as a non-video conversant device, as shown at step 304 . Thus, the fallback logic 132 concludes that an insufficiency exists between the capability features of the calling devices, the insufficiency resulting in an inability to complete the call at the expected service level, as depicted at step 305 . As is known in the industry, call failure due to devices 102 inoperable for the requested service level initiates a trigger or proxy to take terminate the call. In contrast to such conventional approaches, configurations herein employ a trigger, set proxy or other call failure mechanism to invoke fallback logic 132 operable to complete the call at a service level common to the set of capability features of the communications devices, as shown at step 306 .
The invoked fallback logic 132 in the fallback server 130 intercepts the incoming call 140 , as depicted at step 307 , and reroutes the call to fallback device 130 having the fallback logic 132 , as disclosed at step 308 . In this manner, the fallback server 130 operates as a network switch 120 , for routing the call 124 to a call completion server 120 operable to compute a mitigating option 160 and allow the call to complete, as shown at step 309 .
The fallback logic 132 identifies a mitigating option 160 , such that the mitigating option 160 corresponds to a service level employing capability features 112 - 1 , 114 - 1 common to the communications devices 102 , as shown at step 310 . The fallback logic 132 is therefore operable to complete the call automatically, according to predetermined instructions without user intervention or manual selection of operation, consistent with the capability features 112 - 1 . 114 - 1 common to the communications devices 102 , as disclosed at step 311 . Typically, this would involve downgrading the video call to a voice call. The fallback server 130 modifies calling parameters to provide call completion using the common capability features, in which the fallback logic is operable to implement the modified call parameters, as depicted at step 312 .
In the example shown in FIG. 3 , involving a video call, the determined mitigating option includes bifurcating the call 140 into an audio component 142 and a video component 144 , as depicted at step 313 , and continues the audio component 142 in real time via an available voice medium, as depicted at step 314 . The fallback server 130 simultaneously redirects the video component 144 according to a compatible video delivery medium, as shown at step 315 .
The fallback logic 132 captures the video component 144 of the call from the video conversant device 112 , as shown at step 316 , and identifies a video caching mechanism operable to store the video component 144 , such as the video repository 150 , as depicted as step 317 . The video repository 150 may represent a variety of caching options, depending on the capability features of the recipient device 114 such as a video mailbox, a video file (.flv) for subsequent emailing, or a text/email indicative of a URL if the recipient device 114 does not have a video display. Depending on the computed delivery mechanism, the video component is delivered either directly as a user compliant video medium 146 - 1 . . . 146 - 2 ( 146 , generally) to the communications device 114 , shown by arrow 146 - 1 , or indirectly, such as by an IP network 162 to a user device 164 having a browser 166 for URL receipt. The disclosed bifurcating and storage of the video component is employed as an example to illustrate buffering/storage as mitigating omitted functionality in a receiving device. Alternatively, voice only, or the entire video and audio communication stream may be stored and retrieved later by the called party.
The bifurcated call 140 may take a variety of expected service levels 141 , and depending on the initiated call, the mitigating option may be computed. In the example shown, a check is performed, at step 318 , to identify if the call 140 is a video telephony or shared video call. If the call is a video telephony call, then concluding that an insufficiency exists further comprises recognizing an ISDN trigger corresponding to a non-video enabled device, as depicted at step 319 , thus identifying a video telephony call having an integrated audio and video signal, as shown at step 320 . The fallback server 130 bifurcates the integrated audio and video signals in the incoming call 144 into an audio component 142 at the mitigated service level 143 (i.e. voice only) and a video component 144 for fallback server 130 processing, as disclosed at step 321 . The fallback server 130 captures the signals from the video component, as depicted at step 322 , and decodes the audio component 142 to carry the audio portion of the call. The audio portion continues as with a conventional voice call, while the video signals from the video conversant device 112 continue and are captured as the video component 144 by the fallback server 130 . The video repository 150 buffers the captured video signals for subsequent delivery by a user compliant video medium 146 , as computed by the fallback server 130 .
In conventional arrangements, when a 3G-324M Video Call is initiated by a user, if the far-end user is incapable of participating in a Video Call, the call typically fails or, potentially, is downgraded to a voice call. With Video Telephony Fallback, the video call is routed to a Video Telephony Service Node (VTSN). The VTSN terminates the 3G-324M call and allows the initiating user to leave a video for the called party. Depending upon known or inferred called party capabilities, the VTSN either records the video content and forwards it as an MMS or email message or the VTSN sends an SMS, IM or email that contains an RTSP or HTTP link to the Video content. If notification is by sending an SMS, IM or email with a link, the message can be sent immediately without waiting for the full video to be recorded.
As an alternative, the VTSN can terminate the 3G-324M call and immediately establish a voice call to the called party. If that is successful, the VTSN can act as a gateway adapting the voice portion of the calling party's 3G-324M call to the voice call with the called party and vice versa, while providing default video to the calling party and recording the video from the calling party for forwarding as described above. In this case, the VTSN should incorporate interactive voice and video response (IVVR) and interactive voice response (IVR) capabilities, as it is useful to provide a short IVVR session with the calling party and a short IVR session with the called party to explain what is happening before the through voice session is connected. Alternately, the through voice session can be connected, but a voice explanation can be injected into the voice paths in both directions.
In the case of a video sharing call 140 , concluding that an insufficiency exists recognizing a set proxy operation corresponding to a non-video enabled device, intercepting the network 110 call failure processing, as depicted at step 325 . The fallback processing identifies the call 144 as a video sharing call having a video transport medium and a separate audio transport medium, as disclosed at step 326 . The fallback server 130 capturing the signals 144 from the video transport medium, as depicted at step 327 . The fallback logic 132 permits the audio transport medium to carry the audio portion of the call 142 , as shown at step 328 , while buffering the captured signals 144 from the video transport medium for subsequent delivery by a user compliant video medium 146 .
Video Share Fallback provides similar service for subscribers with 3G Video Sharing service when they attempt to share with users whose handsets are not video share compatible. 3G video sharing is typically implemented using the SIP protocol, either with conventional SIP infrastructure or with IMS (the IP Multimedia System defined by the 3GPP).
As with video telephony fallback, a video share session that would otherwise fail is diverted (by a SIP proxy, a session border controller, an IMS CSCF or other IMS gateway function) to the Video Telephony Service Node (VTSN) where the video share is terminated and the video is buffered for subsequent delivery to the called party. Depending upon known or inferred called party capabilities, the VTSN either, records the video content and forwards it as an MMS or email message, or the VTSN sends an SMS, IM or email that contains an RTSP or HTTP link to the Video content. If notification is by sending an SMS with a link, the message can be sent immediately without waiting for the full video to be recorded.
Following call completion, the fallback server 130 identifies an available video delivery medium 146 based on the capability features 114 - 1 of the non-video conversant device 114 , thus determining a video delivery medium consistent with the capability features of a non-video conversant phone, as depicted at step 330 . From among multiple possible available mediums 146 (i.e. email is almost always an option, although may be less desirable than more direct mechanisms), the fallback logic 132 attempts to identify an expedient video medium with which to transport a video component of the call to the non-video conversant user, as disclosed at step 331 . This includes selecting the mitigating option from an ordered list of the expedient video delivery mediums 160 , in which the video delivery mediums are ordered according to efficient delivery to the non-video conversant user 114 , as disclosed at step 332 . In the example arrangement, this may include selecting the expedient video medium from video mail, stored video file, web server caching, still image sequencing, as disclosed at step 333 . The fallback server 132 then delivers notification of the captured video component 146 and the selected expedient video delivery medium to the non-video conversant user 114 , as shown at step 334 This notification is particularly important in the case of, for example, an email of a distinct web server (page) from which the vide component 146 may be retrieved. The fallback server 130 then delivers the cached video component 146 from the repository 150 to the non-video conversant user 114 , as depicted at step 334 . The notification and video component 146 - 1 may be the same communication if a video delivery is made directly to the recipient device 114 .
Further configurations employ a variety of additional factors in determining the mitigating option for delivery. This determination is based on any or all of the following information:
subscriber data the operator has about the called party (typically when the called party is a subscriber on the operator's network).
called party information from the calling party, for example, data about the called party that is stored in the phonebook on the calling party's handset or in a network copy of that phonebook held on behalf of the calling party.
previous experience delivering multimedia content to this called party.
information obtained from failed attempts to establish the original communications, for example what network the called party is on, where they are located and/or what kind of service(s) they have (e.g. their IP address is on a mobile network versus an IP address from a fixed broadband Internet service provider). This class of information is typically available from switches, softswitches, Intelligent Network service control points, SIP proxies, session border controllers and other elements that participate in establishing a multimedia communications session.
information obtained from the failure of other alternate delivery means.
other information about the called party that may become available to the operator providing fallback video communications.
initiating alternate delivery means either immediately (as buffering begins) or once buffering is complete.
storing the video or multimedia content until delivery is compete (or until some holding period has expired).
maintaining records of called parties including which delivery means worked and which didn't and how rapidly they worked.
performing other useful functions as a result of knowing a fallback communications event has occurred, in parallel with or after fallback video communications attempts have been initiated or have succeeded or failed, such as:
Direct marketing including sending targeted text or multimedia messages to recent called parties and calling parties. The principal idea is to promote further adoption of video communications equipment and services so that future communications can proceed directly without the need for fallback video communications. Of course, this marketing channel can be used for other purposes as well, e.g. when the called party's location (perhaps in a country with no mobile video services) indicates they are not a candidate for mobile video services, it may still make sense to promote Internet video equipment or specific country-to-country voice calling plans,
Such direct marketing include sending messages (voice, text or multimedia) to called parties describing how the recent video could have been received live if they had the appropriate handset or service and then making them an offer of the appropriate device and/or service. It also includes delivering messages to calling parties, telling them that their video was (or was not) delivered by alternate means and, if they talk their friend into signing up within the next N days, they get a commission (extra minutes, extra service, cash back, etc.).
Sending alerts. If the called party should have been able to receive the communication but didn't, for example, if the called party is an always open call center or a public safety answering point,
Sending billing information to a billing system or a third party.
analyzing records of calls and call completions and cross-correlating them with other subscriber and non-subscriber data sources for diverse purposes including
measuring service performance,
designing products and marketing programs, for example that seek to increase service adoption.
Those skilled in the art should readily appreciate that the programs and methods for avoiding call failure through fallback processing as defined herein are deliverable to a user processing and rendering device in many forms, including but not limited to a) information permanently stored on non-writeable storage media such as ROM devices, b) information alterably stored on writeable storage media such as floppy disks, magnetic tapes, CDs, RAM devices, and other magnetic and optical media, or c) information conveyed to a computer through communication media, for example using baseband signaling or broadband signaling techniques, as in an electronic network such as the Internet or telephone modem lines. The operations and methods may be implemented in a software executable object or as a set of encoded instructions for execution by a processor responsive to the instructions. Alternatively, the operations and methods disclosed herein may be embodied in whole or in part using hardware components, such as Application Specific Integrated Circuits (ASICs), Field Programmable Gate Arrays (FPGAs), state machines, controllers or other hardware components or devices, or a combination of hardware, software, and firmware components.
While the system and method for avoiding call failure has been particularly shown and described with references to 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 scope of the invention encompassed by the appended claims.
|
Conventional video call attempts encountering a device inoperable according to a desired capability will fail if the receiving device is unable to complete the call at the desired service level (i.e. video). In addition to frustrating the communication attempts between users, another issue is that resources consumed in the attempted but failed exchange are not recoverable, since the call never completed. Accordingly, configurations herein substantially overcome such shortcomings by providing a fallback mechanism that identifies a service level operable by both the initiating device and the receiving device, and completes the call at a lower service level operable by both devices. The disclosed approach allows a call to complete at an alternate service level (i.e. voice instead of video) rather than failing the call completely, resulting in a source of lost revenue to the service provider (operator).
| 7
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to snow removal and more particularly to a snowplow carriage assembly for removing snow by plowing it manually.
2. Prior Art
Heretofore the removal of snow manually at residences by homeowners has been accomplished by use of conventional snow shovels and the use of brooms. The shoveling of snow by homeowners subjects the heart of the shoveler to considerable stress, and even young people have been known to have a heart attack after shoveling snow. Doctors now warn people that if they are fifty years of age, they should not shovel snow.
While a conventional snow shovel can be used to plow the snow in an area for removal without pitching the snow or shoveling it, which is stressful, a conventional snow shovel used for simply plowing the snow still requires a considerable amount of energy input by the user. There is a need for a device for clearing areas of snow by manual plowing of the snow for removal without subjecting the snow remover to excessive harmful stresses.
SUMMARY OF THE INVENTION
The snowplow carriage assembly, according to the invention, is a collapsible or foldable carriage on which is transportably mounted a snowplow. The snowplow is a conventional snow shovel removably and replaceably mounted on the carriage on which it is transported and pushed forwardly for plowing and removing snow from an area to be cleared.
The snowplow carriage assembly is constructed as a structure which can be collapsed and folded into a compact assembly with the snowplow thereon, or off of it, for storage, and can be readily prepared to use by opening the assembly into an expanded or unfolded state for plowing snow. Provision is made for adjustably positioning the snowplow at different acute angles relative to the surface on which the snow is being plowed. The carriage can accommodate different types of snow shovels having different length handles.
BRIEF DESCRIPTION OF THE DRAWINGS
The snowplow carriage assembly, according to the invention, description can be readily understood with reference to the appended claims and drawings in which:
FIG. 1 is a perspective view of a snowplow carriage assembly, according to the invention;
FIG. 2 is a side elevation view of the snowplow carriage assembly in FIG. 1;
FIG. 3 is a side elevation view of the snowplow carriage assembly in FIG. 1, illustrated in a folded state for storage;
FIG. 4 is a section view taken along section line 4--4 in FIG. 1;
FIG. 5 is a fragmentary perspective view of a second embodiment of a snowplow, according to the invention;
FIG. 6 is a fragmentary perspective view of a third embodiment of a snowplow, according to the invention;
FIG. 7 is a perspective elevation view of a second embodiment of a snowplow carriage assembly, according to the invention;
FIG. 8 is a section view taken along section line 8--8 of FIG. 7;
FIG. 9 is a section view taken along section line 9--9 of FIG. 7; and
FIG. 10 is a section view taken along section line 10--10 of FIG. 7.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A snowplow carriage assembly 2, according to the invention, is illustrated in FIG. 1, on which is mounted a snowplow illustrated as a conventional snow shovel. The carriage assembly consists of a single frame which has handles 5, 6 having elongated arms 8, 9 extending therefrom and which can be made tubular, for example. The elongated arms 8, 9 have tubular legs 10, 11 each connected pivotally and the snow shovel is used to function as a blade of the snowplow to the respective arms by a pivot such as a pivot 13. The carriage arms and legs are each provided with wheels 14. The wheels on the arms can be provided with swivels.
Provision is made for the legs 10, 11 to extend away from the arms 8, 9 in an unfolded state of the carriage as shown in FIG. 1 and to be foldable as shown in FIG. 3. A pair of linkage systems in the known form of relatively slidable links 16, 17 are respectively pivotally connected to a corresponding arm and leg. When the links are in an extended condition the individual legs are moved, and held, outwardly spaced away from the corresponding arms. The linkage system link 16 has an end pivotally connected at a pivot 20 to the corresponding leg 11 and has a longitudinal slit 21 in which a pivot pin 22 fixed on the other link 17 slides. The other link 17 is pivotally connected by a pivot 23 to the arm 9. When the carriage is in an unfolded state or condition the links extend from each other as shown in FIGS. 1 and 2. The pin 22 is received in a notch in the end of the slit 21 and locks the corresponding linkage system in an extended condition, and the carriage is held in an opened condition for plowing snow. The links are operable upwardly, as illustrated by an arrow 25 in FIG. 2 to release the pivot pin 22 from the notch so it can slide in the slit 21 to collapse the linkage system in a position shown in FIG. 3 for folding the carriage assembly for storage when not in use.
The two carriage arms 8, 9 are held parallel laterally spaced by two carriage transverse members or cross bars 27, 28 fixed, at ends thereof, axially spaced on the arms. The two cross bars can be made tubular and connected to the arms in any suitable manner such as shown in FIG. 1. The cross bars are arranged so that the upper bar 27 is higher than the lower bar 28 and both are in an inclined plane defined by the arms and the cross bars. This plane makes an acute angle with the horizontal and is the plane in which a snowplow is mounted, as described below, at a suitable acute angle relative to the horizontal, for plowing snow for manual removal thereof.
A snowplow 35 in the form of a conventional snow shovel having a handle 36 and a handle grip 37 is removably and replaceably mounted on the carriage 2 for plowing snow as the carriage is advanced manually. The snowplow or snow shovel is mounted at an angular position relative to the horizontal, as shown in FIG. 2. The carriage 2 is constructed so that in an unfolded condition the snowplow is held in a plane at an angular position relative to the horizontal similar to an acute angle at which snow shovels are used manually to plow snow to clear an area from which snow is being removed by simply plowing.
In order to mount the snowplow on the carriage, the snow shovel is provided with a pair of spaced holders 45, 46 which are fitted axially on the handle 36 of the snow shovel. The holders are constructed so that the upper holder 45 has an upwardly directed hook 50 and the lower holder 46 has a downwardly directed hook 51. These hooks engage the upper cross bar 27 and the lower cross bar respectively on the carriage. The lower hook 51 positions the snow shovel 35 at a position so that the snow will be plowed, for example, along a surface 60. The upper hook maintains the shovel from moving upwardly when snow plowing is taking place. It can be seen that with the holder arrangement illustrated, the shovel handle 36 is subjected to the same type of forces to which it would be subjected if the shovel were being used manually as a plow without being supported and carried on a carriage. The holders are positionable axially spaced on the handle and held in position by bolts 45a, 46a which extend through the handle and have wing nuts on an end thereof so that the bolts can be removed and the snow shovel replaceably removed from the carriage 2.
Snow removal is generally accomplished manually by moving a snow shovel forwardly to plow and move the snow as desired. In order to reduce the workload, snow removal is accomplished by removing snow by plowing a pathway as wide as the shovel 35. People can then walk readily along such a path single file or the path can be widened by making two passes with the snow shovel. The present invention provides for reducing the plowing load in advancing the snow shovel mounted on the carriage by providing for moving the snow laterally as the carriage is advanced for plowing snow.
A snowplow configuration which has a V-shaped front surface is illustrated in FIG. 5. A snow shovel 65 illustrated has a shovel 67 in which a front center section 67a projects forwardly of two trailing opposite side sections 67b, 67c that extend rearwardly of the central section so that as the center section advances, snow being plowed is diverted laterally in two directions by the side sections which trail the center section. The outer side edges of the side sections trail the leading surface of the center section sufficiently so that in effect the shovel is V-shaped. In the V-shaped shovel 67 the side sections 67b, 67c are disposed dimensionally and angularly symmetrically relative to the center section 67a.
Those skilled in the art will understand that the shovel configuration can be that of an asymmetrical V-configuration as well as symmetrical. Moreover, the angle at which the side sections trail rearwardly can be different in the shovel configurations even if the shovel is symmetrical dimensionally. The shovel side sections can be made dimensionally asymmetrical. One side section can extend laterally and rearwardly a greater distance from the center section than the other side section and the respective angle at which the individual sections diverge rearwardly from the center section can be the same or can be different whether the sections are both the same dimensionally or each different dimensionally. Thus, different possibilities of symmetry and asymmetry are possible, resulting by use of same or different angles which the side sections make with the center section and the same or different dimensions of the side sections. In all such cases, the shovel has a V-configuration which has a more open or more closed angle and the sides of such a "V" of different side lengths. Providing the V-configuration makes it possible to provide snowplows for different plowing problems. For example, differences in walks or paths to be plowed can be handled better either by a symmetrical or a non-symmetrical plow depending on the path to be plowed. It is, of course, understood that such V-shaped snowplows would be snow shovels which would generally not be used for shoveling snow and are only for plowing.
The carriage 2 can be used for plowing snow from areas larger than pathways or walks such as driveways. A wider snowplow 70 is illustrated in FIG. 6 as having a shovel 72 which has a conventional handle 73 and is wider than those heretofore described. The wider snow shovel 72 makes it possible to plow an area such as a driveway. The wider snow shovel is illustrated as somewhat arcuate in its height cross section to provide somewhat of a snow scooping action of the snowplow since the shovel is not used on the carriage for shoveling but plowing. The curvature provides the necessary lift to the snow to effectively plow the snow.
Snow shovels generally have handles which have a length on the handle which is straight even if the entire handle is not straight along its full length. Moreover, snow shovels have handles of different lengths. The shovels themselves have different cross section configurations along the shovel height dimension. Generally, snow shovels have a marginal lower edge portion of the height dimension that is arcuate and has curvature along part of the marginal leading edge portion of the shovel so that snow can be scooped up.
The snowplow carriage assembly, according to the invention, makes provision for differences in length of handles of the different snow shovels and for different curvatures along the height of the different snow shovels. Furthermore, provision is made for mounting the snow shovels without need of holders being provided on the shovels for mounting them on a carriage for transport for plowing according to the invention.
A second embodiment of a carriage is illustrated in FIG. 7 in which a carriage 75 is constructed generally similar to the carriage 2 of FIG. 1. This second embodiment carriage is wheeled and has two arms 76, 77 and legs 79, 80 pivotally connected to the respective arms and has linkage systems 82, 83 so that it can be folded or collapsed and unfolded as the first carriage embodiment described. In order to be able to mount snow shovels of different handle lengths, the carriage is provided with an upper cross bar 85 which is movable to different positions axially of the arms for spacing variably with respect to a lower cross bar 87 which is fixed to the two arms. The arms are provided with a plurality of axially spaced holes 88, 89 along the length of the arms for mounting the upper arm 85 at different axial positions axially of the arms in order to accommodate snow shovels of different lengths of handles for mounting and transport on the carriage 75.
The upper cross bar 85 has at each opposite end thereof a curved hook 85a that rests on the corresponding arm 76, 77 as illustrated in FIGS. 7 & 8. Each hook 85a has a hole of equal dimension as the holes 88, 89 on the arms, and the upper cross bar 85 is mounted with the hook holes in registry with the holes on the arms so that bolts 91, 92, having wing nuts 94, can be inserted through the hook and corresponding arms and the upper arm secured to the carriage. The provision of an upper arm construction as shown in FIG. 8 and the mounting holes 88, 89 on the carriage 75 arms 76, 77 provides for variably adjusting the mounting of different types of snow shovels having different length handles, for example.
The second embodiment carriage assembly provides for easily mounting the different snow shovels by use of two split clamps or holders 90, 91 having hooks 90a, 91a engaging the cross bars 85, 87 as shown in FIG. 9 to maintain a snow shovel 100 and its handle 101 in position when plowing snow as described with respect to the first embodiment carriage assembly. The split holders each can also have a compressible liner as shown at 90b, so they can be clamped on different diameter snow shovel handles. They are held assembled by the bolts 105 with a wing nut 106. Snow shovels can easily be replaced on the carriage.
The second embodiment carriage can be adjusted as to the acute angle that the plane cross bars on the arms 76, 77 make relative to the horizontal. The legs 79, 80 are made so that the legs are made with upper lengths or sections 79a, 80a which telescope into lower sections 79b, 80b. The length of the legs is variably adjusted by providing axially spaced holes 110, 111 on the leg sections so that the length of the legs can be varied telescopically and the adjusted length maintained by bolts 112 which extend through the holes in the upper and lower leg sections which are aligned to set the variable length of the legs to vary the acute angle at which a snow shovel will make with the surface on which the snow is being plowed. Thus, the angle of the plow can be varied. Moreover, this adjustability of leg length makes it comfortable for users of different heights to use the snowplow carriage assembly best suited to their height and the angle at which they wish to use as a setting for the snowplow.
While the members of the carriages are described as tubular, they can be made as solid members of any suitable metallic or plastic materials. Components can be made of strong wood with or without reinforcements. The carriage components can be provided as a kit made for easy assembly. Suitable connections are provided for the various components.
It should be noted that the carriage is constructed so that at times the plowing of snow can be carried out with the legs in a retracted or folded position, if desired. This provides a wide range of possible acute angles at which the snowplow will plow the snow when desired. However, the carriage is intended to provide walking support for the users, old or young, and to be used principally as described in an unfolded state supported on all its wheels.
|
A snowplow carriage assembly for removal of snow manually by plowing the snow in an area to be cleared of snow. The carriage is a manually propelled wheeled structure made of a plurality of members pivotally connected for collapsing and folding for storage and unfolding for use in supporting and transporting a snowplow in the form of a replaceable conventional snow shovel having a handle straight length portion. The carriage is configured so that the snow shovel handle is removably mounted thereon inclined from the horizontal defining an acute angle relative to a surface on which snow is being plowed. The snow shovel inclination is variable for establishing different acute angles of the shovel relative to the surface for plowing the snow thereon and removal therefrom.
| 4
|
PRIORITY
[0001] This application claims the benefit under 35 U.S.C. § 119(a) of a Korean patent application filed in the Korean Intellectual Property Office on Aug. 16, 2007 and assigned Serial No. 2007-0082362, the entire disclosure of which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to an apparatus and method for handover between heterogeneous networks. More particularly, the present invention relates to an apparatus and method that provide enhanced heterogeneous network handover using a media independent handover scheme.
[0004] 2. Description of the Related Art
[0005] Handover, or handoff, is a technical procedure for switching a call in progress from the radio coverage area of one base station to another base station while ensuring the continuity of the established call.
[0006] Handover is commonly performed when user equipment, currently in an active communication session, moves between the cells of a homogenous system. With the deployment of various heterogeneous system networks, advanced handover techniques for supporting handover between heterogeneous networks have been developed. Handover between heterogeneous networks (also known as vertical handover) means an inter-technology handover such as a switch between a WiBro network and another standard system network, such as a 2nd generation (2G) network, a 3rd generation (3G) network, or a wireless local area network (WLAN) based on the Institute of Electrical and Electronics Engineers 802.11 (IEEE 802.11) standards.
[0007] Media Independent Handover (MIH) is a standard being developed as part of the IEEE 802.21 standard to enable handover in a heterogeneous network environment. MIH is a seamless intermediate handover technique guaranteeing quality of service (QoS) between heterogeneous networks regardless of media types. MIH provides Event Services, Command Services and Information Services for allowing a mobile node having multiple radio interfaces to switch the communication session in progress to an optimal network regardless of media type without requiring user interface. With such services, the upper layers can perform a handover to an optimal network.
[0008] FIG. 1 illustrates message flows in a conventional inter-system handover procedure. In FIG. 1 , a mobile node (MN) 100 is attempting a handover from a WLAN to a wireless metropolitan area network (WMAN).
[0009] Referring to FIG. 1 , a mobile node (MN) 100 is serviced by a WLAN 101 as a serving network in step S 110 . If a link status changes, the MN 100 transmits an MIH get information request message (MIH_Get_Information.request) to neighbor networks via an MIH Information Service (MIIS) server 102 in step S 115 . The change of link status is determined by comparing a link parameter value with a threshold value. If the link parameter value is greater than the threshold value, it is determined that a change of link status has occurred. The high link parameter value indicates that the received signal strength is weak. Accordingly, the MN 100 determines information about neighboring networks, such as received signal strengths of the different networks, and prepares to perform a handover to the neighboring network having an optimal state. The MIH_Get_Information.request message is formatted as follows and the parameters of the MIH_Get_Information.request message are defined as in table 1.
[0000]
MIH_Get_Information.request (
InfoQueryType,
InfoQueryParameters
)
[0000]
TABLE 1
Valid
Name
Type
Range
Description
InfoQueryType
An integer value corresponding
N/A
The type of query that is specified
to one of the following
types:
1: TLV
2: RDF_DATA
3: RDF_SCHEMA_URL
4: RDF_SCHEMA
InfoQueryParameters
Query type specific parameters
N/A
Query type specific parameters which indicate
the type of information the client may be
interested in.
[0010] The MIH_Get_Information.request is transmitted by MN 100 to request information related to a specific interface, attributes to the network interface as well as entire network capability.
[0011] As shown in table 1, integer values of the InfoQueryType parameter of the MIH_Get_Information.request respectively correspond to TLV, RDF_DATA, RDF_SCHEMA_URL, and RDF_SCHEMA.
[0012] When the InfoQueryType is specified as TLV, the InfoQueryParameters is a binary string. When the InfoQueryType is specified as RDF_DATA, the InfoQueryParameters is a string which contains a SPARQL (Protocol and RDF Query language) query where the SPARQL query is supposed to contain an appropriate query for obtaining expected RDF/XML data. When the InfoQueryType is specified as RDF_SCHEMA_URL, the InfoQueryParameters is a null string. Finally, when InfoQueryType is specified as RDF_SCHEMA, the InfoQueryParameters carries either the URL of the extended schema the query originator wants to obtain or a null string when the URL of the extended schema is unknown.
[0013] In response to the MIH_Get_Information.request message, the MIIS server 102 transmits an MIH get information response message (MIH_Get_Information.response) to the MN 100 in step S 117 . The MIH_Get_Information.response message includes information on the candidate networks that are selected by the MIIS server 102 in consideration of the location of the MN 100 . Upon receiving the MIH_Get_Information.response message, the MN 100 determines link relief information in step S 120 . That is, the link layer of the MN 100 notifies that the current link established by MIH is released within a predetermined time. Accordingly, the MN 100 determines another link to perform handover to a new cell, i.e. a new network.
[0014] Next, the MN 100 receives information required for a new connection from WMANs 103 and 104 as the candidate networks in steps S 125 and S 126 . For simplifying the explanation, it is assumed that two WiBro networks based on the IEEE 802.16 standard are selected as the candidate networks in FIG. 1 . However, the number of the candidate networks can be changed and other the types of networks, such as cellular networks and WLANs, can be utilized.
[0015] Since the candidate networks 103 and 104 are WiBro networks, the connection information includes Downlink MAP (DL MAP), Uplink MAP (UL MAP), Downlink Channel Descript (DCD), and Uplink Channel Descript (UCD).
[0016] If the network connection information is collected, the MN 100 performs a link scanning on the links of the candidate networks 103 and 104 in step S 130 and then transmits a candidate query request message (Candidate_Query. request) including the information on the candidate networks 103 and 104 to the serving network 101 in step S 132 . The Candidate_Query.request includes a link type identifier, network identifiers of the candidate networks, and information about operations required for the current link after handover. Upon receiving the Candidate_Query.request message, the serving network 101 transmits a handover (HO) query resource request message (Query_Resource.request) to the candidate networks 103 and 104 in steps S 135 and S 136 . The candidate networks are selected in consideration of the location of the MN 100 , and the number and types of candidate networks are not limited to the example of FIG. 1 . In a case where five candidate networks are reported by the MIIS server 102 , the serving network 101 requests the radio resource information for handover to the five candidate networks.
[0017] In response to the Query_Resource.request, the respective candidate networks 103 and 104 transmit a query resource response message (Query_Resource.response) containing information on their resources to the service network 101 in steps S 137 and S 138 . Particularly, the handover resource information response message may include handover acceptability for the MN 100 . The serving network 101 determines one of the candidate networks as an optimal network for handover in consideration of the handover acceptability and resource status of the candidate networks 103 and 104 . Next, the serving network 101 transmits a Candidate_Query.response containing information on the HO target network to the MN 100 in step S 140 .
[0018] Assuming that the candidate network 103 is selected as the handover target network, the MN 100 performs operations for establishing a connection to the target network 103 . Since the handover target network 103 is a WiBro network, the MN 100 performs a ranging process for establishing a connection link in step S 145 . After completing the ranging process, the MN 100 determines successful handover completion in step S 147 and is served by the new serving network 103 in step S 150 . Here, the communication link to the old service network 101 is released. In this manner, the vertical handover between heterogeneous networks is performed.
[0019] As described above, in the vertical handover specified by the IEEE 802.21 standard, the MN transmits MIH_Get_Information.request to the MIIS server whenever a handover to a new cell is required, and the MIIS server collects information on the networks in a core network and determines the existence of available heterogeneous networks for handover. The MIIS server transmits the network status information to the MN using the MIH_Get_Information.response message.
[0020] In the conventional standard specification, when a handover is required due to the movement of the MN, the core network predicts a location of the MN using a prediction algorithm and informs the MN of whether a handover to a heterogeneous network is available. In the heterogeneous network environment, however, the network resource management for the vertical handover is very complicated and inefficient real time handover traffic may cause significant network problems. Such problems increase latency and deteriorate communication reliability. That is, the conventional vertical handover method is limited in efficient handover performance due to the latency and communication reliability caused by inaccurate user location and mobility estimated by the core network.
SUMMARY OF THE INVENTION
[0021] An aspect of the present invention is to address at least the above-mentioned problems and/or disadvantages and to provide at least the advantages described below. Accordingly, an aspect of the present invention is to provide a handover method and system in a heterogeneous network environment.
[0022] Another aspect of the present invention is to provide a media independent handover method and system that are capable of improving handover efficiency in a heterogeneous network environment.
[0023] In accordance with an aspect of the present invention, a handover method in a heterogeneous network environment is provided. The method includes generating, at a mobile node, self-location information, transmitting the self-location information to a management server which manages heterogeneous networks, searching, at the management server, surrounding networks using the self-location information, composing a set of candidate networks including at least one of the surrounding networks, transmitting information on the set of candidate networks to mobile node and deciding, at the mobile node, a target handover network among the candidate networks.
[0024] In accordance with another aspect of the present invention, a heterogeneous network handover method is provided. The method includes generating, by a mobile node having multiple standard interfaces, self-location information and self-travel route prediction information, transmitting the self-location information and self-travel route prediction information to a management server which manages heterogeneous networks, searching, at the management server, surrounding networks using the self-location information and self-travel route prediction information, selecting handover candidate networks from among the surrounding networks searched along a travel route extracted from the self-travel route prediction information, transmitting information on the candidate networks to the mobile node and performing, at the mobile node, a handover to one of the candidate networks.
[0025] In accordance with yet another aspect of the present invention, a heterogeneous network handover system is provided. The system includes at least one mobile node for communicating with multiple heterogeneous networks, for generating self-location information, for transmitting the self-location information to a core network, and for performing a handover on the basis of candidate network information received from the network and a management server for managing the heterogeneous networks, for searching surrounding networks using the self-location information received from the mobile node, for selecting at least one of surrounding networks as a set of handover candidate networks, and for transmitting information on the candidate networks to the mobile node.
[0026] In accordance with still another aspect of the present invention, a heterogeneous network handover apparatus is provided. The apparatus includes a plurality of radio interfaces for communication with heterogeneous networks, a self-location information generator for generating self-location information and self-travel route prediction information and a media independent handover function for transmitting a surrounding network information request message containing the self-location information and self-travel route prediction information to a heterogeneous network management server and receiving a reply message in response to the surrounding network information request message.
[0027] Other aspects, advantages, and salient features of the invention will become apparent to those skilled in the art from the following detailed description, which, taken in conjunction with the annexed drawings, discloses exemplary embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] The above and other aspects, features and advantages of certain exemplary embodiments of the present invention will be more apparent from the following detailed description in conjunction with the accompanying drawings, in which:
[0029] FIG. 1 is a flowchart illustrating message flows in a conventional inter-system handover procedure;
[0030] FIG. 2 is a schematic diagram illustrating MIH system architecture according to an exemplary embodiment of the present invention;
[0031] FIG. 3 is a block diagram illustrating an MN having multiple radio interfaces for supporting MIH between heterogeneous networks according to an exemplary embodiment of the present invention; and
[0032] FIGS. 4A and 4B are a message flow diagram illustrating a handover method in a heterogeneous network environment according to an exemplary embodiment of the present invention.
[0033] Throughout the drawings, it should be noted that like reference numbers are used to depict the same or similar elements, features and structures.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0034] The following description with reference to the accompanying drawings is provided to assist in a comprehensive understanding of exemplary embodiments of the invention as defined by the claims and their equivalents. It includes various specific details to assist in that understanding but these are to be regarded as merely exemplary. Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope and spirit of the invention. Also, descriptions of well-known functions and constructions are omitted for clarity and conciseness.
[0035] FIG. 2 is a schematic diagram illustrating MIH system architecture according to an exemplary embodiment of the present invention. In FIG. 2 , the system architecture includes an IEEE 802.11 WLAN and an IEEE 802.16 WMAN. However, the handover system and method of the present invention are not limited thereto. For example, the handover system and method of the present invention can be applied to an MIH system architecture in which other types of WLANs and WMANs and cellular networks coexist.
[0036] Referring to FIG. 2 , an MN 200 is connected to the Internet via an access point (AP) 210 of the WLAN and an access router (AR) 230 of an Internet Protocol (IP) access network. The AR 230 is responsible for IP routing of packets from the MN 200 and acts as a Foreign Agent (FA). The AP 210 communicates with the MN 200 over the WLAN access protocol and acts as a bridge between the WLAN and a wired network.
[0037] As illustrated in FIG. 2 , the WLAN coverage area is overlapped with the WMAN coverage area and the MN 200 moves out of the radio coverage of the AP 210 so as to enter the WMAN area. The WMAN area is defined by the radio coverage of a Radio Access Station (RAS) 240 which provides access service to the MN 200 and manages radio resource. The RAS 240 also provides authentication and security functions. An Access Control Router (ACR) 250 is connected to the IP access network. The ACR is responsible for IP routing and mobility management and performs IP multicast, billing, and mobility control functions.
[0038] A MIIS 260 is placed on a core network and is responsible for managing network resources for supporting handover between the heterogeneous networks. In an exemplary embodiment of the present invention, the MIIS collects the information on the heterogeneous networks connected to the IP access network and provides the network information to the MN 200 in response to a network information request message. Although not shown in FIG. 2 , an Authentication, Authorization, and Accounting (AAA) function is further included in the architecture for performing packet encapsulation as a router of a home network and for authenticating a Home Agent (HA) which performs data tunneling to a currently registered address of the MN and the MN's access.
[0039] In an exemplary embodiment, the MN 200 , AP 210 of the WLAN, and RAS 240 of the WMAN are provided with MIH functions so as to provide MIH services.
[0040] FIG. 3 is a block diagram illustrating an MN having multiple radio interfaces for supporting MIH between heterogeneous networks according to an exemplary embodiment of the present invention. Such MIH functions are supported by other network elements. Although the network elements of the respective networks, equivalent to the base stations, are described with the MIH functions in this example, the present invention is not limited thereto.
[0041] Referring to FIG. 3 , the MN 200 includes a wireless interface unit 310 which is capable of supporting multiple radio interfaces, an MIH function unit 320 , and an MIH user unit (or upper layer unit) 330 . The wireless interface unit 310 is provided with the Physical layer (PHY) and Media Access Control (MAC) layer. In this example, the wireless interface unit 310 is provided with an IEEE 802.11 interface 312 for supporting connection to an IEEE 802.11 WLAN, an IEEE 802.16 interface 314 for supporting connection to an IEEE 802.16 WMAN, and a cellular interface 316 for supporting connection to a cellular network. Of course, other types of radio interfaces can be included in the wireless interface unit 310 in addition to the IEEE 802.11 interface, IEEE 802.16 interface, and cellular interface.
[0042] The MIH function unit 320 provides services to the upper layer unit 330 through a single technology-independent interface and obtains services from the wireless interface unit 310 through a variety of technology-independent interfaces. The MIH function unit 320 includes an event service module 322 , a command service module 324 , and an information service module 326 .
[0043] The event service module 322 provides event classification, event filtering and event reporting corresponding to dynamic changes in link characteristics, link status, and link quality. The event service module 322 also exchanges the event information with the base stations. Here, the base stations may include the AP of a WLAN, an RAS of a WiBro network, a Node B of a Wideband Code Division Multiple Access (WCDMA) network and a Base Transceiver Station (BTS) of a Code division Multiple Access 2000 (CDMA2000) network. The command service module 324 provides the command service which enables MIH users to manage and control link behavior relevant to handovers and mobility. The information service module 326 provides details on the characteristics and services provided by the serving and surrounding networks. The information enables effective system access and effective handover decisions. In an exemplary implementation as illustrated in FIG. 3 , the information service module 326 of the MN 200 provides information on the current location and predicted route of the MN. This information is contained in the network information request message. Accordingly, the MN can quickly receive the information of the surrounding networks and perform handover accurately on the basis of the received information.
[0044] The upper layer unit 330 makes use of the services provided by the MIH function unit 320 . The upper layer unit 330 enables an upper layer application to be seamlessly serviced especially in handover by assistance of the MIH function unit 320 .
[0045] FIGS. 4A and 4B are a message flow diagram illustrating a handover method in a heterogeneous network environment according to an exemplary embodiment of the present invention. In the illustrated example, the handover method is described with a situation in which the MN 200 switches the current WLAN link to a WMAN link. Of course, this is for example only an in no way limits the application of the present invention.
[0046] Referring to FIGS. 4A and 4B , an MN 200 is served by a serving network (WLAN) 401 in step S 410 . If a state of the link connected to the WLAN 401 deteriorates, the MN 200 requests an MIIS 402 for information about surrounding networks. In more detail, the wireless interface unit 310 of FIG. 3 detects the change of the link status of the 802.11 interface 312 and reports the link status change to the MIH function unit 320 . The link status change is detected by comparing a link parameter value to threshold value. If the link parameter value exceeds the threshold value, the wireless interface unit 310 determines that the link state is changed. The change of the link status means, for example, that the received signal strength of the current link is weak. Of course, a change in the link status could indicate deterioration of other parameters. Accordingly, the MN 200 , particularly, the MIH function unit 320 requests information on the surrounding networks in order to prepare for a handover from the current serving network 401 to another network. The MIH function unit 320 requests the MIIS 402 for the surrounding network information using the MIH information service. In this manner, the MN 200 determines the surrounding network information such as received signal strengths and attempts a handover to one of the surrounding networks having an optimal condition for providing services to the MN 200 . In this example, the MN 200 transmits accurate information on its location to the MIIS 401 through the surrounding network information request message.
[0047] The MN 200 , particularly, the MIH function unit 320 generates its own location information and routing information in step S 412 and transmits MIH_Get_Information.request containing the location and routing information to the MIIS 402 in step S 415 . The MIH_Get_Information.request message is formatted as follows and the parameters of the MIH_Get_Information.request message are as in table 2.
[0000]
MIH_Get_Information.request (
InfoQueryType,
InfoQueryParameters,
MIH_LOCATION_REPORT,
MIH_ROUTE_REPORT
)
[0000]
TABLE 2
Valid
Name
Type
Range
Description
InfoQueryType
An integer value
N/A
The type of query
corresponding to one of
that is specified
the following types:
1: TLV
2: RDF_DATA
3: RDF_SCHEMA_URL
4: RDF_SCHEMA
InfoQueryParameters
Query type specific
N/A
Query type specific
parameters
parameters which
indicate the type of
information the
client may be
interested in.
MIH_LOCATION_REPORT
String
N/A
Specifies the
location information
of Mobile Node
MIH_ROUTE_REPORT
String
N/A
Specifies the routing
information of
Mobile Node in
future
[0048] In another exemplary embodiment of the present invention, the MIH_Get_Information.request is formatted as follow and the parameters of the MIH_Get_Information.request are defined as in table 3.
[0000]
MIH_Get_Information.request (
DestinationIdentifier,
InfoQueryBinaryDataList,
InfoQueryRDFDataList,
InfoQueryRDFSchemaURL,
InfoQueryRDFSchemaList,
MaxResponseSize,
MIH_LOCATION_REPORT,
MIH_ROUTE_REPORT
)
[0000]
TABLE 3
Name
Type
Description
Destination
MIF_ID
The local MIHF or a remote
Identifier
MIHF which will be the
destination of this request.
Info Query
LIST(INFO_QUERY_BINARY_DATA)
(Optional)A list of binary
Binary Data List
queries. The order of the queries
in the list identifies the priority
of the query. The first query has
the highest priority to be
processed by MIIS.
Info Query RDF
LIST(INFO_QUERY_RDF_DATA)
(Optional)A list of RDF queries.
Data List
The order of the queries in the
list identifies the priority of the
query. The first query has the
highest priority to be processed
by MIIS.
Info Query RDF
NULL
(Optional)An RDF Schema URL
Schema URL
query.
Info Query RDF
LIST(INFO_QUERY_RDF_SCHEMA)
(Optional)A list of RDF schema
Schema List
queries. The order of the queries
in the list identifies the priority
of the query. The first query has
the highest priority to be
processed by MIIS.
Max Response
UNSIGNED_INT(2)
(Optional)This field specifies the
Size
maximum size of Info Response
parameters (i.e., Info Response
Binary Data List, Info Response
RDF Data List, Info Response
RDF Schema URL and Info
Response RDF Schema List) in
MIH_Get_Information response
message in octets. If this field is
not specified, the maximum size
is set to 65,535. The actual
maximum size forced by the IS
server may be smaller than that
specified by the IS client.
MIH_LOCATION_REPORT
String
Specifies the location
information of Mobile Node
MIH_ROUTE_REPORT
String
Specifies the routing information
of Mobile Node in future
[0049] The MIH_Get_Information.request message is transmitted by MN 200 for requesting information related to specific information, attributes of the network interface as well as entire network capability.
[0050] As shown in tables 2 and 3, an exemplary handover method uses a new MIH_Get_Information.request message format which additionally includes parameters indicating location information and predicted routing information of the MN 200 . This location and routing information is generated by a location information generator (not shown in drawings) in step S 412 . The location information generator estimates the location of the MN 200 using a Location-Based Service (LBS). The parameter MIH_LOCATION_REPORT indicates the current location of the MN 200 which is formatted as coordinate information such as latitude and longitude coordinates used in a Global Positioning System (GPS). The format of the location information should be defined in common with the MIIS 402 . Since the location information of the MN 200 is transmitted to the core network, the MIIS 402 obtains an accurate location of the MN 200 without querying or estimating the location of the MN 200 . Accordingly, the MIIS 402 can evaluate the surrounding networks more accurately, whereby the core network can prepare a handover procedure in advance and, in turn, minimize the handover latency.
[0051] The parameter MIH_ROUTE_REPORT indicates a routing path of the MN 200 predicted from the current location. For example, in a case where the MN is enabled by GPS, the MN 200 can predict its routing path with the support of GPS. When the MN 200 moves along the routing path configured by a navigator, the MN 200 adds the MIH_ROUTE_REPORT parameter to the network information request message to be transmitted to the MIIS 402 . The format of the routing information also should be defined in common with the MIIS 402 . By providing such routing information to the MIIS 402 , the MIIS 402 can quickly determine and provide information on the surrounding networks. Accordingly, the MIIS 402 can predict and schedule the handovers of the MN 200 using the routing information, thereby improving handover efficiency and communication stability especially between the heterogeneous networks.
[0052] The respective integer values of parameter InfoQueryType correspond to TLV, RDF_DATA, RDF_SCHEMA_URL, and RDF_SCHEMA. When the InfoQueryType is specified as TLV, the InfoQueryParameters is a binary string containing encoded information element TLVs. When the InfoQueryType is specified as RDF_DATA, the InfoQueryParameters is a string which contains a SPARQL (Protocol and RDF Query language) query where the SPARQL query is supposed to contain an appropriate query for obtaining expected RDF/XML data. When the InfoQueryType is specified as RDF_SCHEMA_URL, the InfoQueryParameters is a null string. Finally, when InfoQueryType is specified as RDF_SCHEMA, the InfoQueryParameters carries either the URL of the extended schema the query originator wants to obtain or a null string when the URL of the extended schema is unknown.
[0053] In table 3, DestinationIdentifier indicates a local MIH function (MIHF) or a remote MIHF which will be the destination of this request. InforQueryBinaryDataList is an optional parameter indicating a list of binary queries. The order of queries in the list identifies the priority of the query. The first query has the highest priority to be processed by MIIS 402 . Also, InfoQueryRDFDataList is an optional parameter indicating a list of RDF queries. Like the InfoQueryBinaryDataList, the order of the queries in the list identifies the priority of the query. The first query has the highest priority to be processed by the MIIS 402 . InfoQueryRDFSchemaURL is another optional parameter indicating an RDF Schema URL query. Also, InfoQueryRDFSchemaList is an optional parameter indicating a list of RDF schema queries. The order of the queries in the list identifies the priority of the query. The first query has the highest priority to be processed by MIIS 402 . MaxResponseSize is an optional parameter. This parameter specifies the maximum size of Info Response parameters, i.e., Info Response Binary Data List, Info Response RDF Data List, Info Response RDF Schema URL, and Info Response RDF Schema List in MIH_Get_Information.response message in octets. If this field is not specified, the maximum size is set to 65,535. The actual maximum size forced by the IS server may by smaller than that specified by the IS client.
[0054] Upon receiving the network information request message (MIH_Get_Information.request), the MIIS 402 searches for the surrounding networks on the basis of the current location and routing information of the MN 200 and determines candidate networks in step S 416 . At this time, one or more candidate networks can be selected. In the case that the routing information is used, the MIIS 402 can select the candidate networks that can provide the optimal quality of service (QoS) along the travel route of the MN 200 . Accordingly, one or more networks can be selected as the candidate networks. For simplifying the present explanation, one surrounding network, i.e. the WMAN 403 , will be selected as the candidate network using the current location information in FIGS. 4A and 4B . However, more than one surrounding network can be selected as the candidate networks.
[0055] After determining the candidate network, the MIIS 402 transmits a response message (MIH_Get_Information.response) containing the candidate network information to the MN 200 in response to the MIH_Get_Information.request in step S 417 . In a case that the MIH_Get_Information.request received from the MN 200 contains the expected routing information, if the candidate network information changes, for example due to a change in network status, the MIIS 402 may transmit information of another candidate network to the MN 200 or transmit information of the changed condition. This message can be provided to the MIH event service 322 . If the changed candidate network information is received, the MN 200 performs a handover to the changed candidate network.
[0056] If the MIH_Get_Information.response is received, the MN 200 determines link relief information in step 420 . In more detail, the link layer entity of the 802.11 interface 312 of the MN 200 notifies the MIH function unit 320 that the current 802.11 link is to be released in a preset time. Next, the MIH function unit 320 of the MN 200 reports the link relief to the MIH user unit 330 . In response to a link scan request, the 802.16 interface 314 of the interface unit 310 is activated so as to receive network access information broadcast by the 802.16 WMAN 403 in steps S 425 . Since the candidate network is an 802.16 based WiBro network in this example, the network access information is broadcast by the candidate network. However, the candidate network is not limited to the WiBro network. The network access information broadcast by the WiBro network includes UL MAP, DL MAP, DCD, and UCD. The network access information includes information on the initial ranging performed for synchronization between the RAS and MN 200 , and it is broadcasted by the RAS periodically.
[0057] The network access information received through the 802.16 interface 314 is transferred to the MIH user unit (or upper layer unit) 330 . In this manner, the MN 200 performs the link scan process in step S 430 .
[0058] After completing the link scan, the MN 200 , particularly the MIH function unit 320 , transmits a candidate query request message (Candidate_Query.request) to the serving network 401 for initiating the handover in step 432 . The Candidate_Query.request includes a link type identifier, candidate network identifiers, and information about operations required for the current link after handover. Upon receiving the Candidate_Query.request message, the serving network 401 transmits a handover (HO) query resource request message (Query_Resource.request) to the candidate network 403 in step S 435 . Since it is assumed that the WLAN 403 is the only candidate network, the serving network 401 transmits the Query_Resource.request to the WMAN 403 . As described above, the candidate network 403 is the best network selected on the basis of the location information provided by the MN 200 .
[0059] In response to the Query_Resource.request, the candidate network 403 transmits a query resource response message (Query_Resource.response) containing radio resource information to the serving network 401 in step S 437 . Upon receiving the Query_Resource.response, the serving network 401 transmits a Candidate_Query.response to the MN 200 in step S 440 .
[0060] Once the candidate network is determined, the MN 200 performs an operation for connecting to the handover candidate network 403 in step S 445 . In this example, since the handover candidate network 403 is a WiBro network, the MN 200 performs a ranging process for establishing a connection link with the candidate network 403 .
[0061] After completing the ranging process, the 802.16 interface 314 of the interface unit 310 of the MN 200 notifies the MIH function unit of the handover completion and then the MIH function unit 320 notifies the MIH user unit 330 that the link switching is successfully completed in step S 447 . In this manner, the MN 200 completes the handover from the WLAN 401 to WMAN 403 (the WiBro network). Accordingly, the MN 200 can be served by the WLAN 401 , from the WiBro network continuously in step S 450 . Since the MN 200 is connected to the new network 403 , the old link established by the 801.11 interface 312 is released according the relief request of the MIH function unit 320 .
[0062] Although exemplary embodiments of the present invention have been described in detail hereinabove, it should be clearly understood that many variations and/or modifications of the basic inventive concepts herein taught which may appear to those skilled in the present art will still fall within the spirit and scope of the present invention, as defined in the appended claims and the like.
|
An apparatus and method for enhanced heterogeneous network handover using a media independent handover scheme is provided. A heterogeneous network handover method of the present invention includes generating, at a mobile node, self-location information, transmitting the self-location information to a management server which manages heterogeneous networks, searching, at the management server, surrounding networks using the self-location information, composing a set of candidate networks including at least one of the surrounding networks, transmitting information on the set of candidate networks to mobile node and deciding, at the mobile node, a target handover network among the candidate networks. Accordingly, latency during handover in a heterogeneous network can be reduced.
| 7
|
FIELD OF THE INVENTION
The present invention relates to a process and plant to carbonize the vegetable impurities contained in woolen textile manufactured articles.
It is known to carry out a process of carbonization of woolen cloth, in order to remove existing vegetable impurities.
The process of carbonization of the woolen cloth is traditionally carried out on facilities which provide, in sequence, an operation of impregnation of the cloth to be carbonized with an aqueous solution of sulphuric acid, followed by a squeezing operation, and a step or thermal treatment of the same cloth, inside a ventilated chamber with open-loop air circulation, during which the cloth is dried due to water evaporation, and the vegetable impurities are carbonized due to the combined effect of temperature, and of the acid absorbed by the fibre.
The so treated cloth contains therefore a relatively high amount of residual acid, which has to be reduced. For that purpose, the carbonized cloth is usually submitted to a step of intense washing with water, which generally takes place in a separate facility. In particular, then, in the frequently occurring case of carbonization of the grey cloth from weaving, a further function performed by said washing step is that of cleaning the cloth, i.e., removing the lubricating substances of greasy and oily nature, which were previously deposited on the fibre during the course of the preceding spinning and weaving processing steps.
It is in fact customary, due to prevailing economic reasons, not to submit the cloth to be carbonized to a preliminary washing step to remove such lubricating substances, in that carrying out such operation once only, after the carbonization process, is preferred, so to obtain, at the same time, cleaning and removal of the residual acid remaining in the cloth.
Such an operating procedure suffers from the following drawbacks:
the lubricating substances on the cloth to be carbonized, if not removed, hinder the aggressive action of the acid on the vegetable impurities, resulting in an impairment of the quality of carbonization;
during the thermal treatment step of the carbonization process, the low-boiling oils present on the cloth tend to sublime due to the effect of temperature, and are therefore expelled to the outside, with the air, through exhausting chimneys, creating not negligible problems of atmospheric pollution;
the step of cloth washing after the true carbonization requires the consumption of large amounts of water, and produces a corresponding large amount of polluting acid waste liquid, whose economic and environmental consequences constitute the most considerable and important among all problems.
SUMMARY OF THE INVENTION
The process of carbonization of woolen cloth of the present invention is that of overcoming the negative aspects typical of the traditional carbonization process, while at the same time supplying a full set of advantages of qualitative, economic and environmental character.
Such object is achieved according to the present invention by providing a process for carbonizing the vegetable impurities present in woolen textile manufactured articles, wherein the following operations are provided:
treatment of the textile article with chlorinated solvent, until a first deep impregnation thereof is obtained;
treatment of the textile article impregnated with said chlorinated solvent, with an aqueous solution of sulphuric acid, until a second, surface, impregnation is obtained, and
thermal treatment until the evaporation of the chlorinated solvent and of water, and the true carbonization of said vegetable impurities are obtained.
Said chlorinated solvent of the process of the invention is preferably perchloroethylene.
According to a preferred embodiment, a plant for carrying out the carbonization according to the process of the present invention comprises a first chamber for treatment with chlorinated solvent, a second chamber of treatment with an aqueous solution for sulphuric acid, and a third chamber for drying and true carbonization.
BRIEF DESCRIPTION OF THE DRAWING
The characteristics and advantages of a process according to the present invention will become clearer from the following disclosure, given by way of example and without limitation, with reference to the hereto attached sole figure of the drawing which diagrammatically illustrates an embodiment according to the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
A woolen textile article or cloth, once produced, must undergo a process of carbonization, for the purpose of removing the vegetable impurities which are present in it.
According to the present invention, for such a purpose, the woolen cloth undergoes a first operation of treatment with chlorinated solvent, until a first deep impregnation of the cloth is obtained.
The purpose of this first treatment step--in particular in case of carbonization of grey cloth from weaving--is to remove the lubricating substances of greasy and oily character deposited on the fibre during spinning and weaving. In fact, the cleaning of the cloth makes it possible for the vegetable impurities to be more easily attacked by the acid during the following step of true carbonization. However, independently of any cleansing function, the operation of impregnation of the cloth with the solvent is basic and essential for the purposes of the application of the process according to the invention.
In particular and preferably, during this first impregnation or treatment step, as the chlorinated solvent, perchloroethylene is used, and said impregnation, which occurs deeply in the fibre, is carried out by means of a simple washing of the cloth.
Thereafter, the cloth, moist from chlorinated solvent, undergoes a second treatment step, and is impregnated with an aqueous solution of sulphuric acid.
It is known, in fact, that the chlorinated solvents, and in particular perchloroethylene, thanks to their low surface tension are able to rapidly and deeply soak the textile fibres, much more than the aqueous solution. It follows therefrom that if a cloth impregnated with the solvent is subsequently treated with an aqueous solution, this latter does not have the capability to displace the solvent from the fibre, and to replace it, but to a minimum extent, and on the surface only. In other words, the presence of the solvent in the cloth at the time of the second impregnation with the aqueous solution of sulphuric acid, constitutes a protecting element against the penetration of acid into the interior of the fibre. On the other hand, the vegetable impurities contained in the cloth, which are strongly hydrophilic, and on which the solvent is distributed on the surface only, preferentially absorb the aqueous solution of sulphuric acid. In practice, by operating in that way, a selective absorption is accomplished of the aqueous solution of sulphuric acid in the vegetable impurities to be carbonized, the absorption of the acid by the fibre being considerably reduced, as compared to what occurs in the traditional carbonization process.
Finally, the cloth, impregnated with the resulting mixture of chlorinated solvent and aqueous solution of sulphuric acid, is subjected to a step of thermal treatment, during which both solvent and water are evaporated from the cloth, and the vegetable impurities undergo true carbonization due to the combined effect of temperature, and of residual sulphuric acid.
According to a non-limitative example, a plant shown in the hereto attached figure, and embodying the process according to the invention, is essentially constituted by a first chamber or unit of treatment with the chlorinated solvent 11, a second chamber of treatment with the aqueous solution of sulphuric acid 12, and a third chamber of thermal treatment 13 for drying, and the true carbonization. A woolen cloth 14 to be carbonized is continuously fed on a set of rollers 10, through an opening provided with seal elements 15, into the first processing chamber 11, wherein it is subjected to a plurality of sprayings, by means of a set of nozzles 16, with chlorinated solvent. The solvent is then exhausted by a first means 17, or intaking-lip tube, which has the purpose of removing from the woolen cloth 14 most of the solvent applied by nozzles 16.
The woolen cloth 14 is then rinsed by means of a further solvent spray, delivered through a nozzle 18, and is subsequently subjected to the sucking action of a further means 19, or intaking-lip tube, so that on said cloth 14 a determined amount of chlorinated solvent remains.
The woolen cloth 14, moist with solvent, subsequently travels on a further set of rollers 10, and enters, through an opening provided with seal elements 20, the second processing chamber 12, in which a desired and predetermined amount of aqueous solution of sulphuric acid is applied by means of nozzles 21.
The woolen cloth 14, thus impregnated by the resulting mixture of chlorinated solvent and of acidic aqueous solution, passes through a further opening provided with seal elements 22, and enters third chamber 13 where the cloth travels, slidingly guided on a further set of rollers 10, the third chamber 13 being, i.e., the thermal treatment chamber.
Inside third chamber 13, the drying and the true carbonization of the cloth take place, by means of the evaporation of the above-said mixture, and the carbonization of the vegetable impurities due to the combined effect both of temperature, and of the residual sulphuric acid.
Finally, the woolen cloth 14, passing through a last opening provided with seal elements 23, is extracted in a dry and carbonized state from the third chamber 13.
Preferably, inside said third chamber 13 a means is provided, to accomplish a closed-loop circulation of hot air, e.g., by a thermo-fan 24, which is provided with a delivery duct 25 and an intake duct 26, both connected chamber 13.
Inside the air circuit, a refrigerator 27 is provided, which performs the function of de-saturating the recycled air, maintaining it at a constant saturation level, and of simultaneously recovering the solvent and water evaporated from the cloth, which can be sent to a separation tank (not shown in figure).
The impregnation of the woolen cloth 14 with the aqueous solution of sulphuric acid inside the second chamber 12 can be also accomplished by means different from those illustrated, e.g., by spreading by means of plating rollers, or by direct dipping of the fed cloth. In case the direct dipping into a bath of acidic aqueous solution is used, the cloth should be subsequently squeezed by squeezing rollers.
In any case, whatever the means of application of said aqueous solution is, an application must be made possible of a pre-determined and controlled amount of the aqueous solution, so to prepare the damp cloth in such a way as to optimize the true carbonization.
In a similar way, the chamber for treatment with the chlorinated solvent 11 and the thermal-treatment chamber 13 can be modified to account for particular specific requirements within the scope of the method of the present invention.
Summing-up, the process of carbonization and the relevant exemplifying plant according to the present invention, as compared to those presently used in industry, offer a full set of considerable advantages.
First of all, a more uniform and efficient carbonization of the vegetable impurities is obtained, thanks to the preliminary cleaning of the cloth by means of the treatment with chlorinated solvent, which removes the lubricating substances of greasy and oily character.
Then, the elimination is obtained of the phenomena of sublimation of the low-boiling oils during the end thermal treatment of the cloth, and of the related problems of atmospheric pollution, in as much as the thermal treatment chamber is of the type with closed-loop air circulation, and is therefore free from exhausting chimneys leading to the outside.
The limited absorption of acidic aqueous solution on the fabric, due to the protective action performed by the chlorinated solvent, leads consequently to a considerable reduction in the consumption of the processing acid.
Finally, the residual content of acid in the carbonized cloth is so small, as not to require any further steps of washing and removal of the acid from the cloth. This involves, besides the elimination of an additional step, a large water saving, and eliminates the related discharge of aciding polluting effluents.
|
A process and plant to carbonize vegetable impurities in woolen manufactured articles, which makes possible a better and uniform removal of the impurities to be obtained, with a considerable reduction in cost, at the same time avoiding wash water waste and environmental atmospheric pollution, by means of a reduced number of treatment steps.
| 3
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention generally relates to an electro-hydraulic device for actuating a control element of an internal combustion engine. More particularly, the present invention relates to a system and method for regulating a high-pressure hydraulic supply to electro-hydraulic engine valve actuators.
[0003] 2. Description of the Background Art
[0004] The internal combustion engine is well known and has garnered much attention since its creation. Because of its ubiquitous use, substantial efforts are constantly made to improve designs for the internal combustion engine and for its control systems. Of the many advancements made, independent valve actuation and electronic fuel injection were conceived to improve performance and efficiency over cam-based engines.
[0005] With independent valve actuation systems, the engine valves can come in contact with the engine pistons. This valve—piston collision can cause serious engine damage leading to engine failure. Therefore, valve actuation systems are contemplated that prevent such valve-piston collisions from occurring.
[0006] Piston-valve collision has been of particular concern for electro-hydraulic valve-trains on non-freewheeling engines, such as heavy-duty diesel engines. The current solution for solving this problem relies heavily on feedback control based upon valve lift measurements, which is neither reliable nor cost effective. For example, U.S. Pat. No. 6,092,495 describes a method of controlling electronically controlled valves to prevent interference between the valves and a piston. While the system can prevent piston-valve collision, it is flawed because a failure in the electrical control system could cause severe engine damages.
[0007] Thus, there is a need for new and improved systems and methods for valve control in a combustion engine that provide reliable piston-valve clearance.
SUMMARY OF THE INVENTION
[0008] According to one aspect of the present invention, a system and method are provided for regulating high-pressure hydraulic supply to an electro-hydraulic valve actuator. The present invention provides reliable piston-valve clearance.
[0009] Another aspect of the present invention is generally characterized in a valve actuation system for use in an internal combustion engine comprising at least one combustion cylinder having a piston and an engine valve. The valve actuation system includes a hydraulic pump, a high-pressure reservoir, and an electro-hydraulic valve actuator. The hydraulic pump is configured to produce a hydraulic output based on a valve-piston clearance profile of the cylinder of the combustion engine. The high-pressure reservoir is coupled with the hydraulic pump. The electro-hydraulic valve actuator is coupled with the high-pressure reservoir and configured to actuate at least one engine valve of the combustion engine according to an output of the hydraulic pump.
[0010] The above and other features and advantages of the present invention will be further understood from the following description of the preferred embodiments thereof, taken in conjunction with the accompanying drawings wherein like reference numerals are used throughout the various views to designate like parts.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a schematic diagram showing an embodiment of an electro-hydraulic valve actuation system for a combustion engine according to the present invention.
[0012] FIG. 2 is a graph of the piston-valve clearance characteristics of a computer simulation of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0013] An embodiment of an internal combustion engine 100 having an electro-hydraulic valve actuation system according to the present invention is shown in FIG. 1 . The engine 100 includes at least one piston-driven combustion cylinder (not shown) in communication with at least one engine control valve 106 (e.g., intake or exhaust valve), an electro-hydraulic actuator 102 for opening and closing valve 106 , and a hydraulic pump 104 . The hydraulic pump 104 may be a cam-driven pump and is fluidly connected to the electro-hydraulic valve actuator via a high-pressure reservoir 110 .
[0014] In the embodiment shown in FIG. 1 , hydraulic pump 104 includes a plunger 104 b that is driven by a cam 104 a . The geometry (i.e., shape) of the cam 104 a can be selected to drive the plunger 104 b as desired to charge the pressure of the fluid in the high-pressure reservoir 110 . Preferably, the geometry of the cam is selected based on the piston-valve clearance curve for the combustion cylinder, such that when the engine piston is moving close to the valve 106 , the high-pressure begins to drop; that is, the cam 104 a starts to move away from the plunger 104 b . For example, as shown in FIG. 1 , cam 104 a may have concave portions 104 a - 1 and 104 a - 2 corresponding to a crank angle of the engine when the engine piston moves close to the engine valve 106 , thereby allowing plunger 104 b to move toward cam 104 a when piston-valve clearance becomes small.
[0015] Electro-hydraulic actuator 102 includes control valves 102 a and 102 b , which are preferably electric solenoid valves, check valves 102 c and 102 f , control chamber 102 d , and a plunger 102 e . Control valves 102 a and 102 b can be opened and shut to control the direction of plunger 102 e to actuate the engine valve 106 , and can be controlled electronically, such as via an electronic control unit (ECU) or processor (not shown). Control valve 102 a (high-pressure control valve) allows high-pressure hydraulic fluid to travel into the control chamber 102 d , to force the plunger 102 e to travel away toward valve 106 . Hydraulic fluid may be allowed to return to the high-pressure reservoir 110 via check valve 108 one-way only. Opening control valve 102 b (low-pressure control valve) allows high-pressure fluid in the control chamber 102 d to travel to low-pressure, which may be connected to a low-pressure hydraulic fluid supply, such as a regulated low-pressure reservoir (not shown). Check valve 102 f allows hydraulic fluid to flow back to the control chamber 102 d , should the pressure in control chamber 102 d decrease below the pressure of the low pressure hydraulic fluid supply.
[0016] Check valve 102 c allows fluid to flow from the control chamber 102 d , one-way only, to the high-pressure reservoir 110 , when the pressure in the control chamber 102 d exceeds the pressure in the high-pressure reservoir 110 . Thus, even when control valve 102 b is closed, check valve 102 c creates a feedback loop—as the cam 104 b moves away from the plunger 104 a , the pressure in the high-pressure reservoir 110 begins to drop below the pressure in the control chamber 102 d , and check valve 102 c opens. Thus, piston-valve collision can be prevented reliably without reliance on electronic control systems.
[0017] A hydraulic accumulator 112 is in fluid connection to the high-pressure reservoir 110 . The accumulator 112 is able to store excessive hydraulic fluid when the high-pressure control valve 102 a is closed and yet plunger 104 a continues to pump fluid into reservoir 110 . The piston 112 a of the accumulator tends to respond to low-pressure fluctuation more than high frequency fluctuation. Here, the pressure drop due to the cam 104 a shape design as the engine piston moves close to the valve 106 is high frequency. Therefore, the accumulator 112 is preferably slow to react to this fluctuation, which allows the pressure to fluctuate to a significant level such that the check valve 102 c can open.
[0018] In operation, the cam-driven hydraulic pump 104 supplies high-pressure hydraulic fluid to the electro-hydraulic valve actuator 102 . The cam 104 a is preferably mechanically linked to the engine crankshaft (not shown) with a 2:1 ratio (i.e., the engine crankshaft rotates two revolutions while the cam 104 a rotates one revolution). The cam profile is preferably shaped to correspond to the piston-valve clearance profile, so that as the engine piston moves toward the engine valves and the instantaneous piston-valve clearance becomes smaller, the pump plunger 104 b moves toward the cam 104 a . As the plunger 104 b moves toward the cam 104 a , the hydraulic pressure in high-pressure reservoir 110 drops. As a result, check valve 102 c opens and high-pressure hydraulic fluid travels from control chamber 102 d to reservoir 110 , which allows the engine valve 106 to move away from the engine piston to avoid piston-valve collision even when control valve 102 b is still closed. Control valves 102 b is opened to allow hydraulic fluid to return to the low-pressure region. Control valves 102 a and 102 b are closed, and as the engine piston moves away from top-dead center position, the hydraulic pressure in the high-pressure reservoir 110 is built back up. Control valve 102 a is then opened to cycle engine valve 106 for the next combustion event.
[0019] Referring now to FIG. 2 , we assume that the low-pressure control valve 102 b has failed to open before the top dead center to avoid piston-valve collision. FIG. 2 shows a simulation of valve clearance and valve lift, versus timing of the cylinder. The top graph shows the control signal for the high-pressure control valve 102 a , the middle graph shows the control signal for the low-pressure control valve 102 b , and the bottom graph shows valve lift and clearance (piston-valve clearance profile). The bottom axis of each graph is the crank angle of the engine, which corresponds to the position of the piston.
[0020] In operation, high-pressure control valve 102 a is initially closed to allow high-pressure to build up in reservoir 110 . High-pressure control valve 102 a is opened, which causes plunger 102 e to actuate valve 106 to open. The initial valve lift is shown as approximately 12 mm and settles quickly at about 10 mm. As the engine piston approaches the valve 106 , the valve 106 begins to close (i.e., valve lift decreases). One can see that the piston-valve clearance becomes small as the piston approaches top-dead-center, but piston-valve collision is avoided even before the low-pressure control valve 102 b is opened.
[0021] As a result of the novel mechanical design of the present invention, piston-valve collision can be prevented even if there is a failure in the electronic control system.
[0022] While the invention has been described in detail above, the invention is not intended to be limited to the specific embodiments as described. It is evident that those skilled in the art may now make numerous uses and modifications of and departures from the specific embodiments described herein without departing from the inventive concept.
[0023] It will be appreciated that the present invention can be implemented in a number of types of internal combustion engines. The engine can have any number of cylinders.
|
A valve actuation system and method for use in an internal combustion engine including at least one combustion cylinder having a piston and an engine valve. The valve actuation system includes a hydraulic pump, a high-pressure reservoir, and an electro-hydraulic valve actuator. The hydraulic pump is configured to produce a hydraulic output based on a valve-piston clearance profile of at least one cylinder of the combustion engine. The high-pressure reservoir is coupled with the hydraulic pump. The electro-hydraulic valve actuator is coupled with the high-pressure reservoir via a first control valve and configured to actuate at least one engine valve of the combustion engine according to an output of the hydraulic pump.
| 5
|
BACKGROUND OF THE INVENTION
[0001] This invention relates to a vibration isolator assembly that generically refers to a device that absorbs vibrations and dampens relative movement between two structures, such as an isolator mount, bushing assembly, cradle mount assembly, etc.
[0002] A typical vibration isolator includes an external housing and an internal mounting shaft joined by an isolator such as a molded elastomer (e.g., rubber). The elastomer provides isolation between the housing and the mounting shaft. Typically, the elastomer is molded to the housing shaft in a high-temperature molding operation. This provides a desirable bond between the elastomer and the housing, as well as between the elastomer and the mounting shaft. After the molding operation, the elastomer experiences shrinkage as the part cools. Depending on the design, an undesirable effect of this shrinkage is to impart tensile stress to the elastomer. In such cases, fatigue performance of the vibration isolator assembly is generally improved by relieving the stress. One common way of relieving the stress is to pass the external housing through a funnel or reduced diameter opening to permanently reduce the diameter of the assembly. Such an arrangement is shown and described in the prior art representation of FIGS. 11-13 of U.S. Pat. No. 6,094,818, and is also well known to one skilled in the art.
[0003] Also, due to general poor fatigue performance of an elastomer under tensile loading, further enhancements to fatigue life may be realized by going beyond the simple relief of imparted tensile stresses and imparting compressive stress to the elastomer. Unfortunately, conventional methods for reducing the outer diameter of the isolator are limited in their effectiveness when there is a desire to impart compressive stress to the elastomer. This is due, for example, to negative effects on the bonding between the isolator and housing materials, i.e., the adhesive layer bonding between the isolator and housing, and isolator and the mounting shaft. There are also limits on the extent of deformation that the housing material can undergo.
[0004] It will also be appreciated that a substantial amount oftime and money are required to design, redesign, tool, and retool a product. The development cycle requires significant design and engineering time to be sure that the final product meets the final product specifications. If the specifications are altered during the development process, a need exists to remove, modify, and reinstall the assembly in a short time frame. With regard to producing manufactured mounting and vibration isolators for power trains, i.e., engines/transmissions in various consumer and commercial vehicles, as well as a development tool for engineering purposes that allows optimization and tuning of a power train mounting system for improved isolation and performance, a need exists to address tuning and durability issues. If such issues surface late in a program cycle, it is necessary to implement changes without a major redesign or a long retooling time, even though the basic characteristics of the isolator are being modified.
[0005] Thus a need exists to enhance the durability and tuning ability of a vibration isolator assembly. Means to relieve residual tensile stress, as well as vary the level of precompression of the elastomer portion, are desired. A need also exists to vary the travel limits of the elastomer portion. Lastly, there is a need to overcome these problems without major reworking of prototype or production tooling.
SUMMARY OF THE INVENTION
[0006] The present invention discloses a vibration isolator assembly having a housing and a shaft assembly interconnected by an isolator. The shaft assembly includes first and second mating components, the first component of which is connected to the elastomer. The first shaft component forms a cavity of a first dimension to receive the second component having a second dimension slightly greater than the first dimension for altering stress characteristics of the vibration isolator assembly.
[0007] In a preferred embodiment of the invention, the isolator is an elastomer, and the housing may be either metal or non-metal.
[0008] The second mention of the second component of the shaft assembly is pre-selected to relieve molded in tensile stress, or impart compressive stress to the isolator.
[0009] In one embodiment, the first component of the shaft assembly is a split member and the second component is received along the split plane.
[0010] The first and second components of the shaft assembly have a keyed contour relationship to selectively alter spring rate build-up characteristics
[0011] In one embodiment, the first component of the shaft assembly is comprised of first and second mirror portions and the second component is received between the portions.
[0012] A thin layer of elastomer is interposed between the first and second components of the shaft assembly.
[0013] The first and second components of the shaft assembly have an “I” contour relationship to selectively alter spring rate build-up characteristics.
[0014] A primary benefit of the invention resides in the ability to relieve molded in tensile stress and, if desired, impart compressive stress without affecting the housing or bonded layer between the housing and the elastomer material.
[0015] Another benefit of the invention resides in the ability to manipulate spring rate magnitude, rate ratios, rate build-up, and component fatigue characteristics of the vibration isolator assembly.
[0016] Still another benefit resides in reduced tooling costs and reduced lead times associated with different designs so that more options can be made available within the constraints of a fixed or predetermined development budget.
[0017] Still another benefit resides in the ability to manufacture the first components more economically at a lower tolerance of form by employing the layer of elastomer which is produced at precision tolerance through mold design to account for variation and permit easy assembly of the shaft assembly.
[0018] Yet another benefit is the ability to make changes to a design and tuning specifications without impacting a launch schedule of the product.
[0019] Still other benefits and advantages of the invention will become apparent to those skilled in the art upon reading and understanding the following detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] A more complete appreciation of the present invention and many of its advantages may be obtained by referring to the following detailed description in conjunction with the accompanying drawings.
[0021] [0021]FIG. 1 is a cross-sectional view illustrating a conventional vibration isolator assembly or suspension bushing.
[0022] [0022]FIG. 2 is an elevational view of an embodiment of the present invention.
[0023] [0023]FIG. 3 is a cross-sectional view taken generally along the lines 3 - 3 of FIG. 2.
[0024] [0024]FIG. 4 is a perspective view of a second component of the shaft assembly separated from the remainder of the vibration isolator assembly.
[0025] [0025]FIG. 5 illustrates a separation of a first component of the shaft assembly along a split plane for receipt of the second component.
[0026] [0026]FIG. 6 illustrates partial insertion of the second component into the remainder of the vibration isolator assembly.
[0027] [0027]FIG. 7 is a perspective view of the final assembly.
[0028] [0028]FIG. 8 is an elevational view of another embodiment of the present invention, namely, a cradle mount assembly.
[0029] [0029]FIG. 9 is a cross-sectional view taken generally along the lines 9 - 9 of FIG. 8.
[0030] [0030]FIG. 10 is an exploded perspective view of individual components of the assembly.
[0031] [0031]FIG. 11 illustrates a further step in the assembly of the vibration isolator assembly or cradle mount.
[0032] [0032]FIG. 12 shows enlarging the cavity of a first component of the shaft assembly.
[0033] [0033]FIG. 13 illustrates partial insertion of the second component of the shaft assembly.
[0034] [0034]FIG. 14 illustrates the completed assembly of the second embodiment.
[0035] [0035]FIG. 15 is a perspective view of the completed assembly of individual components of a third embodiment.
[0036] [0036]FIG. 16 is a perspective view of another embodiment of the housing, isolator and first component of a shaft assembly.
[0037] [0037]FIG. 17 is a perspective view of a second component of the shaft assembly of the third embodiment.
[0038] [0038]FIG. 18 is a perspective view of a fourth embodiment of the housing, isolator and a first component of the shaft assembly.
[0039] [0039]FIG. 19 is a perspective view of the first component of the shaft assembly.
[0040] [0040]FIG. 20 is a perspective view of the second component of the shaft assembly.
DETAILED DESCRIPTION OF THE INVENTION
[0041] By way of brief description, a conventional vibration isolator assembly A is shown in FIG. 1. The assembly includes a housing A and a shaft B that are interconnected by an isolator such as elastomer C. As noted above, the elastomer is typically mold bonded to the shaft and the housing and provides the vibration damping between the shaft secured to a first structure or component that moves relative to the housing which is secured to a second structure or component.
[0042] A first embodiment of the present invention is shown in FIGS. 2-7. Vibration isolator assembly 20 includes a housing 22 . Typically, the housing is a metal structure, although as will be appreciated in accordance with the present invention, alternative materials including non-metallic materials such as nylon can be used to form the housing. As illustrated in FIGS. 2 and 3, when used as a mount bushing, the housing typically adopts a generally cylindrical conformation, i.e., circular in cross section. Secured to an inner surface 24 of the housing is an isolator 30 . The isolator is often an elastomer or rubber construction because of the ability to isolate and reduce noise and vibration from being transmitted therethrough because of the elastic nature of the material. Rubber is generally an incompressible material that is displaced during loading and exhibits the desirable property that the more the rubber is compressed, the higher the stiffniess. This rate build-up controls noise, vibration, and harshness associated with, for example, the vehicle environment. The elastomer is preferably mold bonded to the inner surface 24 , although it will be appreciated that other bonding arrangements such as an adhesive bond, can be used without departing from the scope and intent of the present invention. Likewise, an inner diameter portion 34 of the isolator is secured to a shaft assembly 40 , which is preferably comprised of first and second components 42 , 44 . The isolator is secured to a first or outer surface 46 of the first component and again is illustrated as being mold bonded thereto. As will become more apparent below, the first component 42 in this embodiment is defined by first and second portions 42 a , 42 b that are separated and have outer surfaces 46 a , 46 b that are bonded to the isolator, respectively. Inner, facing surfaces 48 a , 48 b of the first component are separated along a split plane and slidably engage the second component 44 of the shaft assembly. As perhaps best illustrated in FIG. 2, and FIGS. 4-7, the first and second components 42 , 44 of the shaft assembly have mating, keyed configurations that provide for slidable insertion of the second component into a cavity defined along the split plane between the first and second portions 42 a , 42 b of the first component, and likewise resist relative movement between the first and second components in other directions. This mating, keyed configuration provides an interlocking feature that allows the separate components (here, three separate pieces) to merge and function as a single component. For example, as illustrated in FIG. 2, the first and second portions 42 a , 42 b of the first component have dove-tailed keyways 60 formed on opposite axial sides of central axis 62 . The keyways are dimensioned to receive mating, dovetailed keys or projections 64 that extend outwardly from the second component 44 of the shaft assembly. Thus, with continued reference to FIG. 2, and additional reference to FIGS. 4 and 5, it is seen that the first component 42 includes first and second mirror-image portions 42 a , 42 b having a central rounded portion 66 that merges into generally planar, outer radial portions 68 . The first and second portions 42 a , 42 b are separable or split along the plane 70 that passes through the longitudinal axis 62 . The second component is similarly contoured, having a central rounded portion 76 that merges into generally planar, outer radial portions 78 disposed on diametrically opposite sides of the rounded portion. As will be appreciated, although this contour has met with success, still other variations or contours may be used without departing from the scope and intent of the present invention.
[0043] As represented in FIG. 4, the mirror image portions 42 a , 42 b of the first component of the shaft assembly are integrally bonded to the isolator. The portions are separable along the facing, mating surfaces along split plane 70 . Thus, as shown in FIG. 4, the facing dovetailed key ways 60 define an outer radial cavity portion and the rounded portions 66 a , 66 b define a central cavity portion 80 . When the portions 42 a , 42 b are disposed in abutting relation as shown in FIG. 4, the cavities 80 defined by the keyways present a first dimension of the first component of the shaft assembly that is smaller than a second dimension provided by the preselected, mating contour of the second component. Thus, and as will be appreciated from a comparison of FIGS. 4 and 5, the first and second portions 42 a , 42 b of the first component of the shaft assembly are spread apart or separated along the split plane 70 to enlarge the cavity or opening 80 and allow selective sliding receipt of the second component 44 of the shaft assembly therein. This sliding receipt is represented in FIG. 6, where the second component is partially received into the first component of the shaft assembly. Ultimately, complete insertion of the second component into the first component is achieved and is represented in FIG. 7.
[0044] As noted in the Background discussion above, the isolator is typically an elastomer molded between the housing and shaft, here between the housing and the first component 42 of the shaft assembly. When it cures, the elastomer ends up with residual tensile stress. As noted, the prior art has addressed this in a different manner. Here, using a two-part shaft assembly alters the stress characteristics of the vibration isolator assembly. At a predetermined dimension of the second component 44 , the residual tensile stress in the elastomer is removed upon complete insertion of the second component into the first component. If the second component is made even larger, then a predetermined compressive stress is formed in the isolator/elastomer. All of this is achieved without affecting or adversely impacting on the bond between the housing and elastomer, and likewise between the elastomer and shaft assembly.
[0045] By varying the thickness of the second component, variable compressive stresses can be introduced into the elastomer. This has two basic effects. The first effect is associated with spring rate. The compressive rate characteristics of the main elastomer elements will increase in magnitude, roughly in proportion to the degree of precompression, while the shear rate characteristics of the same elastomer elements will remain relatively unaffected. This results in a change in the compressive-to-shear rate ratio of the final assembly.
[0046] The second effect deals with fatigue life. In general, an elastomer or rubber can tolerate increasing levels of compressive stress under cyclic loading much better than it tolerates smaller amounts of tensile stress. Thus, by introducing compressive stress via this method, fatigue life of the assembly can be enhanced. The forced separation of the molded split shaft assembly relieves the tensile stress resulting from part shrinkage, and imparts or introduces a desired compressive stress to the molded rubber, if desired.
[0047] It is also known in these isolation mount assemblies or bushing assemblies to incorporate one or more openings in the elastomer. Thus, as shown in FIGS. 2-7, the elastomer is radially continuous between the housing and the shaft assembly in one diametrical dimension (e.g., in the vertical direction as shown) and is discontinuous in another diametrical direction (e.g., in the horizontal direction as shown) through the inclusion of openings 90 , 92 . Here, the openings 90 , 92 are generally symmetrical in the vertical and horizontal directions, but need not necessarily be symmetrical or similarly shaped. Likewise, boundary rubber 94 , 96 (FIG. 2) define snubbing rubber extending inwardly from the housing in the horizontal direction. By selectively altering the width dimension of the second component of the shaft assembly, i.e., by extending the planar portions 78 radially outward, the gap between the shaft assembly and the boundary rubber is selectively altered. As the shaft assembly width is increased, the amount of travel that the shaft assembly proceeds through before contacting the boundary rubber on the housing will decrease. This transfers loading and stress more rapidly from the main central rubber elements to the exterior boundary or snubbing elements, and effectively alters the spring rate build-up characteristics. This has the effect of providing additional tuning options and improved fatigue durability.
[0048] The present invention is also useful in other vibration isolator assemblies such as the cradle mount shown in FIGS. 8-14. Since much of the structure and function is substantially identical, reference numerals with a primed suffix refer to like components (e.g., housing is referred to by reference numeral 22 ′), and new numerals identify new components. The primary distinction relates to the frame 100 of the vehicle in which the housing 22 ′ of the cradle mount assembly 20 ′ is also molded to the first component portions 42 a ′, 42 b ′ of the shaft assembly. The subassembly, i.e., housing 22 ′, is initially inserted into the frame 100 , namely opening 102 . Rather than encountering high insertion forces as is typical with conventional structures, smaller friction forces can be provided during insertion of the housing into the frame in accordance with the present invention. Thereafter, the first component portions of the shaft assembly are spread apart (FIG. 12) to accommodate the second component 44 ′. The second component is slidably received therein (FIG. 13), thus altering the stress characteristics of the isolator/elastomer, and also enhancing the abutting engagement force between the housing 22 ′ and the frame 100 .
[0049] The housing 22 ′ is preferably metal, but is should be noted that other composite or hard materials may be used. Likewise, the outer dimension of the housing can relate to any shape such as rectangular, square, circular, triangular, or any other shape or surface depending on the size and requirements needed for the end use. Similarly, the shaft assembly is shown as being located at or near the center point of the housing, although that could be varied. Likewise, although it is preferred to extrude the shaft assembly components from aluminum, occasionally other materials, e.g., cast, extruded, powdered metal, forgings, cold headed steel, or still other materials of construction may be used without departing from the scope and intent of the invention. The number and/or shape of the openings can also be varied, and the elastomer isolator that is bonded to the housing components may be secured thereto with any other type of bonding.
[0050] Similar to the aforementioned embodiments, two additional embodiments are shown in FIGS. 15-20. Since most of the structure and function is substantially identical, reference numerals with a double primed suffix (″) refer to like components (e.g., housing is referred to by reference numeral 22 ″), and new numerals identify new components in the additional embodiment of FIGS. 15-17. Likewise, reference numerals with a triple primed (″) suffix refer to like components (e.g., housing is identified by reference numeral 22 ′″) in the still additional embodiment of FIGS. 18-20, and new numerals identify new components. The primary distinctions relate to the first component and second component of the shaft assembly.
[0051] As shown in FIGS. 15-17, the first and second components 42 ″, 44 ″ of the shaft assembly have mating, keyed configurations that provide for slidable insertion of the second component into a cavity defined by the first component. This mating, keyed configuration provides an interlocking feature that allows the separate components to merge and function as a single component. Preferably, the first component has enlarged dove-tailed keyways 60 ″ formed on opposite axial sides of the central longitudinal axis 62 ″. The keyways are dimensioned to receive mating, dove-tailed keys or projections 64 ″ that extend outwardly from the second component 44 ″ of the shaft assembly. Thus, with continued reference to FIGS. 15-17, it is seen that the first component 42 ″ has a central, rounded (although no circular) portion 66 ″ that merges into generally planar, outer portions 68 ″. The second component is similarly contoured, having a central portion 76 ″ that merges into generally planar, outer portions 78 ″ disposed on diametrically opposite sides of the central portion.
[0052] The facing dovetailed key ways 60 ″ define an outer cavity portion and the non-rounded portions 66 ″ define a central cavity portion 80 ″. The cavities present a first dimension of the first component of the shaft assembly that is smaller than a second dimension provided by the preselected, mating contour of the second component and allow selective sliding receipt of the second component 44 ″ of the shaft assembly therein. Accordingly, as it relates to the first embodiment and specifically when compared with the enlarged dove-tailed projections 64 ″ and keyways 60 ″, this configuration reduces tolerance requirements for the dove-tail locking feature and simplifies assembly of the shaft assembly into the cavity portion.
[0053] As shown in FIGS. 18-20 and as will become more apparent below, the first component 42 ′″ in this embodiment is defined by first and second mirror portions 110 a , 110 b that are separated and have outer surfaces 114 a , 114 b that are bonded to the isolator 30 ′″, respectively. Inner facing surfaces 116 a , 116 b of the first component are separated by the isolator and slidably engage the second component 44 ′″ of the shaft assembly. The first and second components 42 ′″, 44 ′″ have mating configurations that provide for slidable insertion of the second component into a cavity 80 ′″ defined between the first and second portions 110 a , 10 b of the first component and the isolator 30 ′″, and likewise resist relative movement between the first and second components in other directions. This mating configuration provides an interlocking feature that allows the separate components to merge and function as a single component.
[0054] With reference to FIG. 20, it is seen that the second component 44 ′″ of the shaft assembly (sometimes referred to as the spreader component) has a general “I” or I-beam contour with keyed portions 118 a , 118 b extending from a central portion 119 . The first and second portions 110 a , 110 b of the first component have curved end portions 120 a , 120 b (FIG. 19) dimensioned to receive the “I” contour of the second component. The inner facing surfaces 116 a , 116 b of the first and second portions 110 a , 110 b of the first component 42 ′″ have a thin layer or skin 122 of elastomer bonded thereto (FIG. 18). The elastomer 122 bonded to the inner facing surfaces 116 a , 116 b of the first component permits the first component (sometimes referred to as a capture plate of half-shaft) to be manufactured more economically at a lower tolerance of form. The elastomer layer is produced at precision tolerances through mold design thereby taking up any variation in the dimensions of the first component and allowing consistent assembly of the first component and second component. As will be appreciated in accordance with the present embodiment, alternate materials can be used to form the elastomer layer or skin.
[0055] As represented in FIG. 20, the first and second portions 110 a , 110 b of the first component of the shaft assembly are integrally bonded to and separated by the isolator and define a central cavity portion 80 ′″. This cavity defines the first dimension of the first component of the shaft assembly that is smaller than a second dimension provided by the preselected, mating “I” contour of the second component. Thus, the first and second portions 110 a , 110 b of the first component 42 ′″ allow sliding receipt of the second component 44 ′″ of the shaft assembly therein.
[0056] Again, it will be appreciated that the third and fourth embodiments of FIGS. 15-20 use first and second components that are preferably extruded designs because of the ease of manufacture and assembly. The ability to use other shapes, designs, or contours that are not extruded or conducive to extruding should be recognized as being within the scope and intent of the present invention.
[0057] In summary, the manipulation of spring rate magnitude, rate ratios, rate build-up, and component fatigue characteristics is accomplished using a common molded isolator or elastomer and interchangeable shaft assemblies of different designs. This is important since higher tooling costs and longer lead times are typically associated with the isolator/elastomer, while the inserted shaft can be modified quickly and economically. The economical aspect of the vibration isolator assembly means that more options can also be made available within the constraints of a development budget. This highlights yet another feature of the invention wherein the ability to make changes to design and tuning specifications later in the program can be achieved without impacting the launch schedule of the product.
[0058] The invention has been described with reference to the different embodiments. Modifications and alterations will occur to others upon reading and understanding this specification. For example, various other manufacturing steps may be employed or in a different sequence. Likewise, different materials may be used or alternative processes without departing from the present invention. It is intended to include all such modifications and alterations in so far as they come within the scope of the appended claims or the equivalents thereof.
|
A vibration isolator assembly, such as an isolator bushing or cradle mount, includes a housing and an isolator connected to the housing. A shaft assembly includes first and second mating components, the first component being connected to the elastomer and having a cavity of a first dimension for receiving the second component having a different, second dimension therein. The differing dimensions alter the stress characteristics of the vibration isolator assembly. In the preferred arrangement, the shaft assembly includes a first component comprising first and second portions, a thin layer of elastomer interposed between the first and second components and a second component which is inserted between the portions to relieve tensile stress in the isolator and, if desired, to impart a compressive stress in the isolator. The thin layer of elastomer permits the first components to be made more economically. The first component of the shaft assembly is made at a lower dimensional tolerance and subsequently produced to a higher dimensional tolerance by molding the thin layer of elastomer to a precision tolerance.
| 5
|
CROSS REFERENCE TO RELATED APPLICATIONS
This application is the US National Stage of International Application No. PCT/EP2013/056546 filed Mar. 27, 2013, and claims the benefit thereof. The International Application claims the benefit of European Application No. EP12161657 filed Mar. 28, 2012. All of the applications are incorporated by reference herein in their entirety.
FIELD OF INVENTION
The invention relates to a steam turbine system in which the starting up of a steam turbine is improved. The invention furthermore relates to an associated method.
BACKGROUND OF INVENTION
When starting up steam turbines in thermal power stations, the mechanical power is initially limited, since the generator cannot be sufficiently synchronized and operated under load during the starting-up operation. The energy contained in the steam is therefore converted into mechanical work only in a smaller portion than in the normal power mode. This lower extraction of energy resorts in a reduced cooling of the steam as the steam passes through the steam turbine. Significantly higher temperatures than in the normal power mode therefore occur particularly in that region of the steam turbine in which the steam emerges, i.e. in the outgoing steam region. This is true particularly if the losses inside the steam turbine fall if, for example, the low pressure turbine is not in operation.
These higher temperatures necessitate a costly design to guard against said temperatures. In order to avoid the higher temperatures, the following measures have previously been proposed and realized. Firstly, what is referred to as trimming is known. In a system having a high pressure turbine, a medium pressure turbine and a low pressure turbine with resuperheating, the high temperatures occur predominantly in the high pressure outgoing steam and in the low pressure outgoing steam. In order to reduce the temperature in the low pressure outgoing steam, water is injected, i.e. water is additionally supplied to the steam. The temperature is therefore kept within permissible limits. The high pressure outgoing steam temperature is restricted by the mass flow through the high pressure section being increased. At the same time, the mass flow through the medium pressure section and the low pressure section is reduced. The increased pressure ratio in the high pressure section reduces the high pressure outgoing steam temperature. The reduced pressure ratio in the medium pressure section and low pressure section increases the ventilation power in the low pressure section and compensates for the increased power in the high pressure section.
If it does not suffice to reduce the temperature in the high pressure section to the desired extent, the outgoing steam chamber of the high pressure turbine is connected to the condenser by a starting-up line. A nonreturn valve to the cold resuperheating thereby closes and therefore there is no steam extraction point from the high pressure turbine into the resuperheating. The lower pressure level results in a lower high pressure outgoing steam temperature.
In a further approach to reducing the temperature, the mechanical power of the generator is increased. In more precise terms, the generator is intended to supply electrical power as early as in the starting-up mode, i.e. at low and continuously increasing rotational speeds, at which synchronization is not possible. This generated electrical power cannot be output to the mains because of the lack of synchronization. Electric heating elements are therefore provided for using the current generated. The heat generated in the heating elements can be connected into the preheating section of the water steam circuit and used for preheating the feed water.
SUMMARY OF INVENTION
It is an object of the invention to provide a steam turbine system and an associated method for starting up a steam turbine, with which the thermal problems during the starting-up operation can be overcome in a simple manner.
An object of the invention is achieved in particular by the independent patent claims. The dependent patent claims specify advantageous refinements.
In order to achieve an object of the invention, a steam turbine system having the following features is proposed: the steam turbine system has a steam turbine with an incoming steam side, an outgoing steam side, and a turbine housing. The turbine housing has a feed-through for a turbine shaft. A seal is present in said feed-through. The seal here is generally a labyrinth seal. The seal is intended to minimize a fluid flow, i.e. normally a steam flow, through the feed-through. A steam conducting system leads to the seal. The steam turbine is constructed from at least one first sub-section and at least one second sub-section, and a connecting line to a region of low pressure, in particular to a condenser of a thermal power plant, is present between the two sub-sections. The low pressure is understood here as meaning a pressure which is so significantly below the pressure of the steam turbine that, when the connecting line is opened, steam flows from the steam turbine into said region. It is generally appropriate for there to be a connecting line to the condenser. For the feed-through facing the outgoing steam side of the steam turbine, the steam conducting system is designed in such a way that a steam supply to the steam turbine through the steam conducting system is possible for starting up the steam turbine. A steam flow from the outgoing steam side to the connecting line to the region of low pressure can therefore take place for starting up the steam turbine. An incoming steam feed line has a shut-off which can be controlled in such a way that a steam flow from the incoming steam side to the connecting line to the region of low pressure is possible for starting up the steam turbine.
The incoming steam side is the side on which steam is supplied to the steam turbine in the normal power mode. In a high pressure turbine, it is the side on which the live steam coming from a steam generator (not described specifically here) is supplied. In a medium pressure turbine, it is the steam originating from resuperheating. The outgoing steam side is correspondingly the side on which the steam emerges from the steam turbine in the power mode. These terms will be kept to within the scope of this depiction even if, according to aspects of the invention, steam is specifically supplied on the outgoing steam side for the starting-up operation.
One aspect of the invention makes it possible to supply steam from the steam conducting system via the seal. Steam having a lower temperature than the temperature of the live steam or of the resuperheating steam can therefore be selected. The problem, which is explained at the beginning, of the high temperatures in the region in the vicinity of the outgoing steam side during the starting-up operation is therefore avoided. When the steam flows from the outgoing steam side to the connecting line to the region of lower pressure, mechanical work cannot be performed, since the steam flows counter to the direction customary in the power mode. No energy which is worth mentioning and which would lead to cooling of the steam is therefore extracted from the steam. On the contrary, the “ventilation” results in an increase of the temperature. The temperature therefore rises in the steam turbine from the outgoing steam side as far as the region between the turbine sections. A temperature profile which at least qualitatively corresponds to the temperature profile in the power mode is therefore set in the steam turbine.
The incoming steam feed line is normally a live steam line in the high pressure turbine, and normally a resuperheating steam line in the medium pressure turbine. The controllable valves in the incoming steam feed line generally involve a live steam valve or a resuperheating valve.
In one embodiment, the steam conducting system has an intermediate extraction line and/or a locking steam line and/or a water vapor line. During the operation of the steam turbine a significantly higher steam pressure prevails in the turbine housing than outside the turbine housing. The turbine shaft has to be able to rotate in the feed-through in as contact-free a manner as possible. Therefore, a seal providing a complete seal between the turbine shaft and the feed-through for the turbine shaft in the turbine housing cannot be used. A labyrinth seal is normally used as the seal. For this purpose, internals are provided in the feed-through on the turbine housing, said internals reaching for a distance into the feed-through, i.e. reducing the diameter of the feed-through at certain points. Surface-mounted components which increase the diameter of the turbine shaft at certain points are present on the turbine shaft. The internals and surface-mounted components are generally thin plates. The turbine shaft is arranged in such a manner that the surface-mounted components fastened to the turbine shaft project into the space between the internals. The turbine shaft can therefore rotate freely. The steam—in a greatly reduced quantity of steam because of the effect of the seal—flows through the feed-through, i.e. past the internals and the surface-mounted components, because of the higher steam pressure in the turbine housing than in the surroundings of the turbine housing. In the process, the steam pressure of the turbine housing drops in the direction of the surroundings. In order to minimize losses, the steam is extracted in the different regions of the seal and is used at another location in the thermal power station. In that region of the seal which is in the vicinity of the inner region of the turbine housing, there is an intermediate extraction line leading to the intermediate extraction system, in the case of a high pressure turbine. In the case of the medium pressure turbine, an intermediate extraction line is normally not present. Further on the outside, the locking steam is extracted via a locking steam line. The water vapor is extracted via the water vapor line in a region of the seal that is located far on the outside, i.e. in the direction of the region outside the turbine housing. Said steam conducting system can then also be used, according to an aspect of the invention, to supply steam on the outgoing steam side of the steam turbine, as set forth above.
The connecting line to the region of low pressure is preferably attached to, for example flange-mounted on, a steam extraction point. The steam extraction point is in any case located in that region of the steam turbine which is desired for the connecting line. It is therefore possible to avoid further internals directly on the steam turbine.
In one embodiment, there is an auxiliary steam line with which auxiliary steam can be supplied to the intermediate extraction line. Since the intermediate extraction line leads into an intermediate extraction system, normally for the outgoing steam of the low pressure turbine, there should be the possibility of separating the intermediate extraction line from the intermediate extraction system so that the auxiliary steam does not flow off into the intermediate extraction system, but rather is available for the steam supply via the seal.
In one embodiment, there are control devices in order, for the starting, to bring about the desired steam flow from the outgoing steam side to the connecting line to the region of low pressure and the desired steam flow from the incoming steam side to the connecting line to the region of low pressure. This generally includes the fact that valves, such as the live steam valve and the resuperheating steam valve, have to be correspondingly controllable in the incoming steam feed line and that there are corresponding control devices. Similarly, correspondingly controllable valves are required in the steam conducting system to the seal. Furthermore, the pressure should be ascertained at various locations in the steam turbine system in order to be able to determine the corresponding steam flows. By means of the apparatuses described, a substantially automated starting up of the steam turbine can be made possible.
An embodiment of the invention also relates to a thermal power plant comprising the steam turbine system described above. Such a thermal power plant can be started up in a simple manner and is therefore available for the increasingly required operation with a multiplicity of, and optionally rapid, power increases.
Another embodiment of invention also relates to a method for starting up a steam turbine. This particularly involves a method for starting up a steam turbine in a steam turbine system described above. In order to avoid repetition in the description, reference is substantially made to the descriptions regarding the steam turbine system, in which references are already contained to the corresponding method. The method for starting up the steam turbine has the following steps: first of all, the steam turbine is evacuated. A central region of the steam turbine is then connected to a region of low pressure, in particular to a condenser. Steam is then supplied via a seal, which seals off a turbine shaft from a turbine housing. Steam can therefore be supplied to the steam turbine on an outgoing steam side. Similarly, a metered supply of incoming steam on an incoming steam side of the steam turbine takes place in order to achieve a desired rotational speed and/or acceleration and/or power. During the abovementioned measures, it should be ensured that a desired steam flow flows at the same time from the outgoing steam side to the central region of the steam turbine. If, for example, too much steam were to be supplied, then an excessively high pressure would be set in the central region of the steam turbine despite the provided connecting line, and therefore the steam flow from the outgoing steam side to the central region would be undesirably reduced. In this case, either the incoming steam supply should be throttled and/or more steam should be supplied on the outgoing steam side via the seal. If a desired power of the steam turbine is reached, the supply of steam via the seal is ended and the central region of the steam turbine is separated from the region of low pressure. For this purpose, a valve in the connecting line to the region of low pressure is generally closed. The flow, which is customary in the power mode, through the steam turbine from the incoming steam side to the outgoing steam side is then produced. The rising pressure in the steam turbine also causes a nonreturn valve in a steam extraction point to open, and therefore, as is customary in the power mode of a thermal power plant, some of the turbine steam is used at a different location.
The steam turbine can be evacuated, as described above, by connecting the central region of the steam turbine to the region of low pressure. The steps of evacuating the steam turbine and connecting the central region of the steam turbine to the region of low pressure are therefore basically a single step.
In one refinement of the method, in particular if the method involves the starting up of a high pressure turbine, in order to supply steam via the seal, first of all an intermediate extraction line is separated from an intermediate extraction system, i.e. the connection to the outgoing steam of a medium pressure turbine is thus normally separated. Auxiliary steam is then supplied via the intermediate extraction line, and therefore the steam can flow into the seal and from there to the outgoing steam side of the steam turbine.
Alternatively, optionally also additionally, auxiliary steam is not supplied into the intermediate extraction line, but rather locking steam is supplied via a locking steam supply. In this case, the intermediate extraction line is likewise separated from the intermediate extraction system. Steam can also be supplied to the steam turbine on the outgoing steam side via the locking steam supply. For this purpose, normally the desired pressure is set in a locking steam chamber, and therefore steam flows through the locking steam line.
As already mentioned, live steam can be used as the incoming steam for a high pressure turbine. It has likewise already been explained that steam from resuperheating is preferably used as the incoming steam for a medium pressure turbine.
The connection of the central region of the steam turbine to the region of low pressure preferably takes place via a shut-off unit in a line which connects an extraction point to the condenser. There is therefore no need to provide a further line on the cramped steam turbine. It is possible to produce a connection to the condenser via the extraction point. By means of a shut-off unit, this connection can be opened when desired, as described, during the starting-up operation and can otherwise remain closed.
In a variant of the method for starting up a steam turbine, before the evacuation of the steam turbine, the entire steam turbine is subjected to a steam treatment with locking steam or with auxiliary steam supplied via the intermediate extraction line. A moderate first preheating can therefore take place. The subjection to steam treatment with auxiliary steam via the intermediate extraction means is generally possible only in the case of high pressure turbines.
In order to ensure the steam supply via the locking steam supply in a desired manner, a desired pressure can be set in the locking steam chamber. The desired steam flow takes place in this manner.
BRIEF DESCRIPTION OF THE DRAWINGS
Details of embodiments of the invention are described once again in detail with reference to the following figures, in which:
FIG. 1 shows the design of a high pressure turbine, in which auxiliary steam is supplied via the intermediate extraction line for the starting-up operation,
FIG. 2 shows the design of a high pressure turbine, in which locking steam is used for the starting-up operation,
FIG. 3 shows the design of a medium pressure turbine, in which locking steam is used for the starting-up operation.
DETAILED DESCRIPTION OF INVENTION
FIG. 1 illustrates a steam turbine 1 , wherein a high pressure turbine is involved here. The latter has a first turbine section 2 and a second turbine section 3 . A live steam line 4 , in which a live steam valve 5 is arranged, leads as an incoming steam feed line to the first turbine section 2 . Steam can therefore be supplied in a metered manner to an incoming steam side, or live steam side 6 , of the high pressure turbine 1 . An extraction point 8 is attached to a central region 7 of the high pressure turbine 1 , i.e. to the region between the first turbine section 2 and the second turbine section 3 . The extraction point 8 leads via a nonreturn valve 9 to a preheater (not illustrated). The nonreturn valve 9 prevents steam from flowing out of the preheater into the high pressure turbine 1 through the extraction point 8 . A connecting line 10 , frequently called starting-up line, is attached to the extraction point 8 . By means of a connecting valve 11 which is installed in the connecting line 10 , the connection to a condenser (not illustrated) is produced or separated as required. An outgoing steam side 12 is located in a region next to the second turbine section 3 . An outgoing steam line 13 leads from said outgoing steam side to an outgoing steam nonreturn valve 14 . A seal 15 which minimizes the steam flow from a turbine housing into the surroundings is connected to the outgoing steam side 12 of the high pressure turbine 1 on the side facing away from the turbine section 3 . An intermediate extraction line 16 leading into the seal 15 can be seen. The intermediate extraction line 16 can be shut off by an intermediate extraction valve 17 . Auxiliary steam can be supplied to the intermediate extraction line 16 via an auxiliary steam line 18 . In addition to the intermediate extraction line 16 , first of all a locking steam line 19 and, further on the outside, a water vapor line 20 , through which locking steam or water vapor can emerge, are connected to the seal 15 . It is pointed out for the sake of completeness that there is a further seal 15 ′ on the live steam side 6 of the high pressure turbine 1 . An intermediate extraction line 16 ′, a locking steam line 19 ′ and a water vapor line 20 ′ are also arranged there.
In order to start up the high pressure turbine 1 , the following procedure should be selected: first of all, the intermediate extraction valve 17 should be closed in order to subject the system to a steam treatment. The high pressure turbine 1 with the first turbine section 2 and the second turbine section 3 is then subjected to a steam treatment with auxiliary steam which is introduced into the intermediate extraction line 16 via the auxiliary steam line 18 . Also via the intermediate extraction line 16 ′, steam flows to the high pressure turbine 1 via the seal 15 ′. A first preheating of the high pressure turbine 1 therefore takes place. The connecting valve 11 in the connecting line 10 is then opened. The high pressure turbine 1 with the first turbine section 2 and the second turbine section 3 is therefore evacuated. Steam can therefore flow from the central region 7 of the high pressure turbine 1 via the extraction point 8 into the connecting line 10 to the condenser. A desired amount of auxiliary steam is then supplied at a certain pressure via the auxiliary steam line 18 in order to achieve a desired pressure ratio between the outgoing steam side 12 and the central region 7 of the high pressure turbine 1 . This results in a steam flow, which is illustrated by the arrow, through the second turbine section 3 from the outgoing steam side 12 to the central region 7 . By means of a metered opening of the live steam valve 5 , the desired quantity of steam flows to the live steam side 6 via the live steam line 4 . Furthermore, a desired steam flow through the first turbine section 2 , as illustrated by the arrow, then occurs between the live steam side 6 and the central region 7 . The steam flow through the first turbine section 2 and the steam flow through the second turbine section 3 combine in the central region 7 and then flow together into the extraction point 8 and from there via the connecting line 10 to the condenser. The desired rotational speed and/or acceleration and/or power in the first turbine section 2 can be set via the opening of the live steam valve 5 . It is therefore also possible for the pressure ratio between the outgoing steam side 12 and the central region 7 to obtain the desired value. The desired steam flow through the second turbine section 3 is therefore ensured. As soon as the minimum power is reached in the first turbine section 2 , the auxiliary steam supply via the auxiliary steam line 18 is ended. The intermediate extraction valve 17 is opened. The connecting valve 11 in the connecting line 10 is closed. The pressure in the high pressure turbine 1 therefore increases. This furthermore leads to the nonreturn valve 9 to the resuperheating opening automatically because of the pressure. The normal power mode, in which live steam is supplied on the live steam side 6 by the live steam line 4 , is therefore initiated. The steam then flows through the first turbine section 2 and the second turbine section 3 to the outgoing steam side 12 and further through the outgoing steam line 13 via the then open outgoing steam nonreturn valve 14 . Some of the steam is extracted from the central region 7 via the extraction point 8 and flows via the open nonreturn valve 9 to the preheater (not illustrated). It should be explained in addition that some steam escapes in the locking steam lines 19 , 19 ′ and the water vapor lines 20 , 20 ′ during the starting-up operation, since a higher pressure is provided via the intermediate extraction lines 16 , 16 ′.
A further possibility for starting up the high pressure turbine 1 is now illustrated. For this purpose, increased locking steam pressure is used. As can be seen, the design of FIG. 2 virtually corresponds to that of FIG. 1 . Identical features are not explained again in order to avoid repetitions. The sole difference is that there is no auxiliary steam line 18 for the supply of the intermediate extraction line 16 and that the steam flow in the locking steam lines 19 , 19 ′ has a different direction during the starting-up operation. The method for starting up the high pressure turbine 21 is also relatively similar. At the beginning, the intermediate extraction valve 17 should also be closed. The turbine sections 2 and 3 are then subjected to a steam treatment via the locking steam lines 19 and 19 ′. All of the remaining steps and procedures are identical. Admittedly, in order to set the pressure on the outgoing steam side 12 , it is not the auxiliary steam supply 18 , but rather correspondingly the pressure in a locking steam supply which is to be set. For this purpose, the pressure in a locking steam chamber (not illustrated) is correspondingly selected. The starting up of a medium pressure turbine is illustrated below with reference to FIG. 3 . A medium pressure turbine 21 can be seen in FIG. 3 . It has a first turbine section 22 and a second turbine section 23 . Steam originating from resuperheating is introduced into the medium pressure turbine 21 through a resuperheating steam line 24 serving as the incoming steam feed line. In order to regulate the steam flow, a resuperheating valve 25 installed in the resuperheating steam line 24 serves as a controllable shut-off. In the power mode, the steam flows to an incoming steam side 26 , which can also be called the resuperheating steam side here. In the power mode, pressure is removed through the first turbine section 22 and subsequently through the second turbine section 23 . A central region 27 of the medium pressure turbine 21 is located between the turbine sections 22 and 23 . An extraction point 28 leads through a nonreturn valve 29 to a second preheater (not illustrated). The nonreturn valve 29 prevents flow back from the preheater through the extraction point 28 into the medium pressure turbine 21 at too low a pressure in the medium pressure turbine 21 . A connecting line 30 , also called starting-up line, leads from the extraction point 28 to the condenser. In the connecting line 30 there is a connecting valve 31 with which the connecting line 30 can be connected to, and separated from, the condenser. In the normal power mode, the steam flows from an outgoing steam side 32 of the medium pressure turbine into an outgoing steam line 33 and through an outgoing steam nonreturn valve 34 to a second resuperheating. A region of a seal 35 is connected to the outgoing steam side 32 of the medium pressure turbine 21 . An intermediate extraction line is not connected to the seal 35 because of the lower pressure in the medium pressure turbine 21 in comparison to the high pressure turbine 1 . As in the high pressure turbine 1 , a locking steam line 39 and a water vapor line 40 are also connected to the seal 35 in the case of the medium pressure turbine 21 .
In order to start up the medium pressure turbine 21 , the procedure is then as follows: first of all, the medium pressure turbine 21 with the first turbine section 22 and the second turbine section 23 is subjected to a steam treatment with blocking steam which originates from the line 39 . An evacuation then takes place by opening of the connecting valve 31 in the connecting line 30 to the condenser. By setting a desired pressure in the locking steam chamber, a desired pressure ratio between the outgoing steam side 32 and the central region 27 of the medium pressure turbine 21 is produced. A desired steam flow is therefore initiated. In a similar manner as when starting up the high pressure turbine 1 , the resuperheating valve 25 is easily opened, and therefore steam flows through the resuperheating steam line 24 from the first resuperheating (not illustrated) into the incoming steam side 26 . The steam flows from there through the first turbine section 22 to the central region 27 . The resuperheating valve 25 is opened in such a manner that a desired rotational speed and/or acceleration and/or power of the medium pressure turbine 21 , more precisely the first turbine section 22 , is achieved. When a minimum power is achieved, the connecting line 30 is separated from the condenser by the connecting valve 31 being closed. The pressure in the medium pressure turbine 21 therefore rises rapidly. As a result, the nonreturn valve 34 opens. The flow passes correctly through the first turbine section 22 and the second turbine section 23 of the medium pressure turbine 21 with limited ventilation. The two turbine sections 22 and 23 are also referred to as drums 22 and 23 .
For the sake of completeness, it is also indicated that a seal 35 ′ is connected to the incoming steam side 26 ′. Said seal seals off the turbine housing from the turbine shaft on the incoming steam side 26 . Accordingly, a locking steam line 39 ′ and a water vapor line 40 ′ can also be seen here. At the beginning of the above-described starting up of the medium pressure turbine 21 , steam also flows correspondingly through the locking steam line 39 ′ to the medium pressure turbine 21 ′. As soon as steam flows via the resuperheating steam line 24 to the incoming steam side 26 and therefore the pressure rises there, the steam flow flowing through the seal 35 ′ via the locking steam line 39 ′ to the incoming steam side 26 is certainly very low or equal to zero.
Although embodiments of the invention have been illustrated and described in more detail by an exemplary embodiment, the invention is not restricted by the examples disclosed and other variations can be derived therefrom by a person skilled in the art without departing from the scope of protection of the invention.
|
A steam turbine system including a steam turbine is provided, the steam turbine having an incoming and an outgoing steam side, and a turbine housing with a feed-through for a turbine shaft with a seal, whereby a fluid flow through the feed-through can be minimized, and a steam conducting system to the seal is present. The steam turbine includes a first sub-section a second sub-section, and a connecting line to a region of low pressure between two sub-sections. A steam supply through the steam conducting system is possible for starting up the steam turbine such that a steam flow from the outgoing steam side to the connecting line to the region of low pressure is possible, an incoming steam feed line has a shut-off that can be controlled such that a steam flow from the incoming steam side to the connecting line to the region of low pressure.
| 5
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The instant invention relates to improvements on a telephone headset which enables the user to comfortably maintain a telephone in a talking position, while allowing the hands to be free for other activities.
2. Brief Description of the Prior Art
Numerous patents have ben issued which relate to a device for enabling the user to comfortably maintain the telephone in a talking position while allowing the hands to be free for other activities. Nevertheless, devices similar to that of the instant invention have not achieved commercial success.
U.S. Pat. No. 2,481,387 (1949) provides a headset gear with a circular brace hooking onto the telephone earpiece thereby holding the telephone in a position applicable for talking. The disadvantage of this device however, is that the connection between the circular brace holding the telephone receiver and the headband which extends over the user's head is connected by a pivot device. The pivot device would be expected to work effectively with a metal apparatus, however, the use of metal would contribute to the weight of the headset and would be expected to render the device uncomfortable to use. If made from lightweight plastic, the system would appear to be difficult to install without breaking the plastic or preventing breakage during use. An additional drawback of the holder is noted in regard to the curved headband pivotly attached to the holder and adapted to be moved aside by hand. The headband is adapted to pivot outwardly so that it may be readily supported upon the head of the user with the ear portion of the telephone receiver directly overlying the user's ear. However, when the headband is swung back over the telephone receiver handset, it provides for unattractive and awkward storage. In the event of home use, there may not be room on a wall telephone for the storage of the headband and in office use it would give an excessively unattractive appearance to the telephone. It would also be excessively easy to knock the telephone off the telephone body, therefore raising the possibility of putting the telephone out of use.
U.S. Pat. No. 2,721,234 (1955) is another headset device similar to that previously described in U.S. Pat. No. 2,481,387, except that it adds to the standard headband type apparatus, a complicated telephone locking device at one end which locks onto the ring attached to the earpiece of the telephone. The locking device consists of numerous parts and would be complicated and expensive to manufacture. In addition, the headset must remain on the telephone, therefore causing an awkward storage problem. If the headset is removed it would appear to take considerable time to reestablish the position necessary for comfortable use and thus would not be a quick, convenient to use telephone headband apparatus.
U.S. Pat. No. 3,225,147 (1965) is similar to the embodiment of the previously discussed patent. Once again there is a headset which goes over the user's head and an attachment that attaches itself to the earpiece of the telephone. In the patent, there is provided a device which swings the headband back along side the telephone receiver hand piece and which allows for more convenient storage than the previously discussed patents. Again, however, the attachment system of the patent is a complicated one requiring the use of metal parts. The telephone receiver can be removed from the headband, however, the connection pieces are in a nut and bolt type apparatus and would involve time consuming, repeated removal in addition to a potential loss of parts.
SUMMARY OF THE INVENTION
In the instant invention the foregoing complications are overcome and a simple, convenient, easy to manufacture telephone headset head support device is produced. The head support device includes a headband member contoured to conform to the user's head, and a handset attachment member. The headband and the handset attachment member have cooperating interlocking components which releaseably interconnect the two members. The interlocking components can be a hook device on one member and a hook receiving opening in the other member.
A BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a perspective view of an embodiment of the invention;
FIG. 2 is a perspective view of a headband member;
FIG. 3 is a perspective view of a telephone attachment member;
FIG. 4 is a fragmentary perspective view of another embodiment of a headset;
FIG. 5 is a side view of the optional earpiece cup for use with the embodiment of FIG. 4;
FIG. 6 is a side view of the telephone set with the attachment device installed;
FIG. 7 is a perspective view of an alternate embodiment of the invention;
FIG. 8 is a perspective view of the modification of FIG. 7, in combination with a telephone headset;
FIG. 9 is a perspective view of a further embodiment of the invention;
FIG. 10 is a side view of the embodiment of FIG. 9;
FIG. 11 is a side view of a still further embodiment of the invention; and,
FIG. 12 is a perspective view of the modification of FIG. 11, shown in use.
DETAILED DESCRIPTION
The instant invention overcomes the difficulties of the prior U.S. Pat. Nos. 3,225,147 and 2,721,234 through the use of a construction which is of a simple two piece molded type assembly. Each part can be manufactured using simple, well known, molding operations. The production costs would be extremely low thus rendering the device suitable to mass market sales. The device eliminates the need for pivotal arrangements and is not prone to breakage either in manufacture or in use.
In the embodiment, as illustrated in FIG. 1, a headset 10 is shown with the slip body 19 inserted into the flange 14 as would be the case when the headset is fully set up. The supportive headband 12 is preferably formed of plastic, however, other materials can be used provided they are lightweight and inexpensive. The supportive headband 12 is placed over the head of the user in a comfortable position. The flange 14 portion is situated at one end of the supportive headband 12 and is molded as a unitary part of the supportive headband 12. This one piece molding operation is a primary advantage of the instant invention in that it allows for low cost and rapid, automatic manufacture.
The second component part of the invention, as shown in FIG. 1, is the handset attachment member 15. The slip shoulder 18 of the handset attachment member 15 is as wide or wider than the flange 14 members. Extending downward from the slip shoulder 18 is the slip body 19, the upper portion which is molded in a size to fit snugly between the flange 14; a friction fit being preferable. The bottom section 19A of the slip body 19 is molded in a size small enough to fit between the outer portion of the edges 14A of flange 14.
The length L of the bottom section must be long enough to permit the bottom section 19A to fit between the flange edges 14A, and thus must be somewhat longer than the distance L. The collar 16 extends downward from the lower portion of the slip body 19. The interior portion of the collar 16 is molded in a size to fit the inner section, of the handset of a telephone when the outer unscrewable section of the earpiece is removed. The outer dimension of the collar 16 is molded in a size to be flush or near flush to the outer portion of the telephone earpiece. The thickness of the collar 16 must be of a small enough size as to allow the earpiece to be re-screwed securely to the telephone handset.
The supportive headset 20 of FIG. 2 is shown separated from the handset attachment member 30 and shows the individual pieces. The supportive headband 20 is shown with its curvature which fits over the head of the user. For consumer appeal the supportive headset 20 can be manufactured in various sizes to facilitate comfortable fittings. The flanges 22a and 22b are clearly shown extended outward a short distance from either side of one end of the supportive headband 20. The flanges 22a and 22b form a semicircle, which curves a sufficient amount to hold the upper portion of the slip body 34 in place. The curvature of the flanges 22a and 22b must not be curved to the extent in which to inhibit the fit of the lower portion of slip body 34 to fit therebetween. The flanges 22a and 22b are not restricted to the curvature formation as shown in the instant drawings but rather can take various shapes. The supportive headband 20 is shown as being a one piece molded part, preferably of lightweight, durable plastic. The slip shoulder 32 of the handset attachment member 30 is shown extending outward from the slip body 34.
In the preferred embodiment of the slip shoulder 32 the width is equal to that of the distance between the outer edges of the flanges 22a and 22b. This does not, however, put a restriction on the length, except that the slip shoulder 32 must not be narrower than the interior distance between the flanges 22a and 22b. The overlap of the slip shoulder 32 on to the top edges of the flanges 22a and 22b is important in that it prevents the headset attachment member 30 from slipping down through the flanges 22a and 22b. The upper portion of the slip body 34 extends downward from the slip shoulder 32. Although the thickness of the slip body 34 is equal to that of the slip shoulder, which in turn must be same or slightly greater than the distance between the interior of the outer sections of the flanges 22a and 22b and the supportive headband 20, to provide a friction fit. The width "W" of the upper portion of the slip body 34 should be the same or slightly less than the width "W-F" between the interior of flanges 22a and 22b. The width "W" can be dimensioned with respect to width "W-F" so as to provide a friction fit between the flanges 22a and 22b. The lower portion 35 of the slip body 34 extends downward from the upper portion of the slip body 34. The thickness of the lower portion and the upper portion are the same, however, the lower portion 35 of the slip body 34 is narrowwer than that of the upper portion of the slip body 34. The sides of the lower portion 35 form right angles with the bottom edge of the upper portion of the slip body 34. The width of the lower portion of the slip body 34 must be narrower than the distance between the outer curvature of the flanges 22a and 22b in order to facilitate the insertion of the headset attachment member 30 between the flanges 22a and 22b.
Extending downward from said lower portion of the slip body 34 is the collar 36. The collar 36 employs the dimensions as heretofor described in respect to FIG. 1. FIG. 3 shows an additional embodiment of the invention, wherein a lug 38 is incorporated. The lug 38 extends downward from the bottom section of the collar 36 and curves outwardly in the opposite direction from that of the supportive headband 20. The lug 38 serves to further support the telephone in a manner as to position the mouthpiece close to the mouth of the user.
FIG. 4 shows an additional embodiment of th instant invention. The headset 40 is shown the same as described in FIG. 2 with the addition of a second flange 43 and 43b and identical to the first flange 42a and 42b. The second flange 43a and 43b is positioned directly opposite the first flange 42a and 42b at the end of the supportive headband 42. The flange 43a and 43b supports the ear cup attachment member 50 as shown in FIG. 5. The attachment section, the slip shoulder 52 and slip body 54 are the same as described in FIG. 3, however instead of the collar 36 an ear cup 56 is used. The ear cup 56 can be a simple curved plastic cup and an extension of the one cast mold. The invention is not however limited to this and any type of conventional ear cup may be used.
FIG. 6 shows a side view of the headset attachment member 60 as it would be seen attached to a telephone handset 65 ready for use.
FIG. 7 shows an additional embodiment of the instant invention. Headset 70 is shown, as per the previous embodiments, with an additional system for the attachment of the headset attachment member 80. An interlock slot 74 is provided in one end of the supportive headband 72, the interlock slot 74 being narrower in width than that of the supportive headband 72. The headset attachment member 80 is provided, at the top end, with an interlock tongue 76 which is slightly smaller in width than the interlock slot 74, forming a snug fit, preferably a friction fit. Directly below the interlock tongue 76 is the interlock brace 77 which extends outward at a right angle to the interlock tongue 76 in the opposite direction of the supportive headband 72. The interlock brace 77 must have a length at least equal to the width of the supportive headband 72. Extending downward from the interlock brace 77, at a right angle thereto, and parallel to the interlock tongue 76, is the interlock body 78. The collar 79 is positioned as in the previous embodiments.
FIG. 8 shows the headset attachment member 80 in an interlock position with the supportive headband 82. The interlock tongue 86 is inserted into the interlock slot 84, preventing the headset attachment member 80 from tilting in a directon away from the user's mouth. The interlock brace 87 rests on the interlock slot 84, preventing slippage downward. The interlock body 88 rests on the inside of the supportive headband 82, also preventing the headset attachment member 80 from tilting away from the user's face. The rectangular shape of the interlock pieces prevents any side-to-side slippage of the telephone.
A further modification shown in FIG. 9 wherein the headset 90 is seen to include a supportive headband 92 having a hooked portion 94 at one end. An "s" or "Z" shaped section 96 located between the headband 92 and the hooked portion 94 permits the lower end of the supportive headband 92 to be spaced away from the head of the user and thus permit proper relationship between the telephone handset and the ear of the user. A telephone attachment member 98 includes a collar section 100 having a telephone receiving opening 102. An elongated portion 104 includes an opening 106. The dimension D of the opening 106 must be at least equal to the dimension H of the hooked member so as to permit the hooked member to pass through the opening. In use as is shown in FIG. 10, the opening 106 of the telephone attachment member 98 is slipped over the hooked portion 94 of the supportive headband 92, either manually, or due to the weight of the telephone, the telephone attachment member 98 will ride downward with respect to the supportive headband 92 so that the hooked member 94 engages in the upper section 108 of the telephone attachment member 98. It is thus seen that the telephone attachment member 98 and supportive headband 92 can lock together. In use, the telephone attachment member will tend to rotate in the direction of arrow 110, while the supportive headband will tend to rotate in the direction illustrated by arrow 112. Reliance must be made upon the hook and opening assembly to prevent this rotation. It is thus seen that the engagement between the upper end 108 of the telephone attachment member and the lower section 114 of the supportive headband will prevent the aforesaid rotation in cooperation with the action of the hooked member 94.
The modification of FIGS. 9 and 10 is noted to be of extreme value from a manufacturing standpoint in that extremely simple molding configurations are obtained. It should be readily apparent that telephone attachment member 98 can be made using a conventional two piece mold since the member is totally free of undercut or any other configurations which interfere with molding operations. Supportive headband member 92 similarly can be made in a conventional two piece mold thus permitting extremely low cost manufacture. This modification is for these reasons, preferred once the prior modifications for manufacture reasons.
The modification as shown in FIG. 11 is like that shown in FIGS. 9 and 10 with the exception of the hooked member 122. The hooked member 122 is formed with a lip curving outwardly from the headset member 121. The width I of the hooked member 122 must be slightly less than the width J of the telephone attachment member 123. The telephone attachment member 123 is formed as outlined in FIGS. 9 and 10. The telephone attachment member 123 is attached to the headset 121 by slipping the hooked member 122 through the provided opening, as illustrated in FIG. 9, the telephone attachment member being in a position in which the upper portion is parallel with the s or z shaped section 124. The telephone attachment member 123 is then snapped downward resting in the position ready for use, as described in the prior embodiments. The telephone attachment member is held in place by the pressure exerted on it by the differences in width between I and J.
This embodiment again provides for easy manufacturing with the two piece mold system.
FIG. 12 shows the telephone headset 130 in use. For clarity, FIG. 12 is shown in a combination of two planes. The headset 130 is shown as a front view, while the telephone attachment member 132 and telephone 134 is shown on a plane with a 45° angle to that of the headset 130.
|
The telephone handset supporting assembly employs a standard telephone headband which goes over the user's head in a fashion as to be secure, yet comfortable. The headband can be molded as a one piece plastic element. On one side of the headband is a simple interlocking device by which a second part of the assembly can be coupled to the headband. The second part of the assembly is secured to the telephone earpiece and is a lightweight, durable, one piece molded plastic component. The earpiece attachment member is attached to the telephone by unscrewing the telephone earpiece and inserting the earpiece section between the handle portion of the telephone handset and the removeable earpiece. The plastic earpiece attachment member is made of a dimension which will in no way interfere with or damage the telephone, or in any way interact with or interfere with any electronic components of the telephone.
| 7
|
FIELD OF THE INVENTION AND RELATED ART
[0001] The present invention relates to a belt driving apparatus which is mountable in an image forming apparatus such as an electrophotographic copy machine, an electrophotographic printer, etc., to drive multiple (two) belts which are in contact with each other. It also relates to an image forming apparatus in which the above-described belt driving apparatus is mountable.
[0002] There are various belt driving apparatuses which drive multiple (two) belts. One of such belt driving apparatuses is a fixing apparatus which is mounted in an image forming apparatus, such as an electrophotographic copy machine and an electrophotographic printer. More specifically, it is a fixing apparatus of the so-called belt-nip type. A fixing apparatus of this type has an endless heating belt and an endless pressing belt. The endless pressing belt (which hereafter may be referred to simply as pressure belt) is placed in contact with the heating belt (which hereafter may be referred to simply as fixation belt) to form a nip (Japanese Laid-open Patent Application 2007-079034). In operation, a sheet of recording medium which is bearing an unfixed toner image is conveyed through the nip while remaining pinched between the heating belt and pressing belt, whereby the unfixed toner image on the sheet of recording medium is thermally fixed to the sheet of recording medium. For size reduction and cost reduction, some fixing apparatuses of the belt-nip type are provided with only two (minimum number) rollers per belt. In other words, they are reduced in overall thermal capacity by using only two (minimum number) rollers per belt to minimize the length of time necessary for them to reach a temperature range in which they can properly fix a toner image.
[0003] There are serious technical issues regarding fixing apparatuses of the belt-nip type, that is, fixing apparatuses which use an endless fixing belt and/or an endless pressing belt. One of these technical issues is how to prevent the belts of a fixing apparatus of the belt-nip type from shifting (snaking) in a specific direction. More specifically, if the belts shift in the direction perpendicular to their moving direction while they are driven, problems result sometimes such that the belts move out of their preset range, and/or that the belts become damaged across their edge or edges. There are various methods for preventing an endless belt from excessively shifting in the direction perpendicular to its moving direction. One of these methods is to change in attitude one of the two rollers around which the endless belt is wrapped, in such a manner that one of the lengthwise ends of this roller is changed in position to cause the belt to remain in its preset positional range (Japanese Laid-open Patent Application H04-104180).
[0004] As described above, one of the methods for preventing the fixating belt and pressing belt of a fixing apparatus of the belt-nip type from excessively shifting in a specific direction is to structure the fixing apparatus so that the belt supporting rollers can be changed in attitude. However, if a fixing apparatus of the belt-nip type is structured so that its fixing belt and pressing belt can be changed in attitude by changing the upstream roller for the fixing belt, in terms of recording medium conveyance direction, and the upstream roller for the pressing belt, to change in position one of the lengthwise ends of the upstream roller for the fixing belt, and the corresponding lengthwise end of the upstream roller for the pressing belt, it is possible that when a sheet of recording medium is conveyed through the fixing apparatus by the belts, it will become unstable in attitude and behavior. The cause of this problem is that in a case of a fixing apparatus of the belt-nip type structured as described above, when the upstream fixation belt roller and upstream pressure belt roller are changed in attitude so that one of the lengthwise end of the upstream fixation belt roller and the corresponding lengthwise end of the upstream pressure belt roller come closer to each other, and when the upstream fixation belt roller and upstream pressure belt roller are changed in attitude so that one of the lengthwise end of the upstream fixation belt roller and the corresponding lengthwise end of the upstream pressure belt roller move away from each other, the amount by which the lengthwise ends are moved is rather large, and therefore, the amount by which the upstream fixation belt and upstream pressure belt are moved in the direction parallel to the lengthwise direction of the rollers to be corrected in their position is rather large, making it difficult for recording medium to remain stable in attitude and behavior while it is conveyed through the belt-nip. Therefore, in order to ensure that recording medium remains stable in attitude and behavior while it is conveyed through a fixing apparatus of the belt-nip type, it is desired to reduce the amount by which the distance between one end of the lengthwise ends of the upstream roller for the fixation belt, and the corresponding lengthwise end of the upstream roller for the pressure belt, that is, the distance between the fixation belt and pressure belt, on the upstream end of the fixing apparatus.
[0005] Not only does this problem occur to the fixation belt and pressure belt, but also, to any belt driving apparatus which has two (multiple) belts (which are in contact with each other), and is structured so that the two belts are prevented from excessively shifting in the direction perpendicular to their moving direction.
SUMMARY OF THE INVENTION
[0006] The primary object of the present invention is to provide a belt driving apparatus which is significantly smaller in the amount by which the distance between its first and second belts, on the recording medium entrance side of the apparatus, changes, and therefore, is significantly more stable in terms of recording medium conveyance than any of conventional belt driving apparatuses, and also, an image forming apparatus employing such a belt driving apparatus.
[0007] According to an aspect of the present invention, there is provided a belt driving apparatus comprising a first rotatable belt member; a first supporting member rotatably supporting said first belt member; a first steering roller, rotatably supporting said first belt member, for adjusting a position, with respect to a widthwise direction perpendicular to a rotational direction, of said first belt member, wherein one end of said first steering roller is fixed, and the other end thereof is movable; control means for controlling movement of the other end of said first steering roller; a second rotatable belt member contacted to said first belt member; a second supporting member rotatably supporting said second belt member; a second steering roller, rotatably supporting said second belt member, for adjusting a position, with respect to the widthwise direction, of said second belt member, wherein an end of said second steering roller remote from said one end of said first steering roller is fixed, and an end thereof adjacent the other end said second steering roller is movable; and control means for controlling movement of said end of said second steering roller adjacent the other end said second steering roller.
[0008] These and other objects, features, and advantages of the present invention will become more apparent upon consideration of the following description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] FIG. 1 is a schematic sectional view of a typical image forming apparatus to which the present invention is related. It shows the general structure of the apparatus.
[0010] FIG. 2 is a schematic sectional view (at plane perpendicular to moving direction of belts) of the fixing apparatus in the first preferred embodiment of the present invention, and shows the general structure of the apparatus.
[0011] FIG. 3A is an external perspective view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet entrance side, and shows the structure of the mechanisms. FIG. 3B is a left side view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet entrance side, and shows the structure of the mechanisms. FIG. 3C is a schematic drawing which depicts the movement of the pressure belt steering roller of the mechanism for controlling the pressure belt in position.
[0012] FIG. 4A is an external perspective view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet exit side, and shows the structure of the mechanisms. FIG. 4B is a left side view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet exit side, and shows the structure of the mechanisms. FIG. 4C is a schematic drawing which depicts the movement of the pressure belt steering roller of the mechanism for controlling the pressure belt in position.
[0013] FIG. 5 is a flowchart of the sequence for controlling the mechanism for controlling in position the fixation belt of the fixing apparatus in the first embodiment.
[0014] FIG. 6 is a flowchart of the sequence for controlling the mechanism for controlling in position the pressure belt of the fixing apparatus in the first embodiment.
[0015] FIGS. 7( a )- 7 ( e ) are schematic drawings which depict the belt steering movement of the fixation belt steering roller and the pressure belt steering roller of the fixing apparatus in the first embodiment.
[0016] FIG. 8( a ) is an external perspective view of the fixation belt position controlling mechanism and pressure belt position control mechanism of a comparative fixing apparatus, as seen from the recording sheet entrance side of the apparatus. FIG. 8( b ) is a left side (as seen from recording sheet entrance side) view of the fixation belt position control mechanism and pressure belt position control mechanism of the fixing apparatus shown in FIG. 8( a ).
[0017] FIG. 9( a ) is an external perspective view of the fixation belt position control mechanism and pressure belt position control mechanism of the comparative fixing apparatus, as seen from the recording sheet exit side of the apparatus. FIG. 9( b ) is a left side (as seen from recording sheet entrance side) view of the fixation belt position control mechanism and pressure belt position control mechanism of the fixing apparatus shown in FIG. 9( a ).
[0018] FIGS. 10( a )- 10 ( e ) are schematic drawings which depict the belt steering movement of the fixation belt steering roller and pressure belt steering roller of the comparative fixing apparatus.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiment 1
(1) General Description of Image Forming Apparatus
[0019] Hereafter, the first preferred embodiment of the present invention will be described with reference to the appended drawings. FIG. 1 is a schematic sectional view of the image forming apparatus in the first embodiment of the present invention, the fixing apparatus of which is an image heating apparatus (device) in accordance with the present invention. It depicts the overall structure of the apparatus. The image forming apparatus depicted by FIG. 1 is an electrophotographic laser beam printer.
[0020] The image forming apparatus in the first embodiment can be roughly divided into an image forming portion 101 which forms a toner image on a sheet S (recording medium), and a fixing apparatus 111 (image heating apparatus) which fixes an unfixed toner image to the sheet S by heating and pressing the toner image. The image forming portion 101 has the following devices, which will be described next. They are an electrophotographic photosensitive member 102 (image bearing member), a charging device 103 , an exposing apparatus 104 (exposing means), and a developing device 105 (developing means). The photosensitive member 102 is in the form of a drum, and therefore, will be referred to as a photosensitive drum hereafter. The charging device 103 , exposing apparatus 104 , and developing device 105 are in the adjacencies of the peripheral surface of the photosensitive drum 101 . In an image forming operation, the peripheral surface of the photosensitive drum 101 is uniformly charged by the charging device 103 . Then, the uniformly charged portion of the peripheral surface of the photosensitive drum 102 is exposed by the exposing apparatus 104 . More specifically, the uniformly charged portion is scanned by a beam of laser light L projected by the exposing apparatus 104 while being modulated with the digital data of the image to be formed. Thus, an electrostatic latent image is formed on the charged portion of the peripheral surface of the photosensitive drum 101 . This electrostatic latent image is developed by the developing device 105 which uses toner. Thus, a visible image is formed of toner on the peripheral surface of the photosensitive drum 102 (this visible image hereafter will be referred to simply as toner image).
[0021] The image forming apparatus 100 has also a recording sheet feeding-and-conveying cassette 107 , which is in the bottom portion of the apparatus 100 . The cassette 107 stores multiple sheets S in layers. As an image forming operation begins, the sheets S in the cassette 107 are fed into the main assembly of the apparatus 100 one by one, and conveyed to a pair of registration rollers 109 , by a pair of sheet feeder rollers 108 . Then, each sheet S is conveyed to a transfer nip which is between the photosensitive drum 102 and a transfer roller 110 (transferring means), by the pair of registration rollers 109 in synchronism with the arrival of the toner image on the photosensitive drum 102 at the transfer nip. Then, the sheet S is conveyed through the transfer nip while remaining pinched by the peripheral surface of the photosensitive drum 102 and the peripheral surface of the transfer roller 110 . While the sheet S is conveyed through the transfer nip, the toner image on the peripheral surface of the photosensitive drum 102 is electrostatically transferred onto the sheet S by the transfer roller 110 . In other words, the unfixed toner image is borne on one of the surfaces of the sheet S. Then, the sheet S bearing the unfixed toner image is conveyed to the fixing apparatus 111 , and is conveyed through the fixing apparatus 111 . In the fixing apparatus 111 , heat and pressure are applied to the unfixed toner image, whereby the unfixed toner image becomes thermally fixed to the sheet S. Then, the sheet S, bearing the fixed toner image, is conveyed by the fixing apparatus 111 to a pair of discharge rollers 112 . Then, the sheet S is discharged by the pair of discharge rollers 112 into a delivery tray 113 which makes up a part of the top portion of the image forming apparatus. The transfer residual toner, that is, the toner remaining on the peripheral surface of the photosensitive drum 102 after the transfer of the unfixed toner image onto the sheet S, is removed by a cleaning apparatus 106 (cleaning means).
(2) Description of Fixing Apparatus
[0022] In the following description of the fixing apparatus and its structural members, the “lengthwise direction” means the direction perpendicular to the sheet conveyance direction (recording medium conveyance direction), whereas the “widthwise direction” means the direction parallel to the sheet conveyance direction. The “length” of a given member means the measurement of the member in the “lengthwise direction,” whereas the “width” of a given member means the measurement of the member in the “widthwise direction”.
[0023] FIG. 2 is a schematic sectional view of the fixing apparatus, at a plane perpendicular to the lengthwise direction, and shows the general structure of the apparatus. This fixing apparatus is of the belt-nip type. That is, it has a belt driving apparatus, and a pair of belts which are placed in contact with each other to form a nip.
[0024] The fixing apparatus 111 in the first embodiment has a fixation belt unit 10 and a pressure belt unit 20 . The fixation belt unit 10 has a fixation belt 11 , which is an endless belt and is one (first) of the two belts of the fixing apparatus 111 . The fixation belt 11 is supported by a pair of rollers 12 and 13 in such a manner that it can be circularly moved. It is kept stretched also by the pair of rollers 12 and 13 which apply a preset amount of tensile force (120 N for example) to the fixation belt 11 . The roller 12 is a fixation belt driving roller, whereas the roller 13 is a fixation belt steering roller. In other words, the roller 13 has a function of steering the fixation belt 11 and a function of keeping the fixation belt 11 stretched. The fixation belt 11 is a laminar belt. It is made up of a metallic substrate layer, and a silicon rubber layer coated on the substrate layer. The substrate layer is 75 μm in thickness, 380 mm in width, and 200 mm in length. It is made of a magnetic metallic substance such as nickel or stainless steel. The silicon rubber layer is 300 μm in thickness. The fixation belt 11 does not need to be limited in structure and material to the above described ones. That is, any belt may be employed, as long as it is heat resistant and can generate heat by being subjected to the magnetic flux generated by an inductive heating coil 30 as a heat generation source, as will be described later. The fixation belt driver roller 12 is made up of a metallic core 12 a and an elastic layer 12 b . The metallic core 12 a is a solid cylindrical member made of stainless steel, and is 18 mm in external diameter. The elastic layer 12 b is made of heat resistant silicon rubber, and was molded on the peripheral surface of the metallic core 12 a in a manner to entirely cover the peripheral surface of the metallic core 12 a . The fixation belt steering roller 13 is made up of a hollow roller made of stainless steel, for example, and is 20 mm in external diameter and roughly 18 mm in internal diameter. The fixation belt steering roller 13 has the belt steering function and belt tensioning function as described previously. That is, not only does the fixation belt steering roller 13 function as a steering roller for correcting the fixation belt 11 in the position in the “lengthwise direction” of the fixing apparatus 111 (widthwise direction of belt 11 ), but also, it functions as a belt tensioning roller for adjusting the fixating belt 111 n tension.
[0025] The pressure belt unit 20 has an endless pressure belt as the second belt ( FIG. 2 ) of the fixing apparatus 111 . The pressure belt 21 is supported by a pair of rollers 22 and 23 , as supporting members, in such a manner that it can be circularly moved. It is kept stretched also by the pair of rollers 22 and 23 which apply a preset amount of tensile force (100 N for example) to the pressure belt 21 . The roller 22 is a pressure belt driving roller, whereas the roller 23 is a pressure belt steering roller. In other words, the roller 23 has a function of steering the pressure belt 21 and a function of keeping the pressure belt 21 stretched. The pressure belt 21 also is a laminar belt. It is made up of a substrate layer, and a silicon rubber layer coated on the substrate layer. The substrate layer is 75 μm in thickness, 380 mm in width, and 200 mm in length. It is made of polyimide film. The silicon rubber layer is 300 μm in thickness. The pressure belt 21 does not need to be limited in structure and material to the above described ones. That is, any belt may be employed as the pressure belt 21 , as long as it is heat resistant. The pressure belt driving roller 22 is a solid roller made of stainless steel, for example, and is 20 mm in external diameter. The pressure belt steering roller 23 is made up of a hollow roller made of stainless steel, for example, and is 20 mm in external diameter and roughly 18 mm in internal diameter. The pressure belt steering roller 23 has the belt steering function and belt tensioning function as described previously. That is, not only does the pressure belt steering roller 23 function as a steering roller for correcting the pressure belt 21 in its position in the “lengthwise direction” of the fixing apparatus 111 (widthwise direction of belt 21 ), but also, it functions as a belt tensioning roller for adjusting the pressure belt in tension.
[0026] The fixation belt 11 is suspended by the fixation belt driving roller 12 and fixating belt steering roller 13 in such a manner that the portion of the fixation belt 11 , which is moving through the top portion of the loop it forms, remains roughly horizontal. The pressure belt 21 is under the fixation belt 11 , and is in contact with the fixation belt 11 . It is suspended by the pressure belt driving roller 22 and pressure belt steering roller 23 in such a manner that its portion which is moving through the top portion of the loop it forms, is tilted in such a manner that its upstream end, in terms of the moving direction of the fixation belt 21 , is positioned lower than its downstream end. The pressure belt driving roller 22 opposes the fixation belt driving roller 12 with the presence of the fixation belt 11 and pressure belt 21 between the two rollers 22 and 12 . It is kept pressed against the fixation belt driving roller 12 by a pair of springs 71 F and 71 R (which will be described later) so that the outward surface of the pressure belt 21 is kept in contact with the outward surface of the fixation belt 11 . That is, the pressure from the springs 71 F and 71 R is applied to the elastic layer 12 b of the fixation belt driving roller 12 through the pressure belt 21 and fixation belt 11 , whereby the elastic layer 21 b is elastically deformed, forming thereby a part of the fixation nip N. The fixation belt unit 10 is provided with a stay 14 (pressure applying member) formed of stainless steel (SUS), for example. The stay 14 is on the inward side of the fixation belt loop, and is positioned so that its lengthwise direction coincides with the widthwise direction of the fixation belt 11 . The pressure belt unit 11 is provided with a pressure pad 24 (pressing member) formed of silicon rubber, for example. The stay 24 is in on the inward side of the pressure belt loop, and is positioned so that its lengthwise direction coincides with the widthwise direction of the pressure belt 21 . The stay 14 opposes the pressure pad 24 with the presence of the fixation belt 11 and pressure belt 21 between the stay 14 and pressure pad 24 . More specifically, the stay 14 is kept pressed upon the inward surface of the fixation belt 11 by unshown compression springs so that a preset amount (400 N, for example) of contact pressure is maintained between the stay 14 and fixation belt 11 . The pressure pad 24 is kept pressed upon the inward surface of the pressure belt 21 and the peripheral surface of the pressure belt driving roller 22 so that a preset mount (400 N, for example) of contact pressure is maintained between the pressure pad 24 and pressure belt 21 , and between the pressure pad 24 and the pressure belt driving roller 22 . By not only pressing stay 14 upon the inward surface of the fixation belt 11 , but also pressing the pressure pad 24 upon the inward surface of the pressure belt 21 and peripheral surface of the pressure belt driving roller 22 , it is possible to provide a long area of contact between the outward surface of the fixation belt 11 and the outward surface of the pressure belt 21 in terms of the sheet conveyance direction. In other words, it is possible to form a large fixation nip N, the size of which is proportional to the size of the abovementioned area of contact, by the outward surface of the fixation belt 11 and the outward surface of the pressure belt 21 . With the formation of the long and wide fixation nip N, it is possible to make longer the length of time it takes for the sheet S, which is bearing an unfixed toner image T, to be conveyed through the fixation nip N while remaining pinched between the two belts 11 and 21 . Therefore, toner images which are significantly superior in glossiness than those obtainable with the use of any of conventional fixing apparatuses, can be outputted at a significantly higher speed than those reachable by any of conventional fixing apparatuses.
[0027] The typical operation of the fixing apparatus 111 in this embodiment is as follows. As the fixation belt driving roller 12 is rotated by a fixation motor, it circularly moves the fixation belt 11 in the direction indicated by an arrow mark ( FIG. 2 ). The force given to the fixation belt 11 by the fixation motor through the fixation belt driving roller 12 is transmitted from the fixation belt 11 to the pressure belt 21 through the fixation nip N, whereby the pressure belt 21 is rotated in the direction indicated by the arrow mark. In other words, the pressure belt 21 is rotated by the circular movement of the fixation belt 11 . Through the inductive heating coil 30 , high frequency electric current is flowed from an exciter circuit, causing the inductive heating coil 30 to generate magnetic flux, which heats the fixation belt 11 . The surface temperature of the fixation belt 11 is detected by a temperature detecting member, such as a thermistor, which is in the adjacencies of the surface of the fixation belt 11 . The output signal from the temperature detecting member is picked up by a control portion 200 made up of a CPU and memories, such as a RAM, a ROM, and the like. Then, the control portion 200 controls the exciter circuit, based on the output signals, so that the surface temperature of the fixation belt 11 remains in a preset fixation temperature range (target temperature range). While the surface temperature of the fixation belt 11 is kept in the preset fixation range, the sheet S on which the unfixed toner image T is present is introduced into the fixation nip N of the fixing apparatus 111 with the toner image bearing surface of the sheet S facing upward, and is conveyed through the fixation nip N while remaining pinched by the outward surface of the fixation belt 11 and the outward surface of the pressure belt 21 . While the sheet S is conveyed through the fixation nip N, the sheet S and the unfixed toner image T thereon are subjected to the heat from the fixation belt 11 and the pressure from the combination of the pressure belt 21 and fixation belt 11 . Thus, the toner image T becomes thermally fixed to the surface of the sheet S.
[0000] (3) Description of Fixation Belt Position Control Mechanism and Pressure Belt position Control Mechanism
[0028] FIG. 3A is an external perspective view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet entrance side, and shows the structure of the mechanisms. FIG. 3B is a left side view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position (shown in FIG. 3A ), as seen from the recording sheet entrance side, and shows the structure of the mechanisms. FIG. 3C is a schematic drawing which depicts the movement of the pressure belt steering roller of the mechanism for controlling the pressure belt in position. FIG. 4A is an external perspective view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet exit side, and shows the structure of the mechanisms. FIG. 4B is a left side view of the combination of the mechanism for controlling the fixation belt in position, and the mechanism for controlling the pressure belt in position, as seen from the recording sheet exit side, and shows the structure of the mechanisms. FIG. 4C is a schematic drawing which depicts the movement of the pressure belt steering roller of the mechanism for controlling the pressure belt in position.
[0029] First, the mechanism 50 (first correctional means) for controlling the fixation belt in position will be described. This mechanism 50 will be referred to hereafter as a fixation belt position controlling means 50 . The fixation belt position controlling means 50 has a pair of lateral plates 40 F and 40 R (front and rear plates 40 F and 40 R), a pair of steering roller supporting arms 51 F and 51 R, the fixation belt driving roller 12 , and the fixation belt steering roller 13 . The steering roller supporting arms 51 F and 51 R are attached to the front and rear plates 40 F and 40 R, respectively. The front end of metallic core 12 a F of the fixation belt driving roller 12 and the front end 13 a F of the metallic core 13 a of the fixation belt steering roller 13 are supported by the steering roller supporting arm 51 F. The fixation belt steering roller 13 is supported in such a manner that the fixation belt steering roller 13 can be tilted to vertically move the front end 13 a F of its metallic core 13 a . More specifically, the fixation belt driving roller 12 is rotatably supported by the front plate F of the fixing apparatus 111 , and the steering roller supporting arm 51 F of the fixation belt position controlling mechanism 50 of the fixing apparatus 111 , by the lengthwise front end portion 12 a F of its metallic core 12 a ( FIGS. 3A and 3B ). Further, the fixation belt driving roller 12 is rotatably supported by the rear plate 40 R of the fixing apparatus 111 and the steering roller supporting arm 51 R of the fixation belt position control mechanism 50 , by the other lengthwise end (right lengthwise end) 12 a R of the metallic core 12 a ( FIGS. 4A and 4B ). The lengthwise end 13 a F of the metallic core 13 a of the fixation belt steering roller 13 is rotatably supported by the front plate 41 F of the fixing apparatus 111 , and the steering roller supporting front arm 51 F of the fixing apparatus 111 , with the placement of a bearing 52 F between the metallic core end 13 a F and steering roller supporting arm 51 F to make the fixation belt steering roller 13 rotatable ( FIGS. 3A and 3B ). The rear end 13 a R of the metallic core 13 a of the fixation belt steering roller 13 is rotatably supported by the rear plate 41 R of the fixing apparatus 111 , and the steering roller supporting rear arm 51 R, with the placement of a bearing 52 R between the rear front end 13 a R of the metallic core 13 a , and the fixation belt steering roller supporting rear arm 51 R ( FIGS. 4A and 4B ). The bearing 52 F is supported by the steering roller supporting arm 51 F on the front plate 40 F in such a manner that the bearing 52 F can be slid in the direction in which the fixation belt 11 is kept stretched ( FIGS. 3A and 3B ). The frontal plate 40 F is provided with a hole through which the front end portion 13 a F of the metallic core 13 a of the fixation belt steering roller 13 is put. The hole is shaped so that as the fixation belt steering roller 13 is tilted to steer the fixation belt 11 , the front end portion 13 a F is allowed to be vertically displaced. Further, a tension spring 53 F for keeping the bearing 52 F pressed in the belt tensioning direction to provide the fixation belt 11 with a preset amount of tension is attached to the steering roller support arm 51 F. Therefore, of the steering roller support arm 51 F and 51 R, the steering roller support arm 51 F can tilt the fixation belt driving roller 12 in such a manner that the front end 12 a F of the metallic core 12 a of the fixation belt driving roller 12 vertically displaces in an oscillatory manner. Thus, the fixation belt steering roller 13 can be tilted in such a manner that the lengthwise end 13 a R, by which the fixation belt steering roller 13 is supported by the steering roller support arm 51 R, is moved upward or downward as indicated by a pair of arrow marks A 1 or A 2 , respectively, to steer the fixation belt 11 by a preset amount ( FIG. 3B ). That is, the fixation belt position control mechanism 50 is structured so that as the steering roller support arm 51 F is moved in an oscillatory manner, the fixation belt steering roller 13 tilts by a preset angle in such a manner, that the lengthwise end 13 a F of the metallic core 13 a of the fixation belt steering roller 13 moves upward or downward indicated by the pair of arrow marks A 1 and A 2 , respectively ( FIG. 3C ). The steering roller support arm 51 F is provided with a fan-shaped gear 54 , the gear portion of which faces away from the metallic core 13 a . The fan-shaped gear 54 is in engagement with a worm gear 56 attached to the output shaft of a stepping motor 55 . Further, the steering roller support arm 51 R supported by the rear plate 40 R is fitted with a bearing 52 R, which is supported by the steering roller support arm 51 R in such a manner that it is slid in the belt tension direction ( FIGS. 4A and 4B ). It is by this bearing 52 R that the lengthwise rear end portion 13 a R of the metallic core 13 a of the fixation belt steering roller 13 , which is put through the rear plate 40 R in such a manner that it cannot be moved upward or downward, is rotatably supported. Further, the steering roller support arm 51 R is fitted with a tension spring 53 R for keeping the bearing 52 R pressed in the belt tension direction to provide the fixation belt 11 with a preset amount of tension.
[0030] There is a fixation belt position sensor 90 F (belt position detecting first member) for detecting the position of front edge of the fixation belt 11 , on the inward surface of the front plate 40 F. The fixation belt position sensor 90 F is structured so that it can detect the presence of front edge of the fixation belt 11 when the edge is within its preset range, and at the preset limit position in terms of the lengthwise direction of the fixation belt driving roller 13 and fixation belt steering roller 13 . There is also a fixation belt position sensor 90 R (belt position detecting first member) for detecting the position of rear edge of the fixation belt 11 , on the inward surface of the front plate 40 F. The fixation belt position sensor 90 R is structured so that it can detect the presence of the rear edge of the fixation belt 11 when the edge is within its preset range, and at the preset limit position, in terms of the lengthwise direction of the fixation belt driving roller 12 and fixation belt steering roller 13 . The abovementioned preset limit position is on the outward side of the preset range, in terms of the lengthwise direction of the fixation roller driving roller 12 and fixation roller steering roller 13 . As for the angle of the tilt of the fixation belt steering roller 13 , the output of the fixation belt position sensor 90 F and that of the fixation belt position sensor 90 R are inputted into the control portion 200 (controlling means) so that the control portion 200 can control the operation of the stepping motor 55 to keep the fixation belt steering roller 13 in a preset range in terms of tilt.
[0031] Next, the mechanism 60 (second controlling means) for controlling the pressure belt in position will be described. This mechanism hereafter will be referred to as a pressure belt position control mechanism 60 . The pressure belt position control mechanism 60 is made up of a front plate 41 F, a rear plate 41 R, a pair of steering roller supporting arms 61 F and 61 R, the pressure belt driving roller 22 , and the pressure belt steering roller 23 . The steering roller supporting arms 61 F and 61 R are attached to the front and rear plates 41 F and 41 R, respectively. The pressure belt driving roller 22 and pressure belt steering roller 23 are supported by the front and rear plates 41 F and 41 R. The rear end portion 22 a R of the metallic core 22 a of the pressure belt driving roller 22 and the rear end portion 13 a R of the metallic core 13 a of the pressure belt steering roller 23 are supported by the steering roller support arm 61 R. The pressure belt steering roller 23 is supported in such a manner that the pressure belt steering roller 23 can be tilted to vertically move the rear end 23 a R of its metallic core 23 a . The front end portion 23 a F of the metallic core 23 a of the pressure roller driving roller 23 is rotatably supported by the front plate 41 F of the fixing apparatus 111 , and the steering roller support arm 61 F of the pressure belt position control mechanism 60 of the fixing apparatus 111 ( FIGS. 3A and 3B ). The other lengthwise end portion 23 a R of the metallic core 23 a of the pressure belt driving roller 23 is rotatably supported by the rear plate 41 R of the fixing apparatus 111 and the steering roller support arm 61 R of the pressure belt position control mechanism 60 of the fixing apparatus 111 ( FIGS. 4A and 4B ). The lengthwise front end portion 23 a F of the metallic core 23 a of the pressure belt steering roller 23 is rotatably supported by the front plate 41 F of the fixing apparatus 111 and the steering roller support arm 61 F of the fixing apparatus 111 , with the presence of a bearing 62 F between the metallic core end portion 23 a F and steering roller support arm 62 F ( FIGS. 3A and 3B ). The lengthwise other end portion 23 a R of the metallic core 23 a of the pressure belt steering roller 23 is rotatably supported by the rear plate 41 R of the fixing apparatus 111 and the steering roller support arm 61 R, with the presence of a bearing 62 R between the metallic core end portion 23 a R and steering roller support arm 61 R ( FIGS. 4A and 4B ). The bearing 62 R is supported by the steering roller support arm 61 R attached to the rear plate 41 R, in such a manner that it can be slid in the belt tension direction ( FIGS. 4A and 4B ). Further, the metallic core end portion 23 a R of the pressure belt steering roller 23 is put through the rear plate 40 R and is rotatably supported by the bearing 62 R. The steering roller support arm 61 R is fitted with a tension spring 63 R for keeping the bearing 61 R pressed in the belt tension direction to provide the pressure belt 21 with a preset amount of tension. Therefore, of the pair of steering roller support arm 61 F and 61 R, the steering roller support arm 61 R is rotationally movable about the axis of the metallic core end portion 22 a R of the pressure belt driving roller 22 . Therefore, the steering roller support arm 61 R is rotationally (virtually vertically) movable about the axis of the metallic core end portion 22 a R of the pressure belt driving roller 22 . Therefore, the pressure belt steering roller 23 can be tilted (rotationally moved) about the center of the lengthwise metallic core end portion 23 a F of the pressure belt steering roller 23 , which is supported by the steering roller supported by the steering roller support arm 61 F, so that the rear end portion 23 a R of the metallic core 23 a of the pressure belt steering roller 23 moves in the upward or downward direction as indicated by a pair of arrow marks B 1 and B 2 , respectively, to steer the pressure belt 21 by a preset amount ( FIG. 4B ). That is, the pressure belt steering mechanism 60 is structured so that as the steering roller support arm 61 R is rotationally moved, the pressure belt steering roller 23 is rotationally moved (tilted) by a preset angle (amount) about the center of the front end portion 23 a F of the metallic core 23 a of the pressure belt steering roller 23 , in the upward or downward direction indicated by the pair of arrow marks. B 1 and B 2 , respectively ( FIG. 4C ). The steering roller support arm 61 R is provided with a fan-shaped gear 64 , which is on its surface facing away from its rotational axis. The fan-shaped gear 64 is in mesh with a worm gear 66 attached to the output shaft of a stepping motor 65 (for pressure belt steering roller) supported by the rear plate 41 R. Further, steering roller support arm 61 F attached to the front plate F is fitted with a bearing 62 F in such a manner that the bearing 62 F can be slid in the belt tension direction ( FIGS. 4A and 4B ). It is by the bearing 62 F that the front end portion 23 a F of the metallic core 23 a of the pressure belt steering roller 23 , which is put through the front plate F in such a manner that it cannot be vertically moved, is rotatably supported. Further, the steering roller support arm 61 F is fitted with a tension spring 63 F for keeping the bearing 62 F pressed in the belt tension direction to provide the pressure belt 21 with a preset mount of tension.
[0032] There is a pressure belt position sensor 91 R (belt position detecting second member) for detecting the position of the rear edge of the pressure belt 13 , on the inward surface of the rear plate 41 R. The pressure belt position sensor 91 R is structured so that it can detect in position the range in which the lengthwise rear edge of the pressure belt 13 is allowed to move, and the preset positional limit. There is also a pressure belt position sensor 91 F (belt position detecting second member) for detecting the position of the front edge of the pressure belt 13 , on the inward surface of the front plate 41 F. The pressure belt position sensor 91 R is structured so that it can detect in position the range in which the front edge of the fixation belt steering roller 13 is allowed to move, and the positional limit for the shifting of the pressure belt 21 . The above-mentioned position limit for the shifting of the pressure belt 21 is on the outward side of the preset range for the shifting of the pressure belt 13 , in terms of the lengthwise direction of the pressure belt driving roller 22 and pressure roller steering roller 23 . As for the angle of the tilt of the pressure roller steering roller 23 , the outputs of the pressure belt position sensors are inputted into the control portion 200 (controlling means) so that the control portion 200 can control the operation of the stepping motor 65 to keep the pressure roller steering roller 23 in a preset range in terms of tilt.
(4) Description of Belt Position Control of Fixation Belt Position Control Mechanism and Pressure Belt Position Control Mechanism
[0033] FIG. 5 is a flowchart of an example of belt position control of the fixation belt position control mechanism. FIG. 6 is a flowchart of an example of the belt position control of the pressure belt position control mechanism.
[0034] First, referring to FIG. 5 , the belt position control carried out by the control portion 200 to control the fixation belt position controlling means 50 will be described. Referring to FIG. 3A , if the front edge of the fixation belt 11 moves out of the preset range for the front edge of the fixation belt 11 because of the shifting of the fixation belt 11 in the direction indicated by an arrow mark F, for example, the fixation belt position sensor 90 F detects the position of the front edge of the fixation belt 11 , and outputs a signal Sf 1 . Further, if the other edge of the fixation belt 11 moves out of the range preset for the fixation belt 11 , the fixation belt position sensor 90 R detects the position of the other edge of the fixation belt 11 , and outputs a signal Sf 2 .
[0035] In step S 1 , as the signal Sf 1 outputted from the fixation belt position sensor 90 F is picked up by the control portion 200 , the control portion 200 moves to step S 2 . If the control portion 200 takes in the signals Sf 1 and Sf 2 , it takes step S 5 . In step S 2 , the control portion 200 rotates the stepping motor 55 in the direction to cause the output shaft of the stepping motor 55 to rotate in the direction indicated by an arrow mark CW. The rotation of the output shaft of the stepping motor 55 causes the worm gear 56 , whereby the steering roller supporting arm 51 F is rotationally moved, along with the fan-shaped gear 54 , in the downward direction indicated by an arrow mark A 2 . As the steering roller supporting arm 51 F is rotationally moved in the direction indicated by the arrow mark A 2 , the fixation belt steering roller 13 is tilted by the movement of the steering roller supporting arm 51 F, in the direction to cause its front end to move also in the direction indicated by the arrow mark A 2 . As the fixation belt steering roller 13 is tilted as described above, the fixation belt 11 begins to shift toward the other end, that is, in the direction indicated by the arrow mark R. If the other edge of the fixation belt 11 moves beyond the preset range for the other edge, the edge is detected by the fixation belt position sensor 90 R, and the fixation belt position sensor 90 R outputs a signal Sr 2 . In step S 3 , as the control portion 200 takes in the signal Sr 1 from the fixation belt position sensor 90 R, it proceeds to step S 4 , whereas if the control portion 200 takes in signals Sr 1 and Sr 2 , the control portion 200 proceeds to step S 5 . In step S 4 , in response to the signal Sr 1 , the control portion 200 rotates the stepping motor 55 in the direction to cause the output shaft of the stepping motor 55 rotates in the direction indicated by an arrow mark CC. The rotation of the output shaft of the stepping motor 55 causes the worm gear 56 , whereby the steering roller supporting arm 51 F is rotationally moved, along with the fan-shaped gear 54 , in the direction indicated by the arrow mark A 1 . As the steering roller supporting arm 51 F is rotationally moved in the direction indicated by the arrow mark A 1 , the fixation belt steering roller 13 is tilted by the movement of the steering roller supporting arm 51 F, in the direction to cause its front end to move also in the direction indicated by the arrow mark A 1 . As the fixation belt steering roller 13 is tilted as described above, the fixation belt 11 begins to shift toward the other end, that is, in the direction indicated by the arrow mark R. If the front edge of the fixation belt 11 moves beyond the preset range for the front edge, the edge is detected by the fixation belt position sensor 90 F, and the fixation belt position sensor 90 F outputs a signal Sf 1 . If the other edge of the fixation belt 11 moves beyond the preset range for the other edge, the edge is detected by the fixation belt position sensor 90 R, and the fixation belt position sensor 90 R outputs the signal Sf 2 . In step S 1 , as the control portion 200 takes in the output signal Sf 1 of the fixation belt position sensor 90 F, it moves to step S 2 , whereas if it takes in output signals Sf 1 and Sf 2 , it moves to step S 5 . The processes in steps S 2 -S 4 are repeatedly carried out. Thus, the fixation belt 11 continuously and alternately sways frontward and rearward (it continues to snake) while remaining in the preset range in which the fixation belt 11 is allowed to move. In step S 5 , the control portion 200 stops driving the stepping motor 55 , and also, stops the operation of the fixing apparatus 111 by stopping the electric power supply to the exciter coil 30 .
[0036] Next, referring to FIG. 6 , the control carried out by the control portion 200 to make the pressure belt position control mechanism 60 control the pressure belt 13 in position will be described. Referring to FIG. 3A , if one of the edges of the pressure belt 21 moves out of the preset belt movement range because of the shifting of the pressure belt 21 in the direction indicated by the arrow mark F, for example, the belt edge is detected by the pressure belt position sensor 91 F, and the pressure belt position sensor 91 F outputs a signal Sf 3 . Further, if the other edge of the pressure belt 21 moves out of the preset belt range, the belt edge is detected by the pressure belt position sensor 91 R, and the pressure belt position sensor 91 R outputs a signal Sf 4 . In step S 11 , if the control portion 200 picks up the output signal Sf 3 from the pressure belt position sensor 91 F, it moves to step S 12 , whereas if it picks up the output signals Sf 3 and Sf 4 , it moves to step S 15 . In step S 12 , the control portion 200 rotates the stepping motor 65 to rotate the output shaft of the stepping motor 65 in the direction indicated by the arrow mark CW to move the fan-shaped gear 64 downward, that is, the direction indicated by the arrow mark B 2 ( FIG. 4B ) by a preset amount. Thus, the worm gear 66 rotates in response to the rotation of the output shaft of the stepping motor 65 , whereby the steering roller support arm 61 R is moved, along with the fan-shaped gear 64 , in the direction indicated by the arrow mark B 2 . As the steering roller support arm 61 R is rotationally moved in the direction indicated by the arrow mark B 2 , the pressure belt steering roller 23 is tilted as indicated by the arrow mark B 2 . As the pressure roller steering roller 23 is tilted as indicated by the arrow mark B 2 , the pressure belt 21 begins to shift rearward, that is, the direction indicated by an arrow mark R. Then, if the rear edge of the pressure belt 21 moves beyond the preset range for the pressure belt 21 , the rear edge is detected by the pressure belt position sensor 91 R, and the pressure belt position sensor 91 R outputs a signal Sr 3 . Further, if the front rear edge of the pressure belt 21 moves beyond the preset range for the front edge, the front edge detected by the pressure belt position sensor 91 F, and the pressure belt position sensor 91 F output a signal Sr 4 . In step S 13 , if the control portion 200 picks up the output signal Sr 3 from the pressure belt position sensor 91 R, it moves to step S 14 , whereas if it picks up the output signals Sr 3 and Sr 4 , it moves to step S 15 . In step S 14 , the 200 rotates the stepping motor 65 in response to the output signal Sr 3 , to rotate the output shaft of the stepping motor 65 in the direction indicated by an arrow mark CCW to move the fan-shaped gear 64 upward, that is, the direction indicated by the arrow mark B 1 ( FIG. 4B ) by a preset amount. With this rotation of the output shaft of the stepping motor 65 , the worm gear 66 rotates, causing the steering roller support arm 61 R to rotationally move as indicated by the arrow mark B 1 . By this rotational movement of the steering roller support arm 61 R in the direction indicated by the arrow mark B 1 , the pressure roller steering roller 23 is tilted as indicated by the arrow mark B 1 . As the pressure roller steering roller 23 is tilted as indicated by arrow mark B 1 , the pressure belt 21 begins to shift frontward, that is, in the direction indicated by the arrow mark F. If the front edge of the pressure belt 21 moves beyond the preset range while the pressure belt 21 is moving frontward, the front edge is detected by the pressure belt position sensor 91 F, and the pressure belt position sensor 91 F output the signal Sf 3 . Further, if the rear edge moves beyond the preset range, the pressure belt position sensor 91 R detects the rear edge, and outputs the signal Sf 4 . In step S 11 , if the control portion 200 takes in the output signal Sf 3 from the pressure belt position sensor 91 R, it moves to step S 12 , whereas if it takes in both the output signals Sf 3 and Sf 4 , it moves to step S 15 , and repeats the above described processes in steps S 12 -S 14 . Thus, the pressure belt 21 continues to alternately shift frontward and rearward (to snake) within preset pressure belt movement range. In step S 15 , the control portion 200 stops driving the stepping motor 65 , and also, stops the operation of the fixing apparatus 111 by stopping the electric power supply to the inductive heating coil 30 .
[0037] Referring to FIG. 7 , the distance between the fixation belt 11 and pressure belt 21 , on the sheet entrance side of the fixing apparatus is as follows. FIG. 7( a ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt 11 and pressure belt 21 of the fixing apparatus 111 in the first embodiment of the present invention before the starting of the steering of the fixation belt 11 and pressure belt 21 . FIG. 7( b ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt 11 and pressure belt 21 of the fixing apparatus 111 after the fixation belt steering roller 13 was tilted so that its front end was moved downward, and the pressure belt steering roller 23 was tilted so that its rear end was moved upward. FIG. 7( c ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt 11 and pressure belt 21 of the fixing apparatus 111 after the fixation belt steering roller 13 was tilted so that its front end was moved upward, and the pressure belt steering roller 23 was tilted so that its rear end was moved downward. FIG. 7( d ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt 11 and pressure belt 21 of the fixing apparatus 111 after the fixation belt steering roller 13 was tilted so that its front end was moved upward, and the pressure belt steering roller 23 was tilted so that its rear end was moved upward. FIG. 7( e ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt 11 and pressure belt 21 of the fixing apparatus 111 after the fixation belt steering roller 13 was tilted so that its front end was moved downward, and the pressure belt steering roller 23 was tilted so that its rear end was moved downward.
[0038] Referring to FIG. 7( a ), Xf stands for the distance between the front end of the fixation belt steering roller 13 and front end of the pressure roller steering roller 23 , and Xr stands for the distance between the rear end of the fixation belt steering roller 13 and rear end of the pressure roller steering roller 23 . Yu stands for the distance the front end of the fixation belt steering roller 13 moves upward as the steering roller supporting arm 51 F is rotationally moved, and Yd stands for the distance the front end of the fixation belt steering roller 13 moves downward as the steering roller supporting arm 51 F is rotationally moved. Further, Zu stands for the distance the rear end of the pressure roller steering roller 23 moves upward as the steering roller support arm 61 R is rotationally moved, and Zd stands for the distance the rear end of the pressure roller steering roller 23 moves downward as the steering roller support arm 61 R is rotationally moved.
[0039] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( b ),
[0000] Xf=Xf−Yd , and Xr=Xr−Zu.
[0040] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( c ),
[0000] Xf=Xf+Yu , and Xr=Xr+Zd.
[0041] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( d ),
[0000] Xf=Xf+Yu , and Xr=Xr−Zu
[0042] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( e ),
[0000] Xf=Xf−Yd , and Xr=Xr+Zd.
[0043] Substituting actual values for the terms in the formulas given above, for example, if Xf=Xr=20 mm, and Yu=Yd=Zd=Zu=5 mm.
[0044] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( b ),
[0000] Xf=15 mm, and Xr=15 mm.
[0045] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( c ),
[0000] Xf=25 mm, and Xr=25 mm.
[0046] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( d ),
[0000] Xf=25 mm, and Xr=15 mm.
[0047] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 7( e ),
[0000] Xf=15 mm, and Xr=25 mm.
[0048] In other words, the fixing apparatus 111 in the first embodiment changes by no more than 10 mm in the distance between the front end of its fixation belt 11 and pressure belt 21 on the sheet entrance side.
(5) Description of Comparative Fixing Apparatus
[0049] Next, a conventional fixing apparatus as a comparative fixing apparatus to the fixing apparatus 111 in this embodiment will be described about its fixation belt position control mechanism and pressure belt position control mechanism, and their belt position control. FIG. 8( a ) is an external perspective view of the fixation belt position control mechanism and pressure belt position control mechanism of a typical conventional fixing apparatus as a comparative fixing apparatus, as seen from the recording sheet entrance side of the apparatus. It depicts the structure of the conventional fixing apparatus. FIG. 8( b ) is a left side (as seen from recording sheet entrance side) view of the fixation belt position control mechanism and pressure belt position control mechanism of the comparative fixing apparatus shown in FIG. 8( a ). FIG. 9( a ) is an external perspective view of the fixation belt position control mechanism and pressure belt position control mechanism of the comparative fixing apparatus, as seen from the recording sheet exit side of the apparatus. FIG. 9( b ) is the left side (as seen from recording sheet entrance side) view of the fixation belt position control mechanism and pressure belt position control mechanism of the comparative fixing apparatus shown in FIG. 9( a ).
[0050] The comparative fixing apparatus is the same in structure as the fixing apparatus 111 in the first embodiment, except for the fixation belt position controlling means 50 . The members, portions, etc., of the comparative fixing apparatus, which are the same as the counterparts of the fixing apparatus in the first embodiment are given the same referential codes as those given to the counterparts, one for one, and will not be described here. The lengthwise rear end portion 12 a R of the metallic core 12 a of the fixation belt driving roller 12 is rotatably supported by the rear plate 40 R and the steering roller support arm 51 R of the fixing apparatus 111 ( FIGS. 8( a ) and 8 ( b )). The front end portion 12 a F of the fixation belt driving roller 12 is rotatably supported by the front plate 40 F of the fixation belt position controlling means 50 of the fixing apparatus 111 , and the steering roller supporting arm 51 F of the fixation belt position controlling means 50 of the fixing apparatus 111 ( FIGS. 9( a ) and 9 ( b )). Of the rear end portion 12 a R of the metallic core 12 a of the driving roller 12 and the rear end portion 13 a R of the metallic core 13 a of the fixation belt steering roller 13 , which are supported by the steering roller support arm 51 R of the rear plate 40 R, the rear end portion 13 a R of the metallic core of the fixation belt steering roller 13 is movable upward and downward. Further, the steering roller support arm 51 R is rotationally moved upward or downward, respectively, about the axis of the rear end portion of the metallic core 12 a R of the fixation belt driving roller 12 . Thus, as the rear end portion 13 a R of the metallic core 13 a of the fixation belt steering roller 13 is moved upward or downward, the fixation belt steering roller 13 is rotationally moved about the center of the front end portion 13 a F of the metallic core 13 a supported by the steering roller support arm 51 F, in the upward or downward indicated by arrow marks A 1 and A 2 , respectively by a preset amount to steer the fixation belt 11 ( FIG. 8( b )). That is, the fixation belt position controlling means 50 is structured so that as the steering roller support arm 51 R is rotationally moved upward or downward, the fixation belt steering roller 13 is rotationally moved (tilted) by a preset angle about the center of the front portion 13 a F in such a manner that the rear end portion 13 a R moves upward or downward as indicated by the arrow marks A 1 and A 2 , respectively. The fixation belt position controlling means 50 is provided with a stepping motor 55 , which is on the rear plate 40 R, and the worm gear 56 attached to the output shaft of the stepping motor 55 is in mesh with the fan-shaped gear 54 solidly attached to the steering roller support arm 51 R. That is, in the case of the comparative fixing apparatus, the steering roller supporting arm 51 R attached to the rear plate 40 R of the fixation belt position controlling means 50 is enabled to swing upward or downward about the center of the rear portion 12 a R of the metallic core of the driving roller 12 . The principle of the belt position control of the fixation belt position controlling means 50 of the comparative fixing apparatus is the same as that of the belt position control of the fixation belt position controlling means 50 of the fixing apparatus 111 . Thus, the belt shift control of the fixation belt position controlling means 50 of the comparative fixing apparatus will not be described here.
[0051] Referring to FIG. 10 , on the sheet entrance side of the comparative fixing apparatus, the distance between the fixation belt steering roller 13 and pressure roller steering roller 23 changes as follows. FIG. 10( a ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt steering roller 13 and pressure roller steering roller 23 of the comparative fixing apparatus before the starting of the belt steering operation by the fixation belt steering roller 13 and pressure roller steering roller 23 . FIG. 10( b ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt steering roller 13 and pressure roller steering roller 23 after the fixation belt steering roller 13 was tilted so that its rear end was moved upward, and the pressure belt steering roller 23 was tilted so that its rear end was moved downward. FIG. 10( c ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt steering roller 13 and pressure roller steering roller 23 after the fixation belt steering roller 13 was tilted so that its rear end was moved downward, and the pressure belt steering roller 23 was tilted so that its rear end was moved upward. FIG. 10( d ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt steering roller 13 and pressure roller steering roller 23 after the fixation belt steering roller 13 was tilted so that its rear end was moved upward, and the pressure belt steering roller 23 was tilted so that its rear end was moved upward. FIG. 10( e ) is a schematic drawing which shows the positional and attitudinal relationship between the fixation belt steering roller 13 and pressure roller steering roller 23 after the fixation belt steering roller 13 was tilted so that its rear end was moved downward, and the pressure belt steering roller 23 was tilted so that its rear end was moved downward.
[0052] Referring to FIG. 10( a ), Xf stands for the distance between the front end of the fixation belt steering roller 13 and front end of the pressure roller steering roller 23 , and Xr stands for the distance between the rear end of the fixation belt steering roller 13 and rear end of the pressure roller steering roller 23 . Yu stands for the distance the rear end of the fixation belt steering roller 13 moves (upward) as the steering roller supporting arm 51 F is rotationally moved, and Yd stands for the distance the rear end of the fixation roller 13 moves (downward) as the steering roller supporting arm 51 R is rotationally moved. Further, Zu stands for the distance the rear end of the pressure roller steering roller 23 moves (upward) as the steering roller support arm 61 R is rotationally moved, and Zd stands for the distance the rear end of the pressure roller steering roller 23 moves (downward) as the steering roller support arm 61 R is rotationally moved. When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIGS. 10( b ) and 10 ( c ), Xf does not change in value. When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 10( b ), Xr=Xf+Yu+Zd. When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 10( c ), Xr=Xf−Yu−Zd. Substituting actual values for the terms in these equations, for example, Xf=Xr=20 mm, and Yu=Yd=Zu=Zd=5 mm.
[0053] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 10( b ), Xr=30 mm.
[0054] When the fixation belt steering roller 13 and pressure roller steering roller 23 are in the state shown in FIG. 10( c ), Xr=10 mm.
[0055] In other words, in the case of the comparative fixing apparatus, the distance between the fixation belt 11 and pressure belt 21 changes no less than 20 mm on the sheet entrance side. The changes in the distance between the fixation belt 11 and pressure belt 21 on the sheet entrance side makes the sheet S change in attitude and behavior when the sheet S is introduced into, and conveyed through, the fixing apparatus. Even if the fixing apparatus is enabled to tolerate the behavioral instability of the sheet S, problems sometimes occur when recording medium (sheet S) which is small in basis weight is used for a two-sided printing operation. More specifically, a sheet of recording medium, which is small in basis weight, is likely to curl. Thus, it is likely to be curled while it is conveyed through a fixing apparatus. Thus, if it is used as recording medium for a two-sided printing (image forming) operation, it sometimes comes into contact with the surface of the fixation belt 11 when the distance between the fixation belt 11 and fixation belt steering roller 13 reduces. This contact sometimes causes an image forming apparatus to output a print with an unsatisfactory image. Further, even if a sheet of recording medium is small in the amount of the curl which occurred along the leading edge, it may be large enough in the amount of the curl which occurred along the trailing edge for its trailing end to rub against the surface of the fixation belt 11 .
[0056] Compared with the comparative fixing apparatus, the fixing apparatus 111 in the first embodiment was half in the amount of changes in the distance between the fixation belt 11 and pressure belt 21 , on the sheet entrance side. Thus, the sheet S remained more stable in behavior when it was conveyed through the fixing apparatus 111 than when it was conveyed through the comparative fixing apparatus. Thus, the employment of the fixing apparatus 111 in this embodiment by an image forming apparatus can substantially reduce the image forming apparatus in the number of unsatisfactory images.
[Miscellanies]
[0057] In the first embodiment of the present invention, an image heating apparatus in accordance with the present invention was used as a fixing apparatus for an image forming apparatus. More specifically, the first and second belts of the belt driving apparatus in accordance with the present invention were used as the fixation belt and pressure belt, respectively, of the fixing apparatus. However, the usage of the first and second belts of the belt driving apparatus in accordance with the present invention does not need to be limited to the fixation belt and pressure belt of an image heating apparatus (fixing apparatus). For example, they may be used as the endless intermediary transfer belt and endless image bearing belt (image bearing member, which comes into contact with endless intermediary transfer belt) of an image forming apparatus.
[0058] As described above, the present invention can significantly reduce the amount of change in the distance between the first and second belts of a recording medium conveying apparatus (mechanism), and therefore, it can provide a recording medium conveying apparatus (mechanism) which can more reliably convey recording medium than any of conventional recording medium conveying apparatuses (mechanisms).
[0059] While the invention has been described with reference to the structures disclosed herein, it is not confined to the details set forth, and this application is intended to cover such modifications or changes as may come within the purposes of the improvements or the scope of the following claims.
[0060] This application claims priority from Japanese Patent Application No. 175202/2009 filed Jul. 28, 2009 which is hereby incorporated by reference.
|
A belt driving apparatus includes a first rotatable belt member; a first supporting member rotatably supporting the first belt member; a first steering roller, rotatably supporting the first belt member, for adjusting a position, with respect to a widthwise direction perpendicular to a rotational direction, of the first belt member, wherein one end of the first steering roller is fixed, and the other end thereof is movable; control means for controlling movement of the other end of the first steering roller; a second rotatable belt member contacted to the first belt member; a second supporting member rotatably supporting the second belt member; a second steering roller, rotatably supporting the second belt member, for adjusting a position, with respect to the widthwise direction, of the second belt member, wherein an end of the second steering roller remote from the one end of the first steering roller is fixed, and an end thereof adjacent the other end the second steering roller is movable; and control means for controlling movement of the end of the second steering roller adjacent the other end the second steering roller.
| 6
|
FIELD OF THE INVENTION
[0001] This invention concerns systems and methods for time-based servopositioning in the context of linear data recording media such as magnetic tape.
BACKGROUND OF THE INVENTION
[0002] Modern data storage systems use servopositioning (or “servo”) systems to guide their recording and playback components with respect to a recording medium, and thus enable high track density, which increases data storage capacity. Errors in the ability to follow the servopositioning signals on the medium can cause unacceptable reductions in storage capacity, recording/playback rates, and other parameters that are important to consumers (and thus to system manufacturers).
[0003] One type of servo patterns or formats for linear magnetic tape recording systems employs so-called time-based servo techniques, examples of which are disclosed in U.S. Pat. Nos. 5,689,384; 5,930,065; and 6,021,013 (all of which are incorporated by reference in their entireties). Commercial magnetic tape drives such as the IBM model 3570 and drives known under the names “Utrium” and “Accelis,” as described by the Linear Tape Open consortium, use time-based servopositioning systems.
[0004] The advantages of time-based servo systems include very wide dynamic range; inherent track identification; low DC centerline error; and the ability to qualify position error signal (PES) validity by the amplitude of the servo signal. Disadvantages include extreme sensitivity to tape speed during writing; sensitivity to high frequency speed error during reading; and poor scalability to very small track pitches.
SUMMARY OF THE INVENTION
[0005] In general terms, the invention may be embodied in time-based servopositioning systems, methods, and formats, or in data recording media used in association with the same, and therefore this disclosure should be understood in that regard even if only an example of a particular embodiment is described in detail. Similarly, this disclosure should be understood to apply to either analog or digital signals, in accordance with principles known in the art. Thus, the terms “signal,” “data,” and the like may be used interchangeably, and should be understood to apply to either analog or digital representations of information.
[0006] In the most basic embodiment of the invention, a servopositioning system for a data recording system is used in combination with a linear data recording medium, preferably magnetic recording tape. Written or recorded on the medium are a timing reference (for example, a high frequency AC “pilot tone”) and a conventional time-based servo signal. Appropriate circuitry is separately responsive to the two signals so they can be separated from each other. The circuitry produces position error signals by sampling the time-based servo signal at a sampling rate, and also increases the bandwidth of the timing reference signal above that sampling rate. In the preferred embodiment, the two types of signals are written onto the same location of the recording medium, but the high frequency pilot tone signal is written such that its frequency lies in a playback null of the time-based servopositioning system. Any technique for accomplishing this is suitable, but in the most preferred embodiment the two signals are recorded at different azimuth angles with respect to each other (i.e., relative to the playback head of the system).
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] The accompanying drawings show a particular embodiment of the invention as an example, and are not intended to limit the scope of the invention.
[0008] [0008]FIG. 1 is a schematic diagram of one embodiment of the invention.
[0009] [0009]FIGS. 2 a , 2 b , and 3 are schematic views of geometric aspects of the embodiment of FIG. 1. FIG. 2 b is an enlarged view of the portion of FIG. 2 a indicated by the circle designated 2 b.
[0010] [0010]FIG. 4 is a schematic diagram of another aspect of the embodiment of FIG. 1.
[0011] [0011]FIGS. 5 and 6 are schematic diagrams of a preferred embodiment of the invention.
DETAILED DESCRIPTION
[0012] In general terms, the invention can be embodied in an entire system of data recording and playback, including the combination of a drive and a linear recording medium; or as only the recording medium portion of such a system; or as methods for recording or playing back data in combination with the data recording medium. Thus, while the following description may occasionally focus on only one aspect of an entire system (e.g., the recording medium alone) to disclose the preferred embodiment of the invention, this is by way of example only, and not a limitation on the scope of the invention. It should be understood that the full scope of the invention includes other aspects of the system depending on the circumstances, such as combinations of the medium and drive, and methods of using such combinations or relevant portions of them.
[0013] The time-based servo system described in U.S. Pat. Nos. 5,689,384 and 6,021,013 is somewhat immune to speed error (or time-based error) in playback by the use of a reference pulse to compare against the PES (Position Error Signal) pulse. The system is only somewhat immune, because as the frequency of the speed error increases up to the sample rate of the PES system itself the natural immunity generated by the reference normalization procedure decreases.
[0014] Data recording systems using tape media can have considerable time-based error (also known as instantaneous speed variation, or ISV) at frequencies approaching commercially standard PES sample rates. The invention improves the time normalization performance (and thereby the immunity to ISV) of linear data recording systems by effectively increasing the reference time-based bandwidth until it is greater than the PES sample rate.
[0015] [0015]FIG. 1 is a schematic view of one recording system embodiment suitable for this approach, using (for purposes of illustration only) magnetic recording tape as the preferred type of linear recording medium.
[0016] Recording system 20 comprises supply reel 21 , tape 22 , pilot tone recording head 23 , time-based servo write head 24 , verify head 25 , and take-up reel 26 . An AC bias signal 27 is the input to pilot tone recording head 23 . A current pulse signal 29 is the input to time-based servo write head 24 . Verify head 25 produces verify signal 30 that typically passes through a conventional preamplifier (not shown) to become input signal 41 of FIG. 4 (described below).
[0017] [0017]FIGS. 2 a and 2 b schematically show a full-width servo band of height h superimposed on a “sea” of high-density pilot tone 2 produced by pilot tone recording head 23 , which is subsequently used for playback speed tracking. The time-based servo pulses 6 produced by time-based servo write head 24 overwrite this tone. By way of example only, the servo pattern has five pulses 6 per sample 7 . The high-density tone is largely unaffected by the servo pulses because the servo pulses are written using a return-to-zero technique meaning the write current is mostly turned off. In general, the high frequency signal 2 is recorded at a wavelength such that its frequency lies in a playback null of the time-based servopositioning system.
[0018] In the preferred embodiment, the two signals are recorded at different azimuth angles with respect to each other. Referring additionally to FIG. 3, for a given read track width T w and a given slant angle θ, there is a natural spatial frequency null at a wavelength λ HF proportional to the read track width and the tangent of the slant angle θ, or λ HF =T w *tan(θ). Thus, placing the pilot tone in the azimuth null of the time-based servo enables both signals to be available after suitable filtering. For example, given a read track width of 5 micrometers and an angle θ of ±8 degrees, λ HF occurs at the reasonable density of 72,300 flux changes per inch (fci). This density is well within the capability of a tape and a head designed for >150 kbpi data recording. At two meters/second media speed, this density corresponds to a frequency of 2.8 MHz, easily enabling a phase locked loop tracking bandwidth above 50 kHz, or approximately 10 times the typical ISV resonant frequency of the medium. These are examples only and not limitations on the scope of the invention.
[0019] A preferred system to fully utilize this signal structure is shown schematically in FIG. 4 as circuitry 40 . Circuitry 40 receives an input signal 41 produced by the conventional read head preamp (not shown) as described above. This signal is input to both a band reject (“notch”) filter 42 and a band pass filter 44 . Notch filter 42 eliminates the high density pilot tone component but has little effect on the time pulse, because the filter notch is at the same frequency as the natural azimuth loss notch. The filtered time pulse is thereafter processed normally, as described in U.S. Pat. No. 6,021,013, with one crucial difference; the measurement time base normally derived from an external clock is derived from the high-density signal.
[0020] Specifically, the portion of the signal that passes through band pass filter 44 is the input to a phase locked loop (PLL) 46 that produces a measurement time base signal 50 for the time-based demodulator circuit 43 . The band pass is only wide enough to pass the signal and its anticipated FM sidebands, e.g. for the case above, 2.8 MHz±100 kHz. This narrow 200kHz bandwidth is more then eleven decibels quieter than the regular data channel, and therefore this reference tone signal has good signal-to-noise ratio, even when recorded at a low level. (The smaller read track width of the servo read head circuitry makes this narrow band high frequency signal perhaps only 8 db better than the read channel at the same density.) The PLL locks onto this frequency and generates a frequency tracking reference clock for the time-based servo detector circuit. This clock could be any rational multiple of the recorded tone. For example, for the rational multiple of 107 to three, the reference clock signal will be 2.8 MHz×107/3=99.8 MHz.
[0021] The high density signal actually serves at all times as a reference, and therefore has some advantages over the traditional “interval” reference as described in U.S. Pat. No. 6,031,013, particularly at column 7 , line 30 to column 8 , line 2 . First, the need for the “B interval” is eliminated altogether and replaced by the need to know when the “A interval” (or measurement period), as described in the same patent, begins. This enables a higher PES sample rate, because eliminating the reference measurement reduces constraints on the design of the format. Second, since the time-based reference is known at the same time that the PES measurement is known, and because a sampling delay appears to the servo system as if it were a phase lag, there is little PES sampling phase delay, by a factor of as much as one-half the sample time. This enables higher servo performance.
[0022] In the preferred embodiment of this scheme, and as taught in U.S. Pat. No. 6,021,013, multiple PES bursts are recorded together, such as in groups of four or five. The spacing between these pulses should be such that the pulses fall on unique phases of the high frequency tone. For example, if the first pulse in a group of four pulses falls on the zero degree phase of the high frequency signal, the second pulse should fall on the [N cycles plus] ninety degree phase of the next pulse. Similarly, the third pulse should fall on the [N cycles plus] 180 degree phase, and the fourth pulse at the [N cycles plus] 270 degree phase. Since the PES is calculated by taking the average of these four values, any possible bias caused by the high frequency tone may be averaged out according to known principles.
[0023] In another preferred embodiment of the invention, the pilot tone is modulated with a (preferably double) side band AM component without affecting the timing functionality, provided the modulation does not approach 100% negative, which would negate the pilot tone signal entirely. For example, as illustrated in FIG. 5, pilot tone 27 is formed by combining an AC bias signal 28 (for example, a sine wave signal in the range of eighty to three hundred kfci) and modulation carrier 34 (for example, a sine wave signal in the range of approximately twenty to one hundred kfci). The modulation content may comprise linear position (or “LPOS”) data, or auxiliary data (e.g. manufacturing data) as indicated at 31 , and general purpose data such as synchronization signals and error correction/detection data as indicated at 32 . Other content may include encoding data as indicated at 33 , including “biphase” or Manchester encoding, NRZ, NRZI, PR4 and other known encoding techniques; however, quadrature amplitude (“I & Q”) modulation schemes may not be desirable because the primary timing task of the carrier signal is adversely affected. Manchester encoding provides the advantage of simplified decoding due to the simpler embedded clock structure.
[0024] The resolution of the linear position data may be as coarse as 10 cm to as fine as 1 cm, although greater resolution requires greater bandwidth which is undesirable because it reduces the robustness of the signal. Assuming digital modulation bandwidth (double sided) of the pilot tone carrier of approximately 10 KHz and a tape speed of 2 m/s, Manchester encoding would encode 2.5 kbps or 1.25 bits/mm; thus, 125 bits would be encoded in a span of 10 cm, which is sufficient for an accurate LPOS signal. Other more sophisticated encoding schemes could produce as much as 50 bits/cm in the same bandwidth.
[0025] [0025]FIG. 6 is a schematic diagram of the receiver for this embodiment. The AM signal first passes through band pass filter 44 and is an input to the phase locked loop 46 , which tracks its frequency and phase. The primary use of this input is to time the time-based servo pulses, as in the embodiment described above, and also to synchronously demodulate the AM signal by use of an analog multiplier 47 . The output of analog multiplier 47 passes sequentially through a low pass filter 49 ; a detector 51 ; a channel code demodulator 52 ; appropriate encoding 53 for data words, sync signals, and error correction codes, as applicable; and suitable LPOS counters and auxiliary text memory 54 . The result is an output signal 55 that is transferred to the drive controller of the system (not shown).
|
Servopositioning systems, methods, formats, and data recording media used in association with the same, employing additional timing reference information to improve immunity to time-based errors caused by instantaneous speed variations.
| 6
|
This is a division of application Ser. No. 08/375,867, filed on Jan. 20, 1995, now U.S. Pat. No. 5,665,667 which in turn is a continuation-in-part of Ser. No. 08/252,800, filed Jun. 2, 1994, now U.S. Pat. No. 5,536,693.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a process of producing palladium-alkali or palladium/promoter metal/alkali metal catalysts useful in the oxacylation of olefins or diolefins. In particular, effecting the production of vinyl acetate from ethylene, acetic acid and an oxygen containing gas. More particular, the present invention relates to the process of producing palladium-gold-potassium fluid bed catalyst useful in the manufacture of vinyl acetate.
The production of vinyl acetate by reacting ethylene, acetic acid and oxygen together in the gas-phase in the presence of a catalyst containing palladium, gold and an alkali metal acetate promoter is known. The catalyst components are typically supported on a porous carrier material such as silica or alumina.
In early examples of these catalysts, both the palladium and gold were distributed more or less uniformly throughout the carrier (see for example U.S. Pat. Nos. 3,275,680, 3,743,607 and 3,950,400 and GB 1333449). This was subsequently recognized to be a disadvantage since it was found that the material within the inner part of the carrier did not contribute to the reaction since the reactants did not diffuse significantly into the carrier before reaction occurred. In other words, a significant amount of the palladium and gold never came into contact with the reactants.
In order to overcome this problem, new methods of catalyst manufacture were devised with the aim of producing catalysts in which the active components were concentrated in the outermost shell of the support (shell impregnated catalysts). For example, GB Patent No.1500167 claims catalysts in which at least 90% of the palladium and gold is distributed in that part of the carrier particle which is not more than 30% of the particle radius from the surface. GB Patent No. 1283737 teaches that the degree of penetration into the porous carrier can be controlled by pretreating the porous carrier with an alkaline solution of, for example, sodium carbonate or sodium hydroxide.
Another approach which has been found to produce particularly active catalysts is described in U.S. Pat. No. 4,048,096. In this patent shell impregnated catalysts are produced by a process comprising the steps of (1) impregnating a carrier with aqueous solutions of water-soluble palladium and gold compounds, the total volume of the solutions being 95 to 100% of the absorptive capacity of the catalyst support, (2) precipitating water-insoluble palladium and gold compounds on the carrier by soaking the impregnated carrier in a solution of an alkali metal silicate, the amount of alkali metal silicate being such that, after the alkali metal silicate has been in contact with the carrier for 12 to 24 hours, the pH of the solution is from 6.5 to 9.5; (3) converting the water-soluble palladium and gold compounds into palladium and gold metal by treatment with a reducing agent; (4) washing with water; (5) contacting the catalyst with alkali metal acetate and (6) drying the catalyst. Using this method, catalysts having a specific activity of at least 83 grams of vinyl acetate per gram of precious metal per hour measured at 150° C. can allegedly be obtained. Shell impregnated catalyst are also disclosed in U.S. Pat. No. 4,087,622. Finally, U.S. Pat. No. 5,185,308 also discloses shell impregnated Pd--Au catalyst and the process of manufacture. Each of the above patents is primarily concerned with the manufacture of fixed bed catalyst useful in the manufacture of vinyl acetate.
It would be economically beneficial if the oxacylation of olefins or diolefins, in particular the manufacture of vinyl acetate from ethylene, acetic acid and oxygen could be performed in a fluid bed process. However, until the discovery of the process of the present invention, the preparation of Pd--Au--alkali metal catalyst in fluid bed form has not led to a catalyst having the necessary properties which can lead to an economically viable fluid bed process for the manufacture of vinyl acetate.
SUMMARY OF THE INVENTION
It is the primary object of the present invention to provide a process for the manufacture of a fluid bed Pd based catalyst used in the oxacylation of olefins or diolefins.
It is another object of the present invention to provide a process of manufacturing of a fluid bed Pd based or Pd--Au--K catalyst used in the manufacture of vinyl acetate.
Additional objects and advantages of the 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. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
To achieve the foregoing objects of the present invention, the process for manufacture of a fluid bed catalyst having the following formula: Pd--M--A wherein M comprises Ba, Au, Cd, Bi, Cu, Mn, Fe, Co, Ce, U and mixtures thereof, A comprises an alkali metal or mixtures thereof (preferably K) used in the oxacylation of olefins or diolefins, in particular the manufacture of vinyl acetate from ethylene acetic acid and oxygen, comprises milling a fixed bed oxacylation (e.g. vinyl acetate) catalyst precursor comprising Pd--M on a fixed bed support with a fluid bed catalyst aqueous binder material to form a uniform aqueous slurry, spray drying the aqueous slurry to remove the water to form microspheroidal particles of solid fluid bed catalyst precursor, impregnating the microspheroidal particles with a solution of an alkali metal salt to form the fluid bed catalyst. Typically, the weight percent of Pd and alkali in the catalyst are: 0.1 to 5.0 wt % Pd, preferably 0.5 to 2.0 wt %; and alkali greater than 0 to about 10 wt %, preferably 0.01 to 5 wt %. Typically the weight percent of M may range from 0 to about 5%, preferably greater than 0 to 5%, especially preferred being 0.1 to 3%. The balance of the catalyst comprises the inert support material. Depending upon the particular fixed bed catalyst precursor used, the alkali metal acetate may already be present and the need for additional alkali metal salt impregnation after spray drying in some cases may be minimal or non-existent.
Also the need for catalyst to be highly attrition resistant for economical use in fluid bed, will generally require that the catalyst undergo a calcination step at some stage of its preparation. In general it is advantageous for this calcination to occur after the catalyst is spray dried and before the alkali metal salt is added, but with certain fixed bed catalyst precursors the calcination step may be applied after addition of alkali metal salt. After catalyst calcination, a final chemical reduction step may be advantageous. The Pd and other reducible metals present can be reduced with either liquid or gaseous reducing agents as known to those skilled in the art.
A preferred embodiment of the process of the present invention comprises impregnating a fixed bed support material (e.g. silica, zirconia, alumina or mixture thereof) with a metal salt solution of Pd and Au, reducing the metal salts to form metallic Pd and Au on the surface of the support and drying the impregnated support to form the fixed bed catalyst precursor.
In another preferred embodiment of the present invention the drying of the aqueous slurry is performed by spray drying the catalyst slurry at an elevated temperature to form microspheroidal particles of catalyst.
In another preferred embodiment of the present invention a metal salt solution of Au and Pd is prepared to provide a weight ratio of Au to Pd on said resulting catalyst of between 0.10 to 1.00, more preferably 0.2 to 0.8 and especially preferred being 0.25 to 0.75. The specific details of preparation of the salt solutions is conventional and well within the skill of one having ordinary skill in the art. See, for example, U.S. Pat. No. 5,185,308 herein incorporated by reference.
In a preferred embodiment of this aspect of the present invention the alkali metal is selected to be potassium.
DETAILED DESCRIPTION OF THE INVENTION
Reference will now be made in detail to the present preferred embodiments of the invention of which the following examples are set forth for illustrative purposes only.
It has been demonstrated that Pd/Au/K fluid bed catalyst can be obtained by employing the novel procedure set forth below. The procedure comprises impregnating fixed bed support material, in general having a particle size equal to or greater than at least 0.5 mm, preferable at least 3 mm, with an aqueous metal salt solution of Pd and Au, reducing the metal salts to deposit Au and Pd on the support material, drying the support material to form a fixed bed catalyst precursor, milling the fixed bed catalyst precursor with an inert fluid bed aqueous binder to form a uniform aqueous slurry, drying the slurry to remove the water to form microspheroidal particles of catalyst precursor, calcining the dried catalyst and impregnating the spray dried material with a solution of a metal salt of an alkali metal.
Preferably, an aqueous salt solution of Pd and Au are utilized, most preferably an aqueous solution of sodium tetrachloropalladate and chloroauric acid.
A variety of reducing agents may be utilized to precipitate the Pd and Au on the support surface. Typically the precipitation is performed with sodium silicate followed by reduction with hydrazine hydrate.
Size reduction of the dried particles is performed by conventional means such as grinding, crushing, milling, etc. Typically, spray drying of the aqueous slurry is the preferred procedure of removing the water from the aqueous slurry. However, other conventional means of drying the particles to form microspheroidal particles is envisioned in the practice of the present invention.
The dried catalyst is preferably calcined at 400° to 850° C. in air for 1 to 24 hours. Most preferably calcination is between 600° to 700° C. in air for about 1 to 6 hours.
Preferably, an aqueous solution of the metal salt of an alkali metal is utilized. The preferred alkali metal is potassium and an aqueous solution of potassium acetate is typically utilized to impregnate the spray dried particles although other alkali carboxylic salts may be utilized.
In the practice of the present invention suitable fluid bed support/binder materials include silica, alumina, zirconia, and titania among others and mixtures thereof. In general, aqueous sols of these materials are preferred, but fine solid particles which can serve as binders when suspended in liquid medium other than water, for example alcohols such as ethanol, butanol, iso-butanol, are also applicable. Typically 90% of catalyst particles exiting the spray dryer are less than 200 microns in diameter. Preferably 80% of catalyst particles exiting the spray dryer are less than 100 microns in diameter.
Fluid bed catalysts, prepared by this procedure have been demonstrated as very effective for the production of vinyl acetate by reacting ethylene, oxygen, nitrogen and/or CO 2 and acetic acid. Typical feed ratios are between 0.05-0.4 O 2 :0.2-0.7 N 2 /CO 2 :1.0 C 2 H 4 :0.05-0.5 CH 3 COOH, preferably 0.08-0.35 O 2 :0.25-0.65 N 2 :1.0 C 2 H 4 :0.07-0.35 CH 3 COOH, especially preferred being 0.1-0.3 O 2 :0.3-0.6 N 2 :1.0 C 2 H 4 :0.1-0.3 CH 3 COOH.
The following examples are illustrative of our invention.
EXAMPLE 1
Preparation of Fixed Bed Catalyst as Reported in U.S. Pat. No. 5,185,308
A representative fixed bed catalyst of composition 0.91 wt % Pd, 0.34 wt % Au, and 3.2 wt % K on KA-160 silica spheres (5 mm) was prepared as follows:
The appropriate weights of Na 2 PdCl 4 and HAuCl 4 were dissolved in 8.7 ml distilled water and impregnated on 15 g KA-160 silica spheres. The wet solid was allowed to sit undisturbed for several hours. An aqueous solution of sodium metasilicate was then poured onto the wet solid. Again the solid was left undisturbed overnight. An aqueous solution of hydrazine hydrate was then added to the solution covering the catalyst spheres. The wet solid was left undisturbed overnight. The solid was then drained and washed free of chloride with distilled water. The solid was dried at 60° C., the appropriate amount of potassium acetate in aqueous solution was then impregnated upon the solid and the finished catalyst was dried at 60° C.
Evaluation of this catalyst under the following conditions:
Feed: C 2 H 4 :HOAc:O 2 :He=53.1:10.4:7.7:28.6
GHSV: 3850/hr
Temp: 150° C. (at hot spot)
Pressure: 115 psig
Catalyst Charge: 2.50 g
Catalyst Dilution: 30 cc of 4 mm glass beads
produced 94.2% selectivity to vinyl acetate at 8.0% ethylene conversion (calculation based on the reported oxygen conversion of 32.2%).
EXAMPLE 2
Preparation of Fluid Bed Catalyst by the Same Technique as Example 1
An attempt to prepare a fluid bed catalyst by the same method of Example 1 except using a microspheroidal silica support in place of KA-160 was carried out. Inspection of the finished catalyst under a microscope indicated the presence of reduced metal particles mixed with the support as well as "clumps" of agglomerated metal and support. Analysis of the catalyst indicated only 0.16 wt % Pd and 0.072 wt % Au, indicating that most of the metal had been washed away.
Evaluation of 5.0 grams of the catalyst under the conditions of Example 1 yielded only 0.56% ethylene conversion with 86% selectivity to vinyl acetate.
EXAMPLE 3
Preparation of Fluid Bed Catalyst by the Technique of the Present Invention
A catalyst with targeted composition corresponding to 0.90 wt % Pd, 0.40 wt % Au, 3.1 wt % K was prepared by the preferred method using the steps indicated above.
The Na 2 PdCl 4 (8.57 g) and HAuCl 4 (2.18 g) were dissolved in 128 g of distilled water. This solution was then slowly added to 210 g of the spherical silica support (KA-160, Sud Chemie). The solution support mixture was swirled and gently shaken to insure even coverage. This mixture was allowed to sit for two hours at room temperature and essentially all the solution was absorbed into the support. A solution of 15.1 g of sodium metasilicate dissolved in 252 g of distilled water was poured onto the impregnated support. This mixture was allowed to sit for three hours. At this time 26.8 g of hydrazine hydrate was added and the mixture was permitted to sit overnight. The solid spheres were then washed thoroughly with distilled water to remove chloride from the solid. The solid was dried at 60° C. overnight, then the dried solid spheres were crushed. The crushed catalyst (200 g) was milled overnight with 133.3 g of silica sol (30 wt % SiO 2 ) and sufficient water to provide a millable consistency. The catalyst slurry was then spray dried to form microspheroidal particles. A portion of the microspheroidal solid (15 g) was then impregnated with 0.75 g of potassium acetate dissolved in 10 g of distilled water. This solid was dried at 60° C. overnight. Microscopic examination of the finished catalyst indicated well-formed microspheroidal particles.
Evaluation of the catalyst was carried out in a 40 cc fluid bed reactor under the conditions specified in Example 1 except the catalyst bed was composed of 7.5 grams catalyst diluted with sufficient inert silica fluid bed support to produce a total bed volume of 30 cc. An ethylene conversion of 5.2% with 93.7% selectivity to vinyl acetate was obtained, indicating that the preparation method employed was effective.
EXAMPLES 4-8
Effect of Process Variables on Fluid Bed Catalyst Performance
The catalyst prepared in Example 3 was tested in order to determine the effect of oxygen feed concentration, space velocity and temperature on performance. The percent ethylene fed was maintained constant and nitrogen fed was adjusted downward as oxygen or acetic acid levels increased. The following observations were noted:
TABLE I______________________________________Example 4 5 6 7 8______________________________________% O.sub.2 Fed 7.7 15.4 15.4 15.4 15.4% HOA.sub.c Fed 10.4 10.4 15.8 10.4 10.4T (deg-C.) 160 160 160 160 170GHSV 3080 3850 3850 3080 3080C2=Conversion 6.0 7.4 7.7 8.5 10.2(%)VAM 93.0 90.6 92.5 91.2 86.4Selectivity(%)______________________________________
Table I set forth above shows that good selectivity and conversion are maintained over a wide range of feed conditions.
EXAMPLE 9
Dissolved 6.80 g of Na 2 PdCl 4 and 1.73 g of HAuCl 4 in 110 g of distilled H 2 O and impregnated this solution on 200 g of KA-160 silica spheres (5 mm). Allowed wet solid to sit for two hours then added a solution of 12.0 g of Na 2 SiO 3 in 240 g of distilled H 2 O, mixed gently and allowed solid to sit undisturbed for 2 hours. To this mixture was added 21.3 g of 55% hydrazine hydrate. This mixture was allowed to sit overnight. Drained solution from solid and washed solid with fresh distilled H 2 O until negative test for chloride was obtained. The catalyst precursor spheres were then dried overnight at 60° C. 200 g of this catalyst precursor were crushed and mixed with 19.05 g crushed KA-160 (washed to remove Cl), 202.8 g of Snotex-N-30 silica sol (36 wt % solids), and sufficient water to provide a millable consistency to the slurry. This slurry was milled overnight, then spray dried. The microspheroidal catalyst particles were oven dried at 110° C. Elemental analysis of this solid found 0.62 wt % Pd and 0.23 wt % Au.
Dissolved 1.66 g of potassium acetate in 13.5 g of distilled H 2 O and impregnated this solution of 15.85 g of the above microspheroidal particles. After drying the solid contained 9.5 wt % potassium acetate.
EXAMPLES 10 THROUGH 13
A mixture of 14.5 g of the catalyst in Example 9 and sufficient fluidizable silica to provide 30 cc were placed in the fluid bed test reactor. The conditions and results are as follow:
______________________________________Example 10 11 12 13______________________________________% C.sub.2 H.sub.4 fed 50.2 48.4 45.6 45.9% O.sub.2 fed 5.3 8.6 9.7 8.9% HOAc fed 10.3 9.9 13.5 13.7% N.sub.2 fed 34.3 33.1 31.2 31.4Total Flow 380.8 394.3 418.5 415.9Temp (C.) 156 157 165 158Pressure (psig) 115 115 115 115C.sub.2 H.sub.4 conversion (%) 12.9 17.5 20.5 16.2VAM selectivity (%) 90.0 87.7 86.1 89.3______________________________________
EXAMPLE 14
A portion of the catalyst prepared in Example 9 was calcined at 640° C. in air for 2 hours. This sample was reduced in 21% H 2 in N 2 stream, starting at room temperature and ramping the temperature gradually to 100° C. This temperature was held for 3 hours then the catalyst was cooled under N 2 . This sample was evaluated for attrition resistance and found to be sufficiently attrition resistant for commercial use.
EXAMPLE 15
A 16.0 g portion of the catalyst prepared in Example 9 was calcined at 640° C. in air for 2 hours. To this calcined solid was added 1.6 g of potassium acetate dissolved in 13.5 g H 2 O. The catalyst was then dried at 60° C.
EXAMPLES 16 THROUGH 17
16.05 g of the catalyst of Example 15 was mixed with sufficient inert microspheroidal silica to give 33 cc. This catalyst mixture was tested in a fluid bed reactor with the following results.
______________________________________Example 16 17______________________________________% C.sub.2 H.sub.4 fed 47.2 45.2% O.sub.2 fed 6.7 10.5% HOAc fed 14.0 13.4% N.sub.2 fed 32.2 30.9Total Flow 405 422.5Temp (C.) 154 168Pressure (psig) 115 115C.sub.2 H.sub.4 conversion (%) 11.1 16.9VAM selectivity (%) 91.8 83.7______________________________________
EXAMPLE 18
A spray dried catalyst was prepared in the manner described in Example 9 except that it contained 17 wt % silica from the sol and levels of palladium and gold reagents were increased to give 0.69 wt % Pd and 0.25 wt % Au (no potassium acetate). 16 g of this microspheroidal solid was calcined 0.5 hours at 400° C. followed by 2 hours at 640° C. 1.57 g of potassium acetate dissolved in 13.5 g of distilled H 2 O was impregnated upon 15.0 g of the calcined solid. This final catalyst was dried at 60° C.
EXAMPLES 19 THROUGH 21
13.3 g of the catalyst of Example 18 was mixed with sufficient inert microspheroidal silica to give 30 cc. This catalyst mixture was tested in a fluid bed reactor with the following results.
______________________________________Example 19 20 21______________________________________% C.sub.2 H.sub.4 fed 47.9 45.6 44.8% O.sub.2 fed 5.1 9.7 11.1% HOAc fed 14.2 13.6 13.4% N.sub.2 fed 32.7 31.0 30.6Total Flow 399 419 426Temp (C.) 151 158 167Pressure (psig) 115 115 115C.sub.2 H.sub.4 conversion (%) 11.5 15.5 18.7VAM selectivity (%) 92.0 89.3 86.0______________________________________
EXAMPLE 22
Other fixed bed vinyl acetate catalysts which contain the metals distributed essentially throughout the support particle may also be used as the fixed bed precursor of the present invention. For example the Pd/Au containing catalysts described in U.S. Pat. No. 3,743,607 may be advantageously used. A representative preparation of such a catalyst follows:
1 kg of silica support (3 mm) is impregnated with an aqueous solution of 10 g of Pd in the form of PdCl 2 and 0.4 g Au in the form of HAuCl 4 . The thoroughly dried solid is then placed in a solution of 3% hydrazine hydrate at 40° C. After the reduction of the Pd and Au is complete the solid is washed to remove chloride. After drying the catalyst precursor can then be crushed, and milled in the presence of silica sol (sufficient sol to provide ˜20 wt % silica from the sol). Additional water is added until the slurry is of the appropriate viscosity for efficient milling. The milling is continued overnight, then the milled slurry is spray dried to produce microspheroidal catalyst particles which are suitable for use in a fluid bed reactor. Impregnation of these microspheroidal particles with ˜7.0 wt % potassium acetate results in fluid bed catalyst which is both active and selective for the oxidation of ethylene plus acetic acid to vinyl acetate.
EXAMPLE 23
A catalyst containing palladium acetate, cadmium acetate, and potassium acetate is prepared according to the teachings of U.S. Pat. No. 3,759,839. The appropriate amounts of these three reagents are dissolved in acetic acid (sufficient to fill the pore volume of the support) and deposited on silica spheres (5 mm) to give, upon drying, the following composition: 1.5 wt % palladium acetate, 4.5 wt % cadmium acetate, and 4.5 wt % potassium acetate. This fixed bed catalyst can then be used as a precursor in the preparation of a fluid bed vinyl acetate catalyst. The spheres of the fixed bed catalyst are crushed, then ball milled with the appropriate amount of silica sol (Nisson Snotex-N-30) to result in ˜17% silica from sol in the spray dried catalyst. Sufficient water is also added to the slurry to provide a fluid consistency. After sufficient milling (usually overnight is adequate) the slurry can be spray dried to form microspheroidal, fluidizable catalyst particles. This fluidizable catalyst can then be calcined, and reduced with either gaseous reducing agents (such as H 2 or ethylene) or liquid reducing agents (such as aqueous hydrazine), or reduced in situ. When tested in the fluid bed reactor under the conditions described in Example 3, good yields of vinyl acetate are obtained.
While the invention has been described in conjunction with specific embodiments, it is evident that many alterations, 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.
|
A process of producing a fluid bed oxacylation catalyst for olefins and diolefins having the following formula Pd--M--A where
M=Au, Cd, Bi, Cu, Mn, Fe, Co, Ce, U and mixtures thereof,
A=an alkali metal or mixture thereof, and
M is present in the range of from 0 to 5 wt %, comprising milling a fixed bed oxacylation catalyst precursor comprising Pd--M on a fixed support with a fluid bed catalyst aqueous binder material to form a uniform aqueous slurry, drying the aqueous slurry to remove the water to form microspheroidal particles of solid fluid bed catalyst precursor, impregnating the microspheroidal particles with a solution of alkali metal salt to form the fluid bed catalyst. The catalyst is particularly useful in the manufacture of vinyl acetate from ethylene, acetic acid and oxygen.
| 1
|
TECHNICAL FIELD
[0001] The present invention describes a data carrier destruction method for rendering confidential data carriers of paper and likewise unreadable and for their destruction, in a manner safeguarded from access, wherein confidential data carriers are collected at a location of origin in security collection containers, are collected by way of a collection vehicle and finally led to a paper recycling facility, a collection vehicle for picking up and transporting confidential data carriers of paper and likewise, which are collected in security collection containers, for carrying out a data carrier destruction method, as well as the use of a disintegration device for the hydromechanical treatment of confidential data carriers in the form of paper and likewise.
STATE OF THE ART
[0002] Despite the fact that much information is exchanged in an electronic manner nowadays, huge quantities of confidential documents and data carriers, in the form of papers or information carriers of paper or similar material of cellulose or wood pulp still however continue to accumulate in companies, but also in the private sphere. A discrete disposal is of utmost importance in many fields, in the case that these confidential data carriers are no longer required. A disposal which is safeguarded against access by unauthorised third parties has been achieved in recent years by way of various document destruction methods.
[0003] In the simplest case, the confidential documents can be reduced in size into shreds directly on location in offices by way of electromechanical shredding facilities, and thus reduced in size to the extent that they are difficult to be reconstructed. However, with such a procedure, one cannot completely prevent unauthorised persons obtaining access to the confidential document before the shredding process. Correspondingly many shredding appliances are to be procured, depending on the quantity of confidential documents to be destroyed, by which means the access possibilities by third parties are widened to each in shredding facility. The shred size which can be achieved with the obtainable shredding appliances however does not often correspond to the security level which is required in accordance with the confidentiality. Data carriers can also be reconstructed after the shredding due to this.
[0004] A document destruction method of the applicant is known from EP1476376, and this renders an access impossible during the complete procedure and is implemented in a centralised manner. Confidential documents in an office are collected at a central location in a security collection container. The confidential documents are inserted into the security collection container through an insert opening and thereafter can no longer be removed from the sealed and electronically secured security collection container. An undesired access to confidential data carriers can be ruled out, since access obstacles are arranged at the insert opening of the security collection container, and the opening mechanism can only be opened by electronic means. The security collection container is part of a disposal system, in which filled security collection containers are collected which is to say fetched, and exchanged with empty security collection containers. The security collection containers are emptied on location at the customer, into a container of a collection vehicle, likewise in a secured manner, wherein the container can electronically open the opening mechanism of the security collection container in a manner such that an access by third parties is also prevented with the filling transfer of the confidential documents. Means are provided for the blanket surveillance of the transport and each opening of the security collection container, so that the safeguarding from access is protocolled.
[0005] Of course, the container of the collection vehicle also permits no access into its interior, so that a complete safeguarding of the confidential documents from unauthorised access is ensured during the complete destruction process. The collected confidential documents are transported by the collection vehicle to a central disposal facility, usually a certified shredding facility, where these document are reduced in size according to an as high as possible security level, such that the resulting snippets are suitable for paper recycling. Nobody has access to the confidential documents to be shredded, even on ejecting the collected documents out of the container of the collection vehicle into the shredding facility. Surveillance also takes place on ejecting the documents to be destroyed, by which means an unauthorised access safeguard can be confirmed here too. After treatment in the shredding facility, the shreds are conveyed to a paper recycling facility and can be recycled there. This process is represented schematically in FIG. 3 . The possibility of confidential documents getting lost exists, for example in the case of an accident of the collection vehicle on the way to the certified shredding facility 5 , due to the fact that the collected confidential documents, after collection at a location of origin A, are not destroyed until in this facility.
[0006] Now it is possible to provide the collection vehicles with shredding facilities, by which means a so-called mobile shredding can be implemented. Such a system is known for example from WO0170406. The confidential, still readable data carriers collected in the security collection containers can be shredded on location on the collection vehicle after the secured transfer into the container, and be reduced in size according to a define security level, wherein an unauthorised access can likewise be prevented. The on-location shredding however has some disadvantages.
[0007] Particularly powerful cutting mechanisms are to be applied, so that the occurring, differently thick paper types and confidential documents which occur in the most varied of formats can be reduced in size and shredded according to a medium security level. If the size reduction is to be effected with a cross-cut or particle-cut, then such shredding appliances have a loud operating noise, as is known. The applied cutting mechanisms are complex and must be supplied with sufficient energy, in order for a trouble-free size reduction of completely filled security collection containers to be able to be carried out. The shredding appliance must be operated over a longer period of time, with a running motor or engine of the collection vehicle for this. In practise, the power capability of the shredding appliances is not sufficient to be able to reduce in size the fed quantity of confidential data carriers within a short period of time and according to a high security level. It is difficult to commercially and successfully reduce in size the payload quantity of confidential data carriers due to the high intrinsic weight and volume of the shredding appliance. For security reasons and so as to be able to transfer the produced shreds to the paper recycling, the confidential data carriers shredded in a mobile manner must be transported to a certified shredding facility and be post-shredded there once again, before they can be transported into a paper recycling facility for recycling.
DESCRIPTION OF THE INVENTION
[0008] It is the object of the present invention, to provide a data carrier destruction method which prevents access to confidential documents of paper and likewise and includes a destruction step already during the collection of the documents, wherein the possible feed of the destroyed documents to paper recycling remains ensured, and one forgoes the additional treatment in a shredding facility.
[0009] The data carrier destruction method for this only entails a slight increase in effort with regard to apparatus, compared to disposal systems according to the state of the art.
[0010] A further object of the present data carrier destruction method is the implementation of a processing step on location at a location of origin and/or during the transport of the collected documents from the location of origin to a paper recycling facility, wherein the access to the collected, confidential documents is rendered impossible at all times.
[0011] A further object of the invention is the creation of a collection vehicle for the mobile implementation of a data carrier destruction method.
[0012] The advantages which can be attained by the method according to the invention, apart from the destruction with an as high as possible security level, wherein one can achieve the absolute impossibility of being able to reconstruct the confidential data carriers, is additionally the improved retention of the length of the paper fibres due to the tearing, instead of the cutting as occurs when shredding.
[0013] The diversion of the collected, confidential data carriers via a certified shredding facility on the way to a paper recycling facility can finally be avoided. The total investment can be significantly reduced in comparison to mobile shredding facilities, and the energy expense on location for the destruction of the data carriers is significantly lower according to the method according to the invention, than with known mobile shredding methods.
BRIEF DESCRIPTION OF THE DRAWING
[0014] A preferred embodiment example of the subject-matter of the invention is described hereinafter in combination with the accompanying drawings.
[0015] FIG. 1 shows a schematic view of the data carrier destruction method from the location of origin, the filling transfer of the confidential data carriers and the transport up to delivery in a paper recycling facility.
[0016] FIG. 2 shows a perspective view of an embodiment of a collection vehicle for collection, for transport and for the destruction of confidential data carriers,
[0017] FIG. 3 shows a schematic view of the procedure of a data carrier destruction method according to the state of the art, wherein collected confidential data carriers are delivered with and without mobile shredding, to a paper recycling facility via a certified shredding facility
DESCRIPTION
[0018] The data carrier destruction method for the destruction of confidential, personal and/or sensitive documents and data carriers 4 , in the form of papers or information carriers of paper or similar material of cellulose or wood pump, which is to say for rendering all these unreadable, is schematically represented in FIG. 1 .
[0019] The confidential data carriers 4 which are be destroyed are collected in closed security collection containers 1 at a location of origin A. Third parties have no access to the data carriers 4 after the input of the confidential data a carries 4 into the security collection container 1 . The security collection containers 1 which are filled which collected documents and data carriers 4 are transferred by filling into a collection vehicle 2 , wherein emptied security collection containers 1 are again returned back to the location of origin A.
[0020] A disintegration device 20 , also called pulper 20 , which comprises a trough having an interior 201 is located on the collection vehicle. The disintegration device 20 is coupled to a loading device 21 , by way of which the contents of the security collection containers 1 can be filled by transfer into the interior 201 of the disintegration device 20 , securely and without access to unauthorised persons. The loading device 21 can be designed as a lift or lift-and-rotate tipper which lifts the security collection containers 1 vertically relative to the disintegration device 20 . Such a lift can be carried along with the disintegration device 20 and thus with the collection vehicle 2 .
[0021] A circulation device 202 is provided, which circulates the mass of filled-in, confidential data carriers 4 which is located in the interior 210 . The circulation device 202 is designed as a stirrer in FIG. 1 and is arranged in the interior 201 .
[0022] A disintegration fluid, as a rule pure water, which is mixed with the data carriers 4 , is filled into the interior 201 . The confidential documents 4 in the interior 201 are brought into a suspension, which has a mud-like consistency, depending on the mixing ratio of the disintegration fluid to the quantity of documents. The disintegration fluid can selectively contain defibration-assisting chemicals. A mechanical defibration (disintegration) of the confidential data carriers 4 takes place in the disintegration device 20 , due to the circulation device 202 , wherein a hydromechanical defibration takes place in the interior 201 of the disintegration device 20 by way of the addition of the disintegration fluid.
[0023] The confidential data carriers 4 become unreadable and are already disintegrated into fibres within a few minutes, on account of the circulation of the filled-in data carriers 4 amid the action of the disintegration fluid. The confidential documents 4 are rendered unreadable in a targeted manner with this defibration, and are thus destroyed, wherein the resulting fibre length remains significantly larger than is the case after undergoing a shredding process. A destruction of the data carriers 4 according to the security level several is rendered possible with the described method due to the treatment in the interior 201 of the disintegration device 20 , so that the reproduction of the data located on the confidential data carriers 4 , according to the state of the science and the state of the art is impossible, in accordance with DIN standard 66399.
[0024] The disintegration or defibration of the confidential documents 4 in the disintegration device 20 represents the rendering of the data unreadable and simultaneously a recycling step of the paper and this takes place directly after filling into the disintegration device 20 . The disintegration process takes place within a few minutes due to the intrinsic friction and tearing at the circulation device 202 , of the confidential documents 4 with the disintegration fluid. The destruction of the confidential documents 4 which can be achieved by way of this take place immediately after filling into the interior 201 of the disintegration device 20 , wherein only a low energy effort needs to be expended for the one-off loading and the circulation which is carried out at least briefly. Accordingly, the disintegration process can continue to take its course whilst the collection vehicle 2 moves. The arising suspension of defibrated documents and disintegration fluid is moved during the journey even if the circulation device 202 is switched off, by which means a continuous mobile defibration is achieved.
[0025] The collection vehicle 2 transports the suspension of defibrated documents and disintegration fluid into a paper recycling facility 3 , in which the destroyed documents can be recycled for the production of paper. A transport to a certified shredding facility can be done away with on account of the mobile disintegration of the confidential documents 4 . The collected confidential documents 4 are present in a destroyed form according to a high security level and are already in a recyclable form.
[0026] The confidential documents 4 are unreadable and therefore destroyed, even if an undesired opening of the interior 201 and exit of the suspension should occur on the transport route of the collection vehicle 2 to the paper recycling facility 3 .
[0027] The disintegration device 20 can be installed on the loading surface of the collection vehicle 2 in a fixed manner or can be carried along on a trailer, coupled to the collection vehicle 2 . The disintegration device 20 can be arranged in a rotatable manner about a longitudinal axis, so that the circulation device 202 is accordingly designed as a disintegration device rotatable about the longitudinal axis. In a further embodiment, the circulation device can be designed as a rotor which is installed in the interior 201 . All possible circulation devices 202 accordingly require a circulation device drive which drives the circulation of the suspension in the interior 201 . This circulation device drive is usefully connected to the drive of the collection vehicle 2 .
[0028] In a further embodiment, the interior 201 of the disintegration device 20 can be filled with a constant quantity of disintegration fluid before starting the collection route of the collection vehicle 2 , wherein loaded data carriers 4 are simply added to the already existing suspension or to the quantity of disintegration fluid.
[0029] Security collection containers 1 as are already described in EP1476376 of the applicant can be applied, in order to prevent access by unauthorised persons to the confidential data carriers 4 . Thereby, the security collection containers 1 are completely closed and comprise an insert slot which by way of obstacles arranged in the interior of the security collection container 1 prevents confidential data carriers 4 from being able to be removed. An ejection flap is provided with an electromechanical closure. This electromechanical closure can be opened by way of suitable electronics, by way of which the ejection flap can be opened and the confidential data carriers 4 transferred by filling directly into the disintegration device 20 . It is particularly advantageous if the ejection flap of the security collection container 1 is actively connectable to the filling opening of the disintegration device 20 , so that a filling transfer can be achieved in a manner safeguarded from access.
[0030] Additional means are provided, which co-protocol the transport route of the security collection container 1 , for example by way of GPS tracking, and each opening of the ejection flap. The movement of the security collection container 1 can be completely recorded, and it can be proven that no undesired opening by unauthorised parties has taken place, on account of this.
[0031] The collection vehicle 2 can be designed as a tipper, by which means, given a disintegration device 20 fastened thereon, a simplified emptying of the contents from the interior 201 into the paper recycling facility 3 is rendered possible.
[0032] The collection vehicle 2 can also be designed in a manner such that the disintegration device 20 is fastened on a trailer, which is carried along by the collection vehicle 2 . Here too, the disintegration device 20 can also be designed fastened in a tippable manner.
[0033] The contents of the disintegration device 20 after the disintegration procedure, can also be removed from the interior 201 by suitable pump means, above all if the disintegration device 20 is fastened on the collection vehicle 2 in a stationary manner. The pump means can thereby either be fixedly connected to the collection vehicle 2 and/or to the trailer and be designed such that they can also be carried along, or the pump means are installed at the paper recycling facility 3 .
[0034] Trials have found that a mass share of the disintegration fluid of already at least 20% to the mass of the suspension leads to good destruction results. The use of 85% to 98% disintegration fluid to 15% to 2% solid manner which is to say data carrier quantity however is more preferable when using a disintegration device 20 . A metering device is provided, in order to add the disintegration fluid to the quantity of inputted data carriers 4 in a targeted manner. The mass of loaded data carriers 4 is determined by a weighing device of the loading device 21 , and the desired of quantity of disintegration fluid is added in a manner matched to this, by way of a metering device.
[0035] As to how an embodiment of the collection vehicle 2 ′ can look, is described hereinafter by way of FIG. 2 . The collection vehicle 2 ′ comprises a loading device 21 , by way of which confidential data carriers 4 which are to be destroyed can be filled from a security collection container 1 into a fill-in space 22 . The dry, confidential data carriers 4 are transported from the fill-in space 22 into the disintegration device 20 ′, which here is designed as a vertically standing disintegration device 20 ′, wherein the longitudinal axis or rotation axis of the disintegration device 20 ′ is aligned perpendicularly to the longitudinal axis of the collection vehicle 2 ′. Water as a disintegration fluid can be pumped out of a carried-along water tank 23 into the disintegration device 20 ′ in a controlled manner by way of pump means. The circulation device which is applied here but which is not visible can be operated at up to 1500 revolutions per minute, wherein the data carriers 4 within the disintegration fluid can be destroyed to an unreadable extent already after a few minutes.
[0036] The suspension, comprising 2% to 15% solid matter in the form of defibrated, confidential documents can be transported into a dewatering device 24 by way of further pump means, in which dewatering device disintegration fluid is separated from the suspension, so that a mixing ratio of solid matter to water of about one to one results. Here, a drying worm 24 serving as a dewatering device 24 is applied. The separated disintegration fluid is either re-fed to the water tank 23 , a replacement tank 23 ′ or directly to the disintegration device 20 ′. Dewatered suspension which has a significantly higher density than the suspension within the disintegration device 20 ′ can be pumped out of the dewatering device 24 into a storage tank 25 . The dewatered suspension has a mud-like form up to the consistency of a moist mass of paper, and is stored in this storage tank 25 during the transport by the collection vehicle 2 ′.
[0037] The collection vehicle 2 ′ can transport the suspension out of the storage tank 25 to the paper recycling facility 43 and be fed to the recycling there, due to the fact that the destroyed data carriers in the suspension are unreadable. However, it is also possible prior to this to intermediately store the suspension for example at the location of the operator of the collection vehicle 2 ′, since the data carriers are no longer readable. The journeys of the collection vehicle 2 ′ to the paper recycling facility 3 can be reduced to a minimum by way of this.
LIST OF REFERENCE NUMERALS
[0000]
1 security collection container
2 , 2 ′ collection vehicle
20 , 20 ′ disintegration device
201 interior 202 circulation device
21 loading device 22 fill-in space 23 water tank 23 ′ replacement tank 24 dewatering device 25 storage tank
3 paper recycling facility
4 confidential data carriers
A location of origin
5 shredding facility
|
A method for the destruction of data carriers preventing access to the process of rendering confidential data carriers, which consist of paper or similar material, unreadable and allowing the carriers to be destroyed. In the method, confidential data carriers are collected at the point of origin in secure collection containers, removed by a collection vehicle, and are supplied to a paper recycling plant in a final step. The interior of a mobile pulper, which is connected to the collection vehicle, is filled with the confidential data carriers, the carriers are mixed with a pulping fluid and the mixture is blended by an agitator to form a suspension of defibrated documents and pulping fluid, a hydromechanical pulping process taking place in the pulper before the suspension is supplied to the paper recycling plant.
| 3
|
BACKGROUND
1. The Field of the Invention
This invention relates to air pumps and, more particularly to novel systems and methods for reducing sound and vibration from air pumps used in aroma therapy.
2. The Background Art
Various mechanisms for treating an environment with moisture, medicaments, and the like have been developed using boilers, heaters, fans, and so forth. Aroma therapy involves evaporation, distribution, or other entrainment of volatiles, essential oils, or the like into breathing air, an atmosphere of a room, or other enclosed space. Applicant has previously developed various mechanisms for distributing atomized liquids into the atmosphere. Likewise, various systems for heating or dissolving aromatic or oil-based materials in a solvent to promote evaporation into the atmosphere have also been relied upon in the art. Meanwhile, various medical devices provide humidification of a space such as a “steam tent” or the like.
However, in aroma therapy, it would be an advance in the art to accommodate space, aesthetics, weight, stability, simplicity of use, ease of use, storage, and the like. Accordingly, it would be an advance in the art to provide an integrated system having suitable weight for stability, a sufficiently small size so excessive footprint and volume are not occupied on a dresser, table, or a night stand, and otherwise rendering a system easily located on furniture within a room. Likewise, it would be an advance in the art to provide an aesthetically pleasing shape integrating all of the functions required for driving an atomizer of, perfume, essential oils, or other material desired to be distributed within an ambient environment.
It would be an advance in the art to provide an air pump for use in aroma therapy that is virtually silent. Reducing sound by several decibels is very difficult because of the fundamental nature of a vibrating motor driving a diaphragm pump. Accordingly, it would be a substantial advance in the art to create a mechanism for damping, isolating, or both, the mechanical vibration and acoustic vibration within air through a mechanical and fluid systems in order to provide a virtually silent pump. It would also be an advance in the art to provide a pump having long life, inexpensive components, easily replaceable parts, few moving parts, few wearing parts, economical maintenance, and simple assembly and operation.
BRIEF SUMMARY OF THE INVENTION
In view of the foregoing, in accordance with the invention as embodied and broadly described herein, a method and apparatus are disclosed in one embodiment of the present invention as including a system having a housing for a pump driven by an oscillating motor to draw liquids from a reservoir and distribute them through an eductor into the atmosphere.
The method may include adjusting an electronic controller to control at least one of a duration of operation and a duration of a delay between periods of operation of the pump. Operating the pump pressurizes ambient air into a flow that may be through other equipment such as an aquarium or an atomizer.
In some embodiments, the duty cycle may be controlled by controlling the ratio of the duration of operation to the duration of the delay plus the duration of operation. A method may provide a housing, a motor being disposed inside the housing and electrically powered to drive the pump.
In some embodiments, the pump comprises a pump body fitted with a valve plate captured in a pinch slot to support pressure between the pump body and valve plate. Seals positioned about openings passing the flow into and out of the pump may minimize pressure exposure of the structure of the pump. This is an improvement over conventional gaskets by being sized to fit within from about one to about three diameters, typically about two diameters, of the aperture corresponding to each seal.
The method may include the pump disposed within the housing, driven by a motor, and comprising a diaphragm compressing air and providing a flow thereof at a pressure greater than ambient pressure. The motor may have a coil and a magnet operably connected to reciprocate an armature magnet back and forth to move the diaphragm.
A control system operably connected to the coil may control electricity flowing to the coil, including voltage, current, off and on conditions, and so forth. The control system may include an actuator adjustable by a user to selectively and arbitrarily control the duration of delivery of electrical energy to the coil. A user may selectively and arbitrarily control a delay between adjacent periods of continuous delivery of electrical energy to the coil. A user may also arbitrarily control the duration of delivery of electrical energy to the coil and a delay between adjacent periods of continuous delivery of electrical energy to the coil.
A control system may provide infinitely variable adjustment between extremes (max and min values), to be set by a user arbitrarily selecting duration of operation, duration of deactivation between periods of operation of the motor, or both.
In some embodiments, a user may select a first time period corresponding to operation of the pump, arbitrarily selected between a first minimum time and a first maximum time, and selecting by a user a second time period corresponding to a delay in operation of the pump. The delay may be arbitrarily selected between a second minimum time and a second maximum time.
Typically, an apparatus may be constructed to contain a housing, a pump disposed within the housing (typically of a type having a diaphragm compressing air drawn from the ambient), and a magnetic electric motor driving the pump. The motor may be an oscillating type, having a coil and a first magnet (electromagnet) connected to reciprocate an electric field. The electromagnet drives a permanent magnet back and forth to oscillate the diaphragm. The pump may have two diaphragms in symmetric arrangement to reduce vibration.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing features of the present invention will become more fully apparent from the following description and appended claims, taken in conjunction with the accompanying drawings. Understanding that these drawings depict only typical embodiments of the invention and are, therefore, not to be considered limiting of its scope, the invention will be described with additional specificity and detail through use of the accompanying drawings in which:
FIG. 1 is an exploded view of one embodiment of a quite pump apparatus in accordance with the invention;
FIG. 2 is a cross-sectional, side, elevation view of one embodiment of an apparatus with certain items rendered schematically to show their arrangement;
FIG. 3 is an exploded view of a pump for use in an apparatus and method in accordance with the invention as disclosed in FIGS. 1-2 ;
FIG. 4 is an exploded view of the inner housing of the apparatus of FIGS. 1-2 with its liner and other vibration isolation mechanisms;
FIG. 5 is an exploded view of the end cap for the inner housing having the motor magnet potted therein and illustrating an exploded view of the mounting and filter hardware as well as isolation feet for this portion of the inner housing and motor support; and
FIG. 6 is a cross-sectional, side, elevation view of the apparatus of FIG. 1 assembled and illustrating the flow of air therethrough.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
It will be readily understood that the components of the present invention, as generally described and illustrated in the drawings herein, could be arranged and designed in a wide variety of different configurations. Thus, the following more detailed description of the embodiments of the system and method of the present invention, as represented in the drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of various embodiments of the invention. The illustrated embodiments of the invention will be best understood by reference to the drawings, wherein like parts are designated by like numerals throughout.
Referring to FIG. 1 , a system 10 or apparatus 10 may provide a supply of air virtually silently to drive various types of life support or breathable air. For example, a system 10 in accordance with the invention may supply air to an aroma therapy atomizer, aquarium, or the like. In general, an apparatus 10 may include an outer housing 12 . The outer housing 12 may be divided into two portions in order to be able to receive other components therewithin.
In the illustrated embodiment, the outer housing contains electronics 14 or control systems 14 to control the volume, duration, and delay times between delivery of a supply of pressurized air. In the illustrated embodiment, an inner housing assembly 16 or inner housing 16 further provides isolation to separate a motor 18 or the larger and fixed components thereof from a pump 20 within the inner housing 16 .
Mechanical isolation of the inner housing 16 from the outer housing 12 is provided by use of elastomeric components, damping, and decoupling of supports and by supports between the inner housing 16 or the outer housing 12 . Selective positioning of required connections minimizes mechanical advantage and connection between various components.
Moreover, the inner housing 16 is substantially sealed as to any gaps that might pass acoustic vibrations. The exception to the sealing is the path of air actually being inducted and pressurized before being pumped out for use. Even that stream or flow of air is selectively isolated from certain components, passed through tortuous and narrow passages, to filter acoustics while exposed to other components, according to particular needs.
Referring to FIG. 2 , an upper shell 22 of the outer housing 12 is positioned opposite a lower shell 24 of the housing 12 . In the illustrated embodiment, feet 26 are formed of an elastomer selected for its softness and thus damping of vibration. In this way, the outer housing 12 , may be isolated further from its environment, such as a supporting surface, table, dresser, or the like.
The damping ability of the feet 26 in an axial direction (e.g., vertically, for example) may be substantial according to the selection of the elastomer from which the feet 26 are formed. Meanwhile, both the softness of the elastomer and the length or extent of each of the feet 26 also tends to provide radial isolation against any transmission of mechanical vibration therebetween.
In the illustrated embodiment, a seal 28 may be formed as a gasket, ‘O’ ring, or the like. Typically, the gasket 28 may be selected from various elastomers and shaped to provide a substantially hermetic seal between the upper shell 22 and lower shell 24 of the housing 12 . An outlet 30 provides a controlled penetration between the outer housing 12 and the environment. Nevertheless, the outlet 30 in one currently contemplated embodiment is isolated from the other components contained within the outer housing 12 by a long, flexible tube that wraps inside the housing 12 in order to avoid supporting any mechanical connection of force or movement between the outlet 30 fixed to the housing 12 , and any of the contained components therewithin.
Likewise, another penetration is made to support a fitting 32 supporting entrance of an electrical power cord. The length and flexibility of the cord 33 , and its contained components, along with the selection of the softness of the elastomer from which the fitting 32 is fabricated provide for a tight, interference fit between the outer housing 12 and the fitting 32 . For example, fasteners securing the upper shell 22 to the lower shell 24 capture the fitting 32 therebetween and can distort it elastomericaly in order to confirm a tight, hermetic seal therebetween.
The inlet 34 may be engineered as the only aperture 34 through which air may enter into the outer housing 12 . All other penetrations are typically sealed against passage of air and transmission of sound therethrough. Meanwhile, openings such as the inlet 34 are provided highly circuitous paths of small dimension (e.g., from about one hundredth to about one quarter inch hydraulic diameter) in order to attenuate, absorb, and otherwise disrupt and redirect any acoustic waves that might escape from the apparatus 10 therethrough.
In the illustrated embodiment, the inlet 34 feeds air into a filter 36 or filter medium 36 . Thereafter, air is released through a passage from the area of the filter 36 into the interior of the outer housing 12 . The keeper 38 securing the filter medium 36 or filter 36 in position may be vented in various locations to provide passage of air from the inlet 34 into the interior of the housing 12 .
As a practical matter, the difficulty of isolating vibration from mechanical reactions as well as acoustic (sound) waves from the moving components of the apparatus 10 is complicated by the fact that any use of energy, particularly motors, will generate heat. That heat must be dissipated. When it is dissipated, it must be transferred away into some medium such as the ambient air or it may destroy the electrical and electronic components generating that heat.
Accordingly, the need to transfer heat away from electrically active componentry stands in opposition to enclosing and isolating those same components in order to reduce or eliminate acoustic and mechanical vibrational interactions that may cause undesirable noise, chatter, or the like between the apparatus 10 and its environment, including its supporting surface. Thus, the inlet 34 provides cooling air for the motor 18 and the electronics 14 inside the outer housing 12 .
Continuing to refer to FIGS. 1-2 , a control assembly 40 or printed circuit board 40 equipped with the proper circuitry and controls may provide three principle control abilities. A flow control 41 typically controls the power to the motor 18 . By control of power, the net throughput of air, measured by mass flow rate or volumetric flow rate may be controlled.
Meanwhile, a control 42 or controller 42 controls the duration of operation of the motor 18 driving the pump 20 . For example, the duration control 42 may provide an infinitely variable selection of time from zero to any other number selected. In certain presently contemplated embodiments, a minimum time may be provided for the duration control, such as a minimum of 1 minute. Otherwise, the control 42 might have no dead space and might oscillate between an on and off condition indefinitely if improperly adjusted.
Likewise, as a practical matter for typical applications, a duration of from about 10 to about 60 minutes is typically a maximum time an individual may choose to have the pump 20 and motor 18 operating at one session. Similarly, delays of the same amounts may be selected. In one presently contemplated embodiment, times may set at from between 1 second and 60 minutes. Typically, it has been found suitable to permit or to select controls 42 , 43 that may be set at any location on a continuously variable and infinitely variable scale between about 1 minute and 20 minutes.
The controller 43 or delay control 43 provides a user the ability to set arbitrarily and selectively the specific amount of time delay between adjacent durations of operation. For example, the duty cycle of a motor 18 and pump 20 may be controlled by the ratio of total duration of operation divided by the total time of delay plus that duration of operation. Thus, a duty cycle may be described as a fraction of the total elapsed time that the motor 18 and pump 20 are in actual operation. Various knobs 44 a , 44 b , 44 c may control or provide actuation by a user for the flow control 41 , duration control 42 , and delay control 43 , respectively. Here, knob 44 b is identical to, and removed by the cross sectional cut from in front of, knob 44 c in FIG. 2 .
Referring to FIG. 3 , while continuing to refer generally to FIGS. 1-2 the apparatus 10 may enclose within the inner housing 16 a pump 20 . The pump 20 may provide air discharged through an outlet 45 .
Referring to FIG. 3 , the pump 20 may include a pump body 46 or body 46 central thereto. The body 46 may have formed therein a passage 48 , here illustrated as it emerges from two faces of the body 46 . The passage 48 provides an inlet for air coming from within the housing 12 into the pump 20 . Likewise, a passage 50 originates from a face of the body 46 , and eventually exits through the outlet 45 of the pump 20 .
In the illustrated embodiment, a slot 52 or pinch slot 52 receives a valve body 56 therein, thus providing support along a large portion of the periphery of the valve body 56 . Thus, the passages 48 , 50 are operably connected to compression chambers 53 in the respective valve bodies 56 . A retainer 55 may secure the pump body 46 to the inner housing 16 through apertures 90 . The tapered face 58 of each valve body 56 illustrates that each is formed with an angle 59 . Thus, the pinch slot 52 may more easily capture but then tightly secure the valve body 56 once it is fully inserted into the pinch slot 52 .
Covering, and associated with the apertures in the pump body 56 corresponding to the passages 48 , 50 in the pump body, are reeds 60 or flappers 60 secured by keepers 62 . (The generic reference may be used herein to represent all of the specific examples, such as a generic 60 for specifics 60 a , 60 b , here illustrated, and 102 for 102 a , 102 b hereinbelow) The reeds 60 act as one-way valves, each permitting flow in one direction and resisting flow in the opposite direction. Accordingly, each of the compression chambers 53 may draw air in through the passage 48 , then seal off the passage 48 with the reed 60 . Accordingly, the passage 50 may be sealed off against back flow, but opened to be accessible by the reed 60 b opposite the reed 60 a . Actually, the reeds 60 a , 60 b are not exactly opposite one another but rather, each is on an opposite side of the valve body 56 , acts in an opposite direction, and services an aperture for one of the passages 48 , 50 .
Typically, a diaphragm 64 may be formed in a single piece to secure about the chamber 53 . Thus, a diaphragm 64 may form a sealing and a closure for the chamber 53 . Each diaphragm 64 , of which there may be a single diaphragm 64 , or multiple diaphragms 64 , may be secured to the pump 20 by fasteners to a swing arm 66 . The swing arm 66 itself may include a yoke 65 secured to a hinge 68 . Meanwhile, opposite the yoke 65 a magnet 67 secured to the swing arm 66 operates as an armature 67 in conjunction with the drive mechanism.
The yoke 65 , capturing a hinge 68 , such as a resilient tubing may provide a comparatively wear-free, damping, long-lived attachment mechanism. The hinges 68 recessed into the retainer 54 provide a pivot access for each of the swing arms 66 about the yokes 65 thereof.
Various seals 70 may be provided to both limit and secure passage of air through the pump 20 . For example, a seal 70 may be formed as an ‘O’ ring fitted into a slot 72 or groove 72 . Accordingly, the seal 70 provides securement of the flow of air from the passage 50 into the valve body 56 . Likewise a seal 74 may be configured to fit in a groove 76 or slot 76 sealing the passage of air between the passage 48 and the valve body 56 . Thus, the seals 70 , 74 fit between the valve bodies at the grooves 72 , 76 , and against the faces 78 of the pump body to effect their seal.
The diaphragms 64 operate by the oscillation of the armatures 67 driving the swing arms 66 to pivot about their yokes 65 and hinges 68 . Accordingly, the armatures 67 pivot in an almost linear fashion, driven by electromagnetic forces.
The reeds 60 a , 60 b provide substantially instantaneous valving in accordance with the pressure within and without the chamber 53 . Thus, air is drawn into the chamber 53 by the diaphragm 64 as it moves away from the valve body 56 . Similarly, air is pushed back from the diaphragm through the valve body 53 and into the passage 50 by the diaphragm 64 under the control of the reeds 60 b.
Referring to FIG. 4 , while referring generally to FIGS. 1-3 , the inner housing 16 may include a comparatively harder structural component such as a shell 80 . The shell 80 may be provided with an edge 81 to receive a closure. Prior to closure of the shell 80 , a liner 82 may be inserted therewithin. In the illustrated embodiment, the liner 82 is formed of a comparatively soft elastomer selected for its ability to dampen sound and vibration rather than transmitting it therethrough or therealong.
For example, the wall 83 of the liner 82 may be comparatively thin, thus in combination with the soft elastomeric properties of the material thereof may substantially reduce or eliminate any vibration or transmission of vibration along the surface thereof. Meanwhile, by selecting hardness (e.g., softness) for the elastomer from which the liner 82 is molded or otherwise formed, the liner may substantially dampen any vibration or acoustic vibration passing through the wall thereof.
In one embodiment, the liner 82 may be spaced a distance away from the shell 80 in order to provide an air gap therebetween. In the illustrated embodiment, the lip 84 of the liner 82 fits inside the shell 80 . Meanwhile, no continuous source of substantial contact is made between the wall 82 and the shell 80 , except near the relief 85 . The relief 85 is formed in the liner 82 in order to accommodate certain manufacturing components.
For assembling the apparatus 10 , a method may include insertion of the liner 82 into the shell 80 of the inner housing 16 . The shell 80 may be provided with an edge to capture the lip 84 . In one embodiment, a recess or groove inside a shoulder within the interior of the shell 80 captures the lip 84 and secures it, urging it against the outer most contact with the interior surface of the shell 80 .
Meanwhile, inserting the liner 82 a sufficient distance into the shell 80 permits alignment of an aperture 86 in the liner 82 with an aperture 87 in the shell 80 . Each of the liner 82 and the shell 80 may include both upper and lower apertures 86 , 87 , respectively. Upon alignment of the apertures 86 , 87 , a fastener 88 may pas through both apertures 86 , 87 to secure the pump 20 therewithin.
As a practical matter, the fasteners 88 may provide a mechanical coupling between the pump 20 and the shell 80 . Thus, a principal purpose of the shell 80 in the illustrated embodiment is to provide acoustic isolation, of the pump from its environment, notwithstanding vibrational or mechanical vibration isolation is not occur as effectively between the pump and the shell 80 . Rather, the inner housing 16 is mechanically isolated by other mechanisms to be described hereinbelow.
An additional aperture 89 may receive fasteners from the pump. The aperture 89 may be aligned with the aperture 90 to pass a clip 55 from the pump 20 therethrough to register and temporarily secure the pump 20 or align the pump 20 in registration with the shell 80 . Thereafter, an aperture 92 may be aligned with an aperture 93 in order to receive a fastener 94 securing the shell 80 to the pump 20 . Thus, the pump is held rigidly to the shell 80 with the soft elastomer of the liner 82 between a pump 20 and the shell 80 to damp vibrations. Meanwhile, the pump 20 is suspended by three fasteners 88 , 94 providing a secure, 3-point connection in order to minimize misalignment and chatter between the pump 20 and the shell 80 .
The aperture 96 is sized to form an interference fit with the outlet 45 of the pump 20 . The outlet 45 has a diameter larger than that of the aperture 96 . Accordingly, the elastomeric material of the liner 82 stretches to fit around the outlet 45 , thus making an effective acoustic and hermetic seal between the pump 20 and the remaining interior of the outer housing 12 . Because each of the fasteners 88 , 94 may be tightened to compress the liner 82 between the fastener 88 , 94 and the pump 20 , the apertures 86 , 92 may provide clearance fits, which may then be closed by compression according to Poisson's principle controlling distortion of materials.
The outlet 45 feeds air from the pump 20 directly into a chamber 98 or plenum 98 . The chamber 98 may be provided with one or more ports 100 . In the illustrated embodiment, the port 100 a opens downward, while the port 100 b opens upward. Meanwhile, seals 102 a , 102 b seal each port 100 a , 100 b , respectively. In the illustrated embodiment, an adaptor or fixture 104 sometimes referred to as a barbed fitting may fit into the port 100 a to receive a connecting line for conducting air from the pump 20 to a delivery point.
Meanwhile, in the illustrated embodiment, a plug 106 closes off the port 100 b . The ports 100 a , 100 b may be configured as desired with a fitting 104 or a plug 106 . Meanwhile, the seals 102 a , 102 b provide air-tight sealing by a mechanism such as gaskets, ‘O’-rings, or the like.
Legs 108 provide substantially complete radial isolation of mechanical vibrations between the shell 80 and the outer housing 12 . According to the softness (alternative of hardness) of the elastomeric material from which the legs 108 are formed, an additional degree of axial (e.g., vertical) isolation is also provided between the shell 80 and the outer housing 12 .
In the illustrated embodiment, the legs 108 each contain a collar 109 or collar portion 109 that may be fitted with an interference fit in a corresponding aperture (not shown) in the shell 80 . The leg 108 may be stretched to insert the collar 109 into the aperture, into which the resilience of the leg 108 will shorten the length thereof and expand the diameter of the collar 109 to provide the interference fit.
Meanwhile, a neck 110 or neck portion 110 provides an extremely small diameter that is substantially radially unstable. Thus, the softness selected for the elastomeric material of the leg 108 may be further enhanced by the small diameter of the neck 110 . Accordingly, a foot 111 resting on the lower shell 24 of the outer housing 12 can support substantially no lateral (radial) forces to be transmitted between the shell 80 and the outer housing 12 . Meanwhile, the softness of the elastomer of the leg 108 provides additional isolation in an axial direction to both dampen and isolate vibrations generated by the pump and transmitted to the shell 80 from transmitting to the outer housing 12 .
Above the collar 109 a keeper 112 provides securement of the leg 108 within an aperture (not shown) in the shell 80 . The diameter of the keeper 112 may be reduced by stretching the length of the leg 111 , thus providing for insertion of the collar 109 through an aperture. Thereafter, upon release of the extension force the length of the leg 108 will return to an equilibrium position leaving the keeper 112 and the remainder of the leg 108 to capture the shell 80 on either end of the collar 109 .
In general, the liner 82 and the legs 108 may be formed of polymers having elastomeric properties suitable for isolation and damping of mechanical vibration. Likewise, any acoustic vibration transmitted to the shell 80 may be damped thereby to an extent designed by selection of the materials. Meanwhile, the use of an extended length of conduit or tubing formed of soft polymer or elastomer and connected to the fitting 104 will also provide substantial vibration isolation from any mechanical vibration or force that might otherwise be transmitted between the shell 80 and the outer housing 12 .
Referring to FIGS. 5-6 , while continuing to refer generally to FIGS. 1-4 , an end plate 120 forms the completion of the enclosure of the inner housing 16 . In one embodiment, the end plate 120 may include a coupler 122 or coupler portion 122 inserted inside the open end of the shell 80 . The coupler 122 terminates at a face 124 sealed and impervious to any transmission of mass, particularly air. The coupler 122 thus presses the face 124 against the lip 84 of the liner 82 . Accordingly, the coupler 122 serves as a keeper 122 holding the lip 84 into its slot within the shell 80 .
The lip 84 , being made of the same material as the remainder of the liner 82 , thus provides the mechanical damping of vibrations between the coupler and the shell 80 . Perhaps more importantly, the lip 84 thus provides a gasket sealing the interior of the liner 82 against the face 124 . Every opening in the liner 82 may be sealed by compression, an interference fit, or the like. Accordingly, with the exception of the path of pumped air into and out of the pump is substantially sealed against any movement of gas or sound waves (e.g., air) therethrough.
A rim 126 on the end plate 120 may be homogeneously molded with the end plate. In one embodiment, the entire end plate 120 including the coupler 122 , rim 126 , and the coil 127 and coil 128 assembled may be potted together. The end plate 120 may be cast, or may be formed as a partial casting to be potted later with the magnet assembly 129 (e.g., coil 127 and coil 128 ) potted therein. Thus, the end plate 120 may be homogeneously molded as a single piece containing both the coupler 122 and rim 126 and potting the magnet 129 of the motor 130 therewithin.
In the illustrated embodiment, the face 124 may be spaced away from all parts of the magnet 129 . Accordingly, both the coil 127 and the core 128 may be spaced away from the face 124 in order to provide a complete, integral seal thereby. Meanwhile, the coupler 122 may be provided with a detent of some type such as a groove, boss, rise, clip, barb, or the like to engage a corresponding portion of the shell 80 in order to secure the coupler 122 inside the shell 80 .
A portion of the motor 130 , the magnets 67 are illustrated in FIG. 3 . The magnets 67 operate near but without contacting the face 124 . Thus, the magnets 67 may interact with the magnetic core 128 of the motor 130 without actually contacting any part thereof mechanically.
Fasteners 131 inserted through relief locations within the core 128 may secure the motor 30 to the mount 132 . The mount 132 in the illustrated embodiment serves multiple functions. For example, the mount 132 provides a housing 134 to contain a filter 135 or filter medium 135 . That is, sometimes it is proper to speak of a filter as both the housing 134 and the contained filtering media 135 . A keeper 136 or lid 136 may snap into the housing 134 to secure the filter 135 therewithin.
In addition to the filter housing 134 , a mount 132 provides legs 138 to support the motor 130 within the inner housing 16 . In order to maintain the mechanical isolation of a inner housing 16 with respect to the outer housing 12 , the legs 135 may be provided with isolating feet 140 .
In the illustrated embodiment, the feet 140 are formed in a convoluted shape such that an inner portion thereof receives a leg 138 , while the outer portion thereof is offset both radially and axially to extend beyond the inner portion. Thus, radial motion of the leg 138 is isolated by the convoluted shape of the foot 140 . Meanwhile, axial movement due to vibration of the leg 138 is actually taken up and absorbed, by the convolution in the foot 140 . In certain embodiments, the selection of any elastomeric material to form feet 140 may provide sufficient thickness and softness to absorb a substantial portion of any mechanical vibration presented by the leg 138 .
It may be seen from the foregoing that the inner housing 16 remains mechanically isolated from the outer housing 12 . Restraints formed in the outer housing 12 to contain the feet 140 against radial and axial motion will not constrain substantially the leg 138 captured therein. Thus, as explained, the leg 138 may translate axially and radially without requiring movement of the portion of the outermost perimeter of the foot 140 .
It may be seen that the feet 140 , along with the leg 108 positioned at the opposite end of the inner housing 16 provide isolation and damping in three dimensions and nearly perfect isolation in at least two.
The filter housing 134 contains inlet apertures 142 or apertures 142 receiving air from inside the outer housing 12 . Since the filter housing 134 is located outside the shell 80 and its enclosing end plate 120 or cap 120 air must pass near or around the coil 127 and core 128 of the magnet 129 to gain access to the apertures 142 . Thereafter, the air must pass down through the apertures 142 and around the rim surrounding each. Thereafter, the air must pass through the filter medium 135 , up over rims (see FIG. 6 ) on the hidden side of the lid 136 .
Various slots in the rims of the lid 136 may provide preferential release of air to enforce these more circuitous paths towards the nearest wall, and thus through a greater extent of the filter media 135 , instead of the most direct route from the aperture 142 to the outlet 146 . The outlet 146 is connected by a passageway 147 in the filter housing 134 . Air may then pass from the outlet 146 into the cavity 150 of the shell 80 . The cavity 150 is contained within both the liner 82 and the shell 80 .
As can be seen, the path of air provides a draw bringing air from within the surrounding environment into the outer housing 12 through an inlet 34 . From within the interior of the outer housing 12 , air is drawn from a location near the motor 130 , and particularly the coil 127 and core 128 thereof to enter the inlet 142 of the filter housing 134 . After passing through the filter media 135 and through the outlet 146 , the air is free to circulate within the cavity 150 of the inner housing 16 . From a location at or near the top of the cavity 150 , the passage 48 draws in the air into the pump as described hereinabove. Meanwhile, the pump body receives air from the chambers 53 into the passage 50 for discharge through the outlet 45 . From the outlet 45 , air passes into the chamber 98 , which passes the pressurized air out through the fixture 104 into a connecting line to be discharged to the environment. The connecting line (not shown) is formed of a sufficiently soft elastomer of a sufficient length to isolate the inner housing 16 from the outlet 30 and thus the outer housing 12 .
The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The described embodiments are to be considered in all respects only as illustrative, and not restrictive. The scope of the invention is, therefore, indicated by the appended claims, rather than by the foregoing description. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
|
An aromatherapy air pump is damped and largely isolated against acoustic and mechanical transmission of vibrations in three dimensions by a combination of containment within multiple, nested housings and standoffs provided by elastomeric supports having anisotropic geometry. An elastomeric liner as well as unstable legs, physical separations, and hermetic seals combine to provide sound reduction for noise and vibration emanating from the pump and its drive motor.
| 5
|
BACKGROUND
The present invention relates to optical power limiting devices, and in particular, to a laser power limiter employing a plasma generating material comprising a particulate coated surface.
Radiation sensors are adapted to sense radiation over a wide band of wavelengths including infrared and visible light. Sensors are used for mapping, targeting, and the like. It is desirable that the sensors have high sensitivity. However, this sensitivity simultaneously renders the sensor susceptible to damage or destruction from threat radiation such as a high power laser beam directed at the sensor. The most important type of threat radiation is a short pulse, high peak power pulsed laser operating in the visible or infrared wavelength regions. Laser power limiters or "optical fuses" are used to protect sensors from such threat radiation.
At the present time, the two most significant laser power limiters are a gas plasma shutter which operates at infrared wavelengths and a liquid-particulate limiter which operates at visible wavelengths. Both of these devices respond to incident laser radiation and produce a plasma interposed between the incident radiation and a sensor. The plasma blocks the radiation by means of reflection, absorption, and diffraction. However, the gas plasma shutter cannot be used in the visible light region because the gas plasma densities produced by the device are not high enough to attenuate visible light. The liquid-particulate limiter is ineffective for use in the infrared region because no liquid has been found that effectively transmits infrared radiation. Both devices require relatively high turn-on thresholds and exhibit a variable probability of turn-on. The liquid-particulate limiter also cannot handle multi-pulse (high repetition rate) threats without implementation of a complicated means of stirring the fluid. Particulate clumping and dissolution are further problems of the liquid-particulate limiter.
Another laser power limiter device is a gas plasma switch based on the use of particulate plasma formation in a gas. This device, however, although quite useful, has a relatively high turn-on threshold, has a relatively low probability of switching, and is only suitable for use with infrared radiation.
Thus, there has heretofore existed a need for an improved radiation limiter that provides low insertion loss, wide wavelength coverage, fast rise time, multi-pulse protection, high attenuation, and fast recovery times.
SUMMARY OF THE INVENTION
To overcome these limitations, there has been developed a laser power limiter, or optical fuse, which incorporates a coated, optically-transmissive surface that is sacrificed when the coating material is ablated or removed by a focussed high power laser pulse. The optically deteriorated surface then diffusely scatters subsequent radiation, thus reducing laser flux on the sensor. However, in order for the sensor to image the scene subsequent to laser irradiation, the coated optically-transmissive surface is moved (rotated) so that a fresh surface without optical defects is provided for transmission of the light from image scene. This laser power limiter is somewhat limited in that the optical surface must be of good quality in its initial state to allow good imaging of the scene by the sensor. This requirement however requires a high activation threshold that allows significant laser radiation to enter the detector before protection is effected.
The laser power limiter incorporates a layer of plasma generating particulate material (also referred to as a particulate layer) employed between a sensor and a source of laser radiation. The particulate layer is relatively thin and its optical transmissivity is typically between 70% and 90%. A focusing or condensing lens arrangement is disposed in front of the particulate layer to concentrate radiation onto a predetermined focal area of the particulate layer. The focal area is determined as a function of the incident laser radiation energy level that is sufficient to cause sensor damage, known as the damage energy level, and the plasma forming energy threshold of the particulate layer. The particulate layer is preferably located on a surface displaced from the focal plane of the focussing lens arrangement so that the focal area is relatively large. This ensures that a large number of particulates are irradiated, thereby ensuring a high probability of plasma formation. The relatively large focal area further ensures that the energy level required to produce plasma formation produces minimal damage in the supporting structure of the particulate layer.
It is therefore a feature of the invention to provide a laser power limiter that incorporates a relatively thin, optically transmissive surface layer of particulate material that is adapted to generate a plasma when irradiated by laser radiation. Another feature of the invention is to provide a power limiter in which laser radiation is focussed onto a predetermined focal area of a particulate layer in a sufficient amount to ensure plasma formation. Another feature of the invention is to provide a power limiter in which a focusing lens arrangement concentrates laser radiation onto a predetermined focal area of the particulate layer sufficient to limit damage to the supporting material on which the particulate layer is disposed. Yet another feature of the invention is to provide a power limiter in which the focal area is sufficiently large so that an adequate number of particulates are subjected to plasma forming threshold energy. Still another feature of the invention is to provide a power limiter that has multiple damage level radiation thresholds. Still another advantage of the invention is to provide a power limiter that is easily and automatically restored to its unirradiated state. Another feature of the invention is to provide a power limiter that exhibits low insertion loss, wide wavelength coverage including ultraviolet to infrared wavelengths, fast rise time, multi-pulse (high repetition rate) protection, high attenuation, and fast recovery time.
BRIEF DESCRIPTION OF THE DRAWINGS
The various features and advantages of the present invention may be more readily understood with reference to the following detailed description taken in conjunction with the accompanying drawings, wherein like reference numerals designate like structural elements, and in which:
FIG. 1 is an optical schematic showing the optical power limiter in accordance with the principles of the present invention; and
FIG. 2 is an illustration of a second, multiple surface, optical power limiter in accordance with the principles of the present invention.
DETAILED DESCRIPTION
Referring now to the drawings, FIG. 1 shows an optical power limiter 10 in accordance with the principles of the present invention. The optical power limiter 10 comprises supporting structure 12, which is typically a disk shaped window made of an optically transparent material, such as zinc selenide or optical quality glass, for example. The supporting structure 12 is disposed on a shaft 14 and the shaft 14 is operatively coupled to a mechanism (not shown) that enables incremental rotation of the supporting structure 12 as will be explained below. At least one surface of the supporting structure 12 is coated with a layer 16 of plasma forming particulate material, also referred to as a particulate layer 16. A suitable particulate material is finely divided carbon having a grain size of 0.5 microns, for example. In FIG. 1, both surfaces of the supporting structure 12 are coated with a particulate layer 16.
The particulate layer 16 is disposed on the surface of the supporting structure 12, typically by means of a vapor deposition process, or by applying mastic to the surface, for example. The particulate layer 16 is applied to a thickness that provides a transmissivity factor of between 70% and 90%, with 80% transmissivity as a nominal value. This typically requires a particulate layer 16 having a thickness of about 1 micron rms when carbon comprises the particulate material.
Disposed in front of the particulate layer 16 is a focusing lens arrangement, comprising a focussing lens 18 . The focusing lens 18 is adapted to focus incident radiation 20 that comprises an image scene. A collimating lens 32 is disposed behind the supporting means 12 and in front of a sensor 30. The collimating lens 32 is adapted to collimate applied radiation and transmit it to the sensor 30. In the absence of a plasma formed by the power limiter 10, the collimating lens 32 forms an image of an external image scene at the sensor 30.
The particulate layer 16 is disposed in front of a focal plane 22 of the focusing lens 18. The particulate layer 16 may alternatively be positioned behind the focal plane 22. In either case, the position of the particulate layer 16 is selected such that a focal area 24 encompassed by focussed incident radiation 26 satisfies the following two criteria. Firstly, incident radiation 20 having an energy level sufficient to cause damage or destruction of the sensor 30 must be concentrated on the particulate layer 16 to achieve an energy level sufficient to cause the particulate material comprising the particulate layer 16 to explode, ablate, or otherwise form a plasma 28. Secondly, the focal area 24 must be sufficiently large to ensure that an adequate quantity of particulates are exposed to the focussed radiation 26 to ensure formation of an adequate cloud of plasma 28. Accordingly, the size of the focal area 24 is a function of the damage level energy of the particular sensor 30 with which the power limiter 10 is used in conjunction with the plasma formation energy threshold of the plasma forming particulate layer 16.
In operation, incident radiation is brought to focus at the focal plane 22 by the focussing lens 18. In the absence of a plasma 28 formed by the power limiter 10, the collimating lens 32 forms an image of the external image scene at the sensor 30. The light image is detected by the sensor 30 and subsequently converted into a video image. Prior to the application of laser radiation, it will be recognized that image scene radiation is imaged in a normal manner onto the sensor 30 with a slight image quality loss due to absorption and scattering by the particulate layer 16. However, the large spot size on the particulate layer 16 minimizes this effect.
The particulate layer 16 is disposed at a location such that incident radiation 20 having an energy level sufficient to cause damage to the sensor 30 is focussed to an energy level at the particulate layer 16 sufficient to guarantee ablation thereof. This typically occurs in the presence of applied high power laser radiation, such as by a CO 2 laser, for example. The focussed laser radiation produces the plasma 28 by exploding or ablating the particulates comprising the particulate layer 18. The plasma 28 then reflects, absorbs, and diffracts the damaging laser radiation.
Subsequently applied laser radiation, arriving shortly after the first laser pulse, in the case of the high repetition rate laser, for example, is focussed on the ablated damage site and is likewise dissipated by the plasma 28. After the laser pulses cease, the supporting structure 12 is rotated, for example, to a new position to allow unobstructed scene viewing. Typically, rotation of the supporting structure 12 is effected within a period of about 10 milliseconds.
To ensure broadband protection, it is important to have a particulate generated plasma 28 having a plasma density several orders of magnitude higher than is typical for a gas plasma. Such a plasma appears "metallic" at visible wavelengths and at infrared wavelengths. For example, a fully ionized plasma in one atmosphere pressure gas has a plasma frequency of 5×10 13 which is sufficient to reflect 10.6 μm radiation. However, a plasma frequency 20 times higher is required to reflect visible radiation. This plasma frequency is obtained by a near-solid density plasma, such as is provided by an exploded particulate layer 16. It has further been shown that particulate explosion thresholds are far lower than thresholds required for pure gas plasma formation. Accordingly, the power limiter 10 of the present invention has the attribute of lower threshold activation compared to conventional gas plasma devices. The power limiter 10 also exhibits the benefit of reduced bulk damage caused by heat liberated at the damage site. Such damage can cause structural failures in conventional devices. In tests performed with the power limiter 10, plasma formation time has been determined to be approximately 5 nanoseconds, and attenuation factors on the order of 1,000 have been demonstrated.
Referring now to FIG. 2, there is shown a second embodiment of a power limiter 10' in accordance with the principles of the present invention. In this embodiment, a plurality of supporting structures 12 are disposed between the focusing lens 18 and collimating lens 32. At least one surface of each of the plurality of supporting structures 12 is coated with a particulate layer 16 as described above. However, the particulate layer 16 on each of the plurality of supporting structures 12 is formed with decreasing amounts of material, thus providing for relatively increasing transmissivities. Accordingly, the energy threshold at each of the particulate layers 16 increases as progressively concentrated radiation propagates through the successive particulate layers 16. The plasma formation threshold for each particulate layer 16 is set below the damage threshold for the sensor 30. This, again, is a function of the damage level energy of the sensor 30 and the respective focal areas 24 of each particulate layer 16. With this configuration, incident laser pulses are attenuated by respective ones of the particulate layers 16 from left to right (as viewed in FIG. 2).
From the above description, it should now be seen that the optical power limiters 10, 10' of the present invention provide for a surface particulate power limiter that exhibits the characteristics of relatively low insertion loss, wherein the particulate coating typically allows about an 80% energy transmission in its unablated state. The optical power limiters 10, 10' provide broadband coverage providing protection from the visible through infrared wavelengths due to appropriate choice of materials, namely carbon and zinc selenide. The optical power limiters 10, 10' provide fast rise times, typically in the order of 5 nanoseconds. The optical power limiters 10, 10' provide for higher repetition rate protection by reason of the natural occurrence of the damage site or by stacking several particulate layers 16 in series. The optical power limiters 10, 10' provide an attenuation factor of on the order of 1,000. The optical power limiters 10, 10' further exhibit fast recovery allowing a scene to be viewed by a sensor 30 after protective plasma formation by rotation of the supporting structure(s) 12. This recovery period is typically less than 10 milliseconds.
In tests, a zinc selenide window coated with carbon particles was exposed to a solid state laser operating at 0.53 nanometers and in another test, a CO 2 laser operating at a wavelength of 10.6 μm. Carbon particles were coated on a zinc selenide window with a net transmission of 80%. A laser was pulsed with pulses having a 10 microsecond duration. The total beam energy was 44 mJ. In this test, the power limiter 10 transmitted only 4 mJ of energy to the sensor 30 after an initial ablation episode. All subsequent laser pulses were blocked. Using the solid state laser operating in the green portion of the visible spectrum at 0.53 nm wavelength, carbon particles coated on a transparent glass slide, having an effective transmissivity of 75% effected an attenuation factor of 100 for the first and all subsequent laser pulses. Incoming laser radiation 20 in this test was in the order of 10 μJ. From this it will be observed that the threshold for plasma formation is very low. It will further be observed that the attenuation factor becomes much larger for higher laser input energies, which generates higher levels of plasma 28.
Thus there has been described a new and improved surface particulate optical power limiter. It is to be understood that the above-described embodiment is merely illustrative of some of the many specific embodiments which represent applications of the principles of the present invention. Clearly, numerous and other arrangements can be readily devised by those skilled in the art without departing from the scope of the invention.
|
The invention is a laser power limiter. The limiter incorporates a layer of plasma forming particulate material supported optically in front of a sensor. A focussing means is positioned optically forward of the particulate layer to concentrate incident threat radiation on the particulate layer. The position of the particulate layer relative to the focussing means is selected such that the focal area encompassed by concentrated incident radiation encompasses a sufficient number of particulates to insure protective plasma formation and to insure that damage level incident radiation will be concentrated to an energy level exceeding the plasma formation threshold of the particulate material. The particulate layer is supported on a rotating window such that new areas of the layer can be exposed to incident radiation after a damage radiation incident.
| 7
|
This invention relates to a process for increasing near-wellbore permeability of a porous subterranean formation.
BACKGROUND OF THE INVENTION
Most porous formations contain clay minerals, which are crystalline in nature and have lattice-layer silicates and chain silicates. The lattice-layer silicates are formed of combinations of two basic building blocks, a silicone-oxygen tetrahedron, and an aluminum-oxygen-hydroxyl octahedron. These units are polymerized into sheets. Tetrahedral sheets are formed by sharing of corners, while octahedral sheets are formed by sharing of edges. There are two types of octahedral sheets: one in which every octahedral site is filled by a divalent ion and one in which two out of three sites are filled by trivalent ions. The first and second sheets are referred to as trioctahedral and dioctahedral sheets, respectively. The polymerization process can also be continued by hooking together terahedral and octahedral sheets to form a 1:1 composite layer. In the composite layer, the octahedral sheet could also be a dioctahedral one. Similarly, a 2:1 composite layer can also be formed by using two tetrahedral sheets to the central octahedral layer. At 2:1 composite layer could be formed of dioctahedral or trioctahedral sheets.
Clay surfaces of the most common clays have many negatively charged sites, which make them fresh-water sensitive. Previous studies have established that clay occur naturally as either pore-lining or pore-filing minerals. These clay minerals usually are surrounded by saline connate water layer. The cations (e.g., Na + , Ca ++ etc.) from the saline water neutralizes the negative charges in clay minerals. The introduction of fresh water or less saline water into the formation, dilute the connate water and reduce its saline content. Because of this cation-charge deficiency around clay minerals, water molecules can easily invade in between clay platelets and results in swelling or dispersion. Therefore, charge deficiency in the minerals is an important quantity. It determines the forces holding the layers together. With mica group, these forces are relatively large. For smectites the forces are relatively small. The results is that interlayer cations can leave and enter the structure readily. In addition, water and organic molecules can enter and leave readily. Water tends to hydrate interlayer cations and result in a swelling of structure perpendicular to these layers. Organic materials also cause swelling.
Clay materials either were originally deposited during sedimentation, were formed later by the action of heat, pressure, and time on minerals already present, or were precipitated from fluids flowing through the matrix. The major components of clay are smectite, kaolinite, illite and mixed layer (i.e., illite-smectite). The two major mechanisms by which these minerals cause permeability damage are swelling and migration. In swelling, clay imbibes fresh water into its crystalline structure and subsequently increases in volume, plugging the pores in which it resides. Mixed layer and smectite are examples of swelling clays. In migration, clay minerals can be dispersed by contact with a foreign fluid or can be entrained by produced fluids and transported until a restriction is encountered (usually a pore throat), where the entrained particles bridge and restrict flow in the capillary. Kaolinite, illite, chlorite and mixed-layer are examples of migrating clays.
During drilling, if water-based drilling mud is used, mud filtrate will invade and damage the near-wellbore formation to some degree. During completion, the completion fluid can also invade and damage the near-wellbore formation. The cause of the formation damage can be explained by several possible factors including:
1. the invasion of drilling fluid causes clay minerals to swell and to constrict pore throats; this constriction causes a decrease in formation porosity and permeability, and an increase of the capillary effects.
2. the invasion of water-based fluid also causes water blockage due relative-permeability effects (two-phase flow).
The above-mentioned factors and other possible factors subsequently cause permeability reduction. Hydraulic-fracture treatments are often effective in by-passing the clay-related formation damage. However, these treatment techniques of clay-related formation damage, especially in horizontal wells, are difficult to perform and could be uneconomic. Therefore, there is a need in the petroleum industry for a new and improved method of treating clay-related formation damage.
In addition to the conventional acid and hydraulic-fracture treatments, several unconventional methods are disclosed in the literature. The following is a brief description of some of these disclosures.
U.S. Pat. No 4,844,169 presents a method of injecting non-reactive gas (i.e., nitrogen) into the formation at atmospheric temperature to fluidize the clays, including migratable fines, for their removal. Subsequently, an aqueous solution of soft water containing potassium chloride is proposed to be injected into the formation to cause a potassium-sodium cationic exchange within the swellable clays to reduce their swelling. In this method, temperature is kept low and clay structures are not altered. The fluidized clay particles can also block pore throat and subsequently, the treating fluid will be unable to contact the swelling clays. After low-temperature injections, chemical treatments may cause reswelling of the clays.
Canadian patent No. 915,573 discloses a method of treating the near-wellbore formation damage by contacting the formation with heated air or gas at a 121° C. (250° F.) temperature to cause partial dehydration of clays. Thereafter, the near-wellbore formation is treated with non-ionic vinyl pyrrolidone polymer to prevent reswelling of clays. In this 2-step method, the partial dehydration remedies the formation damage temporarily. However, subsequent chemical treatment may not be very effective because of the lack of good contact between the polymer solution and the formation.
Injection of aqueous solution of nitrogen at an elevated temperature of 260° C. to 310° C. (500° F. to 590° F.) to transform montmorillonite clays to more stable illitic-type clays was disclosed in U.S. Pat No. 4,227,575. These illitic-type clays are less sensitive to fresh water. The transformation of montmorillonite clays to illitic-type clays are possible by this method, but the aqueous solution of nitrogen can also trigger swelling of other minerals (e.g. glauconite paloids).
The use of saturated and superheated steam at temperatures of 104° C. to 871° C. (220° F. to 1600° F.) and at pressures of 14.7 to 8000 psia was proposed in U.S. Pat. No. 3,847,222 to treat the near-wellbore formation damage. Subsequent to steam treatment, the injection of guanidine hydrochloride in methanol was shown to achieve better results. In this two-step process, the condensed steam will act as a source of fresh water and cause formation damage in the untreated regions.
The simultaneous injection of steam and vaporized hydrogen chloride to rectify clay-related formation damage is presented in U.S. Pat No. 4,454,917. The purpose of steam is to clean the formation and the purpose of hydrogen chloride is to react with calcium and magnesium salts in the near-wellbore formation to form water-soluble chloride salts. In this process, the condensed steam is also a source of fresh water and could cause formation damage due to reswelling of clay minerals.
Another preventive technique disclosed in Canadian patent No. 1,282,685 is the removal of precursor ions from the injection water using reverse osmosis before injection into the formation. The removal of precursor ions will reduce precipitation in the formation and subsequently reduce the chances of formation damage. In this technique, the removal of precursor ions may not necessarily prevent the swelling and/or migration of clay materials in the formation.
SUMMARY OF THE INVENTION
It is the object of the present invention to provide a new method for increasing the permeability of near-wellbore formation containing hydratable clays, shales and other materials which tend to swell when contacted with fresh water and/or mud filtrate.
It is also the object of the invention to provide a new method for increasing the permeability of near-wellbore formation containing migratable clays, which are fluid velocity sensitive.
It is a further object of the present invention to provide a new method for increasing the permeability of near-wellbore formation whose wettability tends to cause water and/or fluid blockage.
It is thus generally the object of the invention to provide a new method for increasing near-wellbore permeability of any porous formation either containing hydratable clays, shales or other minerals which tend to swell when contacted with fresh water and/or mud filtrate, or a formation which has migratable clays, or a formation whose wettability tends to cause water and/or fluid blockage.
The method in accordance with the present invention consists of exposing the formation to an elevated temperature of . .400°.!. .Iadd.600° .Iaddend.C. or greater to cause dehydration or the clay lattices, vaporization of any blocked water, mud filtrate, or other fluids, and/or destruction of the clay structure.
The porous formation can be effectively treated to improve hydrocarbon permeability either prior to water and/or mud filtrate contact or after damage by water and/or mud filtrate. The heat treatment typically lasts for several hours, preferably more than 4 hours after the desired temperature is reached.
The temperature of this heat treatment is desirably about . .400°.!. .Iadd.600° C. .Iaddend.to 1000° C., preferably 600° to 800° C.
The above heat treatment may be carried out using downhole heaters including electrical resistance or gas heaters with air and/or inert gas injection. The desirable injection pressure must be higher than the reservoir pressure. Use of high frequency dipole heating with or without gas injection is also envisaged.
The advantages of the preset invention is that the high temperature destroys clay structure so that there is no possibility of rehydration and reswelling of clay minerals. Therefore, chemical post treatments are not required. In addition, laboratory tests have shown that the destruction of clay structure not only improves the damaged permeability but also improves the original permeability of the virgin formation.
DETAILED DESCRIPTION OF THE INVENTION
In this invention, a subterranean formation containing one or more hydratable clays, one or more migratable clays, one or more hydratable shales, and/or one or more combinations thereof, where the clays and shales both tend to swell when contacted with fresh water and/or mud filtrate, and/or formation whose wettability tends to cause water and/or fluid blockage, is exposed to an elevated temperature of . .400°.!. .Iadd.600° .Iaddend.C. or higher, either prior to water contact or after the formation has been contacted with water from underground or other sources and therefore has become hydrated and expanded and/or water blocked so as to substantially reduce the permeability of that formation relative to the original permeability of the virgin reservoir.
The porous formation is preferably treated to improve hydrocarbon permeability prior to water and/or fluid contact or after damage by water and/or fluid. The heat treatment typically last for several hours, preferably more than 4 hours after the desired temperature is reached. The three basic principles of formation heat treatment are given below:
1. dehydration of clay lattices,
2. vaporization of any blocked water, mud filtrate, or other fluids, and/or
3. destruction of clay structure.
The temperature ranges for this heated gas treatment are desirably about . .400°.!. .Iadd.600° .Iaddend.C. to 1000° C., preferably 600° C. to 800° C.
The above-mentioned three steps can be carried out using a tubing or wireline-conveyed-downhole heating device placed in the wellbore. Air and/or inert gas (e.g., nitrogen) is preferably injected into the wellbore at atmospheric temperature and at a pressure higher than the reservoir pressure. Air and/or inert gas will be heated as it passes through and/or around the heating device and hot gas will be forced into the formation. The heating device can be made of an electrical-resistance heating element or a gas heater or any device that can generate heat downhole. The near-wellbore formation will be heated by the air and/or inert gas being heated by the downhole heater. This heating process is designed for cased or openhole vertical or horizontal wells. In order to reduce wellbore heat losses in the vertical direction, air and/or inert gas injection through the annular space, for the case of tubing-conveyed heaters, may be provided. For the case of wireline-conveyed heaters, injection of air and/or inert gas into the formation will reduce the heat losses.
The injection of hot air or inert gas can also be carried out by heating air and/or inert gas at the surface.
High-frequency dipole heating is another procedure which can be used in the field. In this case, the formation is heated by high frequency energy transmitted through an antenna located in the wellbore. This heating procedure is suitable only for openhole vertical or horizontal wells. It can also be applied to a newly drilled well before casing is placed into the formation of interest. In this case, it is not required to inject air and/or inert gas into the wellbore to carry the heat into the formation. However, the injection of air and/or inert gas into the formation during heating will prevent heat front propagation towards the antenna and also can mobilize the clay minerals and be beneficial. The high-frequency dipole heating is rapid and propagates into a large area.
By the application of either of the above-mentioned procedures for several hours, depending on the injectivity of the formation and the desired degree of treatment, the permeability of the near-wellbore formation can be increased significantly. The injected heat completely or partially dehydrates the clay-bound water, evaporates the blocked water and/or fluid and destroys the clay structures, thus leaving no possibility of rehydration when the formation is resaturated with formation water.
The invention will now be disclosed, by way of example, with reference to the following two examples:
EXAMPLE 1
Small core plugs, measuring 3.98 centimeters in length and 3.75 centimeters in diameter, were obtained from full-diameter cores, taken from the gas-bearing formation, in a conventional manner. The average porosity was estimated to be 12% and the initial absolute permeability (i.e., at zero connate-water saturation) to air was 17.85 millidarcies (md). This permeability was considered to be the base permeability.
The petrographic studies indicated that the sandstone formation under consideration was of poor quality due to the presence of swelling clays and glauconitic peloids. The formation contained 78% quartz, 9% clays, and 13% glauconite materials. The major components of clay are 58% illite, 38% mixed layer (i.e., illite-smectite), and 4% kaolinite.
The core sample was saturated with produced formation water. The post-brine-desaturation permeability of 5.19 md reflects a 70% decrease in air permeability when a residual-brine phase remains in the core. The core was then saturated with KCd/Polymer mud filtrate. A nitrogen flood was performed to reduce the mud-filtrate saturation, thereby establishing an irreducible mud-filtrate saturation level. At this point a post-mud-filtrate permeability of 2.86 md was measured which indicated an 84% reduction from the initial air permeability.
The core under consideration was subjected to a sequential heat treatment at temperatures ranging from 200° C. to 800° C. During heating, the core was placed into a reactor and heated in a high-temperature oven. A constant pressure of 2,413 kPa was maintained inside the reactor using a regulated nitrogen source and a back-pressure regulator. The heating was maintained for 4 to 6 hours after the desired temperature was reached in the core sample. The permeability of the treated core was measured after cooling the core sample to atmospheric temperature.
The heat treatment of the core under consideration at 200° C. yielded an increased air permeability to 56% below the base permeability. The increase in permeability is most likely attributable to the partial evaporation of the residual mud-filtrate phase. Total evaporation of the mud filtrate during the 200° C. heat treatment did not occur because the internal reactor pressure was maintained at 2,413 kPa, which is above the saturation pressure at this temperature. It was also observed from mass measurements that the total fluid in the core was not evaporated. From the gas analyses conducted at 200° C., hydrocarbon evolution from the core is evident as well as possible degradation of carbon-based minerals.
The second heat treatment at 400° C. revealed a further permeability increase to 11.9% below the base permeability. The mass measurements indicated that the residual fluid was completely evaporated. The reduction of residual hydrocarbons, a more extensive decrease in hydration water and a partial degradation of carbonaceous minerals increased the permeability significantly.
The third heat treatment at 600° C. yielded a 51% increase in air permeability above the base permeability. Further decrease in sample mass indicated that the heating at 600° C. has had a significant effect on the mineral structures. The petrographic studies revealed that the permeability reducing minerals have broken down, resulting in a significant permeability increase. The petrographic studies also revealed that the heating at 600° C. improved the core porosity from 12% to 15%.
A dramatic permeability increase of 764% occurred during the fourth heat treatment at 800° C. An additional decrease in sample mass was also observed. The petrographic studies suggested that the swelling-clay and shale structures were completely destroyed during this heating phase. Even after the rehydration of the test core with formation water (after heating at 800° C.), the permeability was maintained at 622% above the base permeability.
EXAMPLE 2
Heating tests were also carried out on cores taken from the oil-bearing formation. The average porosity of the formation was estimated to be 15% and the air permeability is on the order of 25 md and the oil phase permeability was 0.9 md at 100% oil saturation. The petrographic studies on cores indicated that the formation was a moderately sorted, fine-grained, quartzose sublitharenite with good porosity and moderate permeability. The XRD analysis indicated that quartz material dominated the mineralogy (85%). The total clay content was about 15%. Kaolinite dominated the clay mineralogoy (86%) and illite constituted the remaining 14%. Smectite and mixed-layer illite-smectite clays were not found in the XRD analysis. The reservoir had modified intergranular porosity of about 8% and a supplemental grain moldic porosity of about 3%. The sandstone formation appeared to be sensitive to water and to conditions that could induce fines migration.
The core sample was sequentially exposed to brine, mud filtrate, heat and brine. In these tests, one temperature (800° C.) was used to evaluate the effect of heat on oil-saturated core permeability. It was anticipated that the exposure of an oil-saturated core to heat would result in coking of the oil and eventual reduction in permeability. The experimental setup was modified to flush nitrogen through the core. This way the oil is pushed out of the core as the core is exposed to heat. During the experiment, no liquid phase was seen at the outlet end of the core. In this experiment, the reactor was maintained under 16,500 kPa confining pressure (reservoir pressure). In a field situation, the injection of hot nitrogen would push the near-wellbore fluid far into the reservoir and expedite the heating around the well-bore.
The results indicated that mud filtrate caused substantial (38%) reduction in oil-phase permeability, likely due to a combination of phase trapping and clay deflocculation. However, the high-temperature (800° C.) exposure for four hours increased the oil permeability by about 1000% over the original permeability. Even after rehydration with conate water, permeability was still 748% greater than the initial "undamaged" baseline permeability.
The results of the petrographic studies indicated that most of the kaolinite was destroyed with only a few kaolinite pseudomorphs remaining. SEM studies suggest that the hydrocarbon was not been coked to insoluble carbon. The increase in permeability is mostly due to the destruction of the kaolinite minerals and to the subsequent transport of the degraded clay with hydrocarbon through the pore system.
|
A method of increasing the near-wellbore permeability of porous formation comprises exposing formation to an elevated temperature of . .400°.!. .Iadd.600° .Iaddend.C. or greater to cause dehydration of the clay lattices, vaporization of any blocked water, mud filtrate or other fluids, and/or destruction of the clay structure.
| 4
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of provisional patent application Ser. No. 60/760,334, filed 2006 Jan. 20 by the present inventor.
FEDERALLY SPONSORED RESEARCH
Not Applicable
SEQUENCE LISTING OR PROGRAM
Not Applicable
BACKGROUND OF THE INVENTION
1. Field of Invention
This invention relates to lighting devices, specifically to hands-free devices used to illuminate a user's path.
2. Prior Art
Hikers, climbers, and trail-runners use artificial light to illuminate the trail at night. The introduction of the headlamp allowed hands-free operation of the lighting device, freeing their hands to operate other objects and devices, also minimizing the chance of dropping the lighting device.
However, headlamps have disadvantages. The light is located close to the user's eyes. The shadows cast by objects in the user's path are hidden by the objects themselves. This yields a lack of depth perception, making travel more difficult.
Another disadvantage of locating a light source on a user's head is apparent in cool weather. When a user exhales, the moisture from the user's breath is sharply illuminated. This momentarily blinds the user. This is also detrimental to the user's night-vision.
Headlamps are often bulky and cumbersome. Many people do not like objects on their heads. These users will avoid using headlamps.
These issues are not present with hand-held lights, however, these lights are not hands-free. A user is unable to use trekking poles or other items when using a hand-held light. Also, the natural motion of moving one's arms when walking or running must be stifled. A user is forced to hold the light, which can then be dropped. The user is also unable to put their hands in their pockets, thereby warming them.
One solution for this is a light with a clip. A light with a clip is hands-free, and does not have the same problems as a headlamp; however, its function is limited as well. A clip can be placed in many locations, but cannot be attached at the center of a backpack's hip-belt, as the buckle is there. If the buckle is placed off-center to accommodate a light clipped to the center of the belt, the buckle will be where padding usually is. This requires a hip-belt to have less padding, which decreases a user's comfort.
In addition, a light with a clip, a headlamp and a handheld light can be misplaced, and can be difficult to find when darkness is approaching. They can be buried deep in a pack, or worse, either forgotten at home, or lost on the trail.
Others have come to the conclusion of mounting a light on a user's waist. U.S. Pat. No. 4,849,863 (Gallegos, 1989), U.S. Pat. No. 5,045,979 (Stevens, 1991), U.S. Pat. No. 5,255,168 (Stevens, 1993), U.S. Pat. No. 5,359,501 (Stevens, 1994), and U.S. Pat. No. 6,056,412 (Atlee et al., 2000) all address this issue. All of these patents require a separate device from what a hiker would ordinarily carry, and are largely incompatible with a pack hip-belt. U.S. Pat. No. 4,283,756 (Beamon, 1981), attaches a light to a buckle, but the light flashes and is used solely for safety and not for illumination. It does not illuminate a user's path, and the batteries are in a separate housing, not even attached to the belt. U.S. Pat. No. 5,183,324 (Thomas, 1993) and U.S. Pat. No. 6,499,859 B2 (Petzl et al., 2002) describe a lamp with batteries built in, but it's a single housing, not a buckle of any kind. Finally, U.S. Pat. No. 6,979,098 B2 (Petzl et al., 2005) and U.S. patent application 2006/00561758 A1 (Petzl et al., filed Jan. 28, 2004) describe a swiveling optic system. These describe a binary system, it is either on or off; it is not used to direct a beam of light depending on the angle of the optics.
OBJECTS AND ADVANTAGES
Accordingly, several objects and advantages of the present invention are:
a) to provide a light formed into a hip-belt buckle, of which hikers and climbers ordinarily have with them. b) to provide a light that is a significant distance from the users eyes, so shadows of objects in the trail are visible. c) to provide a light that is a significant distance from the mouth and nose, so it will not illuminate the condensation in user's breath in cooler weather; this will prevent temporarily blinding the user. d) to provide a hands-free light that does not have straps around or object(s) on the user's head. e) to provide a light that is centered on the user's belt, and thus centered with a user's line of sight. f) to provide a light which cannot get separated from the pack unintentionally, therefore making it more difficult to lose; the user will always know where the light is located. g) to provide a light that has either a specific LED arrangement or a lens provided so a wide section of the trail or area in front of the user is illuminated.
Further objects and advantages will become apparent from a consideration of the ensuing description and drawings.
SUMMARY
There is a need for a light source for illuminating a trail with hand free operation and providing a significant distance between a user's eyes and the light source. There is also a need for a light source that is attached to, in other words affixed to or integral with, a belt buckle on a pack.
These needs and others are met by embodiments of the present invention, which comprise a portable light constructed of a light housing attached, either embedded or with a hinge, to a belt buckle, such as a side-release plastic buckle, with a power source, such as a battery(s), embedded within the buckle.
Additional advantages and novel features of the invention will be set forth in part by the description which follows, and in part will become apparent to those skilled in the art upon examination of the following or may be learned by practice of the invention. The advantages of the invention may be realized and attained by the instrumentalities and combinations, particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is illustrated by way of example, and not by way of limitation in the figures of the accompanying drawings in which like reference numerals refer to similar elements and in which:
FIG. 1 a shows an isometric view of a light in a stowed position.
FIG. 1 b shows an isometric view of the light of FIG. 1 a in an “in-use” position.
FIG. 2 shows an exploded view of the light of FIG. 1 a.
FIG. 3 shows a bottom aspect of the light of FIG. 1 a.
FIG. 4 shows a side aspect of the light of FIG. 1 a.
FIG. 5 a shows a front aspect of a housing.
FIG. 5 b shows a sectional view of the housing of FIG. 5 a.
FIGS. 6 a - 6 d show various aspects and exploded views of a second embodiment of a light with single, embedded, high-powered LED.
FIGS. 7 a & 7 b show isometric and exploded views of a third embodiment of a light with a single, high-powered LED and a movable housing.
FIGS. 8 a & 8 b show isometric and exploded views of a fourth embodiment of a light with a swivel lens.
FIGS. 9 a & 9 b show isometric and exploded views of a fifth embodiment of a light embedded in a different buckle.
FIG. 10 shows an isometric view of the device attached centrally to a hip belt strap of a backpack.
DRAWINGS—REFERENCE NUMERALS
10
Housing Assembly
11
Housing body
12
Female Side-release
buckle
14
Bolt
15
Nut
16
Cable
18
5 mm LED
19
Hole (switch)
20
Side Panel
21
Opaque protrusion
22
Switch
23
Button
24
Circuit Board
26
Front Panel
27
Hole
28
Groove
29
Hole
30
Mounting Posts
31
Protrusion (nut)
32
Recess (button)
34
Cavity
36
AAA Battery
38
1W LED
40
Battery Cover
42
Male Buckle
43
Plain Female Buckle
46
Embedded Housing Buckle
48
Swivel Housing Buckle
49
Swivel Housing
50
Swivel Lens Buckle
51
Swivel Lens
52
Adapter Buckle
DETAILED DESCRIPTION
The present invention addresses and solves problems related to light sources, particularly where current light sources do not provide ample space between a user's eyes and the light source to allow user easily discern objects and the shadows they cast at night. The present invention also addresses and solves problems related to providing a light source which is integrated into a pack, specifically a buckle, and permits hands free operation.
The present invention solves the above problems by providing a light as discussed below. One of ordinary skill in the art will realize that the following discussion is illustrative and intended to describe preferred embodiments of the present invention and is not intended to limit the present invention to the embodiments discussed. The present invention has numerous applications where a light is needed for hands free operation. The present invention may be scaled and adapted to many applications and is defined by the claims, which set forth the metes and bounds of the present invention.
Referring now to the drawings, and initially to FIGS. 1-5 , the preferred embodiment of the light of the present invention is described. FIG. 1 a shows the light in the stowed position, and FIG. 1 b shows the light in the “in-use” position. A housing assembly 10 is connected to a 2 inch female side-release buckle 12 on mounting posts 30 with a bolt 14 and a nut 15 . A cable 16 transmits power between buckle 12 and housing assembly 10 . It is fitted into a groove 28 on buckle 12 , and passes through a hole 29 in a housing body 11 . Six white, 5 mm LEDs 18 are mounted in housing assembly 10 . Semi-translucent side panels 20 are mounted to housing body 11 .
FIG. 2 is an exploded view of the light assembly. The housing assembly 10 consists of housing body 11 with an opaque protrusion 21 , a rubber button 23 protecting a switch 22 , a circuit board 24 , LEDs 18 , a front panel 26 , and side panels 20 . Switch 22 , cable 16 , and LEDs 18 are soldered to circuit board 24 . LEDs 18 fit through holes 27 in panel 26 . Panel 26 is mounted to housing body 11 . Button 23 is held in place between switch 22 and a hole 19 in housing body 11 . A recess 32 is cut into buckle 12 so there is no interference with button 23 when light is in stowed position. A battery 36 is mounted in the center of buckle 12 .
Housing body 11 and front panel 26 are made out of a durable polymer, such as polycarbonate or ABS, and may be injection molded. Rubber button 23 can be made out of natural or synthetic rubber, such as Santoprene®. Side panels 20 are made out of a semi-translucent material, such as Plexiglas® or polycarbonate. Battery 36 is a standard AAA battery, and may be either disposable or rechargeable. Buckle 12 is made from a durable polymer, such as nylon, and may be injection molded.
FIG. 3 shows a bottom aspect of the light assembly, showing location of hole 19 and button 23 .
FIG. 4 shows a side aspect of the light assembly, showing a cavity 34 in buckle 12 where battery 36 is mounted. Button 23 protrudes below the bottom of housing body 11 as shown. Nut 15 interferes with a protrusion 31 on mounting post 30 to prevent rotation.
FIG. 5 a is a front view of housing assembly 10 . FIG. 5 b is a sectional side view of housing assembly 10 , showing arrangement of components within housing assembly 10 . FIGS. 5 a and 5 b show orientations of LEDs 18 relative to a plane defined by the bottom of housing body 11 . 1 LED 18 . 1 is mounted at an angle of approximately 15 degrees down from the plane. 2 LEDs 18 . 2 are mounted approximately level with the plane. 3 LEDs 18 . 3 are mounted at an angle 15 degrees up from the plane.
OPERATION
A user of this device would install female buckle 12 and male counterpart onto hipbelt of pack or onto piece of webbing or other strap going around user's waist. User would keep housing assembly 10 in the stowed position ( FIG. 1 ) during the day or whenever the light was not in use. When the user needs illumination in front of him or her, the user simply moves the housing assembly 10 into the “in-use” position ( FIG. 2 ). If user finds light in the exploded position ( FIG. 3 ), user has done something wrong.
When the light is in the “in-use” position, the user would actuate switch 22 by pressing on button 23 , thus turning on or off the light. Recess 32 protects button 23 when housing assembly 10 is in the stowed position, preventing light from accidentally getting turned on. Before use, user would insert battery 36 into buckle 12 . When battery 36 is drained, user removes and replaces battery 36 .
If housing assembly is not staying in position, user tightens bolt 14 . Nut 15 cannot rotate, so only one tool is needed for this adjustment. Tightening bolt 14 moves mounting posts 30 closer together, increasing pressure on housing body 11 , preventing housing assembly 10 from falling down.
Semi-translucent panels 20 are mounted on the side of housing body 11 to limit the amount of light escaping the side. During normal use, user's hands move within close proximity to LEDs. Due to this close proximity, user's hands will become very bright without panels 20 , distracting use and adversely affecting user's night vision. Panels 20 will limit the brightness of the light, yet still allow for illumination to the side of the user.
Opaque protrusion 21 shields a user's direct view of LEDs 18 . By design, LEDs 18 have an intense bright spot at the foremost point in the lens. Without opaque protrusion 21 , user would have a direct view of this intense bright spot, significantly and adversely affecting user's night vision. Protrusion 21 blocks substantially all light from direct view by user, allowing user to develop better night vision. This allows the user to see more around him or her, and makes the light on the trail appear brighter, increasing its effective brightness.
DETAILED DESCRIPTION—ADDITIONAL EMBODIMENTS
FIGS. 6 a - 6 d show various aspects and exploded views of a second embodiment of a light with one fixed, embedded 1W LED. A 1W LED 38 is embedded in a female side-release buckle 46 . LED 38 is powered by either a single or a plurality of AAA batteries 36 which are contained in buckle 46 and enclosed by a battery cover 40 .
FIGS. 7 a - 7 b show isometric and exploded views of a third embodiment of a light with one 1W LED in an adjustable housing. LED 38 is embedded in a swivel housing 49 , which is attached to a female side-release buckle 48 . Throughout the specification and claims, the term “attached” is meant to be interpreted broadly and includes affixing to as well as integral to. Housing 49 is vertically adjustable relative to buckle 48 to direct light where it is desired. Power from batteries 36 to LED 38 is transmitted either by the method described above in the preferred embodiment or as described below.
FIGS. 8 a - 8 b show isometric and exploded views of a fourth embodiment of a light with one fixed, embedded 1W LED with an adjustable lens. LED 38 is embedded in a female side-release buckle 50 . A swivel lens 51 is attached in front of LED 38 , and rotates vertically to direct light.
FIGS. 9 a - 9 b show isometric and exploded view of a fifth embodiment of a light with one fixed, embedded 1W LED. LED 38 is embedded in a female side-release buckle 52 with male protrusions. Buckle 52 mates with a plain female buckle 43 .
In FIGS. 6-9 , LED 38 is powered by a plurality of AAA batteries 36 , which are contained in the respective buckles ( 46 , 48 , 50 , 52 ) and enclosed with a battery cover 40 . The respective female buckles ( 46 , 48 , 50 , 52 ) mate with male buckle 42 .
ADVANTAGES
FIG. 10 shows an isometric view of the preferred embodiment attached centrally to a hip belt strap of a backpack. Female side-release buckle 12 is mounted on a hip belt strap 54 . Male buckle 42 is mounted on a second hip belt strap 54 . Hip belt straps 54 are attached to a backpack 53 . Opaque protrusion 21 prevents light emitted by LEDs 18 from extending upward in the direction of users eyes.
From the description above, a number of advantages of my buckle-mounted light become evident:
a) By mounting a light on a buckle (such as a hip-belt buckle), the light is moved away from the eyes, enabling the user to see shadows, thereby increasing depth perception at night. b) By mounting a light on a buckle, the light is a significant distance from the user's nose and mouth, eliminating the temporary blindness from light reflecting off the condensation in a users breath described above. c) The light is hands-free, without the consequences of a headlamp. d) The buckle is always in the same place on the pack, so the user always knows where the light is. The possibility of forgetting or losing the light, or not being able to find it in the dark is greatly reduced, if not essentially eliminated. e) The light will be centered on the user's waist, due to the position of the buckle.
CONCLUSION, RAMIFICATIONS, AND SCOPE
Accordingly, the reader will see that the buckle-mounted light of this invention provides superior illumination when hiking at night. The visibility of shadows allows for depth perception that was previously unavailable with headlamps. This greatly increases the user's enjoyment and safety of the activity. Also, the difficulty in misplacing the light is a distinct advantage.
Although the description above contains many specificities, these should not be construed as limiting the scope of the invention but as merely providing illustrations of some of the presently preferred embodiments of this invention. For example:
a) LEDs could be set to flash as a safety light. b) Buckle could be smaller or larger. c) Buckle could be a different size than the webbing which it is attached to. d) Battery(s) could be mounted elsewhere in the buckle (such as proximal to where the strap is threaded). e) Battery(s) could be mounted inside housing assembly. f) More or fewer batteries could be used. g) Other battery sizes, configurations, or chemistries could be used, such as AA or lithium ion. h) More or fewer LEDs could be used. i) LED arrangement could be different, either by changing the angles, changing the number of angles, or changing the number of LEDs directed in each angle. j) Buckle could be mounted on sternum strap instead of hip-belt or waist-strap. k) Cable 16 could be eliminated, instead using housing mounting posts 20 for electricity transmission. Such a mechanism could be accomplished with a cup-and-ball system. l) Housing assembly could be detachable. m) If housing assembly was detachable, a harnessing assembly could be made for mounting assembly on head for chores around camp. n) If housing assembly was detachable, batteries could be mounted inside housing assembly, or in buckle using the housing mounting posts for electricity transmission. o) Housing posts could have grooves or ridges that would interact with ridges or grooves on the housing assembly, giving discreet positions for the housing relative to the buckle. p) Other light sources, such as, but not limited to, 3W LED(s) or incandescent bulb(s), could be used instead of the 5 mm or 1W LEDs. q) The light could be mounted on the male member of the buckle, or the buckle could be unisex.
Thus the scope of the invention should be determined by the appended claims and their legal equivalents, rather than by the examples given.
|
A belt buckle with an embedded power source, such as battery(s), and an attached or embedded light source, such as light emitting diodes, for illuminating an area in front of a user, such as a hiker, climber, or trail-runner. The buckle is typically a side-release plastic buckle, and is typically mounted centrally on a pack's hip-belt. The light is adjustable vertically, or has a lens to produce a tall, narrow beam of light for the purpose of illuminating a large section of trail.
| 5
|
COPYRIGHT NOTICE
[0001] A portion of the disclosure of this patent contains material that is subject to copyright protection. The copyright owner has no objection to the reproduction by anyone of the patent document or the patent disclosure as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyright rights whatsoever.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to air cleaning systems for welding chambers. In particular, the present invention relates to an air cleaning system booth, a small footprint and the ability to have many units in a confined area without substantial air handling problems.
[0004] 2. Description of Related Art
[0005] The welding of metal parts and welding to build products is an inherently dangerous endeavor. Not only are the sparks and hot metal pieces easy to start fires, cause burns, and the like, but the gases and dust created during the welding process can be toxic, as well as detrimental, to the product being produced. Generally, welding is carried out in a welding chamber, which controls dust and particulate matter generated by the process of circulating and filtering the air that enters the welding chamber before returning it to the surrounding environment.
[0006] Older welding chamber air filtration systems consist of an air cleaning system, which is positioned on the floor just outside the welding chamber. They are connected to the air flow from the welding chamber by one or more air hoses. Not only does this older system waste valuable floor space, but it adds considerably to the maintenance and cleaning of a welding system.
[0007] A more recent approach to air handling systems for welding chambers, which is superior in many ways to the side mounted units, has been the introduction of the overhead air cleaning system for welding stations. These air cleaning systems have the ability to be in direct connection with the interior of a chamber, eliminating the need for ducting, and also eliminate many of the other problems associated with side mounted air systems and lengthy ducted systems.
[0008] The air cleaning systems contain one of a variety of different types of air filtration devices. One cleaning filter method, in addition to standard charcoal, HEPA and other filter units, is the self cleaning pulsed air filter. These filters comprise a paper or cloth filter, which air moves through trapping particles. At desired intervals, a pulse of reverse flow air is blown through the filter, releasing the trapped particles for collection below the filter. Typically, air cleaning systems provide a door, which must be opened and a collector below the air filter also must be handled and cleaned. These work well, but expose the worker who cleans the unit to the filter and interior of the filter chamber every time the tray needs to be cleaned, exposing the worker and surrounding environment to a higher level of contaminants. In U.S. Pat. No. 4,359,330 issued Nov. 16, 1982 to Copley, there is disclosed a self cleaning pulsed air cleaner designed for use in air cleaning systems. The system describes methods for preventing the recontamination of the air filter after it has been pulsed but, nothing to prevent exposure to the filter every time the collection tray is cleaned.
[0009] In addition to a wide variety of filters, there are several different approaches to the air cleaning system. In U.S. Pat. No. 6,036,736 issued Mar. 14, 2000 to Wallace, et al., there is disclosed a ventilating method wherein an air blower, suitable for fumes filtered by a contaminate filter, a charcoal filter, and a HEPA filter is disclosed. The device is mounted on top of a framed box and includes spark arrestor means. In U.S. Pat. 4,606,260 issued Aug. 19, 1986 to Cox, there is disclosed a movable welding station with a top frame mounted exhaust hood, including charcoal filters. In U.S. Pat. No. 6,758,875 issued Jul. 6, 2004 to Reid et al., there is disclosed a top frame mounted air cleaning system. The system includes a blower housing, frame, filters, shields, and a spark arrestor. This particular air cleaning system has a framing system for supporting the air cleaning on top of the cabinet. The support consists of corner posts with a top corner to corner cross member of long, heavy, metal “beams”. The beams are indicated as relatively tall, and in some embodiments, must be further supported by cross posts (i.e., cross members like the upright posts which add support to the heavy beams of the invention, FIG. 1 and FIG. 2 ). Upright posts and cross beams are a fairly standard construction method for framing systems in general, and as with any older technology, present a variety of problems including their size and greater weight.
[0010] These booths all tend to take up much room on the floor, and are not very cost effective for smaller welding jobs. The problems of the present state of the art would be a greatly reduced different type of welding chamber than currently in use.
BRIEF SUMMARY OF THE INVENTION
[0011] The present invention relates to a new type of welding chamber that, while it can stand alone, allows for a reduced space when multiple chambers are used. The particular configuration is designed such that either side-to-side, back-to-back, or both configurations can be achieved with multiple booths of the present invention.
[0012] Accordingly, in one embodiment of the present invention, there is disclosed a welding booth designed to attach to one or more like welding booths comprising:
a) a left and right side panel wall; b) a back work panel wall comprising one or more adjustable slots and a duct support mounted to a top surface of the panel; c) a plurality of leveling feet; and d) a roof positioned on the top surface of the side and back panels with a roof mounted exhaust extraction port;
wherein the side and back panels are adapted, such that a side or back panel can become the side or back panel of a second welding booth attached to the welding booth.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 is a front perspective view of a welding booth of the present invention.
[0018] FIG. 2 is a back perspective view of a welding booth of the present invention.
[0019] FIG. 3 is a front view of the back panel.
[0020] FIG. 4 is a perspective view of two connected booths with one booth comprising a fume arm.
[0021] FIG. 5 is a perspective view of multiple booths positioned side-by-side and back-to-back with ducting connected to duct supports on the booth.
[0022] FIG. 6 is a perspective view of roof mounted ventilation.
DETAILED DESCRIPTION OF THE INVENTION
[0023] While this invention is susceptible to embodiment in many different forms, there is shown in the drawings, and will herein be described in detail specific embodiments, with the understanding that the present disclosure of such embodiments is to be considered as an example of the principles, and not intended to limit the invention to the specific embodiments shown and described. In the description below, like reference numerals are used to describe the same, similar, or corresponding parts in the several views of the drawings. This detailed description defines the meaning of the terms used herein, and specifically describes embodiments, in order for those skilled in the art to practice the invention.
[0024] The terms “a” or “an”, as used herein, are defined as one or as more than one. The term “plurality”, as used herein, is defined as two or as more than two. The term “another”, as used herein, is defined as at least a second or more. The terms “including” and/or “having”, as used herein, are defined as comprising (i.e., open language). The term “coupled”, as used herein, is defined as connected, although not necessarily directly, and not necessarily mechanically.
[0025] Reference throughout this document to “one embodiment”, “certain embodiments”, and “an embodiment”, or similar terms means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, the appearances of such phrases or in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments without limitation.
[0026] The term “or”, as used herein, is to be interpreted as an inclusive or meaning any one or any combination. Therefore, “A, B or C” means any of the following: “A; B; C; A and B; A and C; B and C; A, B and C”. An exception to this definition will occur only when a combination of elements, functions, steps, or acts are in some way inherently mutually exclusive.
[0027] The drawings featured in the figures are for the purpose of illustrating certain convenient embodiments of the present invention, and are not to be considered as limitation thereto. Term “means” preceding a present participle of an operation indicates a desired function for which there is one or more embodiments, i.e., one or more methods, devices, or apparatuses for achieving the desired function, and that one skilled in the art could select from these or their equivalent in view of the disclosure herein, and use of the term “means” is not intended to be limiting.
[0028] As used herein, the term “welding booth” refers to a chamber enclosed on 3 sides used for welding and for containing the sparks and/or air emissions caused by the welding activity. In the present invention, they are designed for smaller welding jobs, and unlike large cabinets designed for large robotic welding jobs that are enclosed on 4 sides. These booths typically have a relatively small footprint on the floor of around 3 or 4 feet on a side to no more than about 10 or 12 feet on a side. Where appropriate, these chambers could also be used for welding by either a small robotic or a non-robotic means, but in general, designed for operator welding small items because of the smaller size. The welding booth can accommodate smaller jobs than high volume booths, and have the advantage of operating in a smaller warehouse floor area. The welding booth normally consists of an enclosure, consisting of 3 panel sides and a roof mounted on the panels to form and define the enclosure. There is no frame structure like larger welding chambers designed for large robotic applications. In some embodiments, the paneling is solid metal or the like. In one embodiment, the panels are welding steel that is optionally powder coated. As will be shown in the figures, the booths have the advantage of being placed next to one another, or even wall sharing to take up even less floor space.
[0029] The “left and right side panel walls” are essentially identical. A panel is essentially a welded steel (tubing and sheet), powder coated panel wall. Other materials can be utilized, however, steel is presently cost effective and works in this environment. By making them essentially identical inside, two booths can use a common side panel if desired, though walls can be single or double as desired, thus, saving on materials, and not wasting floor space by needing floor space in-between each booth. While a single booth could be free standing, the great advantage of the present invention is the shared wall option. In the shared wall option, two welding booths of the invention share a wall. The left and right walls of the two booths are the same wall. This can be clearly seen in the drawings of the present invention. The panels each have leveling feet. These feet create a space underneath the bottom of the side panels for air circulation, and in addition allow for leveling of the booth on uneven surfaces.
[0030] The “back work panel wall” is the third center panel of the booth. The present booth has no front wall. The back wall and left and right side walls can be attached to one another to create a free standing three wall structure. In other embodiments, the roof attaches to the top surface of the side and back panels to hold them together, and in yet another embodiment, both methods are used to hold the panels together and the structure upright and in a squared off configuration. The back wall is also optionally outfitted with one or more adjustable slots for regulating air circulation in and out of the booth. This can be used to balance air flow and air pressure within the booth. The slots can also be positioned in the roof, but the booth is fitted with at least one of these slots in the back wall or roof. An adjustable slot is an opening that can be adjustably opened or closed to the opposite outside of the panel to allow air circulation to pass through the back panel (or roof) as desired. The back panel also is outfitted with leveling feet, which accomplish the same function as the side panels. Note that in one embodiment, the back wall as well as the side walls can be predrilled for side-to-side or back-to-back use, where the walls are used together and not shared. The back wall is engineered to support overhead ducting, wiring, gas lines and the like, without additional structures and/or hanging anything from the ceiling for support.
[0031] The roof of the present invention is outfitted with a means of resting on the top surface of the two sides and one back panel. As can be seen in the figures, which accompany, the bottom of the roof can be fitted with a slot or bracket, so that the roof stays in place when placed on the 3 walls. The roof can also be screwed, welded, or otherwise attached to the walls as desired. The roof can be a flat type roof, or can be a built up roof as is typical in many welding cabinets of larger size. The recess in the roof can be outfitted with lighting, ductwork, or the like, as well as air flow pass through slots as in the back wall. The roof on its top surface has a vent exit, which passes down to the booth interior. In order for several booths to be used together and to string exhaust tubing along the top of the booths, the back panel is outfitted with a support bracket for supporting exhaust vents (tubing) along the width of the booth while some attachment can partially be to the roof, the back wall placement allows for better support and better usage for booths placed back to back. By supporting the vents on the back wall instead of the roof, they can be strung together easier, and provide more support than those mounted directly on the roof. Multiple connected booths can then be attached by sharing a common side wall or back wall, as desired. While they can also be attached without sharing a common wall, the sharing allows for a reduction in expense, when utilizing the booths together. In other embodiments it's possible to utilize a roof mounted filtration system, such as filters. These systems are known in the art however it's possible to use a single filtration unit mounted to span two or more booths thus saving money and equipment, something not achieved in previous welding system enclosures.
[0032] Now referring to the drawings, FIG. 1 is a front angle perspective of the welding booth of the present invention. Welding booth 1 consists of left panel 2 and right panel 3 . Panels 2 and 3 are constructed of a square tubing frame 5 covered with a steel sheet coating 5 a, and the entire exposed surface powder coated as desired. As can be seen, the frame left panel 2 supports a CO2 bracket 6 for placing a CO2 canister and positioned between left panel 2 and right panel 3 is shelf 7 .
[0033] Likewise, back panel 10 is tubing and sheet metal covered with a powder coating, but has several additional accessories. There are quick connectors 12 for gas, such as CO2 or air. There is also an open shelf 13 , and right above that, a dust clean out drawer 15 for collecting heavier dust. The adjustable air slots 20 with adjustment handles 21 can be seen in this view. The roof 30 is supported on tops 8 of the left 2 and right 3 panels as well as the top of back panel 10 not seen in this view. The roof 30 has electrical connection box 31 positioned in the back right corner for routing electrical and for a working light. The back left corner has quick connect inlets 34 for attaching gas to feed connectors 12 inside the booth 1 . Also seen in this view is exhaust port 32 . This connector can be attached to exhaust tubing and a motor to suck air out of the booth 1 . The exhaust tubing brace 32 a is shown in this embodiment as spanning the entire width of the booth along the back wall 10 , and supported on the top of that wall as well as attached to the roof 30 of the invention booth 1 . In order to further brace this embodiment, triangular braces 33 are placed on roof 30 , and welded in place to give lateral support to the brace 32 .
[0034] FIG. 2 shows a back angle perspective view of booth 1 . In this view, the top of back panel 10 can be seen. It is noted that while the two side panels are the same height in this view, the back panel 10 is taller. Note that the top of back panel 35 can also be seen in this view. FIG. 3 is a full frontal view of the present invention, in addition to multiple adjustable slots 20 . This view shows the entire interior portion of booth 1 . In this view, electrical outlets 38 and electric light switch 39 can be seen. The light is recessed up inside the roof in this embodiment.
[0035] FIG. 4 depicts an embodiment with side-to-side configuration of two units sharing a single side wall. Note wall 40 , which is the left wall of booth 45 and the right wall of booth 46 . This view is from a lower perspective than the previous figures, such that one can see up into the roof, where recess or hanging light fixture 48 can be seen. This view has booth 45 equipped with a retractable fume arm 50 . This arm has the ability to be repositioned as necessary during use, and the small suction head 51 positioned next to the job. Typically fume arms have about a 4 to 8 inch capacity in this environment. With one embodiment being a 6 inch fume arm (referring to diameter). It is clearly designed for small welding jobs as is the entire booth of the present invention.
[0036] FIG. 5 shows a large series of booths in both side-to-side and back-to-back configuration. Booths 60 a and 60 b are positioned back-to-back, and thus, the exhaust tubing braces 32 a are touching and a single exhaust connection 62 is used. As can be seen, the main tubing 63 exhausts to the outside with each pair of booths connected along the main tubing route. Electrical is provided, using conduit 64 with connections to each booth. One can clearly see that in this configuration, several booths can be positioned in a relatively small space on the floor, and conveniently be exhausted at the same time.
[0037] FIG. 6 depicts a perspective view of an embodiment of the present invention where there is a roof mounted filtration system spanning two booths of the present invention. In this embodiment roof 30 has roof mounted filter system 70 . The roof mounted filter system 70 can contain paper filters screens or any other type of filtration unit or means normal for welding type environments. Access to the filter is by door 71 and particulate clearing can be accessed by drawers 72 . By using a single filtration system 70 a further benefit of the present invention is obtained.
[0038] It is clear to one skilled in the art that the drawings herein, are not intended to be limiting. Variations on materials number of attached booths accessories in the booth and the like are within the skill in the art in view of the present disclosure. Nothing in the claims is therefore intended to be limited by the drawings.
|
The present invention relates to a welding booth that has a small foot print and can be joined to other booths for maximization of floor space use.
| 1
|
BACKGROUND OF THE INVENTION
(1) Field of the Invention
The present invention relates to a novel, optically active cyclopropane compound and a liquid crystal composition comprising this optically active cyclopropane compound.
This optically active cyclopropane compound is valuable as an optical switch element material, especially a material of a ferroelectric liquid crystal composition.
In the instant specification, by the term "liquid crystalline substance or material" is meant not only a substance showing a liquid crystalline phase but also a substance or material which is valuable as a constituent of a liquid crystal composition though it is not detected that the substance or material shows a liquid crystalline phase.
(2) Description of the Related Art
As the display system using a liquid crystal display element, which is widely utilized in practice at present, there can be mentioned the twisted nematic type (TN type) and the dynamic scattering type (DS type). In these display systems, display is performed by a nematic liquid crystalline cell comprising a nematic liquid cell as the main component. One defect of the conventional nematic liquid cell is a low response speed, and only a response speed of several milliseconds is obtained. This defect is one cause of the limitation of the application range of the nematic liquid cell. Recently, however, it has been found that a high response speed can be obtained if a smectic liquid crystalline cell is used.
It has been clarified that some optically active smectic liquid crystals have a ferroelectric property, and there are great expectations on the utilization of such liquid crystals. Liquid crystals having a ferroelectric property, that is, ferroelectric liquid crystals, are compounds synthesized by R. B. Meyer et al in 1975, which are represented by 2-methylbutyl 4-(4-n-decyloxybenzilydeneamino)cinnamate (hereinafter referred to as "DOBAMBC"). The compounds are characterized as exhibiting a ferroelectric property in the chiral smectic C phase (hereinafter referred to as "SmC* phase") [J. Physique, 36, L-69 (1975)].
N. A. Clark et al found that a high-response speed of an order of microseconds is obtained in a film cell of DOBAMBC [Appl. Phys. Lett., 36, 89 (1980)], and with this finding as a momentum, the ferroelectric crystal has attracted attention as a material applicable not only to a display system such as a liquid crystal television but also to an optical printer head, an optical Fourier converting element, a light valve, and other optoelectronic elements because of high-speed response characteristics.
Since DOBAMBC has a small spontaneous polarization and is a Schiff base, it has poor physical and chemical stabilities. Accordingly, various physically and chemically stable compounds have been investigated as ferroelectric liquid crystalline materials. At present, research work on the development of ferroelectric liquid crystalline materials is concentrated on an enhancement of the high-speed response characteristic, orientation effect, contrast characteristic, memory characteristic, and threshold value characteristic, and optimization of practical properties such as the temperature dependencies of these characteristics.
However, none of the known ferroelectric liquid crystals, when used alone, shows a large spontaneous polarization, a low viscosity, a long helical pitch and an appropriate molecular tilt angle within a broad temperature range including room temperature such that the above-mentioned practically desired properties are manifested. Therefore, practically, attempts have been made to optimize the foregoing characteristics by mixing several compounds such as a compound having or inducing a large spontaneous polarization, a compound having a low viscosity and compounds having reverse helical pitches. The incorporation of a ferroelectric liquid crystal showing a ferroelectric characteristic within a broad temperature range or a smectic C liquid crystal which is not chiral is effective for obtaining a liquid crystal composition showing a ferroelectric characteristic within a broad temperature range. In connection with liquid crystalline materials used for ferroelectric liquid crystal compositions, it is considered necessary to optimize the physical properties by selecting (1) a compound having or inducing a large spontaneous polarization, (2) a compound considered from the skeleton to have a low viscosity or a compound not degrading the liquid crystalline property of a compound considered from the skeleton to have a low viscosity when both are mixed, (3) a compound having a short helical pitch and capable of unwinding the helical pitch by the addition thereof in a minor amount, and (4) a liquid crystalline substance showing a ferroelectric property within a broad temperature range, among a great: number of compounds differing in the skeleton and optically active group, and mixing them together.
The presence of an optically active group is indispensable for a compound to be a ferroelectric liquid crystal. Amyl alcohol, octyl alcohol and the like are mentioned as the known optical activity source. Although these alcohols are easily available, they are monohydric alcohols having poor reactivity, and chemical modification in the vicinity of the optically active site is limited and the molecular design of a liquid crystalline substance is therefore difficult. As a typical instance of this chemical modification, there can be mentioned only the carbon number-increasing reaction proposed by A. Hallsby et al [Mol. Cryst. Liq. Cryst., 1982 (62), L61] or J. W. Goodby et al [Mol. Cryst. Liq. Cryst., 1984 (110), 175-203].
As the effect of the optically active group or the neighbouring substituent, there can be mentioned the steric factor and electronic factor of the asymmetric source. As the effect on the physical properties of the liquid crystalline material, the former factor has an influence on the symmetry of the liquid crystalline molecule and, for example, control of the range of temperatures showing the liquid crystalline phase becomes possible. The latter factor gives a change to the optically active group or the neighbouring dipole moment and control of the direction and magnitude of the spontaneous polarization, the length and direction of the pitch and the viscosity becomes possible Accordingly, if the effects of the optically active group or the neighbouring substituent are effectively controlled, the molecular design of a compound satisfying the requirements of various characteristics such as temperature range, response speed, viscosity and pitch length, which are imposed on a ferroelectric liquid crystalline material ensuring realization of large-scale liquid crystal panel display, or the design of a composition of such compounds will be easily accomplished.
SUMMARY OF THE INVENTION
We investigated liquid crystalline substances obtained from various asymmetric sources and found optically active cyclopropane compounds having a performance equal or superior to those of liquid crystalline substances obtained from non-cyclic alcohols such as amyl alcohol and octyl alcohol. We have now completed the present invention based on this finding.
It is a primary object of the present invention to provide novel optically active cyclopropane compounds which either exhibit a ferroelectric liquid crystalline characteristic or do not exhibit a ferroelectric liquid crystalline characteristic but can be effectively used as a constituent of a ferroelectric liquid crystal composition, which have a relatively large spontaneous polarization, and which exhibit a high-speed response
In one aspect of the present invention, there is provided an optically active cyclopropane liquid crystalline compound represented by the following formula (1): ##STR4## wherein R represents a linear or branched alkyl group having 4 to 18 carbon atoms or a cycloalkyl group having 4 to 18 carbon atoms, n is 0 or 1, Y 4 represents --CO 2 CH 2 --, --OCO-- or --OCH 2 --, Y 1 , Y 2 and Y 3 independently represent --CO 2 --, --OCO--, --O--, a direct bond or --CH 2 O--, Z 1 , Z 2 , and Z 3 are independently selected from ##STR5## and at least two of the groups optionally selected as Z 1 , Z 2 and Z 3 may be the same or different, A 1 , A 2 and A 3 independently represent a fluorine atom, a bromine atom, a chlorine atom, a cyano group or a hydrogen atom, and the mark ##STR6## indicates an asymmetric carbon atom.
In another aspect of the present invention, there is provided a liquid crystal composition comprising at least one optically active cyclopropane compound represented by the above formula (1).
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows the IR spectrum of the optically active cyclopropane compound obtained in Example 1, and FIG. 2 is a phase diagram of a composition comprising 4'-octylcarbonyloxy-4-(1S-2,2-dimethylcyclopropanemethyloxycarbonyl)biphenyl and 4'-heptylcarbonyloxy-4-(1S-chloro-2-methylbutylcarbonyloxy)biphenyl.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In general, liquid crystalline compounds have a rod-like structure comprising a nuclear portion composed of a benzene ring or the like and a linear portion composed of an alkyl chain or the like. It is known that compounds in which the carbon number of the alkyl chain exceeds a certain level is apt to have the smectic phase. It also is known that compounds having the same skeleton show similar phase systems even if the carbon number of the alkyl chain differs to some extent. Compounds of the formula (1) in which R is an alkyl group having 6 to 14 carbon atoms are apt to show a chiral smectic C phase singly or in the form of a mixture, and they are especially valuable as ferroelectric liquid crystalline materials. Other compounds of the formula (1) can be used as additives to ferroelectric liquid crystals or as ordinary liquid crystalline materials.
The optically active cyclopropane compound of the present invention is valuable as a liquid crystalline substance, especially a ferroelectric liquid crystalline substance. The cyclopropane compound has a larger spontaneous polarization than other linear optically active alcohols Although a compound of the following formula (A): ##STR7## shows a chiral smectic C phase ("SmC* phase") in the case of n=7 to 11 and a compound of the following formula (B): ##STR8## shows a SmC* phase in the case of n=7 to 12, the spontaneous polarization is up to 5 nC/cm 2 even at highest.
In contrast, the compound of the following formula (C) having a cyclopropane ring according to the present invention has a spontaneous polarization of 11 nC/cm 2 , which is more than 2 times that of the compound (A) or (B): ##STR9##
The reason why the cyclopropane compound of the present invention has a larger spontaneous polarization than the non-cyclic optically active alcohol such as amyl alcohol is considered to be that since the asymmetric source is present on the three-membered ring, the rotation freedom of the asymmetric source or neighbouring substituent is reduced and the steric conformation is fixed.
As is illustrated in the example given hereinafter, according to the present invention, there can be provided (1) compounds which do not degrade the liquid crystal characteristic of a compound considered from the skeleton to have a low viscosity when incorporated into this liquid crystalline compound and (2) compounds which have a short helical pitch and provide good compositions in which the helical pitch is unwound by incorporation of small amounts of said compounds.
As the compounds suitable for forming a ferroelectric liquid crystalline composition by mixing them with the optically active cyclopropane compound of the present invention, there can be mentioned compounds of the following groups (1), (2) and (3).
(1) Ferroelectric liquid crystals developed by us in the past, which are disclosed in Japanese Unexamined Patent Publication Nos. 60-67,453, 60-67,586, 60-168,780, 60-168,781 and 60-218,358, and Japanese Patent Application Nos. 59-189,232, 60-22,920, 60-87,034, 60-117,053, 60-144,136, 60-162,654, 60-162,656, 60-250,335, 60-272,834, and No. 60-291,179.
(2) Compounds having a smectic C phase, such as alkyl alkoxybiphenylcarboxylate, alkyl alkylcarbonyloxybiphenylcarboxylate, alkoxyphenyl alkoxybenzoate, alkyloxycarbonylphenyl alkoxybenzoate, alkoxyalkoxyphenyl alkoxybenzoate, alkoxybiphenyl alkoxybenzoate, alkoxyphenyl alkoxybiphenylcarboxylate, alkoxybiphenyl alkylbenzoate, alkoxyphenyl alkylbiphenylcarboxylate, alkylbiphenyl alkoxybenzoate, alkylphenyl alkoxybiphenylcarboxylate, alkoxybiphenyl alkylcarbonyloxybenzoate, alkoxyphenyl alkylcarbonyloxybiphenylcarboxylate, alkylcarbonyloxybiphenyl alkoxybenzoate, alkylcarbonyloxyphenyl alkoxybiphenylcarboxylate, 5-alkyl-2-(4'-alkoxyphenyl)pyrimidine, 5-alkoxy-2-(4'-alkoxyphenyl)pyrimidine, 5-alkyl-2-(4'-alkylcarbonyloxyphenyl)pyrimidine, 5-alkoxy-2-(4'-alkylcarbonyloxyphenyl)pyrimidine, 5-alkyl-2-(4'-alkyloxycarbonylphenyl)pyrimidine, 5-alkoxy-2-(4'-alkyloxycarbonylphenyl)pyrimidine, 5-alkyl-2-(4'-alkoxyphenyl)pyrazine, 5-alkoxy-2-(4'-alkoxyphenyl)pyrazine, 5-alkyl-2-(4'-alkylcarbonyloxyphenyl)pyrazine, 5-alkoxy-2-(4'-alkylcarbonyloxyphenyl)pyrazine, 5-alkyl-2-(4'-alkyloxycarbonylphenyl)pyrazine, 5-alkoxy-2-(4'-alkyloxycarbonylphenyl)pyrazine, 3-(4'-alkylphenyl)-6-alkoxypyridazine, 3-(4'-alkoxyphenyl)-6-alkoxypyridazine, 3-(4'-alkoxyphenyl)-6-alkylpyridazine, 5-(4'-alkylphenyl)-2-(4"-alkoxyphenyl)pyrimidine, 5-(4'-alkoxyphenyl)-2-(4"-alkoxyphenyl)pyrimidine, 5-(4'-alkylphenyl)-2-(4"-alkylcarbonyloxyphenyl)pyrimidine, 5-(4' -alkoxyphenyl)-2-(4"-alkylcarbonyloxyphenyl)pyrimidine, 5-(4'-alkylphenyl)-2-(4"-alkyloxycarbonylphenyl)pyrimidine, 5-(4'-alkoxyphenyl)-2-(4"-alkyloxycarbonylphenyl)pyrimidine, 5-(4'-alkoxyphenyl)-2-(4"-alkoxyphenylcarbonyloxy)pyrimidine, 5-(4'-alkylphenyl)-2-(4"-alkoxyphenylcarbonyloxy)pyrimidine, 5-(4'-alkoxyphenyl)-2-(4"-alkylphenylcarbonyloxy)pyrimidine, alkylphenylcarbonyloxy)pyrimidine, 5-(4'-alkylphenyl)-2-(4"-alkoxyphenyl)-1,2,4-triazine, 5-(4'-alkoxyphenyl)-2-(4"-alkoxyphenyl)-1,2,4-triazine, 5-(4'-alkylphenyl)-2-(4"-alkylcarbonyloxyphenyl)-1,2,4-triazine, 5-(4'-alkoxyphenyl)-2-(4"-alkylcarbonyloxyphenyl)-1,2,4triazine, 5-(4'-alkylphenyl)-2-(4"-alkyloxycarbonylphenyl)-1,2,4-triazine and 5-(4'-alkoxyphenyl)-2-(4"-alkyloxycarbonylphenyl)-1,2,4-triazine.
(3) Ferroelectric liquid crystalline compounds showing a chiral smectic C phase, which are obtained by introducing an asymmetric carbon atom in the alkyl group, alkoxy group, alkylcarbonyloxy group or alkyloxycarbonyl group in the above-mentioned compounds of the group (2).
The cyclopropane compound of the formula (1) is derived, for example, from (+)-1S-2,2-dimethylcyclopropane-carboxylic acid of the following formula (D) as the asymmetric source: ##STR10##
The compound of the formula (D) is synthesized according to a known process as disclosed in Japanese Unexamined Patent Publication No. 59-225,194. More specifically, isobutylene gas is reacted with ethyl diazoacetate in the presence of a catalytic amount of a copper complex of (R)-N-salicylydene-2-amino-1,1-di(2-butoxy-5-t-butylphenyl)-3-phenyl-1-propanol and a catalytic amount of phenylhydrazine and the reaction product is hydrolyzed to obtain the compound of the formula (D). The so-obtained (+)-1S-2,2-dimethyl- cyclopropane-carboxylic acid (D) or its active derivative is reacted with a phenol derivative, or the compound (D) is reduced to (+)-2,2-dimethyl-1S-hydroxymethylcyclopropane according to a known process and this compound is reacted with a benzoic acid derivative, whereby the optically active cyclopropane compound represented by the formula (1) is obtained.
The optically active cyclopropane compound of the present invention has a ferroelectric liquid crystalline characteristic. For example, 4'-octyloxy-4-(1S-2,2-dimethylcyclopropane-methyloxycarbonyl)biphenyl shows the SmC* phase at a temperature of from 27° to 40° C. and has a spontaneous polarization of 11 nC/cm 2 .
The spontaneous polarization of the optically active compound of the present invention is relatively large, as pointed out above.
Although a certain optically active cyclopropane compound included within the scope of the present invention is not a ferroelectric liquid crystal when used alone, this compound can be effectively used as a constituent of a ferroelectric liquid crystal composition. As shown in the examples given hereinafter, some of optically active cyclopropane compounds of the present invention are substances showing no liquid crystalline phase when used alone, but there are included compounds having a short inherent helical pitch such as 0.1 μm and if small amounts of such compounds are incorporated into ferroelectric liquid crystalline compounds or compositions having a reverse helical pitch, there can be obtained ferroelectric liquid crystal compositions having a long helical pitch.
For example, as illustrated in the examples given hereinafter, if S-type optically active cyclopropane compounds of the present invention, which have a counterclockwise helical pitch, are mixed with natural amino acid derivatives, that is, ferroelectric liquid crystals having a clockwise helical pitch and a very large spontaneous polarization, which were developed by us in the past and are disclosed in Japanese Unexamined Patent Publication No. 60-218,358 and Japanese Patent Application Nos. 59-189,232, 60-22,920, 60-87,034, 60-117,053, 60-144,136, 60-162,654, 60-291,179, ferroelectric liquid crystal compositions having an elongated helical pitch providing a good orientation can be obtained.
The optically active cyclopropane compound of the present invention or an optical active liquid crystal composition comprising the optically active cyclopropane compound of the present invention can be added to a nematic liquid crystal for color display of the White-Taylor type, display of the cholesteric-nematic phase transition type and prevention of generation of the reverse domain in a TN-type cell.
Since a liquid crystal composition comprising the cyclopropane compound of the present invention is a smectic liquid crystal, the liquid composition can be used for a memory type display element of the heat writing type or laser writing type.
The present invention will now be described in detail with reference to the following examples that by no means limit the scope of the invention.
In the examples, C, SX, S*, Sc*, Sa, N*, N and I phases represent a crystal phase, a smectic phase not clearly identified, a chiral smectic phase not clearly identified, a chiral smectic C phase, a smectic A phase, a chiral nematic phase, a nematic phase and an isotropic phase, respectively.
The compounds of the present invention were purified by silica gel chromatography and recrystallization from an alcohol or hexane. The measured values of the phase transition points, shown hereinafter, will be influenced by the purities of substances.
EXAMPLE 1
Synthesis of 4'-octylcarbonyloxy-4-(1S-2,2-dimethylcyclopropane-methyloxycarbonyl)biphenyl
(a) A 100-ml three-neck flask equipped with a constant pressure dropping funnel, a magnetic stirrer and a reflux condenser was charged with 30 ml of anhydrous ether and 0.8 g (21.1 millimoles) of lithium aluminum hydride after sufficient substitution of the inner atmosphere with nitrogen The reactor was cooled to 0° C. and 2.1 g (16.3 millimoles) of ethyl (+)-1S-2,2-dimethylcyclopropane-carboxylate obtained according to the known process and 20 ml of anhydrous ether were carefully dropped with stirring over a period of about 15 minutes. After completion of the dropwise addition, the temperature was returned to room temperature and the mixture was stirred for about 1 hour. Then, 20 ml of water was added to the reaction mixture to effect hydrolysis, and an excess of sodium chloride was added and ether extraction carried out. The ether layer was washed with a saturated aqueous solution of sodium chloride and dried on anhydrous magnesium sulfate. Ether was removed by distillation and the residue subjected to distillation under reduced pressure to obtain 1.27 g (12.6 millimoles) of (+)-2,2-dimethyl-1S-hydroxymethylcyclopropane as a fraction boiling at 62 to 63° C under 70 mmHg.
(b) A 100-ml flask was charged with 0.58 g (5.79 millimoles) of (+)-2,2-dimethyl-1S-hydroxymethylcyclopropane, 20 ml of carbon tetrachloride and 5 ml of pyridine, and then 2.0 g (5.91 millimoles) of an acid chloride derivative from 4'-octylcarbonyloxybiphenyl-4-carboxylic acid and 20 ml of carbon tetrachloride were dropped. The mixture was allowed to stand overnight and the reaction liquid was poured into ice water, followed by neutralization with dilute hydrochloric acid, extraction with chloroform, washing, drying and removal of the solvent by distillation. The residue was purified by silica gel column chromatography (developing solvent=chloroform/carbon tetrachloride mixed solvent of 2/5) and recrystallized from ethanol to obtain 0.8 g of 4'-octylcarbonyloxy-4-(lS-2,2-dimethylcyclopropanemethyloxycarbonyl)biphenyl, the infrared (IR) spectrum of which is shown in FIG. 1.
When the obtained compound was sealed in a cell and the transition temperatures were measured, the following results were obtained.
At elevation of temperature:
C-30-Sc*-40-Sa-48-I
At lowering of temperature:
C-9-SX-21-S*-27-Sc*-40-Sa-48
The spontaneous polarization of the above compound was 11 nC/cm 2 as determined according to the Sawyer-Tower method.
EXAMPLE 2
When 4'-octylcarbonyloxy-4-(1S-2,2-dimethylcyclopropane-methyloxycarbonyl)biphenyl obtained in Example 1 was mixed with 4'-heptylcarbonyloxy-4-(1S-chloro-2-methylbutylcarbonyloxy)biphenyl at a weight ratio of 1/1, a composition showing the SmC* phase at a temperature of from 5 to 25° C. was obtained. The phase diagram of the composition is shown in FIG. 2.
EXAMPLE 3
Synthesis of 4'-octyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl
An acid chloride derived from (+)-1S-2,2-dimethylcyclopropane-carboxylic acid was reacted with p-(p'-octyloxyphenyl)-phenol in pyridine as the solvent. The reaction mixture was allowed to stand overnight and poured into ice water, followed by neutralization with dilute hydrochloric acid, extraction with chloroform, washing, drying and removal of the solvent by distillation. The residue was purified by silica gel column chromatography (developing solvent =chloroform/carbon tetrachloride mixed solvent of 1/3) and recrystallized from methanol to obtain 4'-octyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl having a melting point of 72° C.
EXAMPLES 4 through 6
The following compounds were synthesized in the same manner as described in Example 3 except that p-(p'-alkyloxyphenyl)-phenols were used instead of p-(p'-octyloxyphenyl)-phenol.
4'-Butyloxy-4-(1S-2,2-dimethylcyclopropanecarbonyloxy)biphenyl having a melting point of 90° C.
4'-Dodecyloxy-4-(1S-2,2-dimethylcyclopropanecarbonyloxy)biphenyl having a melting point of 70° C.
4'-Hexadecyloxy-4-(1S-2,2-dimethylcyclopropanecarbonyloxy)biphenyl having a melting point of 79° C.
EXAMPLE 7
4'-Octylcarbonyloxy-4-(1S-2,2-dimethylcyclopropanecarbonyloxy)biphenyl was synthesized in the same manner as described in Example 3 except that p-(p'-octylcarbonyloxyphenyl)-phenol was used instead of p-(p'-octyloxyphenyl)-phenol. The melting point of the obtained compound was 72° C.
EXAMPLE 8
4'-Nonyloxycarbonyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl was synthesized in the same manner as described in Example 3 except that p-(p'-nonyloxycarbonyloxyphenyl)-phenol was used instead of p-(p'-octyloxyphenyl)-phenol. The melting point of the obtained compound was 57° C.
EXAMPLE 9
2-[4-(1S-2,2-Dimethylcyclopropane-carbonyloxy)phenyl]-5-dodecylpyrimidine was synthesized in the same manner as described in Example 3 except that 2-(4-hydroxyphenyl)-5-dodecylpyrimidine was used instead of p-(p'-octyloxyphenyl)-phenol. The melting point of the obtained compound was 70° C.
EXAMPLES 10 through 12
The following compounds were synthesized in the same manner as described in Example 3 except that 2-(4-alkoxyphenyl)-5-hydroxypyrimidines were used instead of p-(p'-octyloxyphenyl)-phenol.
2-(4-Heptyloxyphenyl)-5-(1S-2,2-dimethylcyclopropane-carbonyloxy)pyrimidine having a melting point of 96° C. propane-carbonyloxy)pyrimidine having a melting point of 97° C.
2-(4-Dodecyloxyphenyl)-5-(1S-2,2-dimethyl- cyclopropane-carbonyloxy)pyrimidine having a melting point of 102° C.
EXAMPLE 13
Bis-[p-(1S-2,2-dimethylcyclopropane-carbonyloxy)phenyl] was synthesized in the same manner as described in Example 3 except that p,p'-biphenol was used instead of p-(p'-octyloxyphenyl)-phenol. The melting point of the obtained compound was 138° C.
EXAMPLE 14
By mixing compounds of the present invention with compounds having the smectic C phase, there was prepared a composition comprising 4.6% by weight of 4'-butyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 4.6% by weight of 4'-octyloxy-4-(1S-2,2-dimethyl- cyclopropane-carbonyloxy)biphenyl, 4.6% by weight of 4'-dodecyloxy-4-(1S-2,2-dimethylcyclopropanecarbonyloxy)biphenyl, 4.6% by weight of 4'-hexadecyloxy-4(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 4.6% by weight of 4'-nonyloxycarbonyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 4.6% by weight of 2-[4-(1S-2,2-dimethylcyclopropane-carbonyloxy)phenyl]-5-dodecylpyrimidine, 43.4% by weight of 2-(4'-nonyloxy)phenyl-5-nonylpyrimidine and 30.0% by weight of 4-nonyloxyphenyl 4-octyloxybenzoate.
The composition showed the ferroelectric liquid crystalline phase even to a temperature below 0° C. and had the following phase transition points
Sc*-Sa phase transition point: 51° C.
Sa-N* phase transition point: 52° C.
N*-I phase transition point: 62° C.
As apparent from the foregoing description, even an optically active cyclopropane compound included within the scope of the present invention, which is not a ferroelectric liquid crystal when used alone, is effectively used for forming a liquid crystal composition showing ferroelectric characteristics at room temperature by mixing this compound with a compound having the smectic C phase.
EXAMPLE 15
Compounds of the present invention were mixed with a ferroelectric liquid crystal composition having a clockwise helical pitch to obtain a composition having an unwound helical pitch and comprising 4.0% by weight of 4'-butyloxy-4-(1S-2,2-dimethylcyclopropanecarbonyloxy)biphenyl, 4.0% by weight of 4'-octyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 4.0% by weight of 4'-dodecyloxy-4-(1S-2,2-dimethyl- cyclopropane-carbonyloxy)biphenyl, 4.0% by weight of 4'-hexadecyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 4.0% by weight of 4'-nonyloxycarbonyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 4.0% by weight of 2-[4-(1S-2,2-dimethylcyclopropane-carbonyloxy)phenyl)-5-dodecylpyrimidine, 12.4% by weight of (1S,2S)-4"-(4'-octyloxyphenyl)phenyl 1-chloro-2-methylpentanoate, 12.4% by weight of (1S,2S)-4"-(4'-nonylcarbonyloxyphenyl)phenyl 1-chloro-2-methylpentanoate, 12.4% by weight of (1S)-4"-(4'-nonylcarbonyloxyphenyl)phenyl 1-chloro-2-methylbutanoate and 38.8% by weight of (1S,2S)-4"-[4'-(1-chloro-2-methylpentylcarbonyloxy)phenyl]phenyl 4"'-octylcarbonyloxy-3"'-chlorobenzoate. In this composition, the helical pitch of the chiral nematic phase was infinitely diffused, and the orientation was very good.
The composition showed the ferroelectric liquid crystalline phase even to a temperature below 0° C. and had the following phase transition points.
Sc*-Sa phase transition point: 63° C.
Sa-N* phase transition point: 65° C.
N*-I phase transition point: 70° C.
The composition was sealed in a cell formed by spin-coating a polyimide on Nesa glass and rubbing the coating and having a spacer of a polyethylene terephthalate film having a thickness of 2.5 μm, and the composition was gradually cooled from the isotropic phase at a rate of 0.1° C. per minute, whereby a cell having a good orientation was obtained. A rectangular wave of 40 Vp-p was applied to the cell and the electrooptic effect was observed by a polarization microscope. A high-speed response was obtained at a very clear contrast. Thus, it was confirmed that this composition could be applied to liquid crystal display.
As apparent from the foregoing illustration, even optically active compounds of the present invention which are not ferroelectric liquid crystals when used alone are very valuable for forming liquid crystal compositions having a high-response speed and a very good orientation of an unwound helical pitch and showing ferroelectric characteristics at room temperature by mixing these compounds with other ferroelectric liquid crystalline compounds having a reverse helical pitch
EXAMPLE 16
4'-Octyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)phenyl obtained in Example 3 is not a ferroelectric liquid crystalline compound when used alone, but since the inherent helical pitch of this compound is counterclockwise and is as short as 0.1 μm, the compound is very effective for unwinding an inherent clockwise helical pitch of a ferroelectric liquid crystal composition by addition of a small amount of said compound.
The above-mentioned compound obtained in Example 3 was mixed with a clockwise ferroelectric liquid crystal composition and further with Sc phase compounds, which were not chiral, to obtain a composition having an unwound helical pitch and comprising 7.7% by weight of 4'-octyloxy-4-(1S-2,2-dimethylcyclopropane-carbonyloxy)biphenyl, 8.85% by weight of (1S,2S)-4"-(4'-octyloxyphenyl)phenyl 1-chloro-2-methylpentanoate, 3.75% by weight of (1S,2S)-4"-(4'-nonyloxycarbonyloxyphenyl)phenyl 1-chloro-2-methyl-pentanoate, 4.25% by weight of (1S,2S)-4"-(4'-nonylcarbonyloxyphenyl)phenyl 1-chloro-2-methylpentanoate, 4.25% by weight of (1S)-4"-(4'-nonylcarbonyloxyphenyl) 1-chloro-2-methylbutanoate, 7.3% by weight of (1S,2S)-4"-[4'-(1-chloro-2-methylpentylcarbonyloxy)phenyl]-phenyl 4"'-octylcarbonyloxy-3"'chlorobenzoate, 13.15% by weight of (S)-4'-(2"-methylbutyloxy)-phenyl-4-octyloxybenzoic acid, 16.45% by weight of 2-(4'-octyloxy)phenyl-5-octylpyrimidine, 16.45% by weight of 2-(4'-nonyloxy)phenyl-5octylpyrimidine and 16.45% by weight of 2-(4'-decyloxy)phenyl-5-octylpyrimidine. In this composition, the helical pitch of the chiral nematic phase was indefinitely diffused, and the composition had a very good orientation.
The composition showed the ferroelectric liquid crystalline phase even to a temperature lower than the ice point, and the composition had the following phase transition points.
Sc*-Sa phase transition point: 54° C.
Sa-N* phase transition point: 56° C.
N*-I phase transition point: 60° C.
The composition was sealed in a cell formed by spin-coating a polyimide on Nesa glass and rubbing the coating and having a spacer of a polyethylene terephthalate film having a thickness of 2.5 μm, and the composition was gradually cooled from the isotropic phase at a rate of 0.1° C. per minute, whereby a cell having a good orientation was easily obtained A rectangular wave of 40 Vp-p was applied to the cell and the electro-optic effect was observed by a polarization microscope. A very clear contrast was seen. It was proved that the composition could be applied to a liquid crystal display. When the response speed of this cell was measured by using a photosemiconductor, it was found that the response speed required for changing the quantity of transmitted light from 10% to 90% was about 10 microseconds at room temperature, and thus it was confirmed that the response speed was very high.
As apparent from the foregoing illustration, even an optically active cyclopropane compound of the present invention, which is not a ferroelectric liquid crystal when used alone, is valuable for obtaining a liquid crystal composition having a high-speed response characteristic and a very good orientation of an unwound helical pitch and showing a ferroelectric characteristic at room temperature by mixing said compound with a ferroelectric liquid crystalline compound having a reverse helical pitch or a compound showing the smectic C phase.
EXAMPLE 17
2-(4-Decyloxyphenyl)-5-(1S-2,2-dimethylcyclopropane-carbonyloxy)pyrimidine obtained in Example 11 is not a ferroelectric liquid crystalline compound when used alone, but since the inherent helical pitch is counterclockwise and as short as 0.1 μm, the compound is valuable for unwinding the inherent helical pitch of a clockwise ferroelectric liquid crystal composition by addition of a small amount of this compound
This compound obtained in Example 11 was mixed with a clockwise ferroelectric liquid crystal composition and further with an Sc compound which was not chiral, to obtain a composition having an unwound helical pitch and comprising 10.8% by weight of 2-(4-decyloxyphenyl)-5-(1S-2,2-dimethylcyclopropane-carbonyloxy)pyrimidine, 39.2% by weight of (1S,2S)-4"-(4'-octyloxyphenyl)phenyl 1-chloro-2-methylpentanoate, 30.0% by weight of 2-(4'-nonyloxy)phenyl-5-nonylpyrimidine and 20.0% by weight of 4-nonyloxyphenyl 4-octyloxybenzoate. The composition showed the ferroelectric liquid crystalline phase even to a temperature below 0° C. and had the following phase transition points.
Sc*-Sa phase transition point: 47° C.
Sa-N* phase transition point: 53° C.
N*-I phase transition point: 58° C.
The composition was sealed in a cell formed by spin-coating a polyimide on Nesa glass and rubbing the coating and having a spacer of a polyethylene terephthalate film having a thickness of 3.4 μm, and the composition was gradually cooled from the isotropic phase at a rate of 0.1° C. per minute, whereby a cell having a good orientation was easily obtained A rectangular wave of 58 Vp-p was applied to the cell and the electro-optical effect was observed by a polarization microscope. A very clear contrast was seen. Thus, it was proved that the composition could be applied to a liquid crystal display. When the response speed of the cell was measured by using a photosemiconductor, it was found that the response speed required for changing the quantity of transmitted light from 10% to 90% was about 30 microseconds at room temperature, and thus it was confirmed that the response speed was very high.
As apparent from the foregoing illustration, even an optically active cyclopropane compound of the present invention which is not a ferroelectric liquid crystal when used alone is valuable for forming a liquid crystal composition having a ferroelectric characteristic at room temperature, a high response speed and a very good orientation of an unwound helical pitch by mixing this compound with a ferroelectric liquid crystalline compound having a reverse helical pitch or a compound showing the smectic C phase.
|
Disclosed is an optically active cyclopropane compound represented by the formula (1): ##STR1## wherein R is an alkyl or cycloalkyl group, n is 0 or 1, Y 4 is --CO 2 CH 2 --, --OCO-- or --OCH 2 --, Y 1 , Y 2 and Y 3 independently represent --CO 2 --, --OCO--, --O--, a direct bond or --CH 2 O--, Z 1 , Z 2 , and Z 3 independently represent ##STR2## A 1 , A 2 and A 3 independently represent fluorine, bromine, chlorine, a cyano group or hydrogen, and the mark ##STR3## indicates an asymmetric carbon atom. The optically active cyclopropane compound includes a compound which exhibits a ferroelectric liquid crystalline characteristic, and a compound which does not exhibit a ferroelectric liquid characteristic when used alone, but, can be used as a constituent of a ferroelectric liquid crystal composition.
| 2
|
This invention relates to shock absorbing doors especially --although not exclusively--on rolling carts and more particularly to mobile food service equipment which are subject to being bumped by striking other objects.
BACKGROUND OF INVENTION
A rolling cart or mobile food service equipment of the described type may be used in cafeterias or restaurants, for example. These carts may be used to transport trays of food, dirty dishes, or the like. As the carts are rolled around a busy kitchen or dining room, they are likely to bump into any nearby objects. Or perhaps two carts may collide. Possibly a person who is inattentive may run into the cart.
Regardless of why it may happen, the cart is subject to shocks and jolts. The doors on the cart may have either hinges or pins to enable them to swing between opened and closed positions; or, sometimes, the door may hang in any position between being fully open or closed. As the shocks or jolts occur, the pins or hinges may bend or break, especially if the door is standing in a vulnerable position where all of the weight is being carried by the hinge or pin, as distinguished from resting on an underlying surface.
SUMMARY OF INVENTION
Accordingly, an object of the invention is to provide new and improved door mounts which will absorb shocks or jolts without bending or breaking the hinge or other support. Here an object is to provide doors which remain in a stable, fully open or closed position throughout shock causing conditions.
In keeping with these and other objects of the invention, the doors on the cart are supported on the top and bottom by projecting pins which fit into holes in a door sill or mounting blocks. Normally, at least one of the mounting blocks is slidingly supported and held in a fixed position by a spring. When the rolling cart experiences a shock or jolt, the block slides against the bias of the spring in order to absorb the shock. As soon as the shock or jolt condition subsides, the spring bias moves the block back to its normal position.
BRIEF DESCRIPTION OF DRAWINGS
A preferred embodiment is shown in the attached drawing, wherein:
FIG. 1 is a prior art rolling cart with its doors shut;
FIG. 2 is the prior art rolling cart of FIG. 1 with one of its doors in a fixed open position;
FIG. 3 is an elevation view, showing the hinge pins on a door;
FIG. 4 is an exploded view of a shock absorbing door;
FIGS. 5-7 are stop motion views drawing the shock absorbing action of the device of FIG. 4;
FIG. 8 is a fragment of a rolling cart having the inventive door mounted thereon;
FIG. 9 shows the door in a closed position; and
FIG. 10 shows the door as it is swung away from the closed position.
DETAILED DESCRIPTION OF INVENTION
An exemplary rolling cart 20 is mounted on wheels or casters 22 so that it may roll around. In this embodiment, there are two doors 24, 26, each of which is mounted on butt hinges 28-34. The doors may be opened or closed in a locked position by a use of a spring loaded paddle handles 36. The spring in this handle is often broken or jarred out of position.
When the doors are opened (FIG. 2) they may swing around the end of the cart and over a small supporting ledge 38, where they should be latched into place. Ledge 38 is supposed to support the weight of the door in order to relieve the strain on the hinges. Inside the rolling cart, oppositely disposed and vertically aligned supports are positioned to receive trays which may slide into the cart. To facilitate a sliding of trays into and out of the cart, it is desirable to swing the door 270° around the end panel of the cart to fully clear the opening through which the trays may slide.
A problem occurs as the cart rolls because it may strike or be struck by something and stop suddenly with a strong mechanical shock or jolt. The inertia of the door suddenly applies a force to the hinge which may twist the hinge or bend a hinge pin. Also, the projecting butt hinges 28-34 may project outwardly from the side where they may strike or be struck by an object, which might break or twist them.
Still another problem is that a waitress or bus boy might not swing the door all the way around and over ledge 38 so that it is fully supported by ledge 38. Or, if they did so swing the door they might not take enough time to latch it properly in an open position so that it could still swing back and away from the support provided by ledge 38. If the cart or door is struck while the weight of the door is on the hinge, it could bend them.
It should now be apparent that the hinges are probably the most vulnerable parts of the rolling cart.
Accordingly, the inventive shock absorbing door 24 (FIG. 3) has upper and lower hinge pins 44, 46, respectively forming a hinge axis. The spring loaded paddle handle 36 has been deleted in favor of a simple non-moving, recessed handle 48 so that broken latch springs are no longer a problem.
At the upper edge 50 (FIG. 2) of the cart, there is a U-shaped channel member 52 (FIG. 4) which is covered and enclosed by the top panel 54. A sliding block 56, preferably made of a durable plastic such as nylon, has dimensions such that it slides in the channel 52 and is captured within the slot by the top panel 54 (FIG. 2). A compression spring 58 resting on channel partition 59 pushes the block 56 to a normal position against an end panel 60 of the channel 52. The compression spring 58 is resting in a blind horizontal hole 66 in the block 56.
In this position, the hinge pin 44 on the door 24 passes upwardly through a window 62 in the floor of channel 52 and into a hole 64 in the block 56. As shown in FIG. 5, in this normal operating position, the hinge pin is mounted at the edge of the cabinet so that the door may freely swing between an opened and a closed position.
If the cabinet receives a jolt or a shock, the block 56 slides to an OFF normal position, as seen in FIG. 6, compressing the spring 58, in the process. The spring thus absorbs the shock caused energy and the hinge pin is not bent. The window 62 (FIG. 4) is large enough to allow the hinge pin to slide through the full shock absorbing stroke.
After the shock has ended (FIG. 7), the compression spring 58 pushes the block 56 back to its normal position, and the ability of the door to pivot is returned to its normal position.
FIGS. 8-10 show how the shock absorbing door may be used to eliminate the need for the spring biased paddle handle, while making it much more likely that a waitress or bus boy will swing and latch the door over the supporting ledge 38.
More particularly, a detent or rounded dome shaped member 68, 70 is mounted on both the door sill 72 and the supporting ledge 38. A simple way of providing these detents is to turn a bolt into a thread hole, the rounded bolt head forming the detent. The bottom of the door 24 has a nylon or similar somewhat dome-shaped wear resistant piece 74 adjacent the detents 68, 70. The lower hinge pin 46 slidingly rests in a stationary hole 76 in door sill 72. The weight of the door makes it rest on the sill 72 and behind the detent. Thus, the weight of the door causes it to be securely latched in place, while leaving it free to undertake any shock caused travel as represented in FIG. 6.
To open the door, it is only necessary to pull the handle 48. There is a natural tendency to slightly lift the door when the handle is pulled. Also, the pull upon the door, and the mutually camming surfaces of detent 68 and dome shaped wear resistant piece 74 causes the door to lift and pass over detent (FIG. 10), and then drop back to the level of the door at the starting position. The reverse happens when the door is closed.
As the door is swung around to confront the end panel 78 (FIG. 8) on the rolling cart, a waitress or busboy may tend to more or less slam the door, which gives it enough inertia to rise over and latch behind detent 70. The more careful person, who simply pushes the door into place, feels a tactile hand sensation when the door raises, as shown in FIG. 10, to pass over detent 68 or 70. Hence, this person will likely soon, learn to push the door into the latched position, either open or closed.
The foregoing description has described the shock mount on the top of the cabinet. However, it should be understood that similar shock mounts can be provided both above and below the door. Also, other arrangements could be provided such as a pivot block 56 which may swing to absorb a shock.
Those who are skilled in the art will readily perceive how to modify the invention. Therefore, the appended claims are to be construed to cover all equivalent structures which fall within the true scope and spirit of the invention.
|
The invention is a shock mount for a pivoted door on mobile food service equipment or a rolling cart. The shock mount is preferably a sliding block which is spring biased to a normal position. In case of a shock or jolt, the block slides to dissipate the energy resulting from the shock or jolt. A door is pivotally mounted on the sliding block. Detents hold the door in either a closed position or a supported open position. The pivot mount enables the door to move over the detent, while holding the door in either a closed or a supported open position.
| 4
|
CROSS-REFERENCES TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 14/121,856, filed on Mar. 17, 2014, which claims the benefit of U.S. Provisional Application Ser. No. 61/800,782 filed Mar. 15, 2013. The contents of these applications are incorporated by reference herein.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to the field of wheelchairs. Specifically, this invention relates to a wheeled power attachment that converts a manually powered wheelchair into an electrically powered wheelchair.
2. Description of the Related Art
Manually powered wheelchairs come in a variety of sizes for a variety of purposes. Two of the most common are the standard folding wheelchair and the non-folding rigid frame wheelchair 1 (as seen in FIG. 1 ) designed for more active and mobile individuals. Manually powered wheelchairs, regardless of the type of frame, generally include a frame 2 , seating portion 3 , backrest 4 , front castor wheels 5 , and rear wheels 6 having push rims 7 . Each rear wheel 6 has an axle receiver 8 that is aligned with an axle receiver 9 that is connected, directly or indirectly, to the frame 2 . A pin 10 locks each rear wheel 6 , through its axle receiver 8 , to the frame 2 through axle receiver 9 . The wheelchairs are powered by the operator gripping the push rims 7 and pushing clockwise or counterclockwise for the specified direction and speed. However, there are some times when manual wheelchairs are not beneficial, such as propelling long distances, managing uneven terrain, or when the user's deficits are of such degree that manual propulsion becomes painful, exhaustive, or relatively impossible given time or circumstances. In these situations, electrically powered wheelchairs are desired to ease the burden and stress on the operator.
Electrically powered wheelchairs have several drawbacks including the expense, size and weight. Financial, storage, and transportation concerns often make it not practical, or possible, for a user to have both an electric powered and manually powered wheelchair. It is especially inconvenient when traveling to take both types of wheel chairs. Additionally, insurance carriers generally will not pay for a user to have both types of chairs.
As a result, there is a need for a wheeled power base attachment that can convert a manual wheelchair into an electric powered wheelchair. While power attachments for manual wheelchairs exist, those in the prior art do not replace the large rear push wheels, are not controlled by a joystick, do not keep the same height as the manual wheelchair, do not support the necessary posture and positioning of the user, and/or do not have an anti-tip/counterbalance mechanism. None of the prior art power attachments provide for connection through the axle receivers of the standard wheelchair. The failure to attach at the axle receiver makes the prior art attachments more difficult to attach to all types of manual wheelchairs as it generally results in a changed center of gravity for the user. Additionally, the failure of the prior art to allow for removal of the rear wheels complicates operation of the electric powered wheelchair by making maneuverability difficult by retaining the cumbersome large rear wheels despite no longer serving a purpose.
SUMMARY OF THE INVENTION
The present invention converts a manually powered wheelchair into a powered wheelchair by replacing the rear wheels with a power base attachment. The power base attachment consists of drive wheels powered by an electric motor that are operably controlled by a user-controlled joystick. The power base attaches to the manually powered wheelchair frame through the existing axle receivers used to connect the rear wheels. The power base attachment is adjustable to fit manually powered wheelchairs of different heights and widths. Utilization of the existing axle receivers for attachment of the power base maintains the user's center of gravity necessary for balance and function. The power base attachment also includes an anti-tip/counterbalance mechanism that connects between the manually powered wheelchair frame and the frame of the power base attachment. As a user leans backwards in the converted manually powered wheelchair, the anti-tip/counterbalance mechanism slows the backward rotation of the user by resisting the rotational force and then biasing the backrest toward the normal position for safety and stability.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1 is a profile view of a standard rigid frame manually powered wheelchair.
FIG. 2 is a profile front view of the disclosed embodiment.
FIG. 3 is a profile front view of the disclosed embodiment attached to a standard rigid frame manually powered wheelchair.
FIG. 4 is a profile rear view of the disclosed embodiment attached to a standard rigid frame manually powered wheelchair.
FIG. 5 is a profile front view of the frame of the disclosed embodiment.
FIG. 6 is a profile rear view of the frame of the disclosed embodiment.
FIG. 7 is a top view of the frame of the disclosed embodiment with one mounting sleeve removed.
FIG. 8 is a cross section of line 8 - 8 in FIG. 7
FIG. 9 is the exterior view of the frame mounted axle plate and axle receiver of the disclosed embodiment.
FIG. 10 is the interior view of the frame mounted axle plate and axle receiver of the disclosed embodiment.
FIG. 11 is a front view of the disclosed embodiment.
FIG. 12 is a rear view of the disclosed embodiment.
FIG. 13 is a top down view of the disclosed embodiment without the housing cover.
FIG. 14 is a cross section of line 14 - 14 in FIG. 11 .
FIG. 15 is close up view of the disclosed embodiment attached to a manual wheelchair.
DETAILED DESCRIPTION
FIG. 2 discloses the power base attachment 20 which comprises a frame 30 , powered drive wheels 91 , rear castor wheels 94 , hand rails 69 , axle receiver 76 , electrically powered motors 90 in electrical communication with a joystick module 95 , and an anti-tip/counterbalance mechanism 100 . FIGS. 3 and 4 disclose a front and rear side profile views, respectively, of the power base attachment 20 connected to the frame 2 of a manually powered wheelchair 1 . The power base attachment 20 is positioned underneath the seating portion 3 of the manually powered wheelchair 1 where the front end 21 is positioned proximal to the front castor wheels 5 and the back end 22 extends beyond the backrest portion 4 .
FIGS. 5 and 6 further disclose the frame 30 of power base attachment 20 . The frame 30 consists of a rigid portion 31 and an adjustable portion 55 . The rigid portion 31 consists of a support frame 32 and a housing 45 . The support frame 32 comprises a front lateral member 33 , wide longitudinal members 34 , first elbow members, 35 , narrow longitudinal members 36 , second elbow members 37 , rear side members 38 , and a rear lateral member 39 . The front lateral member 33 is positioned at the front end 21 of the power base attachment 20 and is perpendicular to the longitudinal axis 23 of the power base attachment 20 . Wide longitudinal members 34 extend from the lateral ends of the front lateral member 33 towards the back end 22 of the power base attachment 20 . First elbow members 35 are positioned between each wide longitudinal member 34 and the narrowed longitudinal member 36 . The first elbow member 35 is angled perpendicularly toward the longitudinal axis 23 of the power base attachment 20 such that the distance between the narrowed longitudinal members 36 is smaller than the distance between the wide longitudinal members 34 . Second elbow members 37 are positioned between each of the narrowed longitudinal members 36 and each of the rear side members 34 . Each wide longitudinal member 34 , first elbow member 35 , narrowed longitudinal member 36 , second elbow member 37 , and short lateral member 38 are mirrored across the longitudinal axis 23 of the power base attachment 20 . The rear lateral member 39 is positioned between the two second elbow members 37 and is parallel to the front lateral member 33 . A rear lateral bracket 40 is positioned at the approximate midpoint of the rear lateral member 39 . Preferably, the front lateral member 33 , wide longitudinal members 34 , first elbow members 35 , narrowed longitudinal members 36 , second elbow members 37 , rear side members 38 , and rear lateral member 39 are positioned in the same plane. The front lateral member 33 and wide longitudinal members 34 have a first flange 41 extending into the interior space defined by the support frame 32 . Each wide longitudinal members 34 have a second flange 42 extending outwardly from the support frame 32 opposite from the first flange 41 . Two mounting sleeves 43 are mounted on the front lateral member 33 with mounting brackets 52 . The longitudinal axes of the mounting sleeves 43 are aligned and parallel to the front lateral member 33 . Each mounting sleeve 43 is positioned on either side of the longitudinal axis 23 of the power base attachment 20 .
The housing 45 of the rigid portion 31 of the frame 30 comprises a bottom panel 46 , two longitudinal side panels 47 , front panel 48 , middle panel 49 and rear panel 50 . The bottom panel 46 is parallel to the support frame 32 and is connected to the support frame 32 by the front panel 48 , middle panel 49 and rear panel 50 . The front panel 48 is connected to the flange 41 and extends at an angle to the bottom panel 46 . The middle panel 49 is attached to the support frame 32 between the first elbow members 35 and narrow longitudinal members 36 and extends perpendicular relative to the longitudinal axis 23 . The middle panel 49 also connects to the bottom panel 46 and longitudinal side panels 47 and end extends slightly above the support frame 32 . The rear panel 50 is attached to the support frame 32 between the narrow longitudinal members 36 and second elbow members 37 and is positioned perpendicular relative to the longitudinal axis 23 . The rear panel 50 connects to the bottom panel 46 , longitudinal side panels 47 , and rear lateral member 39 and extends above the support frame 32 .
Referring to FIGS. 5 , 6 , and 7 , the adjustable portion 55 consists of a generally U-shaped swing arm 56 having a middle member 57 and two extending side arms 58 . The middle member 57 is positioned parallel and pivotally mounted to the front lateral member 33 through the mounting sleeves 43 . Each of the two extending side arms 58 of the swing arm 56 generally extend from the middle member 57 towards the back end 22 of the power base attachment 20 . Each of the side arms 58 have telescoping portions 61 which extend outwardly from each lateral end of the middle member 57 in a direction parallel to the middle member 57 . The telescoping portions 61 have a smaller circumference than the middle member 57 and telescopically insert within the middle member 57 . Each telescoping portion 61 also has a series of holes 59 equally spaced along the length of the telescoping portion 61 . The side arms 58 may be pulled out of the middle member 57 or pushed into the middle member 57 depending on the width needed. Once the proper width is determined, a specific hole 59 on the telescoping portion 61 is aligned with a hole 60 on the middle member 57 . A bolt or locking pin is inserted into the hole 60 on the middle member 57 and into the hole 59 of the telescoping portion 61 which secures the side arms 58 to the middle member 57 and prevents further lateral movement. The side arms 58 , through the telescoping portions 61 , extend laterally from the middle member 57 then angle towards the rear end 22 of the power base attachment 20 . The angled portion extends upwards over the drive wheels 91 relative to the support frame 32 before becoming parallel and bend at approximately the centerpoint of their length to extend generally parallel to the longitudinal axis 23 of the power base attachment 20 .
Referring to FIGS. 5 , 6 , 9 and 10 , a sleeve 65 is positioned proximal to each rear terminal end of the side arms 58 of the swing arm 56 . Attached to each sleeve 65 is an axle plate 66 having a lateral slot 67 positioned below the sleeve 65 and an adjustment slot 68 positioned above the sleeve 65 . Each axle plate 66 is positioned on the exterior of the sleeve 65 on the side that faces the longitudinal axis 23 . A hand rail 69 , having a frame member 70 and hand rail member 71 , is attached to the axle plate 66 . Frame member 70 forms a “V” shape with a bore hole 72 positioned proximal to the apex. Frame member 70 is secured to the axle plate 66 through bolts or pins 73 which extend through the adjustment slot 68 of the axle plate 66 and holes 74 in the frame member 70 . Extending from one of the frame members 70 is a joystick module bracket 75 (as seen in FIG. 11 ). Hand rail 69 is designed to mimic the push rim 7 of the rear wheel 6 of an industry standard manually powered wheelchair 1 . Each sleeve 65 with the hand rail 69 and axle plate 66 may rotate towards the longitudinal axis 23 of the power base attachment 20 for convenient storage when not in use.
A power base axle receiver 76 , having an axle bore (not shown) there through, is mounted to each axle plate 66 within the lateral slot 67 . The axle bore (not shown) is aligned with the bore hole 72 of the frame member 70 . The power base axle receiver 76 may be adjusted for and aft in a direction parallel to the longitudinal axis 23 of the power base attachment 20 by moving the hand rail 69 through the adjustment slot 68 . This allows the axle receiver 76 to slide in the for/aft position within the lateral slot 67 . Preferably, each axle receiver 76 is adjusted to the same forward/aft position.
The axle bore of the power base axle receiver has a diameter that is equal, or similar, to the diameter of the axle bore of the axle receiver 9 of the manually powered wheelchair 1 . A pin 77 , having industry standard locking mechanisms, including deployment of recessed bearings or a latching pin, is positioned in the axle bore (not shown) of the power base axle receiver 76 . It is industry standard for the axle bore to fit a 0.5 inch pin. The axle plate 66 may be made in a variety of different shapes so long as an axle receiver 76 is mounted proximal the terminal end of the swing arm 56 .
Referring to FIG. 8 , a shock absorber 80 or dampener is positioned in alignment with the longitudinal axis 23 of the power base attachment 20 . The shock absorber 80 is attached at its lower end to the bottom panel 46 of the rigid portion 31 of the frame 30 through a lower shock mount 81 connected to a lower bracket 86 extending from the bottom panel 46 . The shock absorber 80 is attached at its upper end to an upper bracket 82 extending from the middle member 57 of the swing arm 56 through an upper shock mount 83 . The upper bracket 82 is positioned along the midpoint of the middle member 57 and extends away from the middle member 57 towards the back end 22 of the power base attachment 20 . The lower bracket 86 is connected to the bottom panel 46 with a bolt or pin 87 through one of a series of holes 84 in the bottom of panel 46 . The position of the lower bracket 86 on the bottom panel 46 may move toward the front or rear end of the bottom panel 46 by connecting the lower bracket 86 through a different hole 84 .
The height of the terminal ends of the side arms 58 of the swing arm 56 may be adjusted through movement of the shock absorber 80 . As the lower bracket 86 and lower shock mount 81 are moved toward the front of bottom panel 46 , the shock absorber 80 becomes more perpendicular in relation to the longitudinal axis 23 , effectively raising the upper end of shock absorber 80 . As a result, the upper shock mount 83 is raised causing the upper bracket 82 , and resulting swing arm 56 , to rotate upwards within the mounting sleeves 43 . As the swing arm 56 rotates up, the side arms 58 and the power base axle receivers 76 correspondingly rotate upwards effectively raising the position of the power base axle receivers 76 relative to the rigid portion 31 of the frame 30 . Consequently, lower bracket 86 may be adjusted along the longitudinal axis 23 to accommodate varying rear wheel sizes of the manually powered wheelchair such as 24, 25, and 26 inch diameters. Additionally, the attachment point of the upper shock mount 83 to the upper bracket 82 , may be similarly adjusted to various positions on the upper bracket 82 and effectively change the height of the power base axle receiver.
Referring to FIGS. 11 , 12 , and 13 , an electric motor 90 is attached to each wide longitudinal member 34 through attachment to the flange 41 and mirrored flange 42 . Each electric motor 90 is positioned between the drive wheel 91 and a longitudinal side panel 47 of the housing and powers one of the drive wheels 91 . In the preferred embodiment, two batteries 92 and a controller 93 are positioned within the housing 45 . A removable housing cover 51 is placed over the housing 45 and secured over the middle panel 49 and rear panel 50 (as seen in FIG. 2 ).
Still referring to FIGS. 12 and 13 , two castor wheels 94 are mounted to the terminal ends of each rear side member 38 of the support frame 32 . Each castor wheel 94 is able to rotate freely 360 degrees around a vertical axis. A joystick module 95 is attached to the joystick module bracket 75 . A wire or cable 96 extends from the joystick module 95 , along the swing arm 56 , into the housing 45 and to the controller 93 . The controller 93 is electrically connected to each battery 92 and to the respective electric motors 90 .
Referring to FIGS. 4 and 14 , an anti-tip/counterbalance mechanism 100 is attached to the rear lateral bracket 40 of the rear lateral member 39 . The anti-tip/counterbalance mechanism 100 is comprised of a latch 101 , rod 102 , spring 105 , sleeve 109 , base cap 110 and an adjustable pivot joint 111 . The latch 101 is positioned at to the upper end 103 of the rod 102 . The lower end 104 of the rod 102 is positioned within the sleeve 109 and arranged for engagement with a spring 105 . The lower end 104 of the rod 102 has a smaller circumference than the remainder of the rod 102 . The upper end 106 of the spring 105 coils around the lower end 104 of the rod 102 and engages a shoulder created by the smaller circumference of the lower end 104 . The lower end 107 of the spring 105 abuts the base cap 110 . The base cap 110 encapsulates the lower end of the sleeve 109 . A spring adjustment screw 108 is attached to the base cap 110 and may be used to increase or reduce the base line compression of the spring 105 to allow a user a stiffer anti-tip support or a looser anti-tip support. The rod 102 is telescopically arranged with the sleeve 109 in that as the rod 102 is compressed, the rod 102 slides within the sleeve 109 . The spring 105 allows for resilient compression and returns the rod 102 to a static position when no compressive force is applied. An adjustable pivot joint 111 attaches the sleeve 109 to the rear lateral bracket 40 . This pivot joint 111 allows the anti-tip/counterbalance mechanism 100 to rotate around a pivot point on the rear lateral bracket 40 . The sleeve 109 may be adjusted up or down in relation to the rear lateral member 39 by changing the pivot point that attaches the sleeve 109 to the rear lateral bracket 40 .
The latch 101 attaches to an upper frame member 11 located behind the backrest portion 4 of a standard manually powered wheelchair 1 . In the disclosed embodiment the latch 101 is a clamp but other standard latching mechanisms are anticipated so long as the clamping system allows the latch to rotate slightly in relation to the upper frame member during compression. For wheelchairs that do not have an upper frame member for the anti-tip/counter balance mechanism 100 to attach to, an upper cross beam is added (not shown). The upper cross beam connects to the latch as described above and the upper cross beam (not shown) attaches to upper vertical frame members of the standard wheelchair with a similar latching mechanism. In the disclosed embodiment, the pin 77 and axle receiver 76 may be integrally connected. In this embodiment, the pin is not removable from the axle receiver 76 .
To connect the power base attachment 20 to a standard manually powered wheelchair 1 , the pin 10 is removed from the axle receiver 9 of the industry standard manually powered wheelchair 1 and the two rear wheels are removed 6 . The power base attachment 20 is positioned under the seating portion 3 such that the front end 21 of the power base attachment 20 is positioned behind the wheelchair's front castor wheels 5 . The power base axle receivers 76 are adjusted for height as described supra through movement of the shock absorber 80 . The distance between the power base axle receivers 76 is adjusted as described supra through adjustment of the telescoping portions 61 of the side arms 58 . Once fully adjusted, the longitudinal axis of each power base axle receiver 76 is aligned with the longitudinal axis of the corresponding wheelchair axle receiver 9 . As seen in FIG. 15 , the pin 77 is positioned in the axle bore (not shown) of the power base axle receiver 76 and inserted into the axle bore of wheelchair axle receiver 9 of the manually powered wheelchair 1 . In other embodiments the pin 77 may slide within the axle bore of the power base axle receiver, may be removed com completely from the axle bore of the power base axle receiver, or completely remain stationary within the axle bore of the power base axle receiver. Once positioned in the axle bore of the wheelchair axle receiver 9 , the pin is secured through industry standard means including deployment of recessed bearings, latching pin, spring loaded pin, or other suitable means. The process is repeated for the remaining axle pin and axle receiver. In this manner, the front castor wheels 5 , two drive wheels 91 , and two rear castor wheels 94 are all in contact with level ground.
The anti-tip/counterbalance mechanism 100 is positioned so that the latch 101 attaches to the upper frame member 11 of the manually powered wheelchair 1 . The pivot joint 111 is adjusted up or down to ensure the latch 101 is of the appropriate height to latch to the upper frame member 11 . The latch 101 is clamped to the upper frame member 11 . When secured, the latch 9 is located proximal to the center point of the upper frame member 11 . The rear castor wheels also assist in stabilizing the wheelchair and provide added safety as an anti-tip/counterbalance mechanism. In some embodiments the two castor wheels may be replaced with a single castor wheel mounted along the longitudinal axis 23 of the power base attachment 20 . In this embodiment, it is anticipated the rear castor wheel would be located further back from where the anti-tip/counterbalance mechanism 100 attaches to the rear lateral member 39 .
Once the power base attachment 20 is secured, the distance from wheelchair axle receiver and the ground is identical to the height of the manually powered wheelchair with rear wheels. The hand rails 69 are in the approximately the same position as the push rims 7 of the preexisting rear wheels.
In operation, the user manipulates the joystick module 95 to control the direction and speed of the now electrically powered wheelchair. The joystick module 95 sends a signal to the controller 93 via a cable 96 . The controller 93 processes the information and determines the direction and speed of each motor 90 . The controller 93 sends this information to each respective electric motor 90 via a cable. The electric motor 90 , powered by the battery 92 , then operates the drive wheel 91 in a manner to correspond with the user's instructions from the joystick module 95 . The controller and joystick provide for industry standard operation of an electrically powered wheelchair which allow for variable drive speed and direction control. Each electric motor is powered by a rechargeable battery. Typically, each electric motor runs on 24 volts and is a conventional motor used in the electric powered wheelchair industry. In the preferred embodiment there is at least 24 volts of battery powered either through a single battery or a combination of batteries. The controller 93 is electrically connected to the batteries 92 and supplies power to both electric motors 90 and the joystick module 95 through cables. As in standard operation for electrically powered wheel chairs, when the joystick is placed in neutral from a directional position, the electric motor decelerates to allow for a smooth stop. Once stopped and when the joystick is in neutral the drive wheels are locked to prevent movement of the wheelchair when positioned on inclines or uneven terrains.
When the converted wheelchair is in motion, the swing arm 56 and shock absorber 80 assist to dampen the movement of the power base attachment 20 in relation to the manual wheelchair frame 2 . The user's center of gravity remains unchanged due to the power base attachment 20 having the same height and as the rear wheels of the standard wheelchair. The hand rail's 69 identical location to and conformity with the standard push rim, makes the user more comfortable as the hand rail is a familiar point of stability. A user may use the hand rail for transferring, positioning, lifting up for pressure management and for leaning forward.
The anti-tip/counterbalance mechanism 100 enables the wheelchair attached to the power base attachment 20 , to respond as if the manually operated wheels were still attached. The anti-tip/counter balance mechanism 100 allows the user to lean back to reduce pressure on lower extremities and to raise the front end castor wheels 5 several inches off the ground to overcome obstacles. The leaning back and raising of the front castor wheels 5 are accomplished by the user without changing the user's center of gravity. As the chair tilts back, the rod 102 compresses the spring 105 , allowing the user to raise the front castors 5 or to lean back. After compression of the spring 105 during the tilting process, the spring 105 decompresses to push the rod 102 , and resulting back rest and chair, towards the normal position. It is envisioned other anti-tip/counter balance mechanisms may be used to achieve the compression/decompression affect. A hydraulic cylinder, elastic, spring powered telescoping rod or other materials may be suitable to accomplish the compression and decompression mechanism. The anti-tip/counterbalance mechanism 100 assists user's ability to maintain balance as they overcome obstacles without having to adjust for the additional weight of the power drive attachment.
The present disclosure is described above in terms of a preferred illustrative embodiment of a power base attachment. Those skilled in the art will recognize that alternative constructions of such an apparatus can be used in carrying out the present invention. Other aspects, features, and advantages of the present invention may be obtained from a study of this disclosure and the drawings, along with the appended claims.
|
The disclosure describes an improved apparatus for converting a manually-powered wheelchair into an electrically powered wheelchair. The apparatus comprises a frame, at least one powered drive wheel, at least one motor powering said drive wheel, and at least one power base axle receiver capable of connecting with an existing axle receiver of a manually powered wheelchair. The apparatus further includes an anti-tip/counterbalance mechanism to prevent a user from losing control and falling backward when the power base attachment is connected. The apparatus uses the existing axle receiver of a manual wheelchair as a universal connection point and to maintain the center of gravity for a user.
| 0
|
BACKGROUND OF INVENTION
The present invention relates generally to a recording sheet, and more particularly to an inkjet recording sheet, the ink receptive coating thereon and the paper substrate supporting the ink receptive coating.
Paper for recording sheets used in inkjet printing must rapidly absorb the ink to reduce drying time with little or no backside show-through. Further, diffusion of ink laterally on the surface of the recording sheet must be prevented in order to achieve high resolution without blurring. Thus, for obtaining color images having good color density and resolution, with good absorbtivity and water fastness as well as optical brightness, a coated paper for inkjet printing should be able to achieve these results without any substantial dimensional change. For this purpose, the base paper for ink receptive coatings is generally made from bleached chemical pulp to which fillers, dyes, and if required, sizing agents and strength enhancers are added. An example of a typical paper basestock for use in the manufacture of an inkjet recording sheet is disclosed in U.S. Pat. No. 5,589,259.
It is also known that paper substrates for inkjet recording can be improved by applying an under coat or base coat to the paper surface before applying the ink receptive coating. Such base coats generally comprise a pigment and binder where the coated surface has a porous structure resulting in a large amount of pores or voids in the base coat layer. An example of a base coat for an inkjet recording sheet that is subsequently provided with an ink receptive layer is disclosed in U.S. Pat. No. 5,670,242.
Finally, the ink receptive coatings for inkjet paper must provide a surface that is receptive to the inks used for printing. In the past, this result has been achieved through the use of high pigment-to-binder ratios, usually in combination with pigments or coating materials that provide a porus and permeable coating layer. Because of the highly specific requirements for inkjet printing, coating materials used in other printing processes generally are unsatisfactory for inkjet printing.
There are two primary requirements for inkjet printing. The first is that the ink receptive coating, the substrate, and any intermediate base coat must be absorbent enough to immobilize the vehicle of the inks away from the surface so that the inks will not smear. The second requirement is that the ink receptive coating must provide a means for keeping the dyes in the ink on the surface with no spreading, tailing or blurring of the ink drops.
These requirements are achieved in the present invention with a combination of base coat and top coat where the components are matched to achieve a cooperative relationship not found in the prior art.
In conventional inkjet recording sheets, a generally porous fine powder capable of absorbing an ink is coated on a paper surface with a binder. However, when ink is brought into contact with such a coating, the coating is unable to instantaneously absorb the entire amount, and thus it takes a finite time for the inks to be absorbed. This allows the ink drop to spread in a fairly wide range among the particles of the fine powder. The color density tends to be low towards the forward edge of the spread, and the ink tends to spread unnecessarily widely, whereby the entire color density tends to be correspondingly low. This tends to make the sharpness of the printed image low and color blending or blotting is likely to result. However it has now been found possible to overcome these drawbacks by suppressing the unnecessary spread of the ink drop, and to provide a means for the ink drop including its vehicle to be absorbed into the paper substrate as a whole.
For this purpose, according to the present invention, porous particles are provided in both the ink receptive layer and in the base coat layer in a manner such that they work in a cooperative fashion to provide a superior image with good drying capacity.
SUMMARY OF INVENTION
It is the general object of this invention to provide an inkjet recording paper that has superior performance during inkjet printing.
It is another object of the invention to provide a novel combination of basestock, base coat and ink receptive coat to achieve a glossy inkjet paper product having a TAPPI 75° gloss greater than 80%, and an ink drying time of under two minutes, with acceptable intercolor bleed and enhanced density of printed colors.
It is a further object of the present invention to provide a paper basestock for an inkjet recording sheet which has excellent dimensional stability when used with aqueous based inks.
Another object is to provide an improved base coat which has exceptional absorbtion capacity for absorbing the vehicle of inkjet inks.
A further object of the present invention is to provide an improved ink receptive coat which has superior performance for reproducing images.
A typical basestock for the inkjet recording paper of the present invention may have the following preferred characteristics:
______________________________________Basis weight 106 g/m.sup.2Caliper 5.3 milTAPPI Brightness 90%TAPPI Opacity 93%Sheffield Smoothness 150 secondsHercules Size 400 seconds______________________________________
The base coat for the inkjet recording paper of the present invention consists essentially of pigment and binder, including, in a preferred embodiment, a mixture of precipitated calcium carbonate (PCC), calcined clay, and if desired, titanium dioxide, dispersed in a coating binder comprising, as an example, a mixture of polyvinyl acetate and soy protein.
The ink receptive coat for the inkjet recording paper also consists essentially of pigment and binder including, in a preferred embodiment, a pigment component, for example fumed or pyrogenic silica, dispersed in an emulsion prepared from styrene polymerized in the presence of polyvinylpyrrolidone. The use of this emulsion is believed to present a significant departure from the known prior art.
DETAILED DESCRIPTION
The inkjet recording paper of the present invention achieves enhanced properties as a result of a careful combination of basestock, base coat and in particular, the ink receptive coat. The basestock is preferably an alkaline paper having a basis weight in the range of 100-150 g/m 2 with a caliper of at least about 5.0 mil. The basestock is prepared from a bleached wood pulp furnish to which is added a sizing agent such as alkylketene dimer, and fillers such as precipitated calcium carbonate and kaolin clay. An example of a suitable precipitated calcium carbonate is ALBAGLOS supplied by Specialty Minerals. An example of a suitable kaolin clay is ANSILEX supplied by Englehard Chemical Company. The basestock thus formed is preferably size pressed with a mixture of starch and styrene maleic anhydride in a conventional manner. Finished basestock properties (typical values) are, caliper greater than 5.0 mils, and preferably about 5-7 mils; TAPPI opacity of about 90-95%; TAPPI brightness of about 80-95%; Sheffield smoothness of about 100-200 (units are approximately equivalent to cubic centimeters of air per minute times 10); and a Hercules size of about 300-900 seconds. This basestock is particularly advantageous for the novel inkjet sheet of the present invention because it provides exceptional dimensional stability during use.
The preferred base coat for the inkjet recording sheet of the present invention is prepared, in a preferred embodiment, from a formulation comprising a mixture of precipitated calcium carbonate (PCC) and calcined clay (which may also include titanium dioxide and ground calcium carbonate), dispersed in a binder comprising polyvinyl acetate and soy protein. The PCC pigment is incorporated into the coating formulation at a dry weight of from 70-80%. Calcined clay is incorporated into the coating formulation at a dry weight of from about 20-30%, and where desired, up to 10% titanium dioxide may be included to achieve enhanced opacity. Typical binders for the preferred embodiment include polyvinyl acetate (about 10-15%), an example of which is PVA 1103 supplied by National Starch Company, and protein (about 2-5%), an example of which is PROCOTE 200 supplied by Protein Technologies. In addition to these basic ingredients, there may be added sufficient ammonium hydroxide to dissolve the protein and a thickener such as ALCOGUM L28 (supplied by Alco Chemical Company) to reach the target viscosity. A viscosity in the range of from about 2000-3000 centipoise Brookfield (20 rpm, No. 4 spindle) is preferred at a solids content of about 60-65%. The base coat is applied to the basestock at a coat weight in the range 8-10 lbs/ream (ream size 3300 ft 2 ), each side with any suitable coating device known to those skilled in the art (blade coater preferred). The finished base coated sheet has typical properties of basis weight 120-140 g/m 2 ; caliper about 5-7 mils; TAPPI Brightness 80-95%; TAPPI Opacity 90-95%; and Sheffield smoothness of about 100-200 units. The base coated sheet prepared as described above is particularly advantageous for the novel inkjet recording paper of the present invention because of its enhanced absorbtivity.
The ink receptive coat for the inkjet recording paper of the present invention is applied directly over the base coat. It is designed to work synergistically with the base coat to provide superior printed images. The ink receptive coat is prepared from a formulation comprising fumed or pyrogenic silica having a surface area of about 140-200 m 2 /g as measured by the BET method, with an alumina content of from about 0.3-1.3%. A typical fumed silica useful for the present invention is sold under the tradename Degussa MOX 170 supplied by Degussa Company AG. It is desirable that the silica pigment component have a narrow particle size distribution range and large specific surface area to achieve maximum ink absorbtivity. The preferred binder component for the present invention is a mixture of polystyrene and polyvinylpyrrolidone. An example of such a product is POLECTRON 430 supplied by International Specialty Products. POLECTRON 430 is prepared by an emulsion polymerization process at a weight ratio of styrene to polyvinylpyrrolidone of about 70/30. Other suitable binders include polyvinylpyrrolidone, starch, copolymers of vinylpyrrolidone and vinyl acetate, and combinations of these materials. The pigment component of the coating formulation is preferably about 15% by weight, but may range from about 5 to 35%. The remainder comprises binder, on the order of about 85% by weight, but may range from about 65 to 95%. It is believed that the styrene component of the binder acts as a pigment in the coating to reduce bleed while improving the drying time of applied inks. For improved water and smear resistance of the ink jet recording sheet, the coating formulation may also include a cationic agent in the weight percent range of 0.5-10%. An example of such a material is a dispersable polydadmac sold under the tradename poly DADMAC 7544 by Nalco Chemical Company. In addition, where desireable, a fluorescent whitening agent may be added, for example FWA T110 sold by Clariant Company. The ink receptive coat is made up to a solids of about 35-43% and is applied over the base coat by any suitable coating apparatus known to those skilled in the art in an amount of about 3-6 lbs/ream (ream size 3300 ft 2 ) one or both sides.
The invention will be described in further detail with reference to the following Examples. It should be understood, however, that the invention is by no means restricted to these specific Examples.
EXAMPLE I
an inkjet coating drawdown study, the effect of increasing the weight ratio of fumed silica to styrene-vinylpyrrolidone copolymer on image quality, ink drying time and gloss were determined. Previous inkjet prototypes, constructed of an absorbent base coat and a glossy, ink receptive top coat, featured good image quality and high gloss, but they exhibited lengthy ink drying times and persistent tackiness. The purpose of this study was to evaluate a pigment-binder combination of fumed silica and water insoluble styrene-vinylpyrrolidone emulsion copolymer as an ink-receptive top coat. Whereas vinylpyrrolidone homopolymer forms a tacky, water soluble film when applied as a coating, it was hoped that the styrene-vinylpyrrolidone copolymer would provide reasonable ink absorption with a reduced tackiness. The fumed silica, although not as porous as many precipitated synthetic silicas, features a very small agglomerate size (15 nm), and is therefore not as detrimental to gloss as the precipitated and gel silicas.
The experimental top coats were drawn down over a size pressed 80 pound rawstock that was previously base coated with a base coat formulation designed to have high absorbtivity and to be compatible in performance with the top coat formulations. The coating formulations are shown in Table I.
TABLE I______________________________________ Base Coat(60% Solids - 8 lb/side/ream)Precipitated Calcium Carbonate (parts) 65(ALBAGLOS S)Calcined Clay " 25(ANSILEX)Titanium Dioxide " 10Polyvinyl Acetate " 12(NS 1103)Protein " 2(PROCOTE 200)NH.sub.4 OH (as required)Thickener(ALCOGUM L28) (to 2000 cps)Top Coat(dry weight % 3-4 lb/ream) 1 2 3 4 5______________________________________Fumed Silica 15 20 25 30 35(MOX 170)Styrene-Vinylpyrrolidone 85 80 75 70 65(POLECTRON 430)Solids (%) 32 32 30 29 29Viscosity (cps) 700 850 750 630 950______________________________________
After 24-hour storage, the coated samples were supercalendered (4 nips at 600 pli, 110 degrees F.). Test images were printed with an HP Deskjet 693 C inkjet printer. The results demonstrated that increasing the weight fraction of fumed silica in the coating caused both black and color ink density to decrease and both sheet and printed gloss to decrease. However, increasing the weight fraction of fumed silica from 15% to 35% reduced the drying time from 55 to 25 seconds. No effects on edge sharpness, intercolor bleed, or mottle were observed, and likewise, the weight fraction of fumed silica in the coating had no effect on sheet brightness.
EXAMPLE II
Another coating study was conducted to determine the influence of (1) base stock ash and sizing, (2) sizepress ingredients, (3) base coat application, and (4) coating formulation on inkjet print gloss, gamut, bleed and drying properties. It was found that the quality of the print was significantly affected by the base coat application and the top coat formulation. A coating formulation comprising fumed silica and styrene-vinylpyrrolidone (15/85) applied to a base coated sheet was far superior to the same coating applied to a sheet that was not base coated. This demonstrated the need for a double coated rather than a single coated product. Additionally, when a cationic quaternary amine (DADMAC), was added to the coating formulation, a 15-20% improvement was seen in color gamut and ink density along with an improvement in ink bleed. Meanwhile, the introduction of hydrophilic materials (silica/polyvinyl alcohol) to the sizepress to increase water absorbency, resulted in improved ink drying time, but produced a significant decrease in color gamut and optical density. Likewise small differences in internal size and ash levels did not affect inkjet print quality. Table II shows the sizepress, base coat and top coat formulations.
TABLE II______________________________________Size Press FormulationComponent SP-1 SP-2 SP-3______________________________________Styrene Maleic Anhydride 3 -- --Starch (PG 290) 97 -- --Fumed Silica (Mox 170) -- 80 --PVOH (Airvol 107) -- 20 --Styrene Butadiene (Dow 620) -- -- 100Ammonia -- -- PH 8.5Solids (%) 10 15 10______________________________________Base CoatComponent Parts______________________________________Precipitated Calcium Carbonate 75(ALBAGLOS S)Calcined Clay 25(Ansilex)Protein 2(PROCOTE 200)PVAC (NS 1103) 12ALCOGUM (L-28) To 1485 cpsSolids (%) 59.9______________________________________Top CoatComponent TC-1 TC-2______________________________________Fumed Silica 15 15(MOX 170)Styrene-polyvinylpyrrolidone 85 85(POLECTRON 430)Diallyldimethyl Ammonium Chloride -- 5DADMAC (Nalco 7544)T-110 Optical Brightener 1.3 1.3Solids (%) 42.2 38.1Viscosity (cps) Brookfield 5590 3600 Hercules 113/89 106/85______________________________________
The coated sheets were supercalendered and printed on an HP Deskjet 890C printer. Of the conditions that were base coated, base coat weight was 8-9 lb/ream. From the print results, it was found that both paper and print gloss could only be achieved by double coating. When a base coat was not present, both paper and print gloss suffered. The addition of DADMAC increased color gamut and reduced the bleeding tendency of the inks although ink drying time was somewhat longer.
It will be appreciated by those skilled in the art that various changes and modifications can be made in the illustrated embodiments without departing from the spirit of the present invention. All such modifications and changes are intended to be covered by the appended claims.
|
The inkjet recording sheet of the present invention comprises a cellulosic sheet support, e.g., paper, having on at least one surface thereof an inkjet coating comprising, in combination, a porous base coat having a high absorption capacity for absorbing the vehicle of an inkjet ink, and an ink receiving coat having a superior capacity for keeping the dyes in the ink on the surface with minimal spreading, tailing or blurring, to provide a sharp image.
| 8
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a transgenic cell line which has been engineered to constitutively express the α V β 6 integrin receptor, a principal bovine receptor for Foot and Mouth Disease Virus (FMDV). In particular, the invention relates to the transgenic fetal porcine kidney cell line, LFBK α v β 6 , which is useful for the rapid and sensitive detection and identification of FMDV in diagnostic settings and also to identify serotypes and subtypes thereby facilitating vaccine selection procedures. LFBK α v β 6 is highly sensitive and permissive to infection by animal-derived FMDV from all seven serotypes in cell culture. The invention further relates to the transgenic LFBK α v β 6 cells for detection of FMDV from field samples.
2. Description of the Relevant Art
Foot and mouth disease virus (FMDV) is a severe economic concern for meat producing nations since the trade of animal products is prohibited from countries where the virus is confirmed. The rapid spread of the virus among susceptible animals results in severe morbidity and in some cases death, especially in young animals (Grubman and Baxt. 2004. Clin. Microbiol. Rev. 17: 465-493). Foot and mouth disease (FMD) is an extremely contagious viral disease of cloven-hoofed ungulates which include domestic animals (cattle, pigs, sheep, goats, and others) and a variety of wild animals. Infection or vaccination with one of the seven different serotypes does not confer cross-protection to other serotypes or even some subtypes of the same serotype. Vaccines for FMDV are widely used to prevent clinical disease, but since vaccines are serotype and subtype-specific, the virus(es) causing outbreaks must be isolated and serologically characterized for vaccine matching prior to selecting the appropriate vaccine antigen (reviewed in Rodriguez and Gay. 2011. Expert Rev. Vaccines 10:377-387).
Although molecular techniques such as PCR (polymerase chain reaction) coupled with genomic sequencing can be used in samples containing enough virus to rapidly identify the virus serotype and its relationship to other FMDV strains, appropriate vaccine prediction requires virus growth in cell culture to carry out neutralization tests using reference sera. Inefficient recovery of virus from animal samples can delay diagnosis and vaccine selection and thereby hamper rapid implementation of control measures; therefore, virus isolation protocols are designed for maximum sensitivity. Some primary cells, such as bovine thyroid (BTY) cells, are highly susceptible to a wide range of FMDV serotypes (Snowdon, W. A. 1966. Nature 210:1079-1080); however, they are difficult and costly to prepare and lose FMDV susceptibility after multiple passages (House and Yedloutschnig. 1982. Can. J. Comp. Med. 46:186-189). Primary lamb kidney (LK) cells are also very sensitive to FMDV. Unlike BTY cells, LK cells maintain their sensitivity to FMDV infection after cryopreservation; however, their sensitivity decreases after passage (House and House. 1989. Vet. Microbiol. 20:99-109). Immortalized cell lines (e.g. baby hamster kidney (BHK) fibroblasts and porcine kidney epithelial cells), while much easier to maintain, are in many cases less susceptible to specific animal-derived FMDV serotypes (Swaney, L. M. 1976. Amer. J. Vet. Res. 37:1319-1322; Ferris et al. 2006. Vet. Microbiol. 117:130-140; Ferris et al. 2002. Vet. Microbiol. 84:307-316; De Castro, M. P. 1964 . Arch. Inst. Biol. San Paulo 31: 63-78).
Integrins of the α V subgroup have been demonstrated to be FMDV receptors by several laboratories including ours (Ruiz-Saenz et al. 2009. Intervirol. 52:201-212). Of the many α V integrins that have been shown to mediate FMDV attachment, the integrin α V β 6 has been shown to be one of the most efficient receptors for all FMDV serotypes (Jackson et al. 2000. J. Virol. 74:4949-4956; Ferris et al. 2005. J. Virological Methods 127:69-79) and high levels of α V β 6 expression are observed on epithelial cells at the sites of infection in cattle and swine (Monaghan et al. 2005. J. Gen. Virol. 86:2769-2780; O'Donnell et al. 2009. J. Comp. Path. 141:98-112). BTY cells, considered the most sensitive primary cells for FMDV isolation, have high levels of α V β 6 integrin surface expression (King et al. 2011. Vet. Immunol. Immunopath. 140:259-265). Moreover, transient expression of bovine α V and β 6 integrin subunits in baby hamster kidney cells (BHK3-α V β 6 ) (Duque et al. 2004. J. Virol. 78:9773-9781) greatly increased the susceptibility of this cell line to a cow-passaged A24 Cruziero strain that contains an SGD motif in the VP1 (FMD Virus Protein 1) capsid protein (Rieder et al. 2005. J. Virol. 79:12989-12998). Although the BHK3-α V β 6 cells were initially more permissive to the A24-SGD virus than BHK-21 cells were, the BHK3-α V β 6 cells lost integrin expression and sensitivity to the A24-SGD virus after multiple passages (E. Rieder, personal communication).
Swaney derived an immortalized line of fetal porcine kidney (LFBK) cells that had high susceptibility to most FMDV serotypes and the susceptibility was maintained over many passages (Swaney, L. M. 1988. Vet. Microbiol. 18:1-14). Compared to BTY cells, LFBK cells had similar susceptibility to most FMDV serotypes and had equal or better susceptibility than the MVPK (Mengeling-Vaughn Porcine Kidney) cell line, the porcine kidney cell line, IB-RS-2, and fetal bovine kidney cells in the same experiments.
There is a need for a cell line that is easily maintained and is highly susceptible to all serotypes and subtypes of FMDV. The present invention, described below, combines the long-lived FMDV susceptibility of the LFBK cell line with a principal bovine receptor for FMDV, the α V β 6 integrin receptor, to provide a stable cell line which is highly susceptible to FMDV.
SUMMARY OF THE INVENTION
We have developed and characterized a stable transgenic cell line that is highly susceptible to animal-derived FMDV from all seven serotypes and discovered that this cell line greatly facilitates FMDV isolation and growth from field samples ensuring more accurate and more rapid diagnosis of the FMDV serotype involved in an outbreak, when compared to other cells used for diagnosis.
In accordance with this discovery, it is an object of the invention to provide the transgenic fetal porcine kidney cell line, LFBK α v β 6 , engineered to express the α V β 6 integrin receptor, a principal bovine receptor for FMDV.
It is a further object of the invention to provide LFBK α v β 6 cells for the rapid isolation and growth of FMDV serotypes and subtypes from field samples thereby facilitating vaccine selection procedures. LFBK α v β 6 is sensitive and permissive to infection by animal-derived FMDV from all seven serotypes in cell culture.
It is another object of the invention to provide LFBK α v β 6 cells for the rapid and sensitive detection and identification of all seven serotypes of FMDV and multiple subtypes from field samples thereby facilitating vaccine selection procedures.
Other objects and advantages of this invention will become readily apparent from the ensuing description.
BRIEF DESCRIPTION OF THE DRAWINGS
The patent or application file contains at least one drawing executed in color. Copies of this patent or patent application publication with color drawing(s) will be provided by the U.S. Patent and Trademark Office upon request and payment of the necessary fee.
FIGS. 1A-1F depict LFBK-α v β 6 cell characterization. FIGS. 1A-1C show that LFBK-α V β 6 cells maintain long-term expression of β 6 . Mouse anti-human β 6 (Chemicon, CSb6) was used to detect the bovine integrin subunit β 6 . FIG. 1D shows that LFBK-α V β 6 cells maintain long-term susceptibility to A24-SGD. The indicated cells were infected with serial dilutions of either A24-BHK or A24-SGD for plaque determination as described in Example 1. FIG. 1E depicts the relationship between susceptibility and time after seeding. Cells were seeded at the indicated time prior to infection then infected with serial dilutions of the indicated virus for titer determination as described in Example 1. FIG. 1F is a comparison of FMDV A24-BHK and A24-SGD growth in LFBK and LFBK-α V β 6 cells. LFBK and LFBK-α V β 6 cells were seeded in 24-well plates and infected 72 hours later with either A24-BHK or A24-SGD at MOI=0.01. After 1 hour, the monolayers were acid washed and fresh media was added. At the indicated time after infection, the plates were frozen at −70° C., thawed and titrated on LFBK-α V β 6 cells.
FIG. 2 illustrates the susceptibility of 6 cell types to animal-derived FMDV. Cells were infected with the indicated viruses and virus titers were determined for each cell type as described in Example 2. Each solid line is the axis for data generated from the indicated virus strain. Colored points on the solid lines indicate the mean titer of that virus strain in a single cell type (Refer to Table 2 for sample range). Dashed lines specify the log 10 scale of the virus titer in PFU/ml; points located on the outside of the plot correspond to higher virus titers (10 8 ) than those located toward the center (10 2 ).
FIGS. 3A and 3B depict detection of FMDV in diagnostic samples. Wells of 48-well plates seeded with the indicated cells were infected with 38 FMDV-suspect tissue homogenates from Afghanistan, Bolivia and Pakistan (see Table 3 for isolate information). Beginning at 4 hours post infection, each well was scored for the presence of cytopathic effects (CPE). In FIG. 3A , each point on the scatter plot represents the time after infection that a cytopathic effect was first detected in a given well for one diagnostic isolate. “NC” denotes the diagnostic samples that did not induce visible cytopathic effects by 48 hours in the indicated cells. In FIG. 3B , each point on the graph represents the average CPE score for all 38 diagnostic isolates at each time point. 1+, up to 25% of the cell monolayer exhibited visual CPE; 2+, approximately 50% of the cell monolayer exhibited CPE; 3+, approximately 75% of the cell monolayer exhibited CPE; 4+, 100% of the cell monolayer exhibited CPE.
DETAILED DESCRIPTION OF THE INVENTION
Here we report the engineering and comprehensive characterization of the LFBK-α V β 6 cell line, a fetal porcine kidney cell line stably transduced with the bovine α V and β 6 integrin subunits. The expression of the β 6 integrin subunit and the resulting enhanced infectivity of FMDV containing a SGD domain in VP1 were both maintained for at least 100 cell passages. We found that the LFBK-α V β 6 cells were more susceptible to all FMDV serotypes derived from experimentally-infected animals as compared to the LFBK cells from which they were derived and other cells commonly used for FMDV isolation. In a diagnostic sensitivity assay, LFBK-α V β 6 cells were more sensitive than primary lamb kidney cells, the porcine kidney cell line IB-RS-2, and the BHK cell line. LFBK-α V β 6 cells were also able to detect other vesicular disease viruses. Our results support the use of LFBK-α V β 6 cells for FMDV diagnostic purposes.
Our data indicate that the LFBK-α V β 6 cells are excellent for detecting FMDV serotype O isolates. A previous study at PIADC (Plum Island Animal Disease Center) showed that LFBK cell sensitivity to O1 Manisa isolated from cattle was close to the ID 50 observed in primary bovine tongue cells (Pacheco et al. 2010 . Vet. J. 183:46-53); however, we have observed that the transgenic LFBK-α V β 6 cells detect O1 Manisa over one log 10 more efficiently than LFBK cells. Further, Burman and coworkers showed that the integrin-binding domain on the VP1 capsid protein from O1 FMDV binds α V β 6 with the highest affinity among the α V β 3 , α V β 6 and α V β 8 integrins (Burman et al. 2006 . J. Virol. 80:9798-9810). In addition, in our experiments ( FIG. 2 ), O1 Manisa viruses are detected at a level almost two logs better in LFBK-α V β 6 cells than in IB-RS-2 cells that do not express the high levels of α V β 6 (King et al., supra).
BHK-21 cells are widely used for FMDV virus isolation, due to their rapid growth properties and sufficient susceptibility to most serotypes of FMDV. BHK cells generally performed very well in our sensitivity experiments ( FIG. 2 ), detecting cattle-derived A24 with the same sensitivity as primary LK cells; O1 Manisa (from both swine and cattle) was the only serotype where BHK had the least efficient FMDV detection of the cell lines tested. In our diagnostic experiments ( FIG. 3A ), the use of low-passage BHK cells was able to eventually detect FMDV from 18 out of 40 diagnostic tissue samples and in five cases, the detection of a few single infected BHK cells by immunohistochemistry. Taken together, our results with BHK cells clearly indicate that they are not as susceptible to animal-derived isolates as LFBK-α V β 6 cells.
FMDV strain O/TAW/97 does not grow well in primary bovine thyroid cells (BTY) or in cattle; yet, O/TAW/97 grows in the IB-RS-2 porcine kidney cell line and is extremely virulent in swine (Dunn and Donaldson. 1997 . Vet. Rec. 141:174-175). As such, O/TAW/97 has been referred to as a “porcinophillic” virus (Dunn and Donaldson, supra; Knowles et al. 2001 . J. Virol. 75:1551-1556; Pacheco and Mason. 2010 . J. Vet. Sci. 11:133-142). In our experiments this virus also grew poorly in primary lamb kidney cells, forming extremely small plaques. However, O/TAW/97 grew better in the porcine-derived LFBK cells than in the cell lines of swine origin, namely, MVPK and IB-RS-2. The expression of α V β 6 in the LFBK-α V β 6 cells enhanced infectivity of the O/TAW/97 virus over the infectivity levels observed in LFBK cells to a level about the same as seen with the O1 Manisa and O/UKG/2001 viruses.
LFBK-α V β 6 cells have been in use at PIADC for all aspects of FMDV virology with tremendous success. They support the replication of animal-derived virus strains that do not grow well in other cell types (e.g. O1 Manisa, O/TAW/97) and maintain high sensitivity to FMDV for at least 100 subculture passages. They do not require the extraction of animal organs to make primary cells, they grow as efficiently as standard LFBK cells, and they have no special media requirements. We have characterized the FMDV susceptibility of this transduced cell line by infection with animal-derived FMDV from all 7 serotypes as well as recent diagnostic field samples and compared its susceptibility to that of other cell types used for diagnostic FMDV virus isolation. Our results indicate that LFBK-αvβ6 cells are highly permissive for all FMDV serotypes and have excellent performance in a diagnostic setting. Based on the data presented here, LFBK-α V β 6 cells are a valuable tool for the rapid detection and/or isolation of FMDV serotypes in clinical laboratories and are exceptionally suited for all routine FMDV diagnostic and research-based cell applications.
The terms “sample” and “specimen” in the present specification and claims are used in their broadest sense to include any composition that is obtained and/or derived from biological or environmental source, as well as sampling devices (e.g., swabs) which are brought into contact with biological or environmental samples. “Biological samples” include those obtained from an animal, including cloven-hoofed ungulates which include domestic animals (cattle, pigs, sheep, goats, and others) and a variety of wild animals, body fluids such as urine, blood, fecal matter, cerebrospinal fluid (CSF), semen, sputum, and saliva, as well as solid tissue. Also included are samples obtained from food products and food ingredients such as dairy items, meat, meat by-products, and waste. “Environmental samples” include environmental material such as surface matter, soil, water, and industrial materials, as well as material obtained from food and dairy processing instruments, apparatus, equipment, disposable, and non-disposable items. These examples are not to be construed as limiting the sample types applicable to the present invention.
As used herein, the term “cell type,” refers to any cell, regardless of its source or characteristics.
As used herein, the term “microorganism” refers to any organism of microscopic or ultramicroscopic size including, but not limited to, viruses, bacteria, and protozoa.
As used herein, the term “culture” refers to a composition, whether liquid, gel, or solid, which contains one or more microorganisms and/or one or more cells. A culture of organisms and/or cells can be pure or mixed. For example, a “pure culture” of an organism as used herein refers to a culture in which the organisms present are of only one strain of a single species of a particular genus. This is in contrast to a “mixed culture” of organisms which refers to a culture in which more than one strain of a single genus and/or species of microorganism is present.
As used herein, the terms “culture media,” and “cell culture media,” refer to media that are suitable to support maintenance and/or growth of cells in vitro (i.e., cell cultures).
A “primary cell” is a cell which is directly obtained from a tissue or organ of an animal whether or not the cell is in culture.
A “cultured cell” is a cell which has been maintained and/or propagated in vitro. Cultured cells include primary cultured cells and cell lines.
“Primary cultured cells” are primary cells which are in in vitro culture and which preferably, though not necessarily, are capable of undergoing ten or fewer passages in in vitro culture before senescence and/or cessation of proliferation.
The terms “cell line” and “immortalized cell” refer to a cell which is capable of a greater number of cell divisions in vitro before cessation of proliferation and/or senescence as compared to a primary cell from the same source. A cell line includes, but does not require, that the cells be capable of an infinite number of cell divisions in culture. The number of cell divisions may be determined by the number of times a cell population may be passaged (i.e., subcultured) in in vitro culture. Passaging of cells is accomplished by methods known in the art. Briefly, a confluent or subconfluent population of cells which is adhered to a solid substrate (e.g., plastic Petri dish) is released from the substrate (e.g., by enzymatic digestion), and a proportion (e.g., 10%) of the released cells is seeded onto a fresh substrate. The cells are allowed to adhere to the substrate, and to proliferate in the presence of appropriate culture medium. The ability of adhered cells to proliferate may be determined visually by observing increased coverage of the solid substrate over a period of time by the adhered cells. Alternatively, proliferation of adhered cells may be determined by maintaining the initially adhered cells on the solid support over a period of time, removing and counting the adhered cells and observing an increase in the number of maintained adhered cells as compared to the number of initially adhered cells.
Cell lines may be generated spontaneously or by transformation. A “spontaneous cell line” is a cell line which arises during routine culture of cells. A “transformed cell line” refers to a cell line which is generated by the introduction of a “transgene” comprising nucleic acid (usually DNA) into a primary cell or into a finite cell line by way of human intervention
Cell lines include, but are not limited to, finite cell lines and continuous cell lines. As used herein, the term “finite cell line” refers to a cell line which is capable of a limited number of cell divisions prior to senescence.
The term “continuous cell line” refer to a cell line which is capable of more than about 50 (and more preferably, an infinite number of) cell divisions.
The term “transgene” is understood to describe genetic material which has been or is about to be artificially inserted into the genome of a non-human animal, and particularly into a cell of a living non-human mammal. It is to be understood that as used herein the term “transgenic” includes any cell, cell line, or tissue, the genotype of which has been altered by the presence of a heterologous nucleic acid. A transgene may be an “endogenous DNA sequence” or a “heterologous DNA sequence” (i.e., “foreign DNA”). The term “endogenous DNA sequence” refers to a nucleotide sequence which is naturally found in the cell into which it is introduced so long as it does not contain some modification (e.g., a point mutation, the presence of a selectable marker gene, etc.) relative to the naturally-occurring sequence. The term “heterologous DNA sequence” refers to a nucleotide sequence which is ligated to, or is manipulated to become ligated to, a nucleic acid sequence to which it is not ligated in nature, or to which it is ligated at a different location in nature. Heterologous DNA is not endogenous to the cell into which it is introduced, but has been obtained from another cell. Heterologous DNA also includes an endogenous DNA sequence which contains some modification. Generally, although not necessarily, heterologous DNA encodes RNA and proteins that are not normally produced by the cell into which it is expressed.
The term “transduction” is used to refer to the introduction of genetic material into a cell by using a viral vector. As used herein a transduced cell results from a transduction process and contains genetic material it did not contain before the transduction process, whether stably integrated or not.
The term “transformation” refers to a permanent or transient genetic change induced in a cell following the incorporation of new DNA (i.e. DNA exogenous to the cell). Where the cell is a mammalian cell, a permanent genetic change is generally achieved by introduction of the DNA into the genome of the cell Host organisms containing the transformed nucleic acid fragments are referred to as “transgenic” organisms. Thus, isolated polynucleotides can be incorporated into recombinant constructs, typically DNA constructs, capable of introduction into and replication in a host cell. Such a construct can be a vector that includes a replication system and sequences that are capable of transcription and translation of a polypeptide-encoding sequence in a given host cell.
As used herein, the terms “nucleic acid molecule”, “nucleic acid sequence”, “polynucleotide”, “polynucleotide sequence”, “nucleic acid fragment”, “isolated nucleic acid fragment” are used interchangeably herein. These terms encompass nucleotide sequences and the like. A polynucleotide may be a polymer of RNA or DNA that is single- or double-stranded and that optionally contains synthetic, non-natural or altered nucleotide bases. A polynucleotide in the form of a polymer of DNA may be comprised of one or more segments of cDNA, genomic DNA, synthetic DNA, or mixtures thereof.
The term “isolated” polynucleotide refers to a polynucleotide that is substantially free from other nucleic acid sequences, such as other chromosomal and extrachromosomal DNA and RNA, that normally accompany or interact with it as found in its naturally occurring environment. However, isolated polynucleotides may contain polynucleotide sequences which may have originally existed as extrachromosomal DNA but exist as a nucleotide insertion within the isolated polynucleotide. Isolated polynucleotides may be purified from a host cell in which they naturally occur. Conventional nucleic acid purification methods known to skilled artisans may be used to obtain isolated polynucleotides. The term also embraces recombinant polynucleotides and chemically synthesized polynucleotides.
As used herein, “recombinant” refers to a nucleic acid molecule which has been obtained by manipulation of genetic material using restriction enzymes, ligases, and similar genetic engineering techniques as described by, for example, Sambrook et al. 1989. Molecular Cloning: A Laboratory Manual, Second Edition, Cold Spring Harbor Laboratory Press, Cold Spring Harbor, N.Y. or DNA Cloning: A Practical Approach, Vol. I and II (Ed. D. N. Glover), IRL Press, Oxford, 1985. “Recombinant,” as used herein, does not refer to naturally occurring genetic recombinations.
As used herein, the term “chimeric” refers to two or more DNA molecules which are derived from different sources, strains, or species, which do not recombine under natural conditions, or to two or more DNA molecules from the same species, which are linked in a manner that does not occur in the native genome. A “construct” refers to a recombinant nucleic acid, generally recombinant DNA, that has been generated for the purpose of the expression of a specific nucleotide sequence(s), or is to be used in the construction of other recombinant nucleotide sequences. A “chimeric gene construct” refers to a nucleic acid sequence encoding a protein, operably linked to a promoter and/or other regulatory sequences.
As used herein, the term “express” or “expression” is defined to mean transcription alone. “Altered levels” or “altered expression” refers to the production of gene product(s) in transgenic organisms in amounts or proportions that differ from that of normal or non-transformed organisms.
As used herein, the terms “encoding”, “coding”, or “encoded” when used in the context of a specified nucleic acid mean that the nucleic acid comprises the requisite information to guide translation of the nucleotide sequence into a specified protein. The information by which a protein is encoded is specified by the use of codons. A nucleic acid encoding a protein may comprise non-translated sequences (e.g., introns) within translated regions of the nucleic acid or may lack such intervening non-translated sequences (e.g., as in cDNA).
The term “operably linked” refers to the association of two or more nucleic acid fragments on a single nucleic acid fragment so that the function of one is affected by the other. For example, a promoter is operably linked with a coding sequence when it is capable of affecting the expression of that coding sequence (i.e., that the coding sequence is under the transcriptional control of the promoter). Coding sequences can be operably linked to regulatory sequences in sense or antisense orientation.
“Regulatory sequences” refer to nucleotide sequences located upstream (5′ non-coding sequences), within, or downstream (3′ non-coding sequences) of a coding sequence, and which influence the transcription, RNA processing or stability, or translation of the associated coding sequence. Regulatory sequences may include promoters, translation leader sequences, introns, and polyadenylation recognition sequences.
“Promoter” refers to a nucleotide sequence capable of controlling the expression of a coding sequence or functional RNA. In general, a coding sequence is located 3′ to a promoter sequence. The promoter sequence consists of proximal and more distal upstream elements, the latter elements often referred to as enhancers. Accordingly, an “enhancer” is a nucleotide sequence that can stimulate promoter activity and may be an innate element of the promoter or a heterologous element inserted to enhance the level or tissue-specificity of a promoter. Promoters may be derived in their entirety from a native gene or be composed of different elements derived from different promoters found in nature, or even comprise synthetic nucleotide segments. It is understood by those skilled in the art that different promoters may direct the expression of a gene in different tissues or cell types, or at different stages of development, or in response to different environmental conditions. Promoters that cause a nucleic acid fragment to be expressed in most cell types at most times are commonly referred to as “constitutive promoters”.
The “translation leader sequence” refers to a nucleotide sequence located between the promoter sequence of a gene and the coding sequence. The translation leader sequence is present in the fully processed mRNA upstream of the translation start sequence. The translation leader sequence may affect processing of the primary transcript to mRNA, mRNA stability or translation efficiency.
The “3′ non-coding sequences” refer to nucleotide sequences located downstream of a coding sequence and include polyadenylation recognition sequences and other sequences encoding regulatory signals capable of affecting mRNA processing or gene expression. The polyadenylation signal is usually characterized by affecting the addition of polyadenylic acid tracts to the 3′ end of the mRNA precursor.
As used herein, the term “FMD” encompasses disease symptoms in cattle and swine caused by a FMDV infection. Examples of such symptoms include, but are not limited to, vesicles in the mouth, and on the feet. As used herein, a FMDV that is “unable to produce FMD” refers to a virus that can infect a pig, but which does not produce any disease symptoms normally associated with a FMD infection in the pig, or produces such symptoms, but to a lesser degree, or produces a fewer number of such symptoms, or both.
The terms “porcine” and “swine” are used interchangeably herein and refer to any animal that is a member of the family Suidae such as, for example, a pig. “Mammals” include any warm-blooded vertebrates of the Mammalia class, including humans.
The terms “foot and mouth disease virus” and “FMDV”, as used herein, unless otherwise indicated, mean any strain of FMD viruses.
Terms such as “suitable host cell” and “appropriate host cell”, unless otherwise indicated, refer to cells into which RNA molecules (or isolated polynucleotide molecules or viral vectors comprising DNA sequences encoding such RNA molecules) of the present invention can be transformed or transfected. “Suitable host cells” for transfection with such RNA molecules, isolated polynucleotide molecules, or viral vectors, include mammalian, particularly bovine and porcine cells, and are described in further detail below.
A “functional virion” is a virus particle that is able to enter a cell capable of hosting a FMDV, and express genes of its particular RNA genome (either an unmodified genome or a genetically modified genome) within the cell.
In summary, we provide a stable transgenic fetal porcine kidney cell line, LFBK α v β 6 , useful for the rapid isolation and sensitive detection and identification of all seven FMDV serotypes and multiple subtypes in cell culture. The invention provides for highly sensitive detection of FMDV from field samples.
EXAMPLES
Having now generally described this invention, the same will be better understood by reference to certain specific examples, which are included herein only to further illustrate the invention and are not intended to limit the scope of the invention as defined by the claims.
Example 1
LFBK Cells Expressing Bovine α v β 6 Integrin: Growth and Characterization
LFBK cells were propagated in DMEM supplemented with 10% fetal bovine serum and antibiotics as previously described (Piccone et al. 2009 . J. Virol. 83:6681-6688) and used for these experiments between passages 64 and 71. LFBK-α V β 6 cells were propagated in the same manner as LFBK cells and used at the passage indicated in each experiment. BHK cells, used between passages 62 and 67, were propagated in MEM supplemented with 10% calf serum, 10% tryptose phosphate broth and antibiotics. Primary lamb kidney (LK) cells, generously supplied by the APHIS Diagnostic Service Section at PIADC, were propagated in DMEM supplemented with 10% fetal bovine serum, antibiotics and sodium pyruvate and used directly from cryovials or at passage 1 as indicated. IB-RS-2 cells were used between passage 129 and 137 and MVPK cells were used between passages 38 and 41; both of these cell lines were propagated in MEM supplemented with 10% fetal calf serum, nonessential amino acids and antibiotics.
The integrin α V β 6 is an important receptor for FMDV in relevant tissues in vivo. LFBK cells are a transformed cell line that has high sensitivity to most FMDV serotypes but does not express high levels of β 6 integrin protein. In order to merge the enhanced susceptibility of α V β 6 expression with the transformed phenotype of LFBK cells, the bovine α V and β 6 integrin subunits were transduced into LFBK cells. Individual retroviruses expressing the bovine α V (Gen Bank AF239958) or bovine β 6 (GenBank AF468060) integrin subunits (Duque et al., supra) were created with the Pantropic Retroviral Expression System (Clontech PT3346-5) following the manufacturer's protocol. LFBK cells at passage 145 were infected with the α V -expressing retrovirus and neomycin selection was used to select against non-transduced cells. A pool of these cells was infected with the β 6 -expressing retrovirus, then cloned to single cells by terminal dilution. Clones were chosen that showed consistent expression of the β 6 subunit by immunohistochemistry.
Immunohistochemical staining was used to demonstrate the long-term maintenance of β 6 expression in LFBK-α V β 6 cells. The Vectastain ABC kit (Vector Labs, PK-6102) and Vector VIP peroxidase substrate kit (Vector Labs, SK-4600) were used according to the manufacturer's protocols. Mouse anti-human β 6 (Chemicon, CSb6) was used to detect the bovine integrin subunit β 6 at a 1:300 dilution. The mouse monoclonal antibody F19-51 (Yang et al. 2007 . J. Immunol. Methods 321:174-181) was used to detect the FMDV 3D protein at a 1:200 dilution.
Immunohistochemical staining demonstrated the long-term maintenance of β 6 expression in the LFBK-α V β 6 cells for at least 102 cell passages as compared to the non-transduced LFBK cells ( FIG. 1A-C ).
FMDV A24-SGD, an FMDV A24 Cruziero strain serially passed in cattle, has an SGD motif in the G-H loop of VP1 and enhanced infectivity in cells expressing the α V β 6 integrin (Rieder et al., supra). LFBK-α V β 6 cells at various subculture passages and non-transduced LFBK cells were infected with A24-SGD or a cell culture grown control virus (A24-BHK) to confirm the long-term functional maintenance of the α V β 6 integrin.
Cells were seeded 72 hours before infection in 6-well cell culture plates unless otherwise noted. Inoculum volume was 200 μl. 1 hour post adsorption, the inoculum was removed and the cells were overlaid with 50/50 1.2% Gum Tragacanth/2×MEM supplemented with antibiotic/antimycotic. Plates were incubated for 24 hours unless otherwise indicated then simultaneously fixed and stained with Histo-Choice tissue fixative (AMRESCO) containing crystal violet and plaques were counted.
The results of these experiments showed that the LFBK-α V β 6 cells have a 2.5 log increased susceptibility to A24-SGD compared to LFBK cells and that the increased susceptibility is maintained for over 100 passages ( FIG. 1D ). Expression of surface proteins can be delayed due to trypsin treatment during cell subculturing. To determine if increasing the time between seeding and infecting the cells had an effect on susceptibility, LFBK and LFBK-α V β 6 cells were seeded on plates 24, 48 or 72 hours prior to infection with A24-SGD or A24-BHK viruses. It was found that seeding the LFBK-α V β 6 cells 72 hours prior to infection provided only slightly better sensitivity than seeding 24 hours prior to infection ( FIG. 1E ). This result indicates that the LFBK-α V β 6 cells can be infected early after subculturing with only minimal loss of susceptibility.
In order to show that the LFBK-α V β 6 cells support the normal growth progression of FMDV, a multi-step growth curve was performed ( FIG. 1F ). LFBK-α V β 6 or LFBK were seeded in 24 well plates 72 hours before infection with either FMDV A24-BHK (a cell culture-passaged virus containing the wild-type RGD motif in VP1) or FMDV A24-SDG (vesicular fluid from the second bovine passage of the SGD-containing A24-B9 virus described in (Rieder et al., supra) at a multiplicity of 0.01 PFU/cell. The viruses were absorbed for 1 hour with rocking at 37° C. The cells were then acid washed (25 mM MES pH 5.5 in 145 mM NaCl), washed once with growth media, and incubated at 37° C. in 0.5 mL growth media per well. At the indicated time, cells were frozen at −70° C., thawed and virus titer was determined by plaque assay on LFBK-αvβ6 cells.
In this experiment, the replication of A24-BHK was similar in both LFBK and LFBK-α V β 6 cells. While A24-SGD replicated slowly in the non-transduced LFBK cells, this virus grew normally in LFBK-α V β 6 cells, demonstrating that the expression of α V β 6 in LFBK cells complements the defect of non-transduced LFBK cells to support efficient A24-SGD replication.
Example 2
Susceptibility of LFBK-αVβ6 Cells to Animal-Derived FMDV of all Serotypes
In order to determine the susceptibility of LFBK-α V β 6 cells to animal-derived FMDV strains and compare with that of LFBK, primary lamb kidney (LK), BHK, and two swine kidney cells lines (IB-RS-2 and MVPK), each cell type was infected with serial dilutions of infected tissue macerates or vesicular fluid obtained from animals experimentally infected with each of the FMDV serotypes. The viruses used in this experiment are listed in Table 1.
TABLE 1
Animal-derived viruses used in this study.
Sample
Virus
Species
Sample Type
A24 Cruzeiro
swine
Vesicular Fluid (VF)
A24 Cruzeiro
bovine
Pool of Tongue Tissue Homogenate
and Vesicular Fluid
O1 Manisa
bovine
Vesicular Fluid
O1 Manisa
swine
Vesicular Fluid
Asia1 Shamir
bovine
Tongue Tissue Homogenate
Asia1 Shamir
swine
Vesicular Fluid
C3 Resende
swine
Vesicular Fluid
C3 Resende
bovine
Tongue Tissue Homogenate
O Taiwan 1997
swine
Vesicular Fluid
O/TAW/35/1997
O UKG
swine
Vesicular Fluid
UKG/35/2001
SAT1 Zimbabwe
bovine
Tongue Tissue Homogenate
SAT2 SAU2000
bovine
Vesicular Fluid
SAT3 Zimbabwe
bovine
Tongue Tissue Homogenate
For each strain of virus, the LFBK-α V β 6 cells had equal or higher sensitivity to animal-derived FMDV compared to the other cells tested. In some cases, especially with the O serotype FMDV strains, the LFBK-α V β 6 cells supported FMDV replication greater than tenfold higher than most cell types tested ( FIG. 2 ) and Table 2.
TABLE 2
Strain Susceptibility of 6 Cell Types to Animal-Derived FMDV Samples.
Virus Strain
LFBK-
(Species)
α v β 6
LFBK
LK
IB-RS-2
MVPK
BHK
A24 Cruzerio
6.4 ± 0.4 #
3.9 ± 0.4
5.6 ± 0.1
3.9 ± 0.2
2.8 ± 0.6
5.6 ± 0.7
(Cattle)
A24 Cruzerio
7.4 ± 0.2
6.9 ± 0.4
7.0 ± 0.6
6.7 ± 0.4
6.4 ± 0.3
6.8 ± 0.6
(Swine)
O1 Manisa
6.4 ± 0.5
4.9 ± 0.4
4.9 ± 0.8
4.7 ± 0.6
4.3 ± 0.5
4.1 ± 0.6
(Cattle)
O1 Manisa
6.2 ± 0.5
4.9 ± 0.5
4.8 ± 0.5
4.7 ± 0.5
4.6 ± 0.3
4.5 ± 0.2
(Swine)
Asia1
6.0 ± 0.4
5.7 ± 0.3
5.6 ± 0.3
5.3 ± 0.1
5.2 ± 0.3
5.2 ± 0.2
Shamir
(Cattle)
Asia1
7.2 ± 0.2
6.9 ± 0.2
6.8 ± 0.1
6.6 ± 0.3
6.5 ± 1.1
6.6 ± 0.3
Shamir
(Swine)
C3 Resende
5.2 ± 0.6
3.4 ± 0.3
4.3 ± 0.6
2.9 ± 0.4
2.5 ± 0.2
3.6 ± 0.1
(Cattle)
C3 Resende
7.9 ± 0.1
7.5 ± 0.4
7.3 ± 0.1
7.0 ± 0.2
7.0 ± 0.7
7.4 ± 0.1
(Swine)
SAT1/ZIM
7.5 ± 0.5
7.2 ± 0.4
7.0 ± 0.4
6.9 ± 0.1
6.6 ± 0.8
6.6 ± 0.5
(Cattle)
SAT2/SAU
7.0 ± 0.4
6.1 ± 0.3
6.6 ± 0.7
4.8 ± 0.9
6.0 ± 0.8
5.3 ± 0.5
(Cattle)
SAT3/ZIM
6.7 ± 0.2
6.1 ± 0.3
5.9 ± 0.3
5.8 ± 0.5
5.7 ± 0.1
6.1 ± 0.5
(Cattle)
O/TAW/1997
6.8 ± 0.6
5.3 ± 0.1
3.2 ± 0.1
4.7 ± 0.1
4.4 ± 0.6
5.6 ± 0.6
(Swine)
O/UKG/2001
7.2 ± 0.3
5.8 ± 1.4
6.3 ± 0.3
5.5 ± 0.2
5.6 ± 1.0
5.9 ± 0.1
(Swine)
# log 10 PFU/ml ± max-min
These data confirm that LFBK-α V β 6 cells can readily detect all FMDV serotypes in tissues from experimentally-infected animals.
Example 3
Detection of FMDV in Diagnostic Tissue Samples
LK cells, BHK, IB-RS-2 and LFBK-α V β 6 were seeded onto 48-well cell culture plates 48 hours prior to infection. LK cells were seeded directly from storage cryovials. LFBK-α V β 6 cells were seeded at passage 32, IB-RS-2 at passage 136 and BHK-21 at passage 66. Diagnostic lesion tissues were disrupted and virus isolated after centrifugation through a Spin-X purification column (Costar) as described in (Pacheco et al. 2010, supra). 100 μl of a 1:10 dilution of these tissue macerates were used to infect each cell type for 1 hour at 37° C. After adsorption, 400 μl of growth media was added to each well and the plates were incubated at 37° C. Starting at 4 HPI, visual evidence of cytopathic effects was recorded every 2 hours until 20 HPI, then at 24, 28 and 48 HPI. At 48 HPI, all wells were fixed with 50% acetone:50% methanol and wells negative for cytopathic effects were immunohistochemically stained with a monoclonal antibody to FMDV 3D protein to confirm negative results.
Samples from experimentally-infected animals tend to be very high titer and have better integrity than field samples. To more closely mimic diagnostic conditions, we obtained field diagnostic samples from Afghanistan, Bolivia and Pakistan (Table 3).
TABLE 3
Field Diagnostic Samples
Virus Designation
Species
A/AFG/156/2005
Cattle
A/AFG/160/2005
Cattle
O/AFG/210/2004
Cattle
O/BOL/741/2000
Cattle
O/BOL/758/2001
Cattle
A/BOL/803/2001
Cattle
A/BOL/812/2001
Cattle
O/Sargodha/PAK/9/2010
Cattle
O/Islamabad/PAK/10/2010
Cattle
O/Bahawalpur/PAK/11/2010
Cattle
O/Bahawalpur/PAK/12/2010
Buffalo
O/Bahawalpur/PAK/13/2010
Buffalo
O/Rawalpindi/PAK/14/2010
Buffalo
O/Rawalpindi/PAK/15/2010
Buffalo
O/Sahiwal/PAK/16/2010
Buffalo
O/Sargodha/PAK/17/2010
Buffalo
O/Sargodha/PAK/18/2010
Cattle
Asia1/Sargodha/PAK/22/2011
Cattle
Asia1/Sargodha/PAK/23/2011
Cattle
Asia1/Sargodha/PAK/24/2011
Cattle
Asia1/Sargodha/PAK/25/2011
Cattle
Asia1/Sargodha/PAK/26/2011
Cattle
Asia1/Sargodha/PAK/27/2011
Cattle
Asia1/Sargodha/PAK/28/2011
Cattle
Asia1/Sargodha/PAK/29/2011
Cattle
?/Sargodha/PAK/30/2011
Cattle
Asia1/Karachi/PAK/31/2011
Buffalo
Asia1/Karachi/PAK/32/2011
Buffalo
Asia1/Karachi/PAK/33/2011
Buffalo
O/Karachi/PAK/34/2011
Buffalo
Asia1/Karachi/PAK/35/2011
Buffalo
Asia1/Karachi/PAK/36/2011
Buffalo
Asia1/Karachi/PAK/37/2011
Buffalo
O/Karachi/PAK/38/2011
Buffalo
Asia1/Karachi/PAK/39/2011
Buffalo
O/Karachi/PAK/40/2011
Buffalo
O/Karachi/PAK/41/2011
Buffalo
O/Karachi/PAK/42/2011
Buffalo
These samples were processed from tissue according to standard virus isolation procedures and used to infect LFBK-α V β 6 cells and also other cells commonly used for FMDV diagnostics, including LK, IB-RS-2 and BHK cells. FIG. 3A shows the time point at which each diagnostic isolate first showed visible CPE in each cell line. LFBK-α V β 6 was the only cell type in which all clinical samples were detected and scored as CPE positive by 24 h. Few samples yielded virus in all four cell lines. Twelve samples showed CPE in only LFBK-α V β 6 and LK cells. Three of the 38 isolates tested only grew in LFBK-α V β 6 cells. These data thus show that LFBK-α V β 6 cells are the most sensitive to these FMDV field isolates among all the cells tested. In order to rule out the presence of FMDV in non-cytopathic infection, all CPE-negative wells were stained for FMDV 3D antigen after 48 HPI; none of the CPE-negative LK and IB-RS-2 wells reacted with the antibody. 5 CPE-negative BHK wells had individual non-rounded cells that stained positive for antigen (data not shown), indicating these particular FMDV isolates were able to enter BHK cells but not spread efficiently in the culture by 48 h.
FIG. 3B shows the overall CPE progression over time in all 38 virus isolates by plotting the mean CPE score of each isolate at each time point per cell type. On average, the LK and LFBK-αVβ6 cells performed very similarly, both being much more sensitive to the diagnostic isolates than the IB-RS-2 and BHK cells. While the LFBK-α V β 6 cells had slightly faster overall early detection of the isolates than the LK cells, the higher mean CPE score at later times indicates a faster progression of virus replication in the LFBK-α V β 6 cells. Taken together, the enhanced susceptibility, rapid initial detection of CPE, and faster progression of CPE strongly suggests that LFBK-α V β 6 cells are superior to many cells currently used for FMDV diagnostics from tissue specimens.
Example 4
Susceptibility of LFBK-αVβ6 Cells to Other Vesicular Disease-Causing Viruses
Animals exhibiting vesicular lesions may be infected with other agents besides FMDV. In order to determine if LFBK-α V β 6 cells could detect other viruses causing vesicular disease, we inoculated BHK, LK, IB-RS-2, LFBK or LFBK-α V β 6 cells with each of 5 non-FMD viruses causing vesicular disease.
We found that vesicular exanthema of swine virus (VESV) and swine vesicular disease virus (SVDV) replicated as well in LFBK-α V β 6 cells as they did in IB-RS-2 cells (Table 4). Vesicular stomatitis viruses serotype New Jersey (VSV-NJ) grew to similar titers in all the cell lines. LK, LFBK and LFBK-α V β 6 cells supported the growth of bovine papular stomatitis virus (BPSV) as evidenced by the formation of plaques; BPSV grew to a slightly higher titer in LK cells than in LFBK-α V β 6 cells. Infection with bluetongue virus (BTV) only induced cytopathic effects in IB-RS-2 and LK cells by 96 HPI.
TABLE 4
Growth of selected animal-derived vesicular disease viruses.
Cell Types
Virus
LFBK
LFBK-α v β 6
IB-RS-2
BHK
LK
VESV A48 ET 305
6.15 a
6.55
5.8
ND b
3.05
SVDV UKG72
6.2
6.2
6.3
ND
3.05
BSPV New York 2004
3.2
3.05
3.2
ND
3.8
BTV-1 South Africa 1993
ND
ND
3.2
ND
3.05
VSV New Jersey c
7.3
7.05
6.55
6.3
5.8
a Virus titers in log 10 TCID 50 /ml.
b ND, not detected. Limit of detection in this assay is 1.8 log 10 TCID 50 /ml.
c This virus obtained from a pool of experimentally infected animal tissues.
Thus, LFBKαvβ6 cells can support the growth of VESV, SVDV, VSV-NJ and BPSV) as well or better than LFBK, IB-RS-2, BHK and LK.
The LFBKαvβ6 cell line has been deposited with the American Type Culture Collection (ATCC), 10801 University Blvd., Manassas, Va. 20110-2209 on Jul. 11, 2012, under accession number PTA-13047, as a patent deposit under the Budapest Treaty on the International Recognition of the Deposit of Microorganisms for the Purposes of Patent Procedure. The subject cell line has been deposited under conditions that assure that access to the cell line will be available during the pendency of this patent application to one determined by the Commissioner of Patents and Trademarks to be entitled thereto under 37 CFR 1.14 and 35 USC 122. The deposit is available as required by foreign patent laws in countries wherein counterparts of the subject application, or its progeny, are filed. However, it should be understood that the availability of a deposit does not constitute a license to practice the subject invention in derogation of patent rights granted by governmental action.
Further, the subject culture deposits will be stored and made available to the public in accord with the provisions of the Budapest Treaty for the Deposit of Microorganisms, i.e., they will be stored with all the care necessary to keep them viable and uncontaminated for a period of at least five years after the most recent request for the furnishing of a sample of the deposit, and in any case, for a period of at least 30 (thirty) years after the date of deposit or for the enforceable life of any patent which may issue disclosing the cultures. The depositor acknowledges the duty to replace the deposits should the depository be unable to furnish a sample when requested, due to the condition of the deposit(s). All restrictions on the availability to the public of the subject culture deposits will be irrevocably removed upon the granting of a patent disclosing them.
All publications and patents mentioned in this specification are herein incorporated by reference to the same extent as if each individual publication or patent was specifically and individually indicated to be incorporated by reference.
The foregoing description and certain representative embodiments and details of the invention have been presented for purposes of illustration and description of the invention. It is not intended to be exhaustive or to limit the invention to the precise forms disclosed. It will be apparent to practitioners skilled in this art that modifications and variations may be made therein without departing from the scope of the invention.
|
Foot and out disease virus (FMDV) is worldwide problem. Rapid isolation, serotyping and vaccine matching of FMDV from infected animals is critical to enable the implementation of effective vaccination programs and to stop the spread of infection during outbreaks. Current virus isolation protocols use primary cells, known to be susceptible to FMDV, or baby hamster kidney cells (BHK-21) and other cell lines that are not highly sensitive to some strains of FMDV. The α V β 6 integrin is a principal receptor for FMDV. We therefore transduced the porcine kidney cell line, LFBK, to stably express both the α V and β 6 bovine integrin subunits. The LFBK-α V β 6 cell line showed both β 6 expression and enhanced susceptibility to FMDV infection for at least 100 cell passages. LFBK-α V β 6 cells are highly sensitive for detecting all serotypes of FMDV from experimentally infected animals, including the porcinophillic strain O/TAW/97 and are thus a sensitive tool for FMDV isolation.
| 2
|
BACKGROUND OF THE INVENTION
The invention relates to a towing arrangement or hitch for prime movers, in particular for coupling implements with tow bars to an agricultural or utility vehicle.
Agricultural or utility vehicles, in particular, such as agricultural tractors, frequently contain a hitch so that implements can be coupled to and towed by the tractor. For this purpose a towing hook is provided on the prime mover, which is able to engage a clevis in the tow bar of the implement. For tow bars that must be raised from the ground for the coupling process there is an advantage in attaching the towing hook on the utility vehicle so as to be adjustable in height, so that the prime mover can be backed up and the towing hook engaged with the clevis of the tow bar, in order to perform the coupling process. After coupling the towing hook to the tow bar, the towing hook and the tow bar are lifted by a mechanical arrangement.
Certain standards must be observed in the case of tractors with power take-off shafts. For example, the ISO 500/6489 standard requires a fore-and-aft spacing distance of 100 millimeters between the towing hook and the end of the power take-off shaft. This means that the coupling point is located relatively close to the rear of the vehicle cab and is not always visible from the operator's seat, in particular when it is in its lower position. It would be desirable to simplify the coupling process by improving visibility of the coupling point.
In German patent reference DE 1 249 099, a coupling arrangement for tractors is shown in which two levers are arranged under the tractor body, each of which is pivoted at one end about a pin on the tractor body. A towing hook is provided at the other end of each lever. These levers can be raised and lowered by means of a lift shaft, lift arms, chains and drawbar. Thus, the towing hooks move in a circular arc about the axis of the pins. In the lowered position, the towing hooks are located close to the rear of the tractor and are not visible from the operator's seat.
Another similar hitch is shown in European Patent publication EP 0 184 489. In this known hitch the towing hook is pivotally coupled to the vehicle chassis by a pair of spaced apart pivoting links. One link is coupled to the forward end of the towing hook and the other link is coupled to a central portion of the towing hook. The two links determine the curved path through which the towing hook moves as it is raised and lowered. The towing hook is raised by a lifting arrangement which includes a telescoping rod that is attached to a lift rod in the vicinity of the towing hook.
In this hitch the lift lever is located below the vehicle body and thereby reduces the ground clearance of the vehicle. Furthermore, in this location the arrangement is subject to an increased danger of dirt accumulation during operation. Because in its lowered position the towing hook extends further beyond the rear of the tractor than in its locked position, it may, therefore, be visible from the operator's seat in its lowered position. However, during lifting the towing hook is rapidly retracted and disappears from the operator's visual field. That means that the operator is able to capture the clevis of the tow bar only with considerable difficulty when the tow bar is not in the lowest position of the hitch.
SUMMARY OF THE INVENTION
Accordingly, an object of this invention is to provide a hitch of the aforementioned type in which the towing hook is visible from the operator's seat during the entire lifting operation.
Another object of this invention is to provide a hitch which is protected from dirt accumulation during operation.
Another object of this invention is to provide a hitch which can be manufactured at low cost and which meets the requirements of standards.
These and other objects are achieved by the present invention wherein a hitch is built with simple, generally strap-shaped parts connected by joints. The hitch includes at least one spacer pivoted about a horizontal axis from the chassis of the prime mover. Its rear end engages the central region of a lift lever which can be pivoted about a horizontal axis with respect to the spacer. A towing hook is mounted on the aft end of the lift lever. The height of the lift lever can be controlled by pivoting the lift lever. At the second end of the lift lever a joint is provided.
The lift lever is positioned behind the rear of the vehicle, but not under the vehicle body. The lift lever is generally oriented vertically, with an upper end somewhat forward of the lower end with respect to the direction of travel of the vehicle. Therefore, in a locked condition the vehicle ground clearance is not impaired and the danger of dirt accumulation is largely avoided.
The lift lever can be guided in such a way that the towing hook initially moves in a vertical direction. Then, shortly before reaching the operating height, the towing hook changes direction and moves generally in horizontal direction to the operating position. This motion makes possible a constant visual inspection of the coupling point from the operator's seat during its raising or lowering.
In a preferred embodiment at least two connecting links are pivotally connected to each other between a controllable lift arm and the upper end of the lift lever. These links operate as a chain. They transmit tensile forces, but can buckle when the towing hook is locked in its operating position and the lift arm is lowered. This makes it possible for the lift arm or a lift shaft engaging the lift arm to be used also for the operation of other devices, for example, steering arms, without the need for unlocking the components of the hitch.
A stop is provided between the lift arm and one of the connecting links so as to make possible a freely pivoting motion between lift arm and connecting link in the first phase of motion during lifting, but so as to lock the connecting link to the lift arm in a second phase of motion. This shifts the point of engagement from the end of the lift arm to the end of the connecting link in the second phase of motion, and hence the direction of the force applied to the pivoted lift lever is changed. This hitch can be manufactured at low cost and is easy to install.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a schematic side view of the rear region of a vehicle with a hitch according to the invention with the towing hook lowered.
FIG. 2 shows a hitch according to FIG. 1 with a towing hook in operating position.
FIG. 3 shows the schematic view of a hitch according to FIG. 2 as seen from the rear of the vehicle.
DETAILED DESCRIPTION
The center of FIG. 1 shows the gearbox housing 10 of an agricultural tractor, not shown in any further detail. The gearbox housing 10 is part of the support structure (chassis) of the agricultural tractor. A rear axle 12 drives the rear wheels 14, also shown only partially.
A power take-off shaft 16 projects from the rear of the gearbox housing 10, for driving a towed implement (not shown). A retaining plate 18 is attached by bolts 20 to each side of the rear lower region of the gearbox housing 10. The retaining plates 18 extend to the rear beyond the rear end of the gearbox housing.
One end of a spacer 22 is attached to each of the retaining plates 18 so that each spacer 22 can pivot in vertical direction about a horizontal axis 24. The other end 26 of each spacer 22 is connected to the center region of a corresponding one of the lift levers 30 by the horizontal pivot axes 28 arranged to either side of the gearbox housing 10.
The lift levers 30 are configured as metal straps with their upper ends 32 positioned above and forward of their lower ends 34. As best seen in FIG. 3, the lower ends 34 of the lift levers 30 are coupled to a towing plate 36 which carries a towing hook 38. Each upper end 32 is pivotally coupled to a connecting link 42 by a joint 40.
A pair of bell crank-shaped lift arms 44 are pivoted from a fixed horizontal axis 46 which is located above the gearbox housing 10 in the region of the greatest width of the gearbox housing 10. One leg 48 of each lift arm 44 is connected to a piston rod 50 of an associated hydraulic cylinder 52 so that the lift arm 44 can be pivoted about the axis 46 by the hydraulic cylinder 52. In place of the lift arms 44, extended lift arms (not shown) could be used that are directly swung about a pivot by a power-driven lift shaft. The other end 54 of each lift arm 44 is pivotally coupled by joint 58 to a second strap-shaped connecting link 56, which in turn is pivotally coupled to a corresponding one of the connecting links 42.
A stop 60 is attached to each of the lift arms 44 near the joint 58, and extends toward the second connecting link 56. The length of stop 60 is such that the swing angle between the lift arm 44 and the second connecting link 56 is limited to a predetermined amount, as is illustrated by FIG. 2.
Referring now to FIG. 3, a pair of locking pins 62 are supported by the towing plate 36 on each side of the towing hook 38, and a helical spring 64 urges the pins away from each other. The locking pins 62 carry retainers 66, 68 which are coupled to a push-pull cable 70. In the unloaded condition the outer ends of the locking pins 62 project beyond the side surfaces of the towing plate 36. By operating the push-pull cable 70 the two locking pins 62 can be moved towards each other against the force of spring 64 so that their outer ends no longer project beyond the side surfaces of the towing plate 36. The locking pins 62 make possible a locking of the towing plate 36, and therewith also the towing hook 38, to the retaining plates 18, wherein the locking pins 62 engage corresponding bores 72 in the retaining plates 18, as is illustrated in FIG. 3. Pulling on the push-pull cable 70 retracts the locking pins 62 and the lock is released.
When the towing hook 38 reaches its locked position its backside engages a stop 74 which is provided between the retaining plates 18. This stop 74 limits rotation of the towing hook 38 in the clockwise direction past the position shown in FIG. 2).
FIG. 1 shows the lift mechanism in a position with the towing hook 38 lowered to its lowest position on the ground. By extending the piston rod 50 from the hydraulic cylinder 52 the lift arms 44 are rotated about the axis 46 in a counterclockwise direction. The ends of lift arms 44, acting through the second and first connecting links 56, 42, pull the lift levers 30 upward and at a slight forward angle and therewith the towing plate 36 and the towing hook 38. At this time, the connecting links 56, 42 and the lift lever 30 are aligned along a line established by the position of the joints 40 and 58. The joint 58 moves in a circular arc about the axis 46 so that the connecting links 42, 56 and the lift arm 30 are moved to a more nearly vertical orientation of during the lifting.
As the lift arms 30 are lifted, the pivot axis 28 is moved upward in a circular arc, the radius of which is determined by the length of the spacer 22. Due to the movement of pivot axis 28 and the movement of the joint 58, the towing hook 38 initially moves substantially vertically as it is lifted. After the spacer 22 has rotated past a horizontal position, the towing hook 38 begins to move horizontally forward, whereupon the rotation of the lift lever 30 in clockwise direction is accelerated. As a result, the towing hook 38 follows the curved path 76.
This effect is amplified with a certain lift curve in which the angle between the lift arm 44 and the second connecting links 56 has become so small that the stops 60 come into contact with the second connecting links 56 and lock the joints 58.
As a result of the action of the stops 60, the point of alignment of the line formed by the lift levers and connecting links no longer lies in the joint 58, which had described a circle arc about the axis 56, upon further lifting, but in the connecting joint 78 between the first and the second connecting links 42, 56. During further lifting these joints 78 describe a circular arc about the axis 46. In the upper lifting region, therefore, the orientation of the lift levers 30 rapidly becomes more vertical, so that the towing hook 38 moves substantially horizontally as it nears the fully raised position shown in FIG. 2.
When the towing hook 38 finally reaches its operating position, the locking pins 62 are unlocked by the push-pull cable 70 and are forced into the bores 72 by the helical spring 64. The engagement of the locking pins 62 in the retaining plates 18 locks the towing hook 38. The locked position is shown in FIG. 2, and indicated for emphasis with dot-dashed line in FIG. 1.
During operation both locking pins 62 absorb the tensile loads as well as the support forces of the towed implement. Thereby the lift arms 44, connecting links 42, 56 and lift levers 30 remain unloaded during towing. Thus, in the locked position, the lift arms 44 can be used for the operation of other devices, such as steering arms, without the necessity of unlocking the connecting links 42, 56 or the lift levers 30.
The connecting links 42, 56 may be buckled into the position shown in FIG. 2 by the dot-dashed lines 44' and 56'. In this buckled position no force is transmitted from the lift arms 44 to the lift levers 30. The joint 58 moves downward in the circular arc 80 with respect to axis 46 to the point 82. Simultaneously, the joint 78 moves in a circular arc about the joint 40 until it reaches the position 86. The dot-dashed lines 44', 56' and 42' illustrate the new positions of the lift arms and the connecting links.
While the present invention has been described in conjunction with a specific embodiment, it is understood that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, this invention is intended to embrace all such alternatives, modifications and variations which fall within the spirit and scope of the appended claims.
|
A hitch for attaching an implement with a tongue to an agricultural vehicle has at least one spacer bar which is pivotally coupled to the vehicle body about a horizontal axis. A rear end of the spacer bar is pivotally connected to the middle area of a lift arm. A drawbar hook is connected to a rear end of the lift arm and the lift is pivotal about an axis to adjust the height of the drawbar hook. A lift mechanism is pivotally connected to a forward end of the lift arm. This lift mechanism draws the forward end of the lift arm generally upwards. The hitch operates so that the drawbar hook moves substantially vertically and then horizontally when moved from its lowest position to a work height.
| 1
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This non-provisional application claims priority under 35 U.S.C. §119(a) on Patent Application No(s). 101207945 filed in Taiwan, R.O.C. on Apr. 27, 2012, the entire contents of which are hereby incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to card-style solar chargers, and more particularly, to a card-style solar charger comprising an output end disposed on a card-style substrate.
BACKGROUND OF THE INVENTION
[0003] At present, due to the rapid development of the electronic industry, information industry, and communication industry, their products follow the trend toward being lightweight and compact in order for their products not to be portable and space-saving. However, portable electronic products operating outdoors are seldom capable of accessing an external power source but have to be powered by in-built battery (commonly known as secondary batteries.)
[0004] In attempt to solve the aforesaid problem, related prior art discloses providing at least two batteries such that there is always a spare battery for replacing timely an operating battery running out of power. Nonetheless, the aforesaid prior art copes with the aforesaid problem by bringing about a new problem—the weight of the spare battery burdens the user carrying the portable electronic product.
[0005] Another attempt to solve the aforesaid problem involves recharging an operating battery running out of power. A conventional recharging process always takes place at a stationary power-supplying device, such as an electrical outlet, for supplying the recharging power. This conventional recharging process was good until recently. Recent years sees the birth of robust portable electronic device using conventional rechargeable batteries being recharged more often than ever before. Given a portable electronic device equipped with one and only one conventional rechargeable battery, the time taken to recharge the conventional rechargeable battery plus the fact that conventional rechargeable batteries nowadays are recharged more often than ever before means that the recharging-related interruption of the operation of portable electronic devices is inevitably longer and more often than ever before.
[0006] The prior art further discloses eliminating the aforesaid recharging-related interruption by means of solar chargers, as solar chargers can recharge rechargeable batteries continuously and as needed while the rechargeable batteries are operating, provided that sunlight is available. However, conventional solar chargers are disadvantageously bulky and thus not portable.
[0007] The bulkiness weakness led to the advent of ultra-slim conventional solar chargers which remain unfit for thorough elimination of the drawbacks of the related prior art. Ultra-slim solar chargers are not equipped with a power output device and thus have to be connected to a transmission cable and an output connector for outputting power generated from the solar chargers to the charging connector of another electronic device. The aforesaid design of the power output device is so complicated that it not only accounts for the difficulty facing the solar chargers in terms of storage and portability, but also explains why the junction of the transmission cable and the connector or the junction of the transmission cable and the charger is susceptible to circuit severing and contact detachment for long use, thereby posing a safety threat to the charger in operation.
SUMMARY OF THE INVENTION
[0008] It is an objective of the present invention to overcome the aforesaid drawbacks of the prior art, that is, the bulkiness and high weight of conventional solar chargers, simplify the otherwise intricate connection-related design of conventional power output end, enhance the ease of use of conventional solar chargers, and remove risk factors in conventional solar chargers.
[0009] Hence, the present invention provides a card-style solar charger, comprising: a flexible substrate; a solar cell disposed on the flexible substrate and having two electrodes; and a transparent cover membrane disposed on the solar cell, wherein the card-style solar charger is characterized in that: the card-style solar charger has an output end disposed at an end of the flexible substrate and comprising two output electrodes electrically connected to the electrodes of the solar cell. The output end is electrically connected to a connector of a transmission cable for enabling power transmission.
[0010] In an embodiment of the present invention, the card-style solar charger is of a thickness of 1.2 mm.
[0011] In an embodiment of the present invention, the card-style solar cell has a compound thin film made of copper indium gallium selenide (CIGS) and adapted to serve as a sunlight-absorbing material layer.
[0012] The aforesaid card-style solar charger further comprises a converter electrically connected to the output electrodes. The converter increases the output voltage at the output end to 5V.
[0013] The aforesaid card-style solar charger meets ISO/IEC FDIS 7810 ID-1 requirements and is of dimensions of 85.60 mm by 53.98 mm.
[0014] The present invention discloses, in another preferred embodiment thereof, the output electrodes are each of a rectangular shape, such that the output end comprising the output electrodes is electrically connected to a connector as needed.
[0015] In another preferred embodiment, two slit-like openings are disposed at the same end of the card-style solar charger as the output end is. The output end comprises the output electrodes and the openings, wherein the output electrodes and the openings comply with Universal Serial Bus connector (USB connector) specifications in shape.
[0016] In a preferred embodiment, for example, the output end matches an A-type connector for use with a standard USB, whereas the output end matches a Micro-B connector for use with a Micro-USB.
[0017] The present invention further discloses a method for manufacturing the aforesaid card-style solar charger. The method comprises the steps of:
[0018] S1: providing a flexible substrate having an output end having two output electrodes mounted thereon;
[0019] S2: providing on the flexible substrate a solar cell having two electrodes electrically connected to the output electrodes, respectively;
[0020] S3: covering a plastic substrate fully with a transparent cover membrane outside the output electrodes; and
[0021] S4: laminating the transparent cover membrane and the flexible substrate to each other by thermal lamination.
[0022] In a preferred embodiment of the present invention, the output electrodes are of a rectangular shape each such that the output end comprising the output electrodes is electrically connected to a connector as needed.
[0023] In another preferred embodiment of the present invention, two slit-like openings are disposed at the same end of the flexible substrate as the output electrodes are, the output end comprising the output electrodes and the openings, wherein the output electrodes and the openings comply with Universal Serial Bus connector (USB connector) specifications in shape. In an aspect of the preferred embodiment, the output end matches an A-type connector for use with a standard USB. In another aspect of the preferred embodiment, the output end matches a Micro-B connector for use with a Micro-USB.
[0024] Optionally, the aforesaid method further comprises the step of disposing on the card-style solar charger a converter electrically connected to the output electrodes, wherein the converter increases the output voltage at the output end to 5V.
[0025] In conclusion, a card-style solar charger provided by the present invention comes with different output ends to suit different contacts of a connector, and thus users can choose the card-style solar charger equipped with an output end that matches a unique contact of a connector, thereby dispensing with the hassles of connecting the solar charger to an external transmission cable. Due to its card-like appearance and its way of generating solar power, the card-style solar charger is portable, lightweight, compact, easy to use, capable of instant charging, and widely applicable.
[0026] In a situation where sunlight is available steadily, the card-style solar charger of the present invention recharges the rechargeable battery of a portable electronic device in real time as needed while the portable electronic device is operating; hence, the operation of the portable electronic device is unlikely to be interrupted, because the rechargeable battery would not run out of power.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Objectives, features, and advantages of the present invention are hereunder illustrated with specific embodiments in conjunction with the accompanying drawings, in which:
[0028] FIG. 1 is a schematic view of a card-style solar charger according to the present invention;
[0029] FIG. 2 is a schematic view of a layered stacking architecture of the card-style solar charger of FIG. 1 ;
[0030] FIG. 3 is a schematic view as to how to operate the card-style solar charger according to a preferred embodiment of the present invention;
[0031] FIG. 4 is a schematic view as to how to operate the card-style solar charger according to another preferred embodiment of the present invention; and
[0032] FIG. 5 is a schematic view of the card-style solar charger equipped with a converter according to yet another preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Card-Style Solar Charger
[0033] Referring to FIG. 1 and FIG. 2 , the present invention provides a card-style solar charger 1 comprising a flexible substrate 13 , a solar cell 12 , and a transparent cover membrane 11 which are stacked up, with the flexible substrate 13 being at the bottom, the solar cell 12 being in the middle, and the transparent cover membrane 11 being at the top. An output end 10 (whose periphery is indicated by a dashed line for serving an illustrative purpose instead of a restrictive purpose) is disposed at one end of the flexible substrate 13 . The output end 10 comprises two output electrodes 101 . The card-style solar charger 1 is, as its name suggests, card-shaped, resembles a debit card or a credit card which is in wide use, meets ISO/IEC FDIS 7810 ID-1 series requirements, and is of dimensions of 85.60 mm by 53.98 mm. The card-style solar charger 1 of the present invention is lightweight and portable and thus has high applicability.
[0034] The flexible substrate 13 is, as its name suggests, made of a flexible and resilient material, such as PET or any other appropriate plastics. The two output electrodes 101 are mounted on one side at the end of the flexible substrate 13 .
[0035] Referring to FIG. 3 , in a preferred embodiment, an output end 20 (whose periphery is indicated by a dashed line for serving an illustrative purpose instead of a restrictive purpose) disposed at one end of a card-style solar charger 2 comprises two output electrodes 201 . Each of the output electrodes 201 can be of a slender shape or a rectangular shape, provided that each of the output electrodes 201 corresponds in shape to a custom-made dedicated connector 202 or a charging-oriented connector of a conventional electronic device, such that connectors can be electrically connected to the output electrodes 201 as soon as the connectors are inserted into the card-style solar charger 2 .
[0036] Referring to FIG. 4 , in another preferred embodiment, an output end 30 (whose periphery is indicated by a dashed line for serving an illustrative purpose instead of a restrictive purpose) disposed at one end of a card-style solar charger 3 comprises two output electrodes 301 . Each of the output electrodes 301 can be of a slender shape or a rectangular shape. Two slit-like openings 303 are disposed at the same end of the card-style solar charger 3 as the output end 30 is. Shape-related features, such as the depth of the output electrodes 301 and the two openings 303 and the distance between the two openings 303 comply with the specifications of Universal Serial Bus connectors (USB connectors). Hence, once a USB connector 302 (such as an A-type connector for use with a standard USB) is inserted into and electrically connected to the output end 30 , the openings 303 will fix the USB connector 302 in place, and in consequence contacts of the USB connector 302 will be accurately electrically connected to the output electrodes 301 for transmitting power. For example, contacts a, b, c, d serve contact-related functions V Bus , D−, D+, and grounding, respectively. Furthermore, it is feasible that a USB connector of a configuration not described above has an ID contact (not shown), optionally.
[0037] Referring to FIG. 1 and FIG. 2 , the solar cell 12 is a compound thin-film solar cell or any other non-thin-film solar cell which has a layered stacking architecture, such as a silicon solar cell. In this regard, the present invention provides, in a preferred embodiment thereof, the solar cell 12 for use in providing electric power through photoelectrical conversion. For example, the layered stacking architecture of the solar cell 12 is a monolayer or a bilayer. Specifically speaking, the solar cell 12 comprises a substrate 123 , a compound thin film 122 , and a finger electrode 121 . The substrate 123 functions as the positive pole and is made of stainless steel. The compound thin film 122 is disposed between the substrate 123 and the finger electrode 121 and is made of a sunlight-absorbing material, such as copper indium gallium selenide (CIGS); however, the present invention is not limited thereto, as it is also feasible for the compound thin film 122 of the present invention to be replaced with any other compound thin film applicable to the aforesaid cell structure for use in solar power generation. For example, the compound thin film 122 consists of five layers as follows: (1) a lower electrode made of chromium (Cr), molybdenum-sodium (MoNa), and molybdenum (Mo), (2) a sunlight-absorbing material layer made of copper indium gallium selenide (CIGS), (3) a buffer layer made of cadmium sulfide (CdS) or zinc sulfide (ZnS), (4) a window layer made of zinc oxide (ZnO), and (5) a transparent conductive layer (made of aluminum-doped zinc oxide, AZO). The finger electrode 121 functions as a negative pole and is made of silver to thereby form a silver finger electrode. The substrate 123 and the finger electrode 121 are electrically connected to the output electrodes 101 of the flexible substrate, respectively.
[0038] The transparent cover membrane 11 is made of a transparent material and adapted to protect the solar cell 12 by covering the flexible substrate 13 fully. However, the transparent cover membrane 11 does not cover a contact-disposed region of the output electrodes 101 , and thus the contact-disposed region is exposed such that it can come into electrical contact with another device as needed.
[0039] Accordingly, each of the aforesaid card-style solar chargers in a preferred embodiment of the present invention has an output end. The output end comprises the aforesaid output electrodes which are each electrically connected to the electrodes of the solar cell, such that the output ends of the card-style solar chargers are directly electrically connected to different connectors according to the dimensions and shapes of the output electrodes. For example, in several preferred embodiments, the output end is electrically connected to a custom-made dedicated connector, an A-type connector for use with a standard USB, and a Micro-B connector for use with a Micro-USB.
[0040] Referring to FIG. 5 , in another preferred embodiment, a card-style solar charger 4 of the present invention comprises a converter 44 . The converter 44 is electrically connected to output electrodes 401 of an output end 40 (whose periphery is indicated by a dashed line for serving an illustrative purpose instead of a restrictive purpose). The converter 44 increases the output voltage at the output end to 5V so as to render charging faster and more efficient.
[0041] In conclusion, the card-style solar charger not only carries out charging instantly and quickly by means of solar power generation, but is also easy to carry and store because it is compact and lightweight.
[Method for Manufacturing Card-Style Solar Charger]
[0042] A method for manufacturing a card-style solar charger disclosed in the aforesaid preferred embodiments is described in detail below to further prove that the present invention can be readily implemented.
[0043] First, a plastic substrate is provided to serve as a flexible substrate. The aforesaid output electrodes 401 are mounted on the flexible plastic substrate and disposed at recesses formed thereon, wherein the recesses are of appropriate size. In a preferred embodiment, two openings corresponding in position to a USB connector are formed on the plastic substrate.
[0044] Second, a CIGS solar cell of a bilayer structure is produced in the following steps:
I. provide a stainless steel substrate of a thickness less than 200 μm to serve as the positive pole; II. form consecutively on the stainless steel substrate the following: chromium (Cr) layer, molybdenum-sodium (MoNa) layer, and molybdenum (Mo) layer; III. put the aforesaid components in a vacuum chamber at high temperature, introduce selenium gas into the vacuum chamber continuously, and deposit on the molybdenum (Mo) layer by sputter-deposition in the following three stages:
(1) indium (In) and copper gallium (CuGa); (2) copper gallium (CuGa), copper (Cu) and indium (In); and (3) indium (In) and copper-gallium (CuGa);
upon completion of the sputter-deposition process, a sunlight-absorbing material layer is formed;
IV. on the sunlight-absorbing material layer, a buffer layer composed of cadmium sulfide (CdS) or zinc sulfide (ZnS) is formed; V. on the buffer layer, a window layer composed of zinc oxide (ZnO) is formed; and VI. form a transparent conductive layer (AZO) on the window layer.
[0054] Finally, a silver finger electrode which functions as a negative pole is 10 μm thick and is formed on the transparent conductive layer, so as to finalize the production process of the CIGS solar cell.
[0055] The electroplated layer between the stainless steel substrate and the silver finger electrode is 5 μm or less in thickness. The thickness of the battery in its entirety is 220 μm or less in thickness.
[0056] Afterward, the CIGS solar cell thus produced is put in the recesses and on the plastic substrate mounted thereon with the output electrodes 401 . The silver finger electrode and the stainless steel substrate of the CIGS solar cell are connected to the output electrodes 401 on the plastic substrate by wire bonding or soldering.
[0057] At last, outside the output electrodes 401 , the plastic substrate is fully covered with a transparent plastic membrane or a transparent plastic cover which functions as the transparent cover membrane, and then the transparent plastic membrane or the transparent plastic cover and the plastic substrate are laminated to each other by thermal lamination, so as to form the card-style solar charger of the present invention. The card-style solar charger of the present invention is of a thickness of 1.2 mm, but the present invention is not limited thereto. Persons skilled in the art understand that the thickness of the card-style solar charger of the present invention can be configured to range between 0.8 mm and 2 mm as needed.
[0058] Optionally, a converter is disposed on the aforesaid card-style solar charger. The converter is electrically connected to the output electrodes 401 and increases the output voltage at the output end of the card-style solar charger to 5V.
[0059] The present invention is disclosed above by preferred embodiments. However, persons skilled in the art should understand that the preferred embodiments are illustrative of the present invention only, but should not be interpreted as restrictive of the scope of the present invention. Hence, all equivalent modifications and replacements made to the aforesaid embodiments should fall within the scope of the present invention. Accordingly, the legal protection for the present invention should be defined by the appended claims.
|
A card-style solar charger includes a flexible substrate, a solar cell, and a transparent cover membrane which are stacked up in bottom-to-top order and is characterized in that the card-style solar charger has an output end electrically connected to a connector of a transmission cable for supplying electric power. The card-style solar charger comes with different output ends to suit different contacts of a connector. Due to its card-like appearance and its way of generating solar power, the card-style solar charger is portable, lightweight, compact, easy to use, capable of instant charging, and widely applicable.
| 7
|
[0001] The contents of the following Japanese patent application is incorporated herein by reference: No. 2011-042926 filed on Feb. 28, 2011.
BACKGROUND
[0002] 1. Technical Field
[0003] The present invention relates to an optical fiber and a method for manufacturing silica glass. More particularly, the present invention relates to an optical fiber and a method for manufacturing silica glass that achieve low attenuation and are suitable for wavelength division multiplex (WDM) within the wavelength range of 1300 nm to 1625 nm.
[0004] 2. Related Art
[0005] The widespread use of the Internet has been rapidly increasing the amount of information communicated. Therefore, it has been desired to improve the transmission capacity of optical fiber communication systems. Coarse wavelength division multiplexing (CWDM) is a technique for simultaneously transmitting a plurality of optical signals with different wavelengths within the wavelength range of 1300 nm to 1625 nm using the same fiber. This technique, in principle, achieves improved transmission capacity, which is equal to the result of multiplying the transmission capacity of single-wavelength transmission by the number of the wavelengths that enter at the same time. Here, a silica glass-based optical fiber is highly transparent at the wavelengths of 1300 nm to 1600 nm and generally has attenuation of 0.4 dB/km or less. The attenuation is dependent on the wavelength and is expressed by the following Expression 1, where α denotes the attenuation and λ denotes the wavelength.
[0000]
α
=
A
λ
4
+
B
+
C
(
λ
)
Expression
1
[0006] In Expression 1, the first term on the right side denotes the Rayleigh scattering loss, the second term denotes the structural-imperfection-induced loss, and the third term denotes the absorption loss caused by metal impurities and OH groups.
[0007] A conventional silica glass-based optical fiber has a lot of OH groups mixed therein that have an absorption peak in the vicinity of the wavelength of 1383 nm. This makes it difficult to use the optical fiber for WDM transmission within the wavelength range of 1300 nm to 1625 nm. To address this issue, Patent Document 1 discloses a method of fabricating silica glass for an optical fiber having the smallest possible number of OH groups mixed therein and thereby achieving reduced absorption loss at 1383 nm. Furthermore, it is known that the attenuation of the silica glass-based optical fiber may increases in the vicinity of 1383 nm when hydrogen is diffused within the silica glass-based optical fiber (see Non-Patent Documents 1 and 2).
[0008] During the step of spinning an optical fiber base material into an optical fiber, the base material made of silica glass is exposed to high temperature and elongated with high tensile force. Here, it is believed that the base material is rapidly cooled down with its glass structure being broken to generate structural defects, which are generally represented by Expression 2 and referred to as non-bridging oxygen hole centers: NBOHCs).
[0000] ═Si—O Expression 2
[0009] Here, it is known that the concentration of the NBOHCs in the optical fiber is dependent on the tensile force and the cooling rate during the spinning step. It is also known that the concentration of NBOHCs increases as the tensile force or cooling rate increases during the spinning step.
[0010] Furthermore, it is known that hydrogen molecules, which are small, are easily diffused at room temperature within the glass structure of the silica glass of which the optical fiber is made. If hydrogen molecules are diffused within the silica glass, the hydrogen molecules react with NBOHCs to generate OH groups as shown by Expression 3. This results in absorption loss in the vicinity of 1383 nm.
[0000] ═Si—O.+½H 2 →═Si—OH Expression 3
[0011] To prevent such degradation in absorption loss of the optical fiber made of silica glass, the optical fiber may be exposed to a deuterium atmosphere. According to this method, instead of hydrogen, deuterium, which is an isotope of hydrogen, is diffused within the optical fiber to react with the NBOHCs as expressed in Expression 4.
[0000] ═Si—O.+½D 2 →═Si—OD Expression 4
[0012] If the NBOHC defects disappear in this way, hydrogen may later diffuse within the silica glass but does not cause the OH group-induced increase in absorption loss. This reaction easily proceeds at room temperature as disclosed in Patent Document 2. The generated OD groups do not have absorption loss in the wavelength range of 1300 nm to 1625 nm. Therefore, the attenuation in this wavelength range is hardly affected. Accordingly, the method using deuterium is effective in fabricating silica glass optical fibers with low attenuation.
[0013] In some occasions, however, the absorption loss may increase in the vicinity of the wavelength of 1400 nm after the deuterium treatment as shown in FIG. 1 . It has been proved that this increase in absorption loss is unstable and is likely to decrease as the time elapses and ultimately substantially disappears as shown in FIG. 2 . It, however, takes approximately two to three months until the increase in absorption loss disappears. Therefore, such an increase in absorption loss significantly hinders the optical fiber manufacturing. Here, FIG. 1 shows the relation between the wavelength and the absorption loss for an optical fiber that has been treated with deuterium and an untreated optical fiber. Curve 1 represents the attenuation spectrum of the optical fiber that has been treated with deuterium, and Curve 2 represents the attenuation spectrum of the untreated optical fiber. FIG. 2 shows the relation between the days that have elapsed and the absorption loss at the wavelength of 1400 nm.
[0014] Patent Document 3 introduces a hypothesis that the increase in absorption loss at the wavelength of 1400 nm may result from per-oxy linkages (POLs) in the silica glass. When silica glass base materials fabricated under the same conditions are spun into optical fibers, the amount of the increase in absorption loss may vary depending on the spinning conditions. It is, however, not clear how the spinning conditions are related to the amount of POLs generated. The increase in absorption loss at the wavelength of 1400 nm has thus not yet been clarified. Patent Document 3 discloses an optical fiber that achieves reduced increase in absorption loss at the wavelength of 1400 nm. This optical fiber is realized by a low-productivity method that involves a low drawing speed and requires manufacturing condition optimization based on electron spin resonance evaluation.
Patent Document 1: Japanese Patent 3970692 Patent Document 2: EP 1182176 B1 Patent Document 3: Japanese Patent Application Publication No. 2006-030655 Non-Patent Document 1: “New Hydrogen Aging Loss Mechanism in the 1400 nm Window,” K. H. Chang, D. Kalish and M. L. Pearsall; Proceedings OFC 99. Non-Patent Document 2: “Formation of Hydroxyl Due to Reaction of Hydrogen with Silica in Optical Finer Preforms,” J. Stone, J. M. Wiesenfeld, D. Marcuse, C. A. Burrus and S. Yang; Apllied Physics Letters 47, No. 3, 328-330, 1 Aug. 1985.
[0020] In light of the above-described problems, an object of the present invention is to provide a method for manufacturing silica glass that can reduce the increase in absorption loss in the vicinity of the wavelength of 1400 nm that is caused by deuterium treatment and can efficiently fabricate a silica glass optical fiber having low attenuation in the wavelength range of 1300 nm to 1625 nm, and to provide such a silica glass optical fiber.
SUMMARY
[0021] Therefore, it is an object of an aspect of the innovations herein to provide a method for manufacturing silica glass and an optical fiber, which are capable of overcoming the above drawbacks accompanying the related art. The above and other objects can be achieved by combinations described in the claims.
[0022] According to the present invention, a method for manufacturing silica glass includes exposing silica glass to a deuterium-containing atmosphere for a predetermined period of time to diffuse deuterium molecules within the silica glass, maintaining the silica glass at 40° C. or higher, and cooling the silica glass to room temperature. The silica glass is a silica glass-based optical fiber in which a core made of silica glass is provided at a center thereof and contains at least germanium. The core is surrounded by a clad that is made of silica glass and has a lower refractive index than the core. The surface of the silica glass is covered with a resin coating.
[0023] The exposing deactivates a structure in the silica glass that has an absorption loss peak in the vicinity of the wavelength of 630 nm. Prior to the exposing, a first attenuation value is measured in the vicinity of the wavelength of 1383 nm. After the cooling, a second attenuation value is measured in the vicinity of the wavelength of 1383 nm. The increase from the first attenuation value to the second attenuation value is 0.005 dB/km or less.
[0024] The maintaining can also deactivate a structure within the silica glass that has an absorption loss peak in the vicinity of the wavelength of 1400 nm. Prior to the maintaining, a third attenuation value is measured at least in the vicinity of 630 nm. The third attenuation value is equal to or less than a reference value, which is a result of adding 3 dB/km to a value that is obtained through extrapolation for a wavelength of 630 nm using Expression 5 and optimal values for variables A and B in Expression 5, and the optimal values for the variables A and B are determined using attenuation values at a plurality of wavelengths from no less than 700 nm and no more than 1600 nm. Here, Expression 5 is
[0000]
α
=
A
λ
4
+
B
,
[0000] where λ denotes a wavelength and α denotes attenuation. Alternatively, the reference value can be determined in advance based on values measured for a similar fiber.
[0025] During the exposing, a partial pressure of the deuterium in the deuterium-containing atmosphere is preferably 1 to 5 kPa. The exposing is preferably performed in an atmosphere having a temperature of 40° C. or higher. The maintaining is preferably performed after an absorption loss peak is generated in the vicinity of the wavelength of 1383 nm and continues until the generated absorption loss peak is stabilized. The stabilization of the absorption loss peak may indicate that the absorption loss peak becomes equal to or less than 0.35 dB/km. Alternatively, the stabilization of the absorption loss peak may indicate that the absorption loss peak becomes equal to or less than 0.3 dB/km. The maintaining is performed in the air or within a deuterium-containing atmosphere. The method preferably further includes, after the maintaining or after the cooling, exposing the silica glass to a hydrogen-containing atmosphere. After the exposing the silica glass to the hydrogen-containing atmosphere, a fourth attenuation value of the silica glass in the vicinity of the wavelength of 1383 is measured. The fourth attenuation value is equal to or less than 0.35 dB/km.
[0026] According to the present invention, a silica glass-based optical fiber includes a core made of silica glass. The core is positioned at a center of the optical fiber and containing at least germanium. The core is surrounded by a clad made of silica glass. The clad has a lower refractive index than the core. The clad is surrounded by a resin coating. The optical fiber is obtained by exposing silica glass to a deuterium containing atmosphere for a predetermined period of time to diffuse deuterium molecules within the silica glass, maintaining the silica glass at 40° C. or higher, and cooling the silica glass to room temperature. The optical fiber is characterized in that the attenuation at the wavelength of 630 nm is 10 dB/km or lower, the attenuation at the wavelength of 1383 nm is 0.35 dB/km or lower, and the cut-off wavelength is 1260 nm or lower when measured for the optical fiber of 22 m. The clad may partially contain fluorine. The clad has a diameter of 125 μm, and the resin coating has a diameter of 250 μm. The attenuation is 1 dB/turn or lower when the optical fiber is wound around a cylindrical tube of 5 mm.
[0027] The summary clause does not necessarily describe all necessary features of the embodiments of the present invention. The present invention may also be a sub-combination of the features described above. The above and other features and advantages of the present invention will become more apparent from the following description of the embodiments taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 is a graph showing the relation between the wavelength and the absorption loss for an optical fiber that has been treated with deuterium and an untreated optical fiber.
[0029] FIG. 2 is a graph showing the relation between the days that have elapsed and the absorption loss at the wavelength of 1400 nm.
[0030] FIG. 3 is a schematic view illustrating a method for manufacturing a porous core base material.
[0031] FIG. 4 is a schematic view illustrating dehydration and vitrification of a porous core base material.
[0032] FIG. 5 is a schematic view illustrating a method for manufacturing a porous base material.
[0033] FIG. 6 is a schematic view illustrating a method for manufacturing a porous clad base material.
[0034] FIG. 7A is a graph illustrating an initial attenuation spectrum for an optical fiber SMF 1 and showing, in an enlarged view, the values of attenuation in the low-attenuation range of 1300 nm or higher wavelengths.
[0035] FIG. 7B is a graph illustrating an initial attenuation spectrum for the optical fiber SMF 1 and showing the attenuation spectrum for the full range of wavelengths at which attenuation is measured.
[0036] FIG. 8 is a graph illustrating how the attenuation of an optical fiber varies over time at the wavelengths of 630 nm and 1400 nm while the optical fiber is left in a high-temperature atmosphere at 40° C. after deuterium treatment.
[0037] FIG. 9 is a graph illustrating how the attenuation of an optical fiber varies over time, where the optical fiber has been treated at a high temperature of 85° C. after deuterium treatment.
DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0038] Hereinafter, some embodiments of the present invention will be described. The embodiments do not limit the invention according to the claims, and all the combinations of the features described in the embodiments are not necessarily essential to means provided by aspects of the invention.
[0039] <Manufacturing of Optical Fiber Base Material>
[0040] SMP 1
[0041] A silica glass core base material is manufactured using VAD. A clad is deposited on the external surface of the core base material using OVD. In this way, a silica glass-based base material is formed. To begin with, a target material 2 , which is attached to the end of a rotational axis 1 , is rotated while silica glass soot containing Ge is sprayed onto the target material 2 from a burner 3 in order to increase the refractive index of a core portion. In addition, silica glass soot is sprayed from a burner 4 to form a silica glass clad portion. In this way, a porous core base material 5 is fabricated. The porous core base material 5 is thermally treated at the temperature of 1200° C. within a chlorine-containing atmosphere for dehydration. Furthermore, the porous core base material 5 is thermally treated at the temperature of 1500° C. within a dry helium atmosphere containing water of 1 ppm or less for vitrification. In this way, a transparent silica glass core base material 6 was fabricated. (See FIGS. 3 and 4 .)
[0042] The core base material 6 is heated and elongated in such a manner that the outer diameter remains constant. In this way, a core base material 8 (a transparent silica glass core) is fabricated. The core base material 8 is attached to a rotational axis 7 and rotated with respect to the core of the core base material 8 . Silica glass soot is sprayed onto the external surface of the core base material 8 from a burner 9 to deposit a porous silica glass layer. In this way, a porous base material 11 is fabricated that has the core base material 8 and a porous silica clad portion 10 integrated with each other (see FIG. 5 ). The porous base material 11 is thermally treated at the temperature of 1500° C. within a chlorine-containing atmosphere for dehydration and vitrification. In this way, a transparent silica glass base material is fabricated.
[0043] SMP 2
[0044] A silica glass core base material is manufactured using VAD. A first clad and a second clad are deposited onto the external surface of the core base material using OVD. In this way, a silica glass base material is fabricated. The silica glass base material is vitrified in the same manner as in SMP 1 to fabricate a transparent silica glass core base material. The transparent silica glass core base material is heated and elongated in such a manner that the outer diameter remains constant. In this way, a core base material 22 is fabricated. The core base material 22 is attached to a rotational axis 21 and rotated with respect to the core of the core base material 22 while silica glass soot containing F is sprayed onto the external surface of the core base material 22 from a burner 23 to deposit a first clad portion 24 made of silica glass. In this way, a first clad base material 25 is fabricated that has the core base material 22 and the first clad portion 24 integrated with each other (see FIG. 6 ). Furthermore, the first clad base material 25 is attached to a rotational axis and silica glass soot was sprayed onto the first clad base material 25 from a burner to deposit a porous silica glass clad portion. In this way, a porous base material is fabricated that has the first clad base material 25 and the silica glass clad portion integrated with each other. The porous base material is thermally treated at the temperature of 1500° C. within a chlorine-containing atmosphere for dehydration and vitrification. In this way, a transparent silica glass base material is fabricated. A manufacturing method involving spraying a gas containing fluorine may be a known method including, but not limited to, OVD, a plasma method or the like. In this embodiment, a conventional plasma apparatus is shown in FIG. 6 as an example. The method described in the above involves spraying silica glass soot containing fluorine from the burner 23 . It is also possible to use a method according to which a quartz tube doped with fluorine may be arranged so as to surround a core base material and the quartz tube and the core base material may be integrated with each other.
[0045] <Manufacturing of Optical Fiber>
[0046] The transparent silica glass base materials manufactured in SMP 1 and SMP 2 are spun into silica glass optical fibers SMF 1 and SMF 2 . The spinning is performed under such conditions that the temperature within the drawing furnace is set to 2000° C., the drawing speed is set to 1000 m/min, and the drawing tensile force is set to 250 g. The silica glass optical fibers have a diameter of 125 μm. Immediately after the spinning, the surfaces of the silica glass optical fibers were covered with ultraviolet curable acrylic resin. In this way, covered silica glass optical fibers having a diameter of 250 μm are fabricated.
[0047] <Deuterium Treatment of Optical Fiber>
[0048] Process 1
[0049] The silica glass optical fiber SMF 1 of 1.5 km is prepared and its attenuation is measured using the cutback technique. The result is shown as an initial attenuation spectrum 51 in FIGS. 7A and 7B . The fiber is left at room temperature for approximately one day within a nitrogen gas atmosphere containing deuterium of 5%. The total pressure of the atmosphere gas is set to approximately one atmospheric pressure. Accordingly, the partial pressure of the deuterium is approximately 5 kPa. After this, the fiber was left for approximately one day in the air. The attenuation of the fiber was measured, in total, two days after the timing before the deuterium treatment. The result is shown as a attenuation spectrum 52 .
[0050] As shown in FIG. 7A , the attenuation spectrum 51 indicates that the attenuation at the wavelength of 630 nm was 15.1 dB/km. FIG. 7B shows the attenuation spectrum within the full range of wavelengths at which the attenuation is measured. In FIG. 7B , peaks 53 and 54 are generated due to the change in the propagation wavelength range for the high-order modes before and after the measurement using the cutback technique, and not indicative of the intrinsic attenuation for the fundamental mode. According to the attenuation spectrum 51 shown in FIG. 7B , the values of the attenuation at the wavelengths of 750 nm, 1300 nm, and 1550 nm are respectively 3.8 dB/km, 0.35 dB/km, and 0.19 dB/km. Using these three values and least squares approximation, the variables A and B in Expression 5 are calculated. The results are A=1.23 and B=−0.05. Using these values of the variables A and B and Expression 5, the attenuation at the wavelength of 630 nm is extrapolated. The result is 7.7 dB/km. This clearly indicates that an absorption peak is present in the vicinity of 630 nm. It is known that such an absorption peak is caused by NBOHC defects. According to the attenuation spectrum 52 , on the other hand, the attenuation at the wavelength of 630 nm is 9.3 dB/km. This reveals that the deuterium treatment eliminates almost all of the NBOHC defects. Here, the attenuation in the vicinity of 1400 nm increases by approximately 0.1 dB/km. It should be noted that the wavelength of 700 nm or longer is desirably used for approximation curve calculation since the absorption peak in the vicinity of 630 nm continues up to the vicinity of 700 nm. On the other hand, the wavelength of 1600 nm or shorter is desirably used for approximation curve calculation since it is known that the infrared absorption loss of silica glass becomes significant in the long wavelength range over 1600 nm. The wavelength used for approximation curve calculation is desirably selected to avoid the peaks resulting from the high-order modes such as the peaks 53 , 54 in FIG. 7B .
[0051] After this, the same optical fiber is left in the air in a high-temperature atmosphere of 40° C. FIG. 8 shows the change, during this treatment, in attenuation over time at the wavelengths of 630 nm (the value of the attenuation is represented by the left vertical axis) and 1400 nm (the value of the attenuation is represented by the right vertical axis) was as shown in FIG. 8 . Note that the value of the attenuation at the wavelength of 630 nm is represented by the left vertical axis and the value of the attenuation at the wavelength of 1400 nm is represented by the right vertical axis. The attenuation at 1400 nm gradually decrease and, eight days later (one day of the deuterium treatment+one day of being left in the air+six days of the high-temperature treatment), the increase in attenuation at 1400 nm becomes 0.01 dB/km or less, which allows the optical fiber to practically serve as a low-attenuation optical fiber. For confirmation, the high-temperature treatment is continued and it is confirmed that the attenuation substantially returns to the level before the deuterium treatment twenty-one days later.
[0052] After this, the same fiber is cooled at a room temperature of 25° C. and then exposed to hydrogen. This hydrogen treatment is performed under conditions determined in accordance with the specifications of IEC60793-2B1.3. The hydrogen treatment is performed at room temperature within an hydrogen atmosphere with a partial pressure of 1 kPa. The attenuation at the wavelength of 1383 nm is measured. The result is 0.304 dB/km before the hydrogen treatment and 0.304 dB/km after the hydrogen treatment. In other words, the deuterium treatment has deactivated the NBOHC defects and the subsequent hydrogen treatment thus does not increase OH groups.
[0053] Process 2
[0054] The silica glass optical fiber SMF 2 of 10 km is prepared and left for 24 hours at a temperature of 47° C. within a vessel containing a nitrogen gas atmosphere containing deuterium of 1%. The total pressure of the atmosphere gas is set to approximately one atmospheric pressure. Accordingly, the partial pressure of the deuterium is approximately 1 kPa. The atmosphere within the vessel is replaced with a nitrogen gas atmosphere and the optical fiber is left in the vessel for four hours. After this, the optical fiber is removed from the vessel and left in the air to be subjected to high-temperature treatment of 85° C. for ten hours. After this, the temperature is lowered to a room temperature of 25° C.
[0055] The change in attenuation over time is shown in FIG. 9 . In FIG. 9 , the values of the attenuation at 630 nm are represented by the left vertical axis, and the values of the attenuation at 1383 nm and 1400 nm are represented by the right vertical axis. The attenuation at 630 nm is initially 15.8 dB/km, which is higher than the attenuation of a fiber of the same type without NBOHC defects, specifically speaking, 10 dB/km or less, by 5 to 6 dB/km. The attenuation at 630 nm decreases to 9.6 dB/km approximately 30 hours after the start of the deuterium treatment. This proves that the NBOHC defects are bonded with deuterium and thus deactivated. The values of the attenuation at 1383 nm and 1400 nm are respectively 0.297 dB/km and 0.274 dB/km when measured before the start of the deuterium treatment. The values of the attenuation at 1383 nm and 1400 nm respectively increase to 0.454 dB/km and 0.442 dB/km approximately concurrently with the decrease in attenuation at 630 nm. This indicates that POLs or any other types of defects react with the deuterium.
[0056] After this, the values of the attenuation at 1383 nm and 1400 nm rapidly decrease and respectively reach 0.300 dB/km and 0.278 dB/km when the high-temperature treatment ends and the cooling step starts approximately 38 hours after the start of the deuterium treatment. Furthermore, sufficiently cooling the optical fiber to a room temperature of 25° C. sufficiently reduces the stress caused by the thermal expansion of the finer wound around a bobbin. When measured approximately 50 hours later, the values of the attenuation at 1383 nm and 1400 nm are respectively 0.299 dB/km and 0.277 dB/km. Accordingly, the increases from the values measured before the treatment are reduced to 0.005 dB/km or less. As a consequence, fiber with excellent characteristics are obtained.
[0057] While the embodiments of the present invention have been described, the technical scope of the invention is not limited to the above described embodiments. It is apparent to persons skilled in the art that various alterations and improvements can be added to the above-described embodiments. It is also apparent from the scope of the claims that the embodiments added with such alterations or improvements can be included in the technical scope of the invention.
[0058] The operations, procedures, steps, and stages of each process performed by an apparatus, system, program, and method shown in the claims, embodiments, or diagrams can be performed in any order as long as the order is not indicated by “prior to,” “before,” or the like and as long as the output from a previous process is not used in a later process. Even if the process flow is described using phrases such as “first” or “next” in the claims, embodiments, or diagrams, it does not necessarily mean that the process must be performed in this order.
[0059] As made clear from the above, the embodiments of the present invention can be used to realize a method for manufacturing silica glass that can reduce the increase in absorption loss of a silica glass optical fiber in the vicinity of the wavelength of 1400 nm resulting from deuterium treatment and can achieve low attenuation in the wavelength range of 1300 nm to 1625 nm and to realize such an optical fiber.
|
A method for manufacturing deuterium-treated silica glass includes exposing silica glass to a deuterium-containing atmosphere for a predetermined period of time to diffuse deuterium molecules within the silica glass, maintaining the silica glass at 40° C. or higher, and cooling the silica glass to room temperature. The silica glass is a silica glass-based optical fiber having a core made of silica glass, where the core is positioned at a center of the optical fiber and contains at least germanium, and a clad made of silica glass, where the clad surrounds the core and has a lower refractive index than the core. A surface of the silica glass is covered with a resin coating.
| 2
|
This application claims the benefit of U.S Provisional Application No. 60/144,545, filed Jul. 16, 1999.
TECHNICAL FIELD
The present invention relates to directional drilling, particularly to a sonde housing structure for use with a directional drilling bit.
BACKGROUND OF THE INVENTION
Directional drilling is used for boring under or through obstructions such as roadways, concrete lined waterways and large underground utilities to provide a passageway for utility lines without the need for trenching through or excavating around the particular obstruction. This need has been met by the development of a variety of systems for the installation of underground conduits and pipe bursting/replacement systems.
Directional boring apparatus for making holes through soil are well known. The directional borer generally includes a series of drill rods joined end to end to form a drill string. The drill string is pushed though the soil by means of a powerful device such as a hydraulic cylinder. The drill string ends in a bit having a sloped front face that causes the bit and drill string to deviate in the direction of the sloped face in order to steer. The bit may be pushed and rotated and the same time in order to drill straight. See McDonald U.S. Pat. No. 4,694,913, issued Sep. 22, 1987. A spade, bit or head configured for boring is disposed at the end of the drill string and may include an ejection nozzle for water to assist in boring.
Accurate directional boring necessarily requires information regarding the orientation and depth of a cutting or boring tool. Consequently, a sensor and transmitting device (“sonde”) attached to the cutting tool is normally required to prevent mis-boring and re-boring. See, for example, Mercer U.S. Pat. Nos. 5,155,442 and 5,633,589. The sonde includes electronic and electromagnetic components that are sensitive to vibration and may fail if subjected to excessive vibrational shock in service. Since the sonde needs to be positioned adjacent to the cutting or boring head in a drill string in order to provide accurate information regarding the orientation of the cutting head, any vibrations or shock may result in premature failure of the sonde. Additionally, a sonde used in directional boring needs to be housed in a manner that facilitates easy access while simultaneously providing adequate protection to the device.
Sondes have been located inside of a bit assembly, such as shown in Stangl U.S. Pat. No. 4,907,658. More typically, however, the sonde is located in a tubular housing that can be connected and disconnected from the housing. The sonde itself is loaded into a compartment that is isolated from compressed fluid that is supplied to the bit through a separate passage in the sonde housing. See Wentworth PCT Publication No. WO 00/11303, published Mar. 2, 2000, and Cox U.S. Pat. Nos. 5,950,743, 5,934,391, 5,931,240 and 5,899,283 for side load sonde housings wherein a door or cover for the sonde compartment is provided.
End load sonde housings are also known wherein the sonde is loaded into a blind hole at the rear end of the sonde housing, which is then coupled to a trailing component such as a starter rod. A spacer is inserted behind the sonde to hold it in place. These designs avoid the possibility of breakage of a side load door, but replacing the sonde requires disassembly of drill head.
One known side loading sonde housing design is described in commonly-assigned U.S. Pat. No. 6,148,935 and U.S. Pat. No. 6,260,634, the entire contents of which are incorporated for all purposes by reference herein. These patents describes a coupling system known commercially as Splinelok™ wherein the starter rod is connected to the rear end of the sonde housing by a series of interlocking splines that pass torque from the drill string to the sonde housing and bit attached to the front end of the sonde housing.
All sonde housing designs must provide sufficient space for the sonde cavity and for a fluid passage to pass drilling fluid up to the bit, which fluid passage is isolated from the sonde compartment, while maximizing the strength of the housing. The sonde is either battery powered or connected to the surface by a wire which runs through the drill string (“wireline”).
A need persists for a sonde housing that provides for increased security and protection of the sonde while simultaneously affording convenient and rapid access to the sonde. The present invention provides an end load sonde housing system that is easier to access than known end load systems.
SUMMARY OF THE INVENTION
According to the invention, an apparatus for mounting an electronic device therein for use in an underground boring machine includes an elongated housing having an elongated, lengthwise central cavity opening at one end thereof. A cartridge containing a sonde fits in the cavity. A keying mechanism is provided on the cartridge and sonde, and also between the cartridge and the housing, for securing the cartridge and sonde in a predetermined orientation relative to the sonde housing when the cartridge is inserted into the cavity through the opening. The sonde housing also preferably includes a lengthwise fluid passage therein which is isolated from the cavity containing the cartridge. According to preferred forms of the invention, an end cap or plug is also provided which holds the sonde cartridge in its installed position and isolates it from contact with the pressure fluid in configurations where the fluid passage and cavity branch from a common end opening of the housing.
A drill head for use in directional drilling according to the invention includes an elongated housing having an elongated, lengthwise central sonde cavity opening at a front end thereof, a keying mechanism for securing the sonde in a predetermined orientation relative to the housing when the sonde is inserted into the cavity through the opening, a closure device for enclosing the cavity with the sonde therein, and a bit assembly mounted at the front end of the sonde housing, such that upon removal of the bit assembly, the cavity containing the sonde can be accessed. Preferably the sonde is contained within a cartridge as described below. A drill string may be directly connected to a rear end of sonde housing without need for an adapter or starter rod. Preferably fluid passages conduct a pressure fluid through the sonde housing to its front end to further fluid passages in the bit assembly. In this arrangement, the closure device comprises a cap which seals the cavity from the pressure fluid, whether or not the cap forms part of a cartridge for the sonde.
A sonde cartridge according to the invention comprises a tube sized to closely receive a cylindrical sonde therein, the tube having alignment openings therein whereby a pin can be used to secure the tube against movement relative to a sonde housing in which the cartridge is to be installed, an end cap which fits into one end of the tube, a keying device which can engage a notch in the sonde so that the sonde may be installed in a predetermined position within the cartridge, and a fastener for securing the end cap to the tube.
The present invention provides an improved end load sonde housing that is inherently stronger than conventional side load configurations and which provides a nonthreaded mechanism for indexing and maintaining the sonde in the proper clockwise position, thereby minimizing the possibility of misboring.
DESCRIPTION OF DRAWINGS
In the accompanying drawings:
FIG. 1 is a side view of the sonde housing according to the invention;
FIG. 2 is a rear end view of the housing shown in FIG. 1;
FIG. 3 is a lengthwise section taken along the line B—B in FIG. 2;
FIG. 4 is a rear perspective view of the sonde housing of FIG. 1;
FIG. 5 is a directional drill head using the sonde housing of the present invention;
FIG. 6 is a front view of the drill of FIG. 5;
FIG. 7 is a lengthwise section taken along the line A—A in FIG. 6;
FIG. 8 is a side view of a sonde cartridge according to the invention;
FIG. 9 is a front view of the cartridge of FIG. 8;
FIG. 10 is a rear (hook end) view of the cartridge of FIG. 8;
FIG. 11 is a lengthwise section taken along line C—C in FIG. 9;
FIG. 12 is a perspective view of the cartridge shown in FIG. 8;
FIGS. 13-17 are views comparable to FIGS. 8-12, with the cartridge outer tube removed for clarity;
FIG. 18 is an exploded view of the cartridge tube, sonde and cap assembly shown previously;
FIG. 19 is an exploded view of the cartridge, sonde housing and drill bit;
FIG. 20 is a side view of a directional drill employing a second embodiment of the invention wherein the sonde housing functions as a combination of sonde housing and starter rod and wherein the sonde is loaded into the housing from the front end;
FIG. 21 is top view of the directional drill of FIG. 20;
FIG. 22 is a lengthwise section taken along line A—A of FIG. 21;
FIG. 23 is a partial cross section taken along line D—D of FIG. 20;
FIG. 24 is a partial cross section taken along line B—B of FIG. 21;
FIG. 25 is a partial cross section taken along line C—C of FIG. 21;
FIG. 26 is a side view of a sonde cartridge in accordance with the second embodiment of the invention;
FIG. 27 is a top view of the sonde cartridge of FIG. 26;
FIG. 28 is a cross section taken along line B—B of FIG. 27;
FIG. 29 is a lengthwise section taken along line A—A of FIG. 27; and
FIG. 30 is a top view of the sonde housing with a threaded male adapter installed.
DETAILED DESCRIPTION
Referring now to the drawings wherein like reference numerals denote the same and similar parts throughout and in particular FIGS. 1-7, an improved sonde housing 12 according to the invention is illustrated. Sonde housing 12 comprises a generally cylindrical structure with a longitudinal central cavity and, as illustrated, includes joint ends 13 and 15 of non-threaded couplings suitable for coupling the housing to a drill string and mounting an appropriately designed boring bit 14 or other tool. In one embodiment, the sonde housing 12 is configured in accordance with Splinelok™ joint system described in the foregoing patent applications incorporated by reference herein. As set forth in detail below, the geometry of the sonde housing of the invention is especially suited to protecting the combination sensor and transmitting device that comprises a sonde and allowing for transmission of the information collected to the operator via electromagnetic waves or through a wireline.
Sonde 18 transmits radio signals defining the subterranean location of the drill head 14 to an operator and the orientation of the slanted front bit face used for steering. Sonde 18 typically transmits information regarding the position, depth, pitch of the axis relative to gravity and clock position of the apparatus. This information allows the operator to determine which direction bit 14 will go during a steering correction. In order to measure the clock position of bit 14 accurately, sonde 18 must be held in registry relative to particular features on the boring head or bit 14 .
Referring to FIGS. 1-7, sonde housing 12 includes an axially extending, rearwardly opening blind hole. This blind hole, henceforth referred to as the cartridge bore or cavity 22 , is configured to receive a sonde cartridge 20 (FIGS. 8-12) encapsulating sonde 18 . A cross-drilled hole 26 is positioned near the blind end 24 of the cartridge bore 22 . A spiral wound roll pin 30 (FIG. 7) is inserted into hole 26 . This transverse pin 30 serves to orient cartridge 20 when the cartridge is installed in the cartridge bore 22 . At the rear of the cartridge bore 22 , there is a profiled, rearwardly facing, generally annular depression 34 surrounding bore 22 . Depression 34 is shallow, for example ⅜ inch, and is designed to accept a flange 36 of a cap 38 , a component of cartridge 20 . Radial slots 40 extend through sonde housing 12 and into cartridge bore 22 . Slots 40 permit transmission of the sonde signal into the surrounding ground. Without slots 40 , the steel of the housing 12 would shield or block the signals. Alternatively, a wireline (not shown) could be utilized to transmit information. Sonde housing 12 also has an axial fluid passage 16 passing lengthwise through the housing 12 and bit 14 to conduct the drilling fluid around the sonde 18 . Fluid is injected through the drill string to a starter rod 56 and then into passage 16 to provide lubrication to the bit and to carry away debris generated during the drilling operation.
Referring now to FIGS. 8-19, cartridge 20 includes an outer tube 42 designed to provide a snug slip-fit over the sonde 18 . Preferably, tube 42 is formed from a material such as plastic which allows transmission of the radio signal. A U-shaped guide 44 is provided at front end 43 of tube 42 . Guide 44 includes a pair of relieved edges 48 that snap fit into corresponding lengthwise, opposed grooves 54 in tube 42 , securing the guide in the tube and providing for proper longitudinal and clockwise alignment of the cartridge 20 and sonde 18 within housing 12 . Guide 44 has a small, rearwardly extending tab 46 which fits in a corresponding notch in the end of the sonde 18 , thereby preventing rotation of sonde 18 within the cartridge 20 and keying the sonde to a predetermined position relative to cartridge 20 .
Upon installation, roll pin 30 passes through the middle of the “U” of guide 44 . A pair of opposed, frontwardly opening keyhole-shaped slots 50 at the front end 43 of the cartridge extend through the wall of tube 42 . Slots 50 snap over the transverse pin 30 described above, so that the rounded inner ends 52 of slot 50 engage the transverse pin. The mating of the keyhole shaped slots 50 and transverse pin 30 prevent rotation of the cartridge 20 (and therefore of sonde 18 ) within the cartridge bore 22 of housing 12 , maintaining the clockwise orientation of the cartridge within the bore.
After cartridge 20 is inserted into cartridge bore 22 , the cartridge is secured in the cartridge bore with an end cap 38 . Cap 38 may be formed from any appropriate material, such as steel, plastic or aluminum, so long as the cap 38 is capable of sealing the cartridge bore against the entry of high pressure (2000 psi) drilling mud or fluid and bearing the applied load of the fluid. As will be appreciated by reference to FIGS. 3 an 7 , drilling mud or fluid is present at the joint between the sonde housing 12 and the starter rod 56 as it moves from the drill string through the starter rod 56 and into a rear end opening 15 which is slightly larger in diameter than cavity 22 and configured to receive the projecting end of the starter rod therein.
As shown in FIG. 2, passage 16 and cavity 22 both branch from rear opening 15 . In this configuration, the high pressure drilling fluid present in the joint between starter rod 56 and sonde housing 20 will produce a load on the back of cartridge 20 . For example, at 2000 psi with a bore of 1.62 inches, the applied load will be approximately 4140 lbs. Cap 38 is provided with an annular flange or lip 36 that serves to bear the load upon the rearwardly facing depression 34 in housing 12 , protecting sonde 18 from the load. To further aid in protecting sonde 18 against the incursion of drilling fluid into cartridge bore 22 , cap 38 is provided with a series of annular grooves 35 along its midsection for mounting elastomeric O-rings 37 which further seal any gap between the cap and cartridge bore 22 . Additionally, a rubber nub 39 at the end of cap 38 remote from end flange 36 resiliently engages the rear end of sonde 18 .
As previously noted, sonde cartridge 20 receives guide 44 at a position predetermined by slots 54 , and guide 44 in turn is provided with indexing tab or key 46 to position sonde 18 in one orientation within the cartridge. In turn, cartridge 20 has keyhole slots 50 which engage transverse pin 30 to position the cartridge in one of two possible orientations, each 180° apart. However, this arrangement still allows the cartridge 20 and sonde 18 to possibly be inverted 180° upon installation in sonde housing 12 .
To prevent the cartridge and sonde from being installed in the inverted position, flange 36 of cap 38 is provided with an alignment feature. In the illustrated embodiment, the alignment feature comprises lateral wings or tabs 60 . Wings 60 fit only into a profiled portion 62 of recess 34 (FIGS. 3 and 6 ), thereby aligning cartridge 20 in the proper orientation relative to housing 12 . This feature provides the assembler with a means of avoiding a situation where the cartridge is accidentally inverted 180° degrees from the correct clockwise orientation during installation.
Cap 38 is secured to tube 42 by bolts 70 that are received in apertures 72 through the wall of plastic tube 42 and are tightened into threaded holes 73 against a counterbore 74 in cap 38 . The heads of bolts 70 function as shear pins to keep cap 38 aligned as well as providing a means to extract the outer tube 42 and sonde 18 from the cartridge bore 22 . A hook eye 76 on the outer surface of cap 38 provides means for pulling cartridge 20 out of housing bore 22 .
Referring now to FIGS. 20-30, a second embodiment of the sonde housing of the invention is illustrated. In this embodiment, a sonde housing 112 is adapted to be directly connected to the lead end of a drill string (not shown) thereby eliminating the necessity for a starter rod. The elimination of a separate starter rod provides for a simpler construction and assembly. Housing 112 includes a central cavity or bore 122 and, as illustrated incorporates a non-threaded joint 113 , such as the Splinelok™ joint for mounting a downhole tool, such as a bit assembly 114 . Bit assembly 114 , including an interchangeable bit 117 and a bit head 119 , is further described in commonly assigned U.S. patent application Ser. No. 09/393,778, filed Sep. 10, 1999, the contents of which are incorporated by reference herein.
Turning to FIGS. 20-25, the sonde housing 112 consists of a generally cylindrical body including a cartridge bore 122 extending rearwardly from a forward end 182 , the forward end 182 being adapted to receive a drill bit 114 or similar tool. As illustrated, sonde housing 112 is incorporates the Splinelok™ joint system described in pending U.S. patent application Ser. No. 09/212,042, filed Dec. 15, 1998, the disclosure of which is incorporated herein for all purposes. As shown in FIG. 30, a threaded adapter 100 may be mounted on sonde housing 112 upon removal of bit assembly 114 to provide for use of other bits or back reamers tools adapted for threaded connection.
Sonde housing 112 includes a threaded aperture 180 for receiving a male end of a leading drill rod (not shown) and a passageway 178 for a wireline in case where a wireline-type sonde is used. Passageway 178 is sealed by a plastic or rubber plug, not shown, prior to use to prevent pressure fluid from entering the sonde compartment. Such a plug is either completely solid, or else may be formed around the wire line. As shown in FIG. 24, housing 112 also include a pair of fluid passageways 116 that extend the length of the housing to allow flow of drilling fluid from the drill string through the housing to the bit assembly 114 . Cartridge bore 122 extends longitudinally along a portion of the length of housing 112 from the forward end of housing 112 . As illustrated, cartridge bore 122 terminates in a blind or, in the case of a wire-line type sonde, a semi-blind end 124 .
As best illustrated in FIGS. 20-22, 23 and 25 , bit assembly 114 is retained on the forward end of sonde housing with two pairs of solid steel anchor pins 184 that pass through apertures 188 in housing 112 . Anchor pins 184 pass through holes in the male end 186 of bit assembly 114 to secure the bit to the housing 112 . Anchor pins 184 are formed with a pair of rounded, circumferential grooves 187 that are spaced for alignment with a retainer hole 192 that passes through housing 112 and is substantially perpendicular to apertures 188 . Retainer holes 192 are aligned to intersect the grooves 187 of anchor pins 184 so that a retainer 190 inserted in retainer hole 192 fits into grooves 186 of anchor pins 184 , locking the anchor pins in position. Preferably, retainers 190 are roll pins, i.e. a flat sheet of steel rolled into a tube. Resilient engagement between retainers 190 and the walls of retainer holes 192 and/or interference with anchor pins 184 maintain retainers 190 in place upon installation. However, other engagement mechanisms between the bit assembly and sonde housing, such as the splined connections shown in the above-cited PCT publication, or even a threaded connection, may also be employed. A threaded connection is, however, more difficult to use and is not preferred. Similarly, bit assembly 114 may be replaced by the bit 14 discussed in connection with the first embodiment above.
Referring now to FIGS. 26-29, a sonde cartridge 120 for use in connection with the front loading sonde housing of the invention includes an outer plastic tube 142 and an end cap 138 generally similar to cap 38 and tube 42 discussed above. A retainer 130 such as a roll pin passes through tube 142 and a transverse hole in sleeve 147 adjacent to a rear end 143 of cartridge 120 to secure cartridge 120 in the sonde housing. Sleeve 147 may be formed from an elastomeric material to provide a resilient cushion for sonde 18 .
Cap 138 includes an annular flange 136 designed to fit into a shallow depression 134 (FIG. 22) formed at the forward end of cartridge bore 122 . Cap 138 also includes a key or tab 146 at its rear end that indexes against the notch in sonde 18 to position the sonde at the proper clockwise orientation within the tube 142 . Sonde housing 112 includes a cross-drilled hole 126 that passes through the housing and cartridge bore 122 . A transverse retainer, such as a roll pin 130 is inserted through the cross-drilled hole 126 .
Tube 142 includes an aperture 172 that extends through the wall of plastic tube 142 for receiving a bolts or screws 170 in order to secure cap 138 onto the tube. Bolt 170 is tightened into one or more holes 174 in cap 138 to secure the cap 138 and sonde 18 in cartridge 122 . The front end of cap 138 may include a recessed crossbar 135 that serves as a handle for pulling cartridge 120 from bore 122 . Flange 136 is provided with wings 160 that engage profiled recess 162 of cartridge bore 122 . As previously discussed, wings 160 in conjunction with profiled section 162 prevent the cartridge 120 from being accidentally inverted from the proper clockwise orientation when installed in cartridge bore 122 . Although guide 44 is absent in this embodiment, keying of the sonde position is still accomplished because the tab 146 and holes 174 are in a predetermined alignment, and a similar keyed connection is maintained between wings 160 and profiled recess 162 . Upon installation of cartridge 22 , keyholes grooves 150 fit over and stop against transverse pin 130 .
Fluid passages 116 terminate at a rear end opening 201 in the bit assembly, which communicates with fluid channels 216 in the bit assembly. The arrangement of the first embodiment is thus reversed, with cap 138 performing the same functions but now facing frontwardly at the joint between the bit assembly and the sonde housing. As such, upon removal of the bit, which occurs frequently, this embodiment of the invention allows ready access to the sonde and the same time.
As will be appreciated by those skilled in the art the sonde housing of the invention provides for securing a sonde in an indexed position with a combination of orienting features that require the installation of the sonde in the proper orientation. Furthermore, as opposed to other end load design, the sonde housing described herein, in combination with the Splinelok™ joint maintains a bit or tool in a known clockwise orientation with the sonde. Thus, as opposed to designs that utilize thread-on type tool joints, the orientation of the tool relative to the sonde is not dependent upon the orientation of a threaded tool connection. This feature represents a substantial advantage over prior art designs that are susceptible to mis-orientation due to the use of a threaded tool connection.
Additionally, the sonde housing described above provides proper sonde orientation in an end loading housing that structurally superior to side load configurations that by design weaken the torsional and bending strength of a housing, require complicated closure mechanisms, and/or are more likely to fail.
While certain embodiments of the invention have been illustrated for the purposes of this disclosure, numerous changes in the method and apparatus of the invention presented herein may be made by those skilled in the art, such changes being embodied within the scope and spirit of the present invention as defined in the appended claims.
|
An apparatus for mounting an electronic device therein for use in an underground boring machine includes an elongated housing having an elongated, lengthwise central cavity opening at one end thereof, a cartridge containing a sonde therein, which cartridge fits in the cavity; and a keying mechanism for securing the cartridge and sonde in a predetermined orientation relative to the housing when the cartridge is inserted into the cavity through the opening. One or more lengthwise fluid passages isolated from the cavity extend through the housing. A sonde housing of the invention may be used with a drill string and bit assembly in directional boring.
| 4
|
BACKGROUND
[0001] 1. Technical Field
[0002] This invention relates to compositions and methods for prevention and treatment of obesity and obesity related metabolic syndrome using microorganisms.
[0003] 2. Description of Related Art
[0004] Obesity is an epidemic, stigmatized, and costly disease that is rarely curable and is increasing in prevalence in most of the world. It poses a major risk for various serious chronic diseases. Excess weight poses major risks for a number of serious metabolic diseases, such as hypertension, type II diabetes, dyslipidemia, arteriosclerosis, ischemic heart disease, fatty liver disease, gallstones, osteoarthritis, reproductive and gastrointestinal cancers, and sleep apnea. The main prescription products currently approved for obesity are sibutramine (Abbott's Meridia®) and Orlistat™ (Roche's Xenical™). Sibutramine inhibits the re-uptake of noradrenaline and serotonin, controlling appetite and therefore decreasing food intake. Sibutramine, however, has well known side effects associated with sympathomimetic properties, affecting heart rate and blood pressure. In contrast to sibutramine, Orlistat™ acts locally. Orlistat™ is a gastric and pancreatic lipase inhibitor that prevents fat hydrolysis, thus reduces dietary fat absorption by approximately 30%. However, undigested fat along the gastrointestinal tract causes side effects, which is not only uncomfortable but also socially unacceptable. Therefore, a new type of anti-obesity treatment needs to be actively sought because the current pharmaceutical drugs are not ideal for the treatment of obesity.
REFERENCES CITED
[0000]
1. B. S. Drew, A. F. Dixon, J. B. Dixon, Vasc. Health Risk Manag. 3, 817 (2007)
2. P. G. Kopelman, Nature 404, 635 (2000)
3. Must et al., J. Am. Med. Assoc. 282, 1523 (1999)
4. R. Padwal, S K Li, D C Lau, Cochrane DatabaseSyst. Rev. 3, CD004094 (2003)
5. R. S. Padwal, S. R. Majumdar, Lancet 369, 71 (2007)
6. J. Rolls, D. J. Shide, M. L. Thorwart, J. S. Ulbrecht, Obes. Res. 6, 1 (1998)
7. G. A. Bray et al., Obes. Res. 7, 189 (1999)
8. R. Guercolini, Int. J. Obes. Relat. Metab. Disord. 21, S12 (1997)
9. J. B. Hauptman, F. S. Jeunet, D. Hartmann, Am. J. Clin. Nutr. 55, 309S(1992)
10. J. O. Hill, et al., Am. J. Clin. Nutr. 69, 1108 (1999)
11. R. E. Ley, P. J. Turnbaugh, S. Klein, J. I. Gordon, Nature 444, 1022 (2006)
12. P. J. Turnbaugh, R. E. Ley, M. A. Mahowald, V. Magrini, E. R. Mardis, J. I. Gordon, Nature 444, 1027 (2006)
13. P. J. Turnbaugh, F. Backhed, L. Fulton, J. I. Gordon, Cell Host Microbe 3, 213 (2008)
14. W. H. Lin, C. F. Hwang, et al., Food Microb. 23, 74 (2006)
15. Appl Environ Microbiol. 59, 15 (1993)
16. R. Leenen et al., Am. J. Physiol. 263, E913 (1992)
17. Y. Keno et al., Int. J. Obes. 15, 205 (1991)
18. Molavi, N. Rasouli, P. A. Kern, Curr. Opin. Cardiol. 21, 479 (2006).
19. R. T. Spiotta, G. B. Luma, Am. Fam. Physician 78, 1052 (2008)
20. S. Rand, J. ChronicDis. 40, 911 (1987)
21. National Heart Lung and Blood Institute, Obes. Res. 6; 51S(1998)
22. J. O. Hill, Endocr. Rev. 27, 750 (2006)23. C. Thompson-Chagoyon, J. Maldonado, A. Gil, Dig. Dis. Sci. 52, 2069 (2007)
23. C. Thompson-Chagoyon, J. Maldonado, A. Gil, Dig. Dis. Sci. 52, 2069 (2007)
24. B. Stecher, W. D. Hardt, Trends. Microbiol. 16, 107 (2008)
25. Isolauri, M. Kalliomaki, K. Laitinen, S. Salminen, Curr Pharm Des. 14, 1368 (2008)
26. W. Jia, H. Li, L. Zao, J. K. Nicholson, Nature Rev. Drug Disc. 7, 123 (2008)
SUMMARY OF THE INVENTION
Technical Problem
[0031] Recent evidence showed that gut microbiota plays an intricate role in the regulation of body weight (11-13). The transplantation experiments of the microbiota from obese and lean mice into microbe-free mice also proved that the compositional change of microbiota in the gastrointestinal (GI) tract resulted in differences in the efficiency of caloric extraction from food, eventually contributing to differential body weights (12, 13). These results suggest that small changes in caloric extraction in the GI tract by xenobiotically manipulated intestinal bacteria can lead to a meaningful reduction in body weight. Given that fat is degraded as fatty acid (FA) before absorption into body, removal of FA in the GI tract by the transplantation of a FA-extracting bacterium might be an idea for decreasing fat uptake by host body to treat obesity. In fact, reduction of dietary fat uptake in body by removing available FA is a better choice than by inhibiting fat hydrolysis that result in unavoidable undigested fat problem.
[0032] It's an object of the present invention to provide prevention or treatment of obesity and obesity related metabolic syndrome using microorganisms. Particularly, this invention provides a method and pharmaceutical compositions for reducing the dietary intake of fat by removing fatty acids for absorption. It is another object of the present invention to provide pharmaceutical compositions for obesity without side effects, unlike current pharmaceutical drugs, sibutramine and Orlistat™.
Technical Solution
[0033] In this invention, a probiotic strain, Lactobacillus acidophilus , was mutagenized to isolate a mutant that has enhanced capacity for FA removal. Administration of this fatty acid robbing microbe, FARM, to rats resulted in weight loss that was equal to that caused by the most popular anti-obesity pharmaceutical, Orlistat™. Therefore, this invention provides a method to reduce FA absorption in the GI tract by administration of probiotic strain with enhanced capacity for FA absorption and thus its removal from the GI tract of the host. This invention provides a microbial drug for obesity.
[0034] Based on experimental data, this invention provides a pharmaceutical composition for prevention or treatment of obesity and obesity related metabolic syndrome, comprising microorganisms which can colonize and extract free fatty acids in the gastrointestinal tract of mammals. Preferably, the microorganisms are from gut microbiota or derived from gut microbiota. More preferably, the micoorganisms are probiotic strains.
[0035] In the examples of this invention, Lactobacillus acidophilus FARM 1 KCTC 11513BP, Lactobacillus acidophilus FARM2 KCTC 11514BP, Lactobacillus acidophilus FARM3 KCTC 11515BP are obtained from a commercial probiotic strain, Lactobacillus acidophilus , by improving its capability of FA absorption.
[0036] This invention provides FARM which can colonize in the GI tract and has enhanced FA absorption capacity as active ingredient of dietary supplement for prevention or treatment of obesity and obesity related metabolic syndrome.
[0037] In this invention, the term “dietary supplement” is intended to mean any food with specific health function in addition to its nutrient function, including nutraceuticals, functional food, designer food, health food. The purpose of a dietary supplement according to an aspect of the present invention is in preventing or treating obesity and obesity related metabolic syndrome.
[0038] This invention also provides FARM which can colonize in the GI tract and has enhanced FA absorption capacity, Lactobacillus acidophilus FARM 1 KCTC 11513BP, Lactobacillus acidophilus FARM2 KCTC 11514BP, Lactobacillus acidophilus FARM3 KCTC 11515BP.
[0039] This invention also provides a method for treating obesity and obesity related metabolic syndrome by administration of FARM which can colonize in the GI tract and has enhanced FA absorption capacity. This invention provides an effective method for obesity and obesity related metabolic syndrome by reducing dietary energy intake after administration of FARM.
Advantageous Effects
[0040] Extra caloric intake from dietary fat is the most important determinant of obesity as it can be observed from rapid increases in underdeveloped countries. For the vast majority of humans, even caloric intake exceeding 1% more than caloric expenditure results in the accumulation of body fat, thereby leads to obesity.
[0041] This invention demonstrated that transplantation of xenobiotically manipulated Lactobacillus , FARM, actively extract FA in the GI tract to limit caloric intake by host, which showed anti-obesity effect as much as the most popular anti-obesity pharmaceutical drug, Orlistat™. Moreover, FARM as an anti-obesity drug has obvious advantages over the current pharmaceuticals for obesity. First, it does not act on the brain, but acts peripherally and, therefore, has a superior risk-benefit profile to centrally acting drugs, such as sibutramine. Second, FARM does not act on lipid hydrolysis that causes the unavoidable side effect of the GI tract such as anal leakage and oily spotting. Third, FARM is a Lactobacillus strain which is a beneficial probiotic and conveys considerable safety as a drug candidate.
[0042] Since gut microbiota is associated with various complex diseases such as infectious disease, obesity, cancer, allergic diseases etc., the transplantation of living intestinal bacteria xenobiotically modified into a host has strong potential to treat the various microbiota-related diseases. The present invention also proved the hypothesis that the transplantation of specifically manipulated intestinal bacteria can successfully change microbial flora in the GI tract to treat the diseases of a host.
BRIEF DESCRIPTION OF THE DRAWINGS
[0043] FIG. 1 . is a graph illustrating Fatty acid extraction capability of FARM Lactobacillus in accordance with an exemplary aspect of the present invention;
[0044] FIG. 2 . is a graph illustrating the change of the caloric intake by host colonized with FARM Lactobacillus in accordance with an exemplary aspect of the present invention;
[0045] FIG. 3 . is a graph illustrating the change in body weight of host colonized with FARM Lactobacillus in accordance with an exemplary aspect of the present invention;
[0046] FIG. 4 . shows visceral fat analysis of the host colonized with FARM Lactobacillus measured using MRI and analyzed with an image analysis program (Image J, USA) in accordance with an exemplary aspect of the present invention;
[0047] FIG. 5 . shows MRI images of the visceral fat accumulation of the rats fed high fat diet only and with FARM daily after 22 weeks in accordance with an exemplary aspect of the present invention;
[0048] FIG. 6 . shows a change of plasma lipid profiles in rats in accordance with an exemplary aspect of the present invention. (TG, as in triglycerides; TC, as in total cholesterol; HDL, as in high-density lipoprotein cholesterol; LDL, as in low-density lipoprotein cholesterol);
[0049] FIG. 7 . shows a change of plasma insulin and leptin concentrations in rats in accordance with an exemplary aspect of the present invention;
[0050] FIG. 8 . shows a change of blood glucose concentrations in rats in accordance with an exemplary aspect of the present invention;
[0051] FIG. 9 . illustrates the comparison of in vitro FA absorption capacity of FARM Lactobacillus in accordance with an exemplary aspect of the present invention; and
[0052] FIG. 10 . illustrates the reduction of caloric intake by FARM Lactobacillus or Orlistatin accordance with an exemplary aspect of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Best Mode
[0053] FARM Strain with Enhanced FA Absorption Capacity
[0054] A commercial probiotic strain, Lactobacillus acidophilus KCTC 3179 was mutagenized by N-methyl-N-nitro-N-nitrosoguanidine (NTG) to isolate mutants that has the increased capability of FA absorption. We initially isolated a mutant absorbing/robbing free fatty acid 2.1 times more from its surrounding environment than the wild type strain. The identified mutant, fatty acid robbing microbe 1 (FARM1) was deposited at Korean Collection for Type Cultures, Korea Research Institute of Bioscience and Biotechnology (KRIBB), 111 Gwahangno, Yuseong-gu, Daejeon 305-806, Republic of Korea, on May 19, 2009 under accession number KCTC 11513BP. FARM1 was again mutagenized by 4-nitroquinoline 1-oxide (4NQO) to isolate a mutant, FARM2, with more improved extraction of free FA. FARM2 was deposited at Korean Collection for Type Cultures, Korea Research Institute of Bioscience and Biotechnology (KRIBB), 111 Gwahangno, Yuseong-gu, Daejeon 305-806, Republic of Korea, on May 19, 2009 under accession number KCTC 11514BP. The mutagenesis yield the FARM2 mutant that absorbed 14 C labeled palmitic acid up to 3.1 times more than the wild type strain. With the identified FARM strains, the abilities of acidification during its growth and colonization in host gastrointestinal tract after consumption were examined since these are the most important characteristics of edible Lactobacillus . Both mutants, FARM1 and FARM2, maintained normal growth and acidification activity during yogurt fermentation. The mutant strains also colonized successfully the GI tract of rats after administration of the mutants as a yogurt form. These results indicate that both FARM1 and FARM2 functions as a normal Lactobacillus except their capability of enhanced FA extraction.
[0000] Reduction of Caloric Intake by Host that was Colonized with FARMs which Extract Free FA in GI Tract
[0055] Intestinal bacteria with an enhanced capacity for FA extraction could colonize the small intestine, where most FAs are absorbed into the body. The FARM could actively absorbs FAs in the small intestine and function as a bio-sequestrant, resulting in the removal of FAs that are available for absorption by the host's body. Subsequently, the FAs sequestered by the fast FA-extracting bacteria would be gradually transferred to the large intestine for fecal excretion, thereby reducing caloric extraction by the host.
[0056] To test whether FARMs actually extract fatty acid in the GI tract of a host to reduce caloric extraction by a host body, we fed the FARM-fermented yogurts into rats for 8 weeks to colonize the GI tract of the rats. After colonizing the GI tract of rats with FARMs and normal Lactobacillus, 14 C labeled triolein was orally administrated to rats to assess FA absorption in the rats by measuring radioactivity of FA, the digested product of 14 C labeled triolein, in their blood. The rats colonized with FARMs showed higher capability of FA extraction from its surrounding environment while it showed less FA uptake capability by their body in a dose dependant manner. The rats colonized with FARM1 and FARM2 reduced FA absorption up to 35% and 47%, respectively, compared to rats colonized with wild-type Lactobacillus . This result implies that both FARM1 and FARM2 successfully extracted absorbable FA in the GI tract of the rats, thereby reducing caloric extraction by host body.
The Effect of Caloric Extraction by FARMs in the GI Tract on Obesity
[0057] The effect of caloric extraction by FARMs in the GI tract on obesity was evaluated by feeding yogurt fermented with FARMs to male rats for 22 weeks while inducing obesity by diet. Daily administration of 3 ml of yogurt containing about 10 9 CFU per ml of either wild-type L. acidophilus or FARMs, resulted in the successful colonization in the GI tract of the rats after 4 weeks. As expected, colonization of FARM1 and FARM2 in the rats reduced body weight gain up to 15% and 19%, each, compared to the rats colonized with 3179 strain.
[0058] Extra-caloric intake in mammals mainly accumulates as visceral fat so that the visceral fat is correlated with whole-body weight. In this work, we measured the visceral fat area using open-type 0.3 Tesla MRI at the end of feeding experiments. The visceral fat contents of the control rats without feeding any Lactobacillus and rats colonized with wild-type L. acidophilus , FARM1 or FARM2 were 27%, 24%, 14%, and 13%, respectively. These results clearly showed that colonization of the GI tract of rats with FARMs reduced both body weight gain and visceral fat accumulation, indicating that FARMs actually absorb FA in the GI tract of host. Consequently, it reduce FA intake by host, thereby reducing visceral fat accumulation and body weight gain.
Analysis of the Biochemical Parameters of Serum Relating to Metabolic Syndrome
[0059] Since obesity is associated with metabolic syndrome such as insulin resistance, glucose tolerance, dyslipidemia, coronary artery disease, etc., the biochemical parameters of serum relating to metabolic syndrome were analyzed at the end of feeding experiments. The levels of TG, TC and LDL-cholesterol in the control rats without feeding any Lactobacillus and rat colonized with wild-type L. acidophilus 3179, were higher than those in FARM1 and FARM2 groups while HDL-cholesterol levels were reversed, low in the control groups but high in the FARM groups. FARM strains also showed an anti-diabetic effect as expected from their anti-obesity effect. Feeding FARM1 and FARM2 significantly reduced the serum insulin levels about 23% and 30%, respectively, compared to the untreated control. Also, FARM1 and FARM2 significantly reduced the average serum leptin levels to 20% and 45%, respectively, compared to the untreated control. The serum glucose levels were slightly lower in FARM1 and FARM2 group (107.6 mg/dl and 108.4 mg/dl), compared to untreated and 3179 control (122.1 mg/dl and 123.4 mg/dl). As a body gains weight, the body is known to become less sensitive to leptin and insulin as well as have a worsening plasma lipid profile, which leads to increased plasma concentrations of leptin, insulin, glucose, LDL cholesterol and total cholesterol. Our results showed that FARMs is effective in inhibiting insensitivity of insulin and leptin and improving the blood lipid profile by inhibiting the gain of body weight. The biochemical analyses on rat serums solidify the potential of FARM as an effective treatment for obesity.
The Possibility to Use FARM as a Living Anti-Obesity Drug
[0060] Because the mice colonized with FARMs showed reduction in FA absorption by a host to eventually inhibit body weight gain and visceral fat accumulation, we explored the possibility to use FARM as a living anti-obesity drug for diet-induced obesity after further improvement of free FA absorption capability of FARM. FARM2 went through 3 rd round mutagenesis with EMS to generate Lactobacillus with better fatty acid extraction capability. We were able to isolate a mutant, FARM3 that extracts free fatty acid 5 times faster than the wild type strain. FARM3 was deposited at Korean Collection for Type Cultures, Korea Research Institute of Bioscience and Biotechnology (KRIBB), 111 Gwahangno, Yuseong-gu, Daejeon 305-806, Republic of Korea, on May 19, 2009 under accession number KCTC 11515BP.
[0061] Daily administration of 3 ml of the yogurt fermented with FARM3 to male SD rats for 4 weeks resulted in reduction of body weight about 18%, compared to the wild-type Lactobacillus 3179 feeding group. The degree of body weight reduction by FARM3 were basically similar to those of the rat to which pharmaceutically effective dose of Orlistat™ was administered. Other than effective reduction of body weight, FARM3-feeding rats did not produce oily feces unlike Orlistat™ feeding group. These results implicate that FARM3 can be used as a living anti-obesity drug that is not only safe but also effective as much as pharmaceutical drugs.
[0062] The technological aspect of this invention is not limited to FARM or probiotics. It is clear to anybody with general knowledge that the technological aspect of this invention can be applied to any microbes which can colonize GI tract of mammals, especially human and contribute to the reduction in intake of dietary fat.
EXAMPLES
[0063] The present invention may be better understood with reference to the accompanying examples that are intended for purposes of illustration only and should not be construed to limit the scope of the invention, as defined by the claims appended hereto.
Reagents
[0064] Reagents were from Sigma™ except: [1-14C]-palmitic acid (PerkinElmer™ Life Sciences), liquid scintillation cocktail (LSC, PerkinElmer™ Life Sciences), [carboxyl-14C]-triolein (Research Products International™), Man-Rogosa-Sharpe (MRS, Difco), Orlistat™ (Xenical™, Roche). The sterilizable 384-well plate and 384-pin replicator were from Nunc™. Membrane semi-dry system was from Bio-Rad™. X-ray film was from Kodak™. Gel-Pro™ analyzer software was from Media Cybernetics™. L. acidophilus KCTC3179 is a human-derived Lactobacillus strain from the Korea Collection for Type Cultures (KCTC). Anaerobic culture was carried out in an anaerobic jar (BBL Gas-Pack anaerobic systems). Male Sprague-Dawley (SD) rats were obtained from Dae Han Biolink™ Co., Ltd. MRI images were obtained with a Bruker Biospec™ 47/40 4.7-Tesla instrument (Bruker) and analyzed with Image J (NIH). Serum was analyzed with a Rat/Mouse ELISA kit (LINCO™ research), a Leptin ELISA kit (R&D Systems™), a blood glucose meter (Accu-Chek™), and cholesterol ELISA kits (Asan™ Pharm. Co), respectively.
[0000] Obtaining FARM from Mutagenesis
[0065] Lactobacillus KCTC3179 cells were grown statically in MRS medium, pH 7.2, at 37° C. in a BBL Gas-Pack for anaerobic culture in this experiment, otherwise noted. Chemical mutagenesis of Lactobacillus KCTC3179 was performed as described below to obtain a FARM1 mutant. After 24 h culture of Lactobacillus KCTC317.9, the N-methyl-N-nitro-N-nitrosoguanidine (NTG) was added to a final concentration of 2 mg/ml into the MRS broth containing KCTC 3179 cells. After shaking at 25° C. for 30 min, Lactobacillus were washed three times with fresh MRS broth and resuspended in the fresh MRS broth. After serial dilution, the treated cells were spread on MRS agar plate and incubated at 37° C. under anaerobic conditions. After 48 h, the mutant colonies were transferred into a separate well of 384-well plate containing 50 μl of MRS broth. The inoculated colonies were cultured under anaerobic condition at 37° C. without shaking. After overnight incubation, plate was replicated using a 384-pin replicator into two new plates, one with fresh MRS broth and another with the same broth containing 0.1 nCi/ml of 14 C-palmitic acid. Then, plates were wrapped with parafilm and incubated at 37° C. for 30 min with gentle shaking. After incubation, 2 μl of the 14 C-labeled culture in each well was transferred with a 384-pin replicator onto nylon membrane. After drying the membrane with the semi-dry system, the free 14 C-palmitic acid in the bacterial spots on the membrane was removed by washing with MRS broth for three times. The washed membrane was exposed to X-ray film at −80° C. for 3 days. After development, the X-ray film was scanned and the relative dot density was analyzed with Gel-Pro™ analyzer software. High dot density colonies were selected and the strain with the most fatty acid extracting/robbing capability was identified and named as fatty acid robbing microbe 1 (FARM1). After obtaining FARM1 from NTG mutagenesis, 4-nitroquinoline 1-oxide (4NQO) was treated to FARM1 for generation of 2nd-round mutant FARM2 and ethylmethane sulphonate (EMS) was treated to FARM2 to generate 3rd-round mutant FARM3, respectively.
Evaluation of In Vitro Fatty Acid Extraction Capability
[0066] To evaluate the in vitro fatty acid extraction capability of identified strain, the radioactivity of Lactobacillus was measured after in vitro incubation with 14 C labeled palmitic acid. First, L. acidophilus or identified FARM strains were inoculated into 2 ml of MRS broth and incubated. At the end of the exponential growth phase, the cell density was estimated again by measuring the absorbance at 600 nm. The cells were harvested by centrifugation and resuspended into fresh MRS broth containing 1 nCi/ml of 14 C-palmitic acid. After an additional incubation for 1 h at 37° C., the 14 C-labeled cells were washed 3 times with MRS broth. After resuspension in 1 ml of fresh MRS broth, 200 μl of the cell suspension were carefully transferred into a 4 ml scintillation vial containing 2 ml of liquid scintillation cocktail. The mixture was vigorously vortexed for 1 min and then the 14 C activity was determined by a liquid scintillation spectrophotometry.
Evaluation of Acid Production Ability
[0067] For testing acid production, the L. acidophilus was cultured at 37° C. in MRS broth until the end of the exponential growth phase. One ml of cell culture was inoculated into a bottle containing 100 ml of sterile reconstituted skim milk (10%) and glucose (2%). The pH changes of yogurt were determined after incubation for 24 h, 48 h and 72 h, respectively. For cell growth measurement, 5 ml of the resultant yogurt after 48 h culture was transferred to a 15 ml conical tube and vortexed vigorously. Then, 1 ml of the homogenized sample was serially diluted with sterile PBS and 50 μl from each dilution was plated on a MRS plate. The plates were cultured under anaerobic conditions for 48 h to count the visible colonies.
Animal Experiment
[0068] All procedures performed with animals were in accordance with established guidelines and were reviewed and approved by the Institutional Animal Care and Use Committee. Male SD rats with body weight ranged at 200-220 g were housed two in each cage and provided normal rat food and water ad libitum during the first week. All animals were kept under 12-h light and dark cycle until the end of the experiment. The temperature was kept constant at 22±1° C. and the humidity was 40-50%. After 1 wk of familiarization in this environment, the rats were randomly divided into control or experimental groups (n=14 per group): control group (high fat diet only), 3179 group (high fat diet with yogurt fermented by L. acidophilus KCTC3179 strain), FARM group (high fat diet with yogurt fermented by FARM mutant, respectively). The high fat diet used in this study was made with standard rat food (complex-carbohydrate 60%, protein 22%, fat 3.5%, fiber 5%, crude ash 8%, calcium 0.6%, and phosphorus 1.2%) plus 20% pig lard. The composition of the high fat diet is as follows; complex-carbohydrate 48%, protein 17.6%, fat 22.8%, fiber 4%, crude ash 6.4%, calcium 0.48%, and phosphorus 0.96%. The yogurt for feeding was fermented with 10% non-fat milk, 2% sugar, and 1% of L. acidophilus culture at a concentration of ≧10 9 /ml. Through experiment periods, rats had free access to each diet while 3 ml of fermented yogurt was administered orally for the purpose of each experiment. Body weight was measured every week between 9 and 10 A.M after 12 h fasting.
1. Gastrointestinal Tract Colonization Ability
[0069] After 8 weeks of L. acidophilus feeding for colonization, four rats of each control or experimental group were randomly selected and killed under anesthesia with ether. The gastrointestinal organs including stomach and small intestine from rats were collected immediately and weighted. Samples were transferred into 50 ml conical tubes and diluted with sterile saline to give a 10-fold dilution (wt/vol). Then, samples in saline were homogenized with a homogenizer to release the content of gastrointestinal organs. After serial dilution, the homogenates were plated on a lactobacillus selective agar plates and incubated anaerobically for 48 h. The numbers of viable lactobacilli were assessed by counting the colonies formed in the selected plates and expressed as log 10 CFU per gram (wet weight) of various regions of the gastrointestinal organs.
2. In Vivo Effect of Farms on the Induction of the Diet-Induced Obesity
[0070] The long-chain triglyceride, triolein, was used as the substrate in this experiment. [ 14 C] labeled triolein in benzene solution was kept at −70° C. until the day before use. About 1 μCi of [ 14 C] labeled triolein was added per ml of unlabeled triolein and the solvent was evaporated at RT under nitrogen for overnight. The triolein mixture was administered in an amount of 0.5 mmol/100 g of body weight to the animals after feeding Lactobacillus for 22 weeks. After oral administration, blood samples were collected by cardiac puncture at 120 min, 240 min, 360 min, 480 min and 600 min, respectively. 0.1 ml of each serum sample was mixed immediately with 1.8 ml of LSC and the 14 C activity was determined by a liquid scintillation spectrophotometry. In vivo effect of FARMs on the induction of the diet-induced obesity was investigated by measuring in vivo fatty acid absorption abilities of FARMs after feeding yogurt fermented with Lactobacillus.
3. MRI Analysis of the Visceral Fat Content
[0071] Magnetic resonance imaging (MRI) analysis was performed to measure the abdominal subcutaneous and visceral fat with a Bruker Biospec™ 47/40 4.7-Tesla instrument. Rats were anesthetized with a combination of Zoletil™ (25 mg/kg) and Rompun™ (10 mg/kg). To obtain images, the rats were placed prone position in the magnet. MRIs were recorded using the body coil as the transmitter and receiver. A series of T1-weighted transaxial scans for the measurement of intra-abdominal and subcutaneous fat were acquired from a region extending from 8 cm above to 8 cm below the 4th and 5th lumbar interspace. Intra-abdominal and subcutaneous fat areas were measured using an Image J program.
4. Serum Biochemical Analysis
[0072] Blood samples of experiment rats were collected at the beginning and at 22-wks to determine the serum biochemical values. All animals were fasted overnight prior to blood collection. The whole blood samples of the rats were collected by cardiac puncture under anesthesia with aether. After centrifugation at 2,000×g for 10 min at 4° C., serum samples were aliquoted and stored at −70° C. until analysis. Serum was analyzed for biochemical characteristics with available kits, such as insulin (Rat/Mouse ELISA kit), leptin (Leptin ELISA kit) and serum glucose levels (blood glucose meter). Serum total cholesterol, HDL-cholesterol, LDL-cholesterol, and triglyceride concentration was detected with ELISA kits.
5. Effect of FARM3 on Diet-Induced Obesity
[0073] The 3 month old male SD rats were given high-fat feed (described above) for 8 weeks to develop diet-induced obesity with average body weight of 425 g. The rats were randomly divided into groups (n=14 per group) and received fermented yogurt or drug under continued high-fat diet conditions: 3179 group (high fat diet with yogurt fermented by L. acidophilus KCTC 3179 strain), FARM3 group (high fat diet with yogurt fermented by FARM3 mutant), Orlistat™ (high fat diet with Xenical™ in an amount of 200 mg/kg diet).
6. Statistical Analysis
[0074] All data were expressed as mean±standard deviation. Statistical comparisons were performed by analysis of variance (ANOVA) test. A value of P<0.05 was considered statistically significant.
Results
1. Different Fatty Acid Extraction Capabilities of Farms and Reduction of Caloric Intake
[0075] FIG. 1 shows the different fatty acid extraction capabilities of FARMs from their surrounding environment.
[0076] Fatty acid extraction capability of FARMs was inversely related to caloric intake by host in which its GI tract was colonized with FARMs. Lactobacillus acidophilus KCTC 3179 (labeled as “3179”) were mutagenized with N-methyl-N-nitro-N-nitrosoguanidine (NTG) to generate FARM1 having increased fatty acid extraction capability. FARM1 was again mutagenized with 4-nitroquinoline 1-oxide (4NQO) to generate FARM2 having better FA extraction capability. FA extraction capabilities of FARMs were determined by measuring the radioactivity in Lactobacilli using liquid scintillation spectroscopy after incubation of Lactobacilli with 1 nCi/ml of 14 C labeled palmitic acid for 1 hour. Values are mean CPM±standard deviation (n=4).
[0077] FIG. 2 shows the reduction of caloric intake in host that was colonized with FARMs. The GI tracts of the SD rats were colonized for 8 weeks with either FARMs or L. acidophilus KCTC 3179. After administration of 14 C-labeled triolein into the rats colonized with different Lactobacilli (FARM1, FARM2, KCTC 3179) and rats without feeding of Lactobacillus (control), blood samples were collected for the analysis of radioactivity to determine the relative caloric intake by host.
[0078] The FA extraction capability of FARM is inversely correlated to the absorption of FA by host.
2. Acid Production Ability
[0079] Each of Lactobacillus cells was inoculated into the sterile reconstituted skim milk supplemented with 2% glucose to make yogurt. The pH values of the each yogurt were determined at the indicated time points (24 h, 48 h and 72 h) to measure their acidification activities. Values are means±SEM of 10 samples each.
[0080] Table 1 displays the acidification characteristics of milk by Lactobacillus acidophilus KCTC 3179, FARM1 and FARM2.
[0000]
TABLE 1
Values are means + SEM of 10 samples each.
pH Values Of Yogurt
Time
3179
FARM1
FARM2
24
6.78 ± 0.16
7.12 ± 0.16
6.59 ± 0.24
48
3.82 ± 0.24
4.42 ± 0.05
3.77 ± 0.14
72
3.66 ± 0.13
3.97 ± 0.12
3.69 ± 0.12
3. Colonization Ability in the GI Tract
[0081] After feeding rats yogurt fermented with Lactobacillus acidophilus KCTC 3179, FARM1 and FARM2 for 8 weeks each, the samples of stomach and small intestine from each group were taken to count the colonies forming unit (CFU). Control means rats without feeding any yogurt. Values are means±SEM of 5 samples each.
[0082] Table 2 displays the colonization of Lactobacillus KCTC 3179, FARM1 and FARM2 in the GI tract of rats.
[0000]
TABLE 2
Values are means + SEMof5sampleseach.
Log 10 [CFU of lactobacilli/g(wet weight) of organ]
Strain
Stomach
Small Intestine
control
Non-detectable
6.64 ± 0.22
3179
8.54 ± 0.20
8.64 ± 0.14
FARM1
8.61 ± 0.19
8.50 ± 0.19
FARM2
8.50 ± 0.22
8.63 ± 0.23
4. Colonization Ability Under Diet-Induced Obesity
[0083] After feeding rats high fat diet with yogurt fermented with Lactobacillus acidophilus KCTC 3179, FARM1 and FARM2 for 4 weeks each, the samples of stomach and small intestine from each sample were taken to count the colonies forming unit (CFU). Control means rats without feeding any yogurt. Values are means±SEM of 5 samples each.
[0084] Table 3 displays the colonization of Lactobacillus KCTC 3179, FARM1 and FARM2 in the GI tract of rats while inducing obesity by diet.
[0000]
TABLE 3
Values are means + SEMof5sampleseach.
Log 10 [CFU of lactobacilli/g (wet weight) of organ]
Strain
Stomach
Small Intestine
control
Non-detectable
5.98 ± 0.21
3179
8.15 ± 0.29
9.14 ± 0.24
FARM1
8.32 ± 0.23
8.89 ± 0.22
FARM2
8.19 ± 0.17
9.05 ± 0.19
5. The Effect of Caloric Extraction by FARMs in the GI Tract on the Induction of the Diet-Induced Obesity.
[0085] FIG. 3 shows the changes in body weight of host that was colonized with Lactobacillus.
[0086] Three months old Male SD rats (200-220 g) were randomly divided into four groups (n=14 per group); rats fed high fat diet only (control) and rats fed with Lactobacilli (KCTC 3179, FARM1, or FARM2) daily for 22 weeks. Change in body weight is displayed as mean±SEM.
[0087] FIG. 4 shows the visceral fat analysis of host that was colonized with Lactobacillus . The visceral fat areas of the experiment groups of the rats were measured using Magnetic resonance imaging (MRI) after finishing the feeding experiment and analyzed with an image analysis program (Image J, USA). Differences in visceral fat accumulation among the experiment groups of the rats are displayed as mean±SEM.
[0088] FIG. 5 shows the visceral fat images of MRI in host that were colonized with Lactobacillus.
[0089] Representative images of the visceral fat accumulation of the rats fed high fat diet only (control) and with Lactobacilli (KCTC 3179, FARM1, or FARM2) daily after 22 weeks.
[0000] 6. The Comparison of the Blood Serum Parameters after Feeding Lactobacillus 3179 or FARM Strains
[0090] Three months old Male SD rats (200-220 g) were randomly divided into four groups (n=14 per group), and fed high fat diet only or with Lactobacilli for 22 weeks; control group (high fat diet only), 3179 group (high fat diet with yogurt fermented by L. acidophilus KCTC 3179 strain), FARM group (high fat diet with yogurt fermented by FARM mutant, respectively). The blood samples of experimental rats were collected at the beginning and at the end of the experimental period, and analyzed for the change of the blood serum parameters. All data were expressed as mean±SEM. Statistical comparisons were performed by analysis of variance (ANOVA) test. A value of p<0.05 was considered statistically significant.
[0091] FIG. 6 shows the change of plasma lipid profiles in rats. TG, triglycerides; TC, total cholesterol; HDL, high-density lipoprotein cholesterol; LDL, low-density lipoprotein cholesterol.
[0092] FIG. 7 shows the change of plasma insulin and leptin concentrations in rats.
[0093] FIG. 8 shows the change of blood glucose concentrations in rats.
7. Effect of FARM3 on Diet-Induced Obesity
[0094] FIG. 9 shows in vitro fatty acid extraction capability of FARM3 from their surrounding environment. FARM2 was mutagenized with ethylmethane sulphonate (EMS) to generate FARM3 with better fatty acid extraction capability. Fatty acid extraction capability of FARM3 was determined by measuring the radioactivity in Lactobacilli using liquid scintillation spectroscopy after incubation of Lactobacilli with 1 nCi/ml of 14C labeled palmitic acid for 1 hour. Values are mean±standard deviation (n=4).
[0095] FIG. 10 shows the reduction of caloric intake by Lactobacillus or Orlistat™
[0096] The 3 month old male SD rats were given high-fat feed for 8 weeks to develop diet-induced obesity with average body weight of 425 g. The diet-induced obese rats were administered daily yogurt fermented with wild-type Lactobacillus 3179 (∘, high fat diet with yogurt fermented by L. acidophilus KCTC3179 strain), yogurt fermented with FARM3 (, high fat diet with yogurt fermented by FARM3) or Orlistat™ (Δ, high fat diet with Xenical™ 200 mg/kg diet) under continued high-fat diet condition for 4 weeks. Change in body weight (n=14) is displayed as mean±SEM.
|
The present invention relates to prevention and treatment of obesity and obesity related metabolic syndrome, particularly to prevention and treatment of obesity by change of intestinal flora. In the present invention, it was ascertained that the characteristics of intestinal bacteria are transformed by administration of a microorganism preparation which improves free fatty acid absorption by the bacteria, and free fatty acid absorption in the gastrointestinal tract is thereby decreased by introduction thereof. The present invention provides a method for preventing and treating obesity and obesity related metabolic syndrome, a pharmaceutical composition and diet supplement for prevention and treatment thereof, and a modified probiotic strains usable for such purposes on the basis of these experimental results. The present invention shows a weight loss effect equal to that of orlistat which is most widely used as an anti-obesity therapeutic agent. The present invention shows that the absorption of fatty acids in the gastrointestinal tract is blocked by improving the characteristics of intestinal bacteria and transplanting them, thereby enabling the treatment of obesity.
| 0
|
FIELD OF THE INVENTION
A flush and fill system for a water storage tank which delivers consistent volumes of water per flush over a wide range of water supply pressures and supply rates.
BACKGROUND OF THE INVENTION
The environmental concerns regarding availability of water for any purpose, especially for sewage disposal, and of disposing of water used for sewage purposes, has led to severe limitations on the amount of water which is permitted for each flush of a commode. Historically commode flushing systems were permitted to use whatever amount of water was convenient to flush the commode and reliably remove the contents of the bowl. Cycles using several gallons were acceptable.
Now that has profoundly changed. In certain areas crowded with people, the resulting demand for water and the amount of effluent they generate seriously compromise the availability of the water and of the disposal plants which ultimately receive it. As a consequence, governmental units regularly require that new commode installations be reliably flushed with only a few quarts of water, instead of gallons.
A properly designed commode can indeed flush reliably with such a short flush, but only if it is reliably supplied, each time, with a known and specified volume of water delivered under known and specified conditions. However, conventional commode supply and flush systems are susceptible to substantial variations not only from installation to installation, but from flush to flush in the same installation. This makes it most difficult for a manufacturer to design a product for a short flush which is reliable under all circumstances.
It is an object of this invention to provide a flush and fill system for a commode tank whose delivery is volumetrically consistent regardless of differences or variations in water supply pressure or re-supply rates of flow.
In the conventional art, a commode tank is filled and kept closed and at rest until a flush cycle is started. When it is, a flush valve in the bottom of the tank is opened and the contents of the tank are discharged into the commode. The problem arises that with a conventional float-controlled supply valve, the supply valve opens to re-supply the tank even while the tank is emptying, because the float valve which follows the surface of the water in the tank as the tank empties opens the valve before the tank is emptied.
Such an arrangement is tolerable if one can assume that the flow rate of re-supply is consistent and known relative to the rate of discharge from the tank to the commode. This is far from a reliable assumption. Especially for short flushes, variations in water supply pressures and related flow rates can cause the amount of water actually delivered in a given period of time to vary as much as 30% above and below that which is needed for an optimum flush. Such variations either way from an optimum flush are undesirable. Too little water can make an insufficient flush, which will require a subsequent flush thereby wasting water. Too much wasted water frustrates the very purpose of having a short flush commode in the first place.
This invention overcomes the disadvantages of the prior art by requiring that the contents of the tank at rest be delivered to the commode before refilling of water to the tank is started. Deferral of refilling is not per sea new concept. For example, see Antunez U.S. Pat. No. 4,840,196 issued Jun. 29, 1989. However the invention contemplated in that patent involves a complexity of valving concepts which it is an object of this invention to overcome, and which will permit the use of known and proved conventional tank valves.
BRIEF DESCRIPTION OF THE INVENTION
A flush and refill system according to this invention is fitted into a water tank. The water tank has an outlet port with a flush valve seat in it that is adapted to be opened and closed by a flush valve plug mounted to a vertically extending post. Buoyancy means is provided for this post. This post may, if desired, also function as an overflow pipe that is open at its top and bottom, with its lower end discharging into the outlet port. Optionally it may instead be a closed post which together with the flush valve plug and buoyancy means will be buoyant when not forced against the valve seat. In any event, the post has an engagement surface that moves vertically as a part of the post when the post moves up and down.
A level responsive water supply valve receives water under system pressure for refilling the tank. It includes level responsive means such as a float on a float arm. When the water in the tank reaches a storage level, the float and its arm will shut off incoming water. When the water level lowers after the flush valve is opened, then if the float is permitted to lower, the valve will open to refill the tank.
According to a feature of this invention, when the post is raised to open the flush valve, it also rises to prevent the supply valve from opening so long as the post is sufficiently buoyant, i.e., when there is sufficient water in the tank to hold the post in a sufficiently elevated position such that the water supply valve will be restrained to its upper, closed position.
When sufficient water has left the tank, the flush valve will close, and the post will lower to permit the supply valve to open. Notice that the resupply of the tank cannot start until the tank is substantially empty.
According to a preferred but optional feature of this invention, the water supply valve is a conventional float activated ballcock valve and the post serves to prevent the lowering of its float until after the discharge of water from the tank is substantially complete.
According to a preferred but optional feature of the invention, the post is open at both of its ends. A peripheral enlargement in its mid-length will constitute the buoyant means while the passage through the post is not flooded.
According to an optional feature of the invention, the post may instead control an off-on valve in series with the ballcock valve to prevent flow therethrough while the tank water level is lowering from its full to its empty level.
The above and other features of this invention will be fully understood from the following detailed description and the accompanying drawings, in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a vertical cross-section partly in schematic notation showing the presently-preferred embodiment of the invention in its storage condition;
FIG. 2 is a view similar to FIG. 1 showing the invention in its flushing condition;
FIG. 3 is a view similar to FIG. 1 showing the invention in its refilling condition;
FIG. 4 is a cross-section taken at line 4--4 in FIG. 1; and
FIG. 5 is a top view, partly in schematic notation, showing another embodiment of the invention; and
FIG. 6 is a cross-section showing another embodiment of buoyant means.
DETAILED DESCRIPTION OF THE INVENTION
The invention will best be understood from an examination of FIGS. 1-3, which show a sequence from storage (FIG. 1), through flush discharge (FIG. 2), through tank refilling (FIG. 3), after which the stored condition of FIG. 1 will resume.
The system is installed in a water tank 10 having a bottom 11 and a peripheral sidewall 12. An outlet port 13 is formed on the bottom, through which water will be discharged into the commode (not shown). A flush valve 15 is fitted in the outlet port. It includes a tapered valve seat 16, mounted to a conventional spud (not shown), in accordance with known arrangements.
A valve plug 20 is fitted to a post 21. The plug has a valve face 22 tapered downwardly to match valve seat 16 in order to close the flush valve. As shown by arrow 23, a chain 24 is fastened to the post to lift it to start a flush cycle. The chain will be coupled to a conventional pivoted handle and arm for the purpose of lifting the post.
Buoyancy means 25, such as an enlarged medial portion 26 of the post is incorporated in the post. The post includes a central passage 27 open from top to bottom. The medial portion is enlarged internally and externally, and is ring-like. The weight of the post, of the valve plug and of the buoyancy means (if a separate buoyancy means is used as shown in FIG. 6) relative to the buoyant effect of the buoyancy means is selected so that when the valve plug is separated from the valve seat, the post will rise, and can exert enough upward force to accomplish the delay to be described below. This assembly will usually be quite light in weight.
In its preferred form, the post will be a hollow tube, open at its upper and lower ends. It can thereby function as an overflow pipe for the tank when the flush valve is closed. If preferred, an overflow pipe can be supplied separately, and the post may be a closed rod. However the post is made, it will include an engagement surface 28, preferably at the upper end of the post, for a purpose next to be described.
A tank valve 40 is fitted in the tank and connected to a source of water under pressure from a supply pipe 41. Many kinds of valves may be used, but a conventional float-controlled ballcock valve of the type shown in Autunez U.S. Pat. No. 3,389,887, issued Jun. 25, 1968 is especially useful. The details of such a valve are very well known and need no description here. Reference may be had to this Antunez patent for further details.
The valve is controlled by a float 42 pivotally mounted to the valve body 43 by an arm 44. At the upper position shown in FIG. 1, the valve is closed to flow. Below this position (FIG. 3) the valve is open to flow. The valve discharges water into the system in two ways. The first is through a supply outlet 45, directly into the tank, and the other is through a bowl refill tube 46.
The bowl refill tube is intended to deliver a minor amount of water to the bowl after the major flush discharge to provide a gas seal in the bowl. This is a known arrangement. This tube may be made quite rigid and can be attached to valve body 43. It includes a bend 47 and a depending length 48 which extends downwardly into the post to stabilize the post against excessive wobbling. It is long enough to remain in the post in all of the post positions without impeding the vertical movement of the post.
The operation of this system will be understood from the foregoing. When the system is in its rest, stored, condition (FIG. 1) with the tank full to its full level, the flush valve remains closed, because the buoyancy of the buoyancy member will be overcome by the downward differential pressure on the valve plug (the water pressure above it, versus the atmospheric pressure beneath it.)
To start a cycle, the chain is pulled up to separate the valve plug from the valve seat. This terminates the net force holding the flush valve closed, and the buoyancy means quickly raises the post to the position shown in FIG. 2. Then the engagement surface engages the float arm and holds it at or above the level at which the tank valve can open. In fact, it might raise the float above its rest level.
This condition continues until the water level in the tank falls below the buoyancy means. Then the post will drop (FIG. 3) and the flush valve will close. This enables the tank valve to reopen and resupply the tank with water.
The post shown in FIGS. 1-3 is interesting in its performance. Simply placed in a pool of water, it will sink, and will have no buoyant property. Assume now that it is closed at its lower end. Then it would be buoyant because there is no water in it.
Next, assume that the lower end is exposed only to air and not to water. Then, because of the radial enlargement it will be buoyant, and will remain buoyant until the passage is flooded. This circumstance exists immediately after the post is raised.
While the post is closed on the valve seat, the passage drains down out into the flow channels to the bowl. It is filled with air, because these flow channels are vented.
When the post is pulled upwardly, water from the tank rushes through the valve seat. This is its preferred flow path, and water will not back up into the post passage. When the water level lowers sufficiently, the valve plug will close the valve seat, but then buoyancy is meaningless, because water will flood the top side of the valve plug, and overcome any buoyancy of the post.
This is a surprisingly simple post construction. In a field where savings of fractions of cents can contribute to the attractiveness of a product, this is a considerable advantage.
FIG. 6 shows another embodiment of a post 50, in which separate buoyancy means 51 is attached to the post. Preferably it will be a ring 52 of foam plastic material which can be slided up and down the post to establish the level at which the post is to lose its buoyant property.
It should be noted that the tank valve will have remained closed during almost the entire period in which the tank was emptying. No replacement water was supplied during this time. Therefore the flush cycle will have delivered an exact amount of water under flow conditions entirely determined by the geometry of the tank, and independent of the time it takes to refill the tank. Further, the time-rate of water discharge from the tank is entirely determined by the geometry of the commode installation. Both time and volume of each flush are remarkably consistent, and also consistent between different installations of the same design.
The engagement means on the post shown in FIGS. 1-3 are intended to engage either the float arm or an extension from it. It may be preferred to have the post react with a lighter-weight device effective on the tank valve not directly, but in series with it. FIG. 5 schematically shows the same kind of tank valve 51 as in FIGS. 1-3, but which is not reacted by the post. It is controlled in part by a float and arm 52. Instead, a control valve 60 is plumbed into the supply line ahead of tank valve 51. It is an off-on valve under control of a control arm 52 that reacts with post 62. When the post is in its upper position as in FIG. 2, it will raise the control arm and close valve 60 which prevents flow through valve 51 regardless of the position of the float.
When the post lowers and the flush valve is closed the control arm will move downwardly and enable the tank valve to supply water so long as the float is below the storage level. While useful, this arrangement does involve an additional valve and will rarely be preferred.
This invention is not to be limited by the embodiments shown in the drawings and described in the description, which are given by way of example and not of limitation, but only in accordance with the scope of the appended claims.
|
A consistent-delivery flush and fill system for a water tank. A vertically movable post with a central passage carries a valve plug to open and close a valve seat for a discharge port from the tank. Buoyancy means on the post respond to the water level in the tank. A tank valve supplies water to the tank. When the tank is full the tank valve is closed. Engagement means on the post prevents the tank valve from opening until the tank is substantially emptied, at which time the valve plug closes the discharge port and enables the tank valve to open, having delivered a substantially constant volume of water from flush-to-flush.
| 4
|
FIELD OF THE INVENTION
[0001] The present invention relates to a cleaning apparatus and particularly relates to a cleaning apparatus which cleans wafers polished by chemical mechanical polishing (CMP: Chemical Mechanical Polishing) or the like.
BACKGROUND OF THE INVENTION
[0002] Wafers of semiconductor devices, electronic parts, or the like undergo various processes such as cutting and polishing. Recently, development in semiconductor techniques have promoted miniaturization and multi-layer interconnection in the design rules of semiconductor integrated circuits, and increase in the diameter of wafers have been also promoted in order to reduce cost. Therefore, when a next pattern is formed on a pattern-formed layer without processing in a conventional manner, forming a good pattern in the next layer is difficult due to the irregularities of the previous layer, defects, or the like are easily generated.
[0003] Therefore, a planarization process in which the surface of the pattern-formed layer is planarized and the pattern of the next layer is then formed is carried out. CMP has been frequently carried out in the planarization process. Polishing of a wafer by CMP is carried out by retaining the wafer by a polishing head, bringing the wafer into contact with a polishing pad with a pressure while supplying slurry, which is a mixture of an abrasive and a chemical agent, and rotating the wafer and/or the polishing pad in this state.
[0004] Large amounts of particles of, for example, the used abrasive, metal impurities contained in the chemical agent, ions and fine particles of the metal used in metal wiring on the wafer, or the like are adhering on the wafer surface after polishing by the CMP. Since these particles, or the like have adverse effects on semiconductor devices or the like which serve as products, the surfaces of wafers after polishing have to be cleaned to have high cleanliness so that the particles, ions and fine particles of the metal impurities, or the like, are removed.
[0005] For example, the following polishing apparatus and substrate processing apparatus are known as conventional techniques relating to such a cleaning apparatus. In this conventional technique, primary to fourth four cleaning machines (cleaning processing chambers) for cleaning wafers, which have undergone CMP polishing, are separated from each other by dividing walls and arranged in one direction. In addition, transporting mechanisms for sequentially transporting wafers to next cleaning machines are provided. The primary and secondary cleaning machines rotate roll-like sponges, which are disposed above and below, and press the sponges against a first surface and a second surface of the wafer, thereby cleaning the first surface and the second surface of the wafer. The third cleaning machine presses a hemispherical sponge against the wafer while rotating the sponge, thereby cleaning the wafer. The fourth cleaning machine subjects the second surface of the wafer to rinse cleaning and cleans the first surface by pressing a hemispherical sponge against the first surface while rotating the sponge. A spin dry function for drying the wafer after the cleaning by rotating the wafer at a high speed is provided. At the top of each of the primary to fourth cleaning machines, a filter fan unit comprising a clean air filter is provided, and clean air without particles is always blown downwardly from the filter fan unit (for example, see Patent Document 1).
[0006] For example, a following substrate processing method is known as another conventional technique related to the cleaning apparatus. In this conventional technique, first to fourth four cleaning processing chambers for cleaning wafers, which have undergone CMP polishing, are arranged in one direction. In addition, transporting apparatus for sequentially transporting wafers to next cleaning processing chambers are provided. The first cleaning processing chamber causes an organic alkaline treatment liquid to drip from a cleaning fluid supplying nozzle and drive a pair of rotating brushes to rotate in the opposite directions, thereby bringing both the first and second surfaces of a wafer into contact with protruding portions of the pair of rotating brushes and cleaning the wafer. When cleaning using the organic alkaline treatment liquid is completed, pure water is supplied to both the first and second surfaces of the wafer, thereby cleaning particles, or the like which have got away from the wafer. The second cleaning processing chamber causes an organic acid treatment liquid from a cleaning fluid supplying nozzle and drives a pair of rotating brushes to rotate in the opposite directions, thereby bringing both the first and second surfaces of the wafer into contact with protruding portions of the pair of rotating brushes and cleaning the wafer. When the cleaning using the organic acid treatment liquid is completed, pure water is supplied to both the first and second surfaces of the wafer, thereby cleaning metal impurities, or the like which have got away from the wafer. The third cleaning processing chamber supplies pure water to the first surface of the wafer to form a liquid film, at the same time, supplies a highly-oxidative treatment liquid to the second surface of the wafer, and cleans the wafer while rotating the wafer. Then, the fourth cleaning processing chamber subjects both the first and second surfaces of the wafer to precision cleaning by pure water excited by ultrasonic waves and then subjects the wafer to spin drying. In this precision cleaning, fine particles, metal impurities, or the like adsorbed on the part of dishing or the like generated in metal wiring on the wafer can be reliably cleaned. In the fourth cleaning processing chamber, a discharge duct for discharging pure water during cleaning or after cleaning is provided (for example, see Patent Document 2).
[0007] [Patent Document 1] Japanese Patent Application Laid-Open (kokai) No. 2003-309089 (pages 8, 18, 19, and FIG. 1)
[0008] [Patent Document 2] Japanese Patent Application Laid-Open (kokai) No. 2002-299300 (pages 5, 10 to 13, FIG. 2, and FIG. 4)
[0009] In the conventional technique described in Patent Document 1, wafers, which have undergone polishing of CMP, are subjected to cleaning processes while the wafers are sequentially transported from the primary to fourth cleaning machines and dried in the last fourth cleaning machine so as to finish the cleaning process. Since the wafers are sequentially processed in the four cleaning machines, which are arranged in one direction, one by one, the processing number of wafers per unit time in the entire cleaning apparatus is limited by the cleaning time of the cleaning machine that has the longest processing time among the four cleaning machines. When the cleaning process of wafers is stopped due to failure or the like of any of the four cleaning machines, insufficient processing is caused in the wafers in process such as pretreatment. Furthermore, the transporting order from the primary cleaning machine to the last fourth cleaning machine is fixed in the cleaning apparatus due to the structure thereof, and the processing order cannot be changed in accordance with, for example, cleaning treatment processes. In the entire primary to fourth cleaning machines, purified clean air is always supplied from the above thereof by the filter fan unit.
[0010] In the conventional technique described in Patent Document 2, the point that a cleaning process is carried out while sequentially transporting wafers after polishing from the first to fourth cleaning processing chambers and the wafers are dried in the last cleaning processing chamber to finish the cleaning process is approximately the same as the conventional technique described in above described Patent Document 1. Then, in the conventional technique described in above described Patent Document 2, the pure water used merely in the precision cleaning of the fourth cleaning processing chamber is discharged from the discharge duct. The pure water that is used merely in precision cleaning and maintaining not-largely deteriorated purity can be conceivably recycled in the series of cleaning processes starting from a removing process of an abrasive or the like adhering on the wafers after polishing.
[0011] Thus, technical problems to be solved are generated in order to subject wafers that have undergone polishing to various cleaning processes or to subject wafers that have undergone polishing to many cleaning processes while reducing the usage amount of pure water, to increase the processing speed of wafers per unit floor area and significantly improve the operating rate, to enable change or rearrangement of a plurality of cleaning processing chambers to optimum arrangement in accordance with the cleaning treatment processes or the like to prevent generation of defects in wafers that are in process of, for example, pre-treatment, to reduce the cost of supplying equipment and simplify the configuration of the apparatus, and to suppress transmission of the vibration that is generated in the cleaning processing chambers in an upper-layer side to other cleaning processing chambers, and obtain always stable cleaning property. It is an object of the present invention to solve these problems.
SUMMARY OF THE INVENTION
[0012] The present invention has been proposed for achieving the above described objects, and the invention according to claim 1 provides a cleaning apparatus comprising: cleaning lines comprised of lower and upper two levels, each of the levels comprising a plurality of cleaning processing chambers which subjects a wafer, which has undergone polishing, to a required cleaning process and drying; a center transporting means comprising a function of transporting the wafer, which has undergone polishing, into or transporting the processed wafer to each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines; and an inter-chamber transporting means for sequentially transporting the wafer to the adjacent cleaning processing chamber in each of the lower-layer and upper-layer cleaning lines.
[0013] According to this configuration, when a series of processes is to be carried out merely in the lower-layer cleaning line, the wafer, which has undergone polishing such as chemical mechanical polishing, is transported to the cleaning processing chamber in the former side in the lower-layer cleaning line by the center transporting means. The transported wafer is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is subjected to a drying process in the last cleaning processing chamber and carried out therefrom.
[0014] When a series of processes is to be carried out merely in the upper-layer cleaning line, the wafer, which has undergone polishing, is transported into the cleaning processing chamber in the former side in the upper-layer cleaning line by the center transporting means. The transported wafer is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is subjected to a drying process in the last cleaning processing chamber and carried out therefrom.
[0015] When processing is to be carried out sequentially from the lower-layer cleaning line to the upper-layer cleaning line, the wafer, which has undergone polishing, is transported into the cleaning processing chamber in the former side in the lower-layer cleaning line by the center transporting means. The transported wafer is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is carried out from the cleaning processing chamber in the latter-side by the center transporting means. Then, the wafer is transported into the cleaning processing chamber in the former side in the upper-layer cleaning line by the center transporting means. The transported wafer is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-layer transporting means, and the wafer is subjected to a drying process in the last cleaning processing chamber in the upper-layer cleaning line and carried out therefrom.
[0016] When processing is to be carried out in parallel in the lower-layer cleaning line and the upper-layer cleaning line, the wafer, which has undergone polishing, is transported into the cleaning processing chamber in the former side in the lower-layer cleaning line by the center transporting means, and the wafer is subjected to required cleaning processes and drying and carried out therefrom. Approximately in parallel with this process, another wafer, which has undergone polishing, is transported into the cleaning processing chamber in the former side in the upper-layer cleaning line by the center transporting means. In this manner, parallel processing of the wafers is carried out by simultaneously operating the lower-layer and upper-layer cleaning lines.
[0017] The invention according to claim 2 provides the cleaning apparatus wherein even when either one of the lower-layer or upper-layer cleaning lines is stopped, the other cleaning line can be operated.
[0018] According to this configuration, even when either one of the lower-layer or upper-layer cleaning lines is stopped for some reason, cleaning processes are carried out in the other cleaning line. Therefore, the cleaning processing function as the entire apparatus can be always maintained.
[0019] The invention according to claim 3 provides the cleaning apparatus, wherein each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines can be replaced by another cleaning processing chamber with approximately the same shape.
[0020] According to this configuration, the plurality of cleaning processing chambers in the lower-layer and upper-layer cleaning lines can be replaced or rearranged so that optimal cleaning processing functions can be obtained in accordance with the cleaning treatment process and the like of the wafer.
[0021] The invention according to claim 4 provides a cleaning apparatus comprising: cleaning lines comprised of lower and upper two levels, each of the levels comprising a plurality of cleaning processing chambers which subjects a wafer, which has undergone polishing, to a required cleaning process and drying; a center transporting means comprising a function of transporting a wafer to be processed into or transporting the processed wafer to each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines; an inter-chamber transporting means for sequentially transporting the wafer to the adjacent cleaning processing chamber in each of the lower-layer and upper-layer cleaning lines; and an introducing means for introducing pure water used in the cleaning processing chamber, which carries out precision cleaning in a latter side in the upper-layer cleaning line, into the cleaning processing chamber, which carries out rough cleaning in a former side in the lower-layer cleaning line, as washing water for the rough cleaning.
[0022] According to this configuration, when a series of processes from rough cleaning to precision cleaning is to be carried out merely in the lower-layer cleaning line, the wafer, which has undergone polishing such as chemical mechanical polishing, is transported into the cleaning processing chamber in the former side in the lower-layer cleaning line by the center transporting means. The transported wafer is subjected to required cleaning processes including rough cleaning while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is subjected to precision cleaning and a drying process in the cleaning processing chamber in the latter side and carried out therefrom.
[0023] When a series of processes from rough cleaning to precision cleaning is to be carried out merely in the upper-layer cleaning line, the wafer, which has undergone polishing, is transported into the cleaning processing chamber, which carries out rough cleaning in the former side in the upper-layer cleaning line, by the center transporting means. The transported wafer is subjected to required cleaning processes including rough cleaning while the wafer is sequentially transported to the adjacent cleaning processing chamber by the inter-chamber transporting means, and the wafer is subjected to precision cleaning and a drying process in the cleaning chamber in the latter side and carried out therefrom.
[0024] When processing is to be carried out sequentially from the lower-layer cleaning line to the upper-layer cleaning line, the wafer, which has undergone polishing, is transported into the cleaning processing chamber, which carries out rough cleaning in the former side in the lower-layer cleaning line, by the center transporting means. The transported wafer is subjected to required cleaning processes including rough cleaning while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is then carried out therefrom by the center transporting means. Then, the wafer is further transported into the cleaning processing chamber in the latter side in the upper-layer cleaning line by the center transporting means. The transported wafer is subjected to required cleaning processes including precision cleaning and a drying process while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is carried out therefrom. In this course, the pure water used in precision cleaning in the cleaning processing chamber in the latter side in the upper-layer cleaning line is reutilized by being introduced into the cleaning processing chamber, which carries out rough cleaning in the former side in the lower-layer cleaning line as washing water for the rough cleaning.
[0025] When a series of processes from rough cleaning to precision cleaning is to be carried out in parallel respectively in the upper-layer cleaning line and the lower-layer cleaning line, the wafer, which has undergone polishing, is transported into the cleaning processing chamber, which carries out rough cleaning in the former side in the upper-layer cleaning line, by the center transporting means. The transported wafer is subjected to required cleaning processes including rough cleaning while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is subjected to precision cleaning and a drying process in the cleaning processing chamber in the latter-side and carried out therefrom. Approximately in parallel with this process, another wafer, which has undergone polishing, is transported into the cleaning processing chamber, which carries out rough cleaning in the former side in the lower-layer cleaning line, by the center transporting means, and the wafer is subjected to rough cleaning utilizing the pure water used in precision cleaning in the cleaning processing chamber in the latter side in the upper-layer cleaning line as washing water and subjected to a required cleaning process. Then, the wafer is subjected to precision cleaning and a drying process in the cleaning processing chamber in the latter side while the wafer is sequentially transported to the adjacent cleaning processing chambers by the inter-chamber transporting means, and the wafer is carried out therefrom. As described above, while arbitrarily utilizing the pure water used in the precision cleaning in the upper-layer cleaning line as the washing water for rough cleaning in the lower-layer cleaning line, the parallel processing of the wafer is carried out by simultaneously operating the lower-layer and upper-layer cleaning lines.
[0026] The invention according to claim 5 provides the cleaning apparatus wherein the introducing means comprising a washing water retention chamber for temporarily retaining the pure water used in the cleaning processing chamber for carrying out precision cleaning, washing water piping connecting the washing water retention chamber to the cleaning processing chamber for carrying out the rough cleaning, and a regulating valve provided in the washing water piping for regulating supplying of the washing water to the cleaning processing chamber, which carries out the rough cleaning.
[0027] According to this configuration, the pure water used in the precision cleaning in the cleaning processing chamber in the latter side in the upper-layer cleaning line is once retained in the washing water retention chamber. When rough cleaning is to be carried out in the cleaning processing chamber in the former side in the lower-layer cleaning line, the water is introduced from the washing water retention chamber into the cleaning processing chamber for the rough cleaning as the washing water for the rough cleaning via the washing water piping while the supplying amount thereof is regulated to an appropriate amount by the regulating valve.
[0028] The invention according to claim 6 provides the cleaning apparatus, wherein the introduction of the washing water by the introducing means from the cleaning processing chamber, which carries out precision cleaning, to the cleaning processing chamber, which carries out the rough cleaning, is carried out by difference in the head of water between the upper-layer cleaning line and the lower-layer cleaning line.
[0029] According to this configuration, the pure water used in the precision cleaning in the cleaning processing chamber in the latter side in the upper-layer cleaning line is introduced into the cleaning processing chamber for rough cleaning in the lower-layer cleaning line as washing water by utilizing the difference in the head of water between the upper-layer cleaning line and the lower-layer cleaning line.
[0030] The invention according to claim 7 provides the cleaning apparatus wherein the cleaning processing chamber, which carries out precision cleaning in the latter side in the upper-layer cleaning line, is communicated with the cleaning processing chamber, which carries out the rough cleaning in the former side in the lower-layer cleaning line, by an air duct, and clean air supplied from a clean air supplying unit to the cleaning processing chamber, which carries out the precision cleaning, is sent to the cleaning processing chamber, which carries out the rough cleaning, via the air duct.
[0031] According to this configuration, the clean air supplied from the clean air supplying unit to the cleaning processing chamber, which carries out precision cleaning in the upper-layer cleaning line, is not just discharged, but is blown into the cleaning processing chamber, which carries out rough cleaning in the lower-layer cleaning line, via the air duct and is reutilized as the air for the clean ambient of the cleaning processing chamber, which carries out rough cleaning.
[0032] The invention according to claim 8 provides a cleaning apparatus, wherein the wafer, which has undergone polishing, is subjected to a required cleaning process including the rough cleaning in the cleaning processing chamber in the former side in the lower-layer cleaning line, and the wafer is then transported to the cleaning processing chamber in the latter side in the upper-layer cleaning line by the center transporting means and subjected to a required cleaning process including the precision cleaning and a drying process so as to subject the wafer to a series of required processes.
[0033] According to this configuration, rough cleaning with respect to the wafer, which has undergone polishing, is carried out in the cleaning processing chamber for rough cleaning in the lower-layer cleaning line, and the precision cleaning thereafter is carried out in the cleaning processing chamber for precision cleaning in the upper-layer cleaning line. Therefore, the pure water and clean air used in the cleaning processing chamber for precision cleaning can be effectively reutilized as the washing water and the air for the clean ambient in the cleaning processing chamber for the rough cleaning.
[0034] The invention according to claim 9 provides the cleaning apparatus, wherein at least each of the cleaning processing chambers in the upper-layer cleaning line is attached to an apparatus frame via an anti-vibration means.
[0035] According to this configuration, transmission of the vibration generated upon operation of at least the cleaning processing chambers in the upper-layer cleaning line to the other cleaning processing chambers, the transporting means, or the like can be suppressed.
[0036] The invention according to claim 10 provides the cleaning apparatus, wherein even when either one of the cleaning lines among the lower-layer or upper-layer cleaning lines is stopped, the other cleaning line can be operated.
[0037] According to this configuration, even when either one of the lower-layer or upper-layer cleaning lines is stopped for some reason, the cleaning processes from rough cleaning to precision cleaning is carried out in the other cleaning line. Therefore, the cleaning processing function as the entire apparatus is always maintained.
[0038] The invention according to claim 11 provides the cleaning apparatus, wherein each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines can be replaced by another cleaning processing chamber with an approximately the same shape.
[0039] According to this configuration, the plurality of cleaning processing chambers in the lower-layer and upper-layer cleaning lines can be replaced or rearranged so that optimal cleaning processing functions can be obtained in accordance with the cleaning treatment process and the like of the wafer.
[0040] The invention according to claim 1 is provided with cleaning lines comprised of lower and upper two levels, each of the levels comprising a plurality of cleaning processing chambers which subjects a wafer, which has undergone polishing, to a required cleaning process and drying; a center transporting means comprising a function of transporting the wafer, which has undergone polishing, into or transporting the processed wafer from each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines; and an inter-chamber transporting means for sequentially transporting the wafer to the adjacent cleaning processing chamber in each of the lower-layer and upper-layer cleaning lines. Therefore, any of the processing merely by the lower-layer cleaning line, processing merely by the upper-layer cleaning line, and successive processing from the lower-layer cleaning line to the upper-layer cleaning line can be carried out, and the wafer, which has undergone polishing, can be subjected to various cleaning processes. Moreover, parallel processing can be carried out in the lower-layer and upper-layer cleaning lines, the processing speed of the wafer per unit floor area can be increased, the operating rate can be significantly improved, and various wafers to be subjected to different cleaning processes can be simultaneously processed. Moreover, there are advantages that carry in/out of the wafers with respect to the lower-layer and upper-layer cleaning processing chambers can be directly carried out by the common center transporting means, and the apparatus configuration can be simplified.
[0041] In the invention according to claim 2 , even when either one of the lower-layer or upper-layer cleaning lines is stopped, the other cleaning line can be operated. Therefore, there is an advantage that defects are not generated in the wafer in process of pre-treatment or the like since the cleaning processing function as the entire apparatus is always maintained.
[0042] In the invention according to claim 3 , each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines can be replaced by another cleaning processing chamber with approximately the same shape. Therefore, there is an advantage that the plurality of cleaning processing chambers in the cleaning lines can be replaced or rearranged to an optimum arrangement.
[0043] The invention according to claim 4 is provided with cleaning lines comprised of lower and upper two levels, each of the levels comprising a plurality of cleaning processing chambers which subjects a wafer, which has undergone polishing, to a required cleaning process and drying; a center transporting means comprising a function of transporting a wafer to be processed into or transporting the processed wafer from each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines; an inter-chamber transporting means for sequentially transporting the wafer to the adjacent cleaning processing chamber in each of the lower-layer and upper-layer cleaning lines; and an introducing means for introducing pure water used in the cleaning processing chamber, which carries out precision cleaning in a latter side in the upper-layer cleaning line, into the cleaning processing chamber, which carries out rough cleaning in a former side in the lower-layer cleaning line, as washing water for the rough cleaning. Therefore, either the series of processes from rough cleaning to precision cleaning merely by the lower-layer cleaning line or merely by the upper-layer cleaning line or a successive process from rough cleaning to precision cleaning from the lower-layer cleaning line to the upper-layer cleaning line can be carried out, and the wafer, which has undergone polishing, can be subjected to various cleaning processes. Moreover, parallel processing from rough cleaning to precision cleaning in the lower-layer and upper-layer cleaning lines can be carried out, the processing speed of the wafer per unit floor area can be increased, the operating rate can be significantly improved, and various wafers to be subjected to different cleaning processes can be simultaneously processed. Moreover, in the above described processing modes, upon rough cleaning in the former side in the lower-layer cleaning line, the pure water used in the precision cleaning in the cleaning processing chamber in the latter side in the upper-layer cleaning line can be reutilized as the washing water for the rough cleaning, and the usage amount of pure water can be reduced. Furthermore, there are advantages that carry in/out of the wafers with respect to the cleaning processing chambers of the lower-layer and upper-layer can be directly carried out by the common center transporting means, and the apparatus configuration can be simplified.
[0044] In the invention according to claim 5 , the introducing means comprising a washing water retention chamber for temporarily retaining the pure water used in the cleaning processing chamber for carrying out precision cleaning, washing water piping connecting the washing water retention chamber to the cleaning processing chamber for carrying out the rough cleaning, and a regulating valve provided in the washing water piping for regulating supplying of the washing water to the cleaning processing chamber, which carries out the rough cleaning. Therefore, the pure water used in the precision cleaning in the upper-layer cleaning line is once retained in the washing water retention chamber, and, when rough cleaning is to be carried out in the cleaning processing chamber in the lower-layer cleaning line, the pure water retained in the washing water retention chamber can be introduced into the cleaning processing chamber for the rough cleaning while the supplying amount thereof is regulated to an appropriate amount by the regulating valve. Thus, there are advantages that the usage amount of pure water can be reduced, and the rough cleaning with respect to the wafer, which has undergone polishing, can be appropriately carried out.
[0045] In the invention according to claim 6 , the introduction of the washing water by the introducing means from the cleaning processing chamber, which carries out precision cleaning, to the cleaning processing chamber, which carries out the rough cleaning, is carried out by difference in the head of water between the upper-layer cleaning line and the lower-layer cleaning line. Therefore, there are advantages that the pure water used in precision cleaning in the upper-layer cleaning line can be reutilized by introducing the water to the cleaning processing chamber for rough cleaning in the lower-layer cleaning line without using a pump or the like and the usage amount of pure water can be reduced while simplifying the apparatus configuration.
[0046] The invention according to claim 7 is configured so that the cleaning processing chamber, which carries out precision cleaning in the latter side in the upper-layer cleaning line, is communicated with the cleaning processing chamber, which carries out the rough cleaning in the former side in the lower-layer cleaning line, by an air duct, and clean air supplied from a clean air supplying unit to the cleaning processing chamber, which carries out the precision cleaning, is sent to the cleaning processing chamber, which carries out the rough cleaning, via the air duct. Therefore, the clean air supplied to the cleaning processing chamber, which carries out precision cleaning in the upper-layer cleaning line, can be reutilized as the air for the clean ambient of the cleaning processing chamber, which carries out rough cleaning in the lower-layer cleaning line. Thus, there is an advantage that the cost of the clean air supplying equipment can be reduced.
[0047] The invention according to claim 8 is configured so that the wafer, which has undergone polishing, is subjected to a required cleaning process including the rough cleaning in the cleaning processing chamber in the former side in the lower-layer cleaning line, and the wafer is then transported to the cleaning processing chamber in the latter side in the upper-layer cleaning line by the center transporting means and subjected to a required cleaning process including the precision cleaning and a drying process so as to subject the wafer to a series of required processes. Therefore, there is an advantage that the pure water and clean air used in the cleaning processing chamber for precision cleaning in the upper-layer cleaning line can be effectively reutilized as the washing water and the air for the clean ambient in the cleaning processing chamber for rough cleaning in the lower-layer cleaning line.
[0048] In the invention according to claim 9 , at least each of the cleaning processing chambers in the upper-layer cleaning line is attached to an apparatus frame via an anti-vibration means. Therefore, there are advantages that transmission of the vibration generated upon operation of at least each of the cleaning processing chambers in the upper-layer cleaning line to the other cleaning processing chambers, the transporting means, or the like can be suppressed, and always stable cleaning performance and transport of the wafer can be carried out.
[0049] In the invention according to claim 10 , even when either one of the cleaning lines among the lower-layer or upper-layer cleaning lines is stopped, the other cleaning line can be operated. Therefore, there is an advantage that defects are not generated in the wafers in process of, for example, pretreatment or the like since the cleaning processing function as the entire apparatus can be always maintained.
[0050] In the invention according to claim 11 , each of the cleaning processing chambers in the lower-layer and upper-layer cleaning lines can be replaced by another cleaning processing chamber with an approximately the same shape. Therefore, there is an advantage that the plurality of cleaning processing chambers in the cleaning lines can be replaced or rearranged to an optimal arrangement in accordance with the cleaning treatment process and the like of the wafers.
BRIEF DESCRIPTION OF THE DRAWINGS
[0051] FIGS. 1A and 1B are drawings showing a cleaning apparatus according to the invention of claims 1 to 3 , wherein (a) is a plan view and (b) is a side view.
[0052] FIGS. 2A and 2B are drawings showing a cleaning apparatus according to the invention of claims 4 to 11 , wherein (a) is a plan view and (b) is a side view.
[0053] FIG. 3 is a configuration diagram showing an introducing means for introducing washing water to a cleaning processing chamber that carries out rough cleaning and an air duct for supplying clean air.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0054] First of all, a preferred embodiment of the present invention according to claims 1 to 3 of the present invention will be described with reference to a drawing. FIGS. 1A and 1B are drawings showing a cleaning apparatus, wherein (a) is a plan view and (b) is a side view.
[0055] The configuration of the cleaning apparatus according to the present embodiment will be described first. In FIG. 1 , the cleaning apparatus 2 is disposed in a chemical mechanical polishing apparatus 1 . The chemical mechanical polishing apparatus 1 mainly comprises, other than the cleaning apparatus 2 , a load port unit 3 , a polishing apparatus 4 , a first, transporting machine 5 , a center transporting machine 6 serving as a center transporting means, an option chamber 7 , and an apparatus control unit (not shown).
[0056] The load port unit 3 comprises product wafer load ports 3 a and 3 a , a dummy wafer load port 3 b , and a monitor wafer load port 3 c . A cassette 8 storing in which a plurality of wafers W are stored is placed in each of the load ports 3 a , 3 b , and 3 c.
[0057] The polishing apparatus 4 is mainly comprises three platens 4 a , 4 b , and 4 c arranged in a part in one side of the chemical mechanical polishing apparatus 1 and two polishing heads (not shown) which are movably provided in the arrangement direction of the three platens 4 a , 4 b , and 4 c . Each of the platens 4 a , 4 b , and 4 c is formed to have a disk-like shape and rotates in one direction when it is driven by a motor (not shown). A polishing pad is attached on the upper surface of each of the platens 4 a , 4 b , and 4 c , and slurry is supplied onto the polishing pad from a nozzle (not shown).
[0058] Among the three platens 4 a , 4 b , and 4 c , the left and right platens 4 a and 4 c are used in polishing of a first polishing target film (for example, Cu film), and the center platen 4 b is used in polishing of a second polishing target film (for example, Ta film). In polishing of both of them, the type of supplied slurry, the rotating speed of the polishing heads, the rotating speed of the platens 4 a , 4 b , and 4 c , the thrust force of the polishing head, the material of the polishing pads, or the like are changed.
[0059] In the polishing apparatus 4 , the wafers W are retained by the polishing heads, the wafers are brought into contact with the polishing pads with a pressure while supplying the slurry from the nozzles to the polishing pads, and chemical mechanical polishing of the wafers W are carried out in this state by rotating the platens 4 a , 4 b , and 4 c and the polishing heads.
[0060] The cleaning apparatus 2 is disposed in the other side of the chemical mechanical polishing apparatus 1 so that the cleaning apparatus is opposed to the polishing apparatus 4 . The cleaning apparatus 2 comprises two levels including a lower-layer cleaning line 2 A comprising four cleaning processing chambers 2 a to 2 d and an upper-layer cleaning line 2 B similarly comprising four cleaning processing chambers 2 e to 2 h.
[0061] The four cleaning processing chambers 2 a to 2 d in the lower-layer cleaning line 2 A comprises: for example, the cleaning processing chamber 2 a which cleans the wafer W by rubbing the first surface and the second surface of the wafer by sponge brushes, the cleaning processing chamber 2 b which cleans the wafer W by causing steam to be jetted onto the first surface and the second surface of the wafer, the cleaning processing chamber 2 c which cleans the wafer W by ultrasonic waves, and the cleaning processing chamber 2 d which removes remaining dust by subjecting the first surface of the wafer W to an etching process of as light degree, then subjects the wafer to rinse cleaning, and subjects the wafer to spin drying at last.
[0062] The four cleaning processing chambers 2 e to 2 h in the upper-layer cleaning line 2 B are configured in the manner approximately same as the four cleaning processing chambers 2 a to 2 d in the lower-layer cleaning line 2 A.
[0063] Note that the cleaning processing chambers 2 a to 2 h in the lower-layer and upper-layer cleaning lines 2 A and 2 B can be replaced or rearranged by cleaning processing chambers with approximately the same outer shapes and different cleaning processing functions. The lower-layer and upper-layer cleaning lines 2 A and 2 B are configured so that at least either one of them is always operated.
[0064] Inter-chamber transporting machines 9 serving as inter-chamber transporting means are disposed between the cleaning processing chambers 2 a to 2 h in the lower-layer and upper-layer cleaning lines 2 A and 2 B respectively. The inter-chamber transporting machine 9 sequentially transports the wafer W to adjacent cleaning processing chambers (for example, 2 a and 2 b ).
[0065] The first transporting machine 5 picks up the unpolished wafer W from the cassette 8 placed in the product wafer load port 3 a , 3 a and transports the wafer to a wafer standby position 10 . Also, the first transporting machine 5 directly receives the wafer W, which has undergone cleaning processes in the lower-layer or upper-layer cleaning line 2 A or 2 B, from the last cleaning processing chamber 2 d or 2 h thereof and transports the wafer into the product wafer load port 3 a and 3 a.
[0066] The center transporting machine 6 receives the unpolished wafer W from the wafer standby position 10 and transports the wafer into the polishing apparatus 4 via a passing position 11 . The transporting machine also receives the wafer W, which has undergone polishing, via the passing position 11 and transports the wafer to each of the cleaning processing chambers 2 a to 2 h of the lower-layer and upper-layer cleaning lines 2 A and 2 B. The center transporting machine 6 comprises a function of directly carrying in/out into or from any of the cleaning processing chambers 2 a to 2 h of the lower-layer and upper-layer cleaning lines 2 A and 2 B. Therefore, a front transporting opening 12 for carrying in/out the wafer W is provided in each of the cleaning processing chambers 2 a to 2 h of the lower-layer and upper-layer cleaning lines 2 A and 2 B.
[0067] The option chamber 7 comprising functions of subjecting the wafer W, which has not undergone polishing, has undergone polishing, or has undergone a cleaning process, to a predetermined process, film-thickness measurement, or the like in addition to the above described polishing and cleaning process, then passing the wafer W to the center transporting machine 6 , and transporting the wafer to a required next process via the center transporting machine 6 . The front transporting opening 12 for carrying in/out the wafer W is also provided in the option chamber 7 .
[0068] The working of the cleaning apparatus, which is configured in the above described manner, will next be described. In the cleaning apparatus of the present embodiment, the cleaning lines 2 A and 2 B are configured to have two levels of the lower-layer and the upper-layer; therefore, various cleaning processing modes such as (a) carrying out a series of cleaning processes merely by the lower-layer cleaning line 2 A, (b) carrying out a series of cleaning processes merely by the upper-layer cleaning line 2 B, (c) carrying out cleaning processes sequentially from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B, and (d) carrying out cleaning processes in parallel in the lower-layer cleaning line 2 A and the upper-layer cleaning line 2 B can be employed. Hereinafter, these modes will be sequentially described.
[0069] (a) This is the case in which a series of cleaning processes is carried out merely in the lower-layer cleaning line 2 A. In this case, the wafer W, which has undergone chemical mechanical polishing in the polishing apparatus 4 , is received by the center transporting machine 6 via the passing position 11 and transported to the cleaning processing chamber 2 a which is in the start-point side in the lower-layer cleaning line 2 A. The transported wafer W is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning chambers 2 b , 2 c , and 2 d by the inter-chamber transporting machines 9 , and a drying process is carried out in the last cleaning processing chamber 2 d to finish the cleaning process.
[0070] After the cleaning process is finished, the wafer W is directly passed from the last cleaning processing chamber 2 d to the first transporting machine 5 and transported to the product wafer load port 3 a and 3 a.
[0071] (b) This is the case in which a series of cleaning processes are carried out merely in the upper-layer cleaning line 2 B. In this case, the wafer W, which has undergone chemical mechanical polishing, is directly transported to the cleaning processing chamber 2 e which is in the start-point side of the upper-layer cleaning line 2 B by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers 2 f , 2 g , and 2 h by the inter-chamber transporting machines 9 , and a drying process is carried out in the last cleaning processing chamber 2 h to finish the cleaning process.
[0072] After the cleaning process is finished, the wafer W is directly passed from the last cleaning processing chamber 2 h to the first transporting machine 5 and transported to the product wafer load port 3 a and 3 a.
[0073] (c) This is the case in which cleaning processes are sequentially carried out from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B. In this case, first, the wafer W, which has undergone chemical mechanical polishing, is transported to the cleaning processing chamber 2 a in the start-point side of the lower-layer cleaning line 2 A by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers 2 b , 2 c , and 2 d by the inter-chamber transporting machines 9 .
[0074] Then, at any of the points when a cleaning process is carried out merely by the cleaning processing chamber 2 a in the start-point side, when cleaning processes are carried out by the two cleaning processing chambers 2 a and 2 b , when cleaning processes are carried out by the three cleaning processing chambers 2 a , 2 b , and 2 c , or when cleaning processes are carried out until the last cleaning processing chamber 2 d , the wafer W is transported from the corresponding cleaning processing chamber 2 a , 2 b , 2 c , or 2 d by the center transporting machine 6 . Then, the wafer is transported to the cleaning processing chamber 2 in the start-point side of the upper-layer cleaning line 2 B by the center transporting machine 6 .
[0075] The wafer W transported to the upper-layer cleaning line 2 B is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers 2 f , 2 g , and 2 h by the inter-chamber transporting machines 9 , and the wafer is subjected to a drying process in the last cleaning processing chamber 2 h , thereby finishing the cleaning processes from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B.
[0076] After the cleaning processes are finished, the wafer W is passed from the last cleaning processing chamber 2 h of the upper-layer cleaning line 2 B to the first transporting machine 5 and transported to the product wafer load port 3 a and 3 a.
[0077] (d) This is the case in which cleaning processes are carried out in parallel in the lower-layer cleaning line 2 A and the upper-layer cleaning line 2 B. In this case, the wafer W, which has undergone chemical mechanical polishing, is transported to the start-point side cleaning processing chamber 2 a of the lower-layer cleaning line 2 A by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers 2 b , 2 c , and 2 d by the inter-chamber transporting machines 9 . The cleaning-process-finished wafer W is passed from the last cleaning processing chamber 2 d to the first transporting machine 5 and transported to the product wafer port 3 a and 3 a.
[0078] Approximately in parallel with this process, another wafer W, which has undergone chemical mechanical polishing, is transported to the cleaning processing chamber 2 e in the start-point side of the upper-layer cleaning line 2 B by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes while the wafer is sequentially transported to the adjacent cleaning processing chambers 2 f , 2 g , and 2 h by the inter-chamber transporting machines 9 . The cleaning-process-finished wafer W is passed from the last cleaning processing chamber 2 h to the first transporting machine 5 and transported to the product wafer load port 3 a and 3 a . In this manner, the parallel processing of the wafers W is carried out by simultaneously operating the lower-layer and upper-layer cleaning lines 2 A and 2 B.
[0079] As described above, the cleaning processing chambers 2 a to 2 d of the lower-layer cleaning line 2 A and the cleaning processing chambers 2 e to 2 h of the upper-layer cleaning line 2 B are comprised of those approximately the same cleaning processing functions. The lower-layer and upper-layer cleaning lines 2 A and 2 B are configured so that at least either one of them is always operated.
[0080] Therefore, in the case in which cleaning processes are carried out merely in the lower-layer cleaning line 2 A or the upper-layer cleaning line 2 B, when either one of the cleaning lines is stopped for some reasons, required cleaning processes can be carried out without causing any troubles by switching execution of the cleaning processes to the other cleaning line.
[0081] A preferred embodiment of the invention according to claims 4 to 11 of the present invention will next be described in detail with reference to drawings. FIGS. 2A and 2B show drawings showing a cleaning apparatus of the invention according to claims 4 to 11 , wherein (a) is a plan view and (b) is a side view. FIG. 2 is a configuration diagram showing an introducing means for introducing washing water to the cleaning processing chamber which carries out rough cleaning in the lower-layer cleaning line and an air duct for supplying clean air.
[0082] The configurations common with the configurations described for the invention according to claims 1 to 3 based on FIGS. 1A and 1B are denoted by the same reference numerals, and redundant descriptions thereof will be omitted.
[0083] In the invention according to claims 4 toll, the plurality of cleaning processing chambers 2 a to 2 d and 2 e to 2 h are comprised of two levels, the lower-layer cleaning line 2 A and the upper-layer cleaning line 2 B. Therefore, the vibration generated upon operation of each of the cleaning processing chambers 2 e to 2 h in the upper-layer cleaning line 2 B is readily transmitted to other cleaning processing chambers, the transporting means, or the like. Therefore, at least each of the cleaning processing chambers 2 e to 2 h of the upper-layer cleaning line 2 B is disposed on an apparatus frame via anti-vibration rubber (not shown) or the like serving as an anti-vibration means. As a result, transmission of the vibration generated upon operation of at least the cleaning processing chambers 2 e to 2 h of the upper-layer cleaning line 2 B to the other cleaning processing chambers, transporting means, or the like can be suppressed.
[0084] The four cleaning processing chambers 2 a to 2 d in the lower-layer cleaning line 2 A comprises: for example, the cleaning processing chamber 2 a which causes a required processing liquid to drip, rubs the first surface and the second surface of the wafer by sponge brushes, and then supplies pure water to the first and second surfaces of the wafer W so as to wash away particles and the like that have got away from the wafer W; the cleaning processing chamber 2 b which cleans the wafer W by causing steam to be jetted onto the first surface and the second surface of the wafer; the cleaning processing chamber 2 c which cleans the wafer W by pure water excited by ultrasonic waves; and the cleaning processing chamber 2 d which removes remaining dust by subjecting the first surface of the wafer W to an etching process of a slight degree by chemical solutions, then subjects the wafer to rinse cleaning, and subjects the wafer to spin drying at last. As described above, the cleaning line 2 A is comprised of the cleaning processing chambers 2 a to 2 d which carry out a series of processes of the cleaning processing chamber 2 a which carries out so-called rough cleaning to the cleaning processing chambers 2 c and 2 d which carry out precision cleaning.
[0085] In approximately the same manner as the four cleaning processing chambers 2 a to 2 d in the lower-layer cleaning line 2 A, the four cleaning processing chambers 2 e to 2 h in the above described upper-layer cleaning line 2 B are also comprised of the cleaning processing chambers 2 e to 2 h which carry out a series of processes of the cleaning processing chamber 2 e which carries out rough cleaning to the cleaning processing chambers 2 g and 2 h which carry out precision cleaning.
[0086] The rough cleaning herein for cleaning the wafer W on which slurry or the like is adhering immediately after CMP polishing does not require highly purified pure water. Therefore, in the present embodiment, the large amount of pure water used for rinsing upon precision cleaning in the cleaning processing chambers 2 g and 2 h in the upper-layer cleaning line 2 B is not just wasted but is reutilized as washing water for carrying out rough cleaning for washing away particles, dispersed chemical solutions, or the like in the cleaning processing chamber 2 a of the lower-layer cleaning line 2 A.
[0087] Also, in the cleaning processing chamber 2 a which carries out rough cleaning, the air for clean ambient does not require highly purified air. Therefore, in the present embodiment, the clean air processed by a HEPA filter (super-performance filter) or the like and supplied to the cleaning processing chambers 2 g and 2 h which carry out precision cleaning in the upper-layer cleaning line 2 B is not just discharged, but is blown into the cleaning processing chamber 2 a , which carries out rough cleaning in the lower-layer cleaning line 2 A, via the air duct and reutilized as air for the clean ambient of the cleaning processing chamber 2 a.
[0088] FIGS. 2A and 2B show the introducing means 9 for introducing washing water from the cleaning processing chamber 2 h ( 2 g ), which carries out precision cleaning in the upper-layer cleaning line 2 B, to the cleaning processing chamber 2 a , which carries out rough cleaning in the lower-layer cleaning line 2 A, and the air duct 14 for supplying clean air. The introducing means 9 comprises: a washing water retention chamber 10 , which temporarily retains pure water used in the cleaning processing chamber 2 h ( 2 g ), which carries out precision cleaning in the upper-layer cleaning line 2 B; washing water piping 11 connecting the washing water retention chamber 10 to the cleaning processing chamber 2 a , which carries out rough cleaning in the lower-layer cleaning line 2 A; and a regulating valve 12 , which is provided in the clean water piping 11 and regulates supply of washing water to the cleaning processing chamber 2 a which carries out the rough cleaning.
[0089] Then, the pure water used in precision cleaning in the cleaning processing chamber 2 h ( 2 g ) in the latter side in the upper-layer cleaning line 2 B is once retained in the washing water retention chamber 10 and supplied to the cleaning processing chamber 2 a for rough cleaning in the lower-layer cleaning line 2 A as washing water for the rough cleaning by utilizing the difference between the heads of water between the upper-layer cleaning line 2 B and the lower-layer cleaning line 2 A without using a pump or the like. In this course, the supplying amount thereof is appropriately regulated by the regulating valve 12 , thereby saving the usage amount of pure water and appropriately carrying out rough cleaning with respect to the wafer W after polishing.
[0090] The cleaning processing chamber 2 h ( 2 g ), which carries out precision cleaning in the latter side in the upper-layer cleaning line 2 B, and the cleaning processing chamber 2 a , which carries out rough cleaning in the former side in the lower-layer cleaning line 2 A, are communicated by the air duct 14 . The clean air processed by a HEPA filter or the like in a clean air supplying unit 13 and supplied to the cleaning processing chamber 2 g and 2 h , which carries out precision cleaning in the upper-layer cleaning line 2 B, is sent to the cleaning processing chamber 2 a , which carries out rough cleaning in the lower-layer cleaning line 2 A, via the air duct 14 and is reutilized as the air for the clean environment of the cleaning processing chamber 2 a.
[0091] The washing water for rough cleaning and the air for the cleaning ambient introduced into the cleaning processing chamber 2 a for rough cleaning is discharged to outside from a water/air discharge outlet 15 provided in the bottom of the cleaning processing chamber 2 a.
[0092] Note that the cleaning processing chambers 2 a to 2 h in the lower-layer and upper-layer cleaning lines 2 A and 2 B can be replaced or rearranged by cleaning processing chambers with approximately the same outer shapes and different cleaning processing functions. The lower-layer and upper-layer cleaning lines 2 A and 2 B are configured so that at least either one of them is always operated.
[0093] Inter-chamber transporting machines 16 serving as inter-chamber transporting means are disposed between the cleaning processing chambers 2 a to 2 h in the lower-layer and upper-layer cleaning lines 2 A and 2 B respectively. The inter-chamber transporting machine 16 sequentially transports the wafer W to adjacent cleaning processing chambers (for example, 2 a and 2 b ).
[0094] The first transporting machine 5 picks up the unpolished wafer W from the cassette 8 placed in the product wafer load port 3 a , 3 a and transports the wafer to a wafer standby position 17 . Also, the first transporting machine 5 directly receives the wafer W, which has undergone cleaning processes in the lower-layer or upper-layer cleaning line 2 A and 2 B, from the last cleaning processing chamber 2 d or 2 h thereof and transports the wafer into the product wafer load port 3 a and 3 a.
[0095] The center transporting machine 6 receives the unpolished wafer W from the wafer standby position 17 and transports the wafer into the polishing apparatus 4 via a passing position 18 . The transporting machine also receives the wafer W, which has undergone polishing, via the passing position 18 and transports the wafer to each of the cleaning processing chambers 2 a to 2 h of the lower-layer and upper-layer cleaning lines 2 A and 2 B. The center transporting machine 6 comprises a function of directly carrying in/out into or from any of the cleaning processing chambers 2 a to 2 h of the lower-layer and upper-layer cleaning lines 2 A and 2 B. Therefore, a front transporting opening 19 for carrying in/out the wafer W is provided in each of the cleaning processing chambers 2 a to 2 h of the lower-layer and upper-layer cleaning lines 2 A and 2 B.
[0096] The option chamber 7 comprises functions of subjecting the wafer W, which has not undergone polishing, has undergone polishing, or has undergone a cleaning process, to a predetermined process, film-thickness measurement, or the like in addition to the above described polishing and cleaning process, then passing the wafer W to the center transporting machine 6 , and transporting the wafer to a required next process via the center transporting machine 6 . The front transporting opening 19 for carrying in/out the wafer W is also provided in the option chamber 7 .
[0097] The working of the cleaning apparatus, which is configured in the above described manner, will next be described. In the cleaning apparatus of the present embodiment, the cleaning lines 2 A and 2 B are configured to have two levels of the lower-layer and the upper-layer; therefore, various cleaning processing modes such as (a) carrying out a series of cleaning processes from rough cleaning to precision cleaning merely by the lower-layer cleaning line 2 A, (b) carrying out a series of cleaning processes from rough cleaning to precision cleaning merely by the upper-layer cleaning line 2 B, (c) carrying out cleaning processes from rough cleaning to precision cleaning sequentially from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B, and (d) carrying out a series of cleaning processes in parallel from rough cleaning to precision cleaning respectively in the upper-layer cleaning line 2 B and the lower-layer cleaning line 2 A can be employed. Hereinafter, these modes will be sequentially described.
[0098] (a) This is the case in which a series of cleaning processes from rough cleaning to precision cleaning is carried out merely in the lower-layer cleaning line 2 A. In this case, the wafer W, which has undergone chemical mechanical polishing in the polishing apparatus 4 , is received by the center transporting machine 6 via the passing position 18 and transported to the cleaning processing chamber 2 a , which is in the starting-end side in the lower-layer cleaning line 2 A and carries out rough cleaning. The transported wafer W is subjected to required cleaning processes including rough cleaning while the wafer is transported to the adjacent cleaning chamber 2 b by the inter-chamber transporting machine 16 , precision cleaning and a drying process is carried out in cleaning processing chambers 2 c and 2 d in the latter-side, and the cleaning process is finished. After the cleaning process is finished, the wafer W is directly passed from the last cleaning processing chamber 2 d to the first transporting machine 5 and transported into the product wafer load port 3 a or 3 a.
[0099] (b) This is the case in which a series of cleaning processes from rough cleaning to precision cleaning are carried out merely in the upper-layer cleaning line 2 B. In this case, the wafer W, which has undergone chemical mechanical polishing, is directly transported to the cleaning processing chamber 2 e , which is in the starting-end side of the upper-layer cleaning line 2 B and carries out rough cleaning, by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes while the wafer is transported to the adjacent cleaning processing chamber 2 f by the inter-chamber transporting machine 16 , the wafer is subjected to precision cleaning and a drying process in the latter-side cleaning processing chambers 2 g and 2 h , and the cleaning process is finished. In this process, since each of the cleaning processing chambers 2 e to 2 h in the upper-layer cleaning line 2 B is disposed on the apparatus frame via anti-vibration rubber or the like serving as an anti-vibration means, transmission of the vibration that is generated upon operation of each of the cleaning processing chambers 2 e to 2 h to the transporting machines 5 , 6 , 16 , or the like can be suppressed, and stable transporting of the wafer W can be carried out. After the cleaning process is finished, the wafer W is directly passed from the last cleaning processing chamber 2 h to the first transporting machine 5 and transported to the product wafer load port 3 a or 3 a.
[0100] (c) This is the case in which cleaning processes from rough cleaning to precision cleaning are sequentially carried out from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B. In this case, first, the wafer W, which has undergone chemical mechanical polishing, is transported to the cleaning processing chamber 2 a in the starting-end side of the lower-layer cleaning line 2 A by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes including rough cleaning while the wafer is transported to the adjacent cleaning processing chamber 2 b by the inter-chamber transporting machines 16 . Then, at the point when required cleaning processes including rough cleaning are carried out in the two cleaning processing chambers 2 a and 2 b in the lower-layer cleaning line 2 A, the wafer W is carried out by the center transporting machine 6 and subsequently transported into the cleaning processing chamber 2 g in the latter side in the upper-layer cleaning line 2 B by the center transporting machine 6 . The transported wafer W is subjected to a required cleaning process including precision cleaning while the wafer is transported to the adjacent cleaning processing chamber 2 h by the inter-chamber transporting machine 16 , a drying process is carried out in the last cleaning processing chamber 2 h , and the cleaning process from rough cleaning to precision cleaning from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B is finished.
[0101] In this process, the pure water and clean air used in the cleaning processing chambers 2 g and 2 h , which carries out precision cleaning in the latter side in the upper-layer cleaning line 2 B, is introduced into the cleaning processing chamber 2 a as the washing water and the air for clean ambient of the cleaning processing chamber 2 a , which carries out rough cleaning in the lower-layer cleaning line 2 A, and effectively reutilized. Also, in the manner similar to that described above, transmission of the vibration generated upon operation of the cleaning processing chambers 2 g and 2 h in the upper-layer cleaning line 2 B to the cleaning processing chambers 2 a and 2 b in the lower-layer cleaning line 2 A and the transporting machines 5 , 6 , 16 , or the like can be suppressed, thereby providing stable cleaning performance and transport of the wafer W. When the cleaning process from rough cleaning to precision cleaning is finished, the wafer W is passed from the last cleaning processing chamber 2 h in the upper-layer cleaning line 2 B to the first transporting machine 5 and transported to the product wafer load port 3 a , 3 a.
[0102] (d) This is the case in which a series of cleaning processes from rough cleaning to precision cleaning is carried out in parallel respectively in the upper-layer cleaning line 2 B and the lower-layer cleaning line 2 A. In this case, the wafer W, which has undergone chemical mechanical polishing, is transported to the starting-end side cleaning processing chamber 2 e , which carries out rough cleaning in the upper-layer cleaning line 2 B, by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes including rough cleaning while the wafer is transported to the adjacent cleaning processing chamber 2 f by the inter-chamber transporting machine 16 , precision cleaning and a drying process is carried out in the latter-side cleaning processing chambers 2 g and 2 h , and the cleaning process is finished. The cleaning-process-finished wafer W is passed from the last cleaning processing chamber 2 h to the first transporting machine 5 and transported to the product wafer port 3 a , 3 a.
[0103] Approximately in parallel with this process, another wafer W, which has undergone chemical mechanical polishing, is transported to the cleaning processing chamber 2 a , which carries out rough cleaning in the starting-end side of the lower-layer cleaning line 2 A, by the center transporting machine 6 . The transported wafer W is subjected to required cleaning processes including rough cleaning while the wafer is transported to the adjacent cleaning processing chamber 2 b by the inter-chamber transporting machine 9 , precision cleaning and a drying process is carried out in the latter-side cleaning processing chambers 2 c and 2 d , and the cleaning process is finished. The cleaning-process-finished wafer W is passed from the last cleaning processing chamber 2 d to the first transporting machine 5 and transported to the product wafer load port 3 a and 3 a . In this process, the pure water and clean air used in the cleaning processing chambers 2 g and 2 h , which carries out precision cleaning in the latter side in the upper-layer cleaning line 2 B, is reutilized by being introduced into the cleaning processing chamber 2 a as the washing water and air for the clean ambient of the cleaning processing chamber 2 a , which carries out rough cleaning in the lower-layer cleaning line 2 A. Also, in the manner described above, transmission of the vibration generated upon operation of each of the cleaning processing chambers 2 e to 2 h in the upper-layer cleaning line 2 B to each of the cleaning processing chambers 2 a to 2 d in the lower-layer cleaning line 2 A and each of the transporting machines 5 , 6 , 16 , or the like can be suppressed, thereby realizing stable cleaning performance and transport of the wafer W. In this manner, the parallel processing of the wafer W is carried out by simultaneously operating each of the upper-layer and lower-layer cleaning lines 2 A and 2 B while arbitrarily reutilizing the pure water and clean air used in the precision cleaning in the upper-layer cleaning line 2 B as the washing water for rough cleaning and air for the purified ambient in the lower-layer cleaning line 2 A.
[0104] As described above, each of the cleaning processing chambers 2 a to 2 d in the lower-layer cleaning line 2 A and the cleaning processing chambers 2 e to 2 h of the upper-layer cleaning line 2 B are comprised of those approximately the same cleaning processing functions. The lower-layer and upper-layer cleaning lines 2 A and 2 B are configured so that at least either one of them is always operated. Therefore, in the case in which cleaning processes are carried out merely in the lower-layer cleaning line 2 A or merely in the upper-layer cleaning line 2 B, when either one of the cleaning lines is stopped for some reason, a required cleaning process can be carried out without any problem by switching execution of the cleaning process to the other cleaning line.
[0105] Each of the cleaning processing chambers 2 a to 2 d and 2 e to 2 h in the lower-layer and upper-layer cleaning lines 2 A and 2 B can be rearranged or replaced by cleaning processing chambers with approximately the same outer shapes and different cleaning processing functions. Therefore, when each of the cleaning processing chambers 2 a to 2 d and 2 e to 2 h are replaced or rearranged, the cleaning processing functions of each of the cleaning lines 2 A or 2 B can be arbitrarily changed.
[0106] As described above, in the cleaning apparatus according to the present embodiment, the wafer W, which has undergone chemical mechanical polishing, can be subjected to various cleaning processes, for example, successive processes can be carried out from the lower-layer cleaning line 2 A to the upper-layer cleaning line 2 B.
[0107] Parallel processing can be carried out in the lower-layer and upper-layer cleaning lines 2 A and 2 B, the processing speed of the wafer W per unit floor area can be increased, and the operating rate can be significantly improved.
[0108] Various wafers W to be subjected to different cleaning processes can be processed at the same time.
[0109] Carry in/out of the wafer W with respect to each of the cleaning processing chambers 2 a to 2 d and 2 e and 2 h of the lower-layer and upper-layer can be directly carried out by the common center transporting machine 6 , and the apparatus configuration can be simplified.
[0110] Upon rough cleaning in the former side in the lower-layer cleaning line 2 A, the pure water used in precision cleaning in the cleaning processing chamber in the latter side in the upper-layer cleaning line 2 B can be reutilized as the washing water for the rough cleaning, and the usage amount of pure water can be reduced.
[0111] The clean air supplied to the cleaning processing chamber, which carries out precision cleaning in the upper-layer cleaning line 2 B, is reutilized as the air for the clean ambient of the cleaning processing chamber, which carries out rough cleaning in the lower-layer cleaning line 2 A; thus, the cost of clean air supplying equipment can be reduced.
[0112] Transmission of the vibration generated upon operation of at least the cleaning processing chambers 2 e to h in the upper-layer cleaning line 2 B to the other cleaning processing chambers, each of the transporting machines, or the like can be suppressed; thus, always stable cleaning performance and transport of the wafer can be carried out.
[0113] The cleaning processing function of the entire cleaning apparatus is always maintained; thus, defects are not generated in in-process wafers W of pretreatment or the like.
[0114] In accordance with the cleaning treatment processes, or the like of the wafers W, the plurality of cleaning processing chambers 2 a to 2 d and 2 e to 2 h in each of the cleaning lines 2 A and 2 B can be replaced or rearranged to an optimal arrangement.
[0115] Various modifications can be made in the present invention without departing the spirit of the present invention, and it goes without saying that the present invention pertains to the modifications.
|
It is an object of the invention to provide a cleaning apparatus which can subject wafers that have undergone polishing to various cleaning processes while reducing the usage amount of pure water, increase the processing speed of wafers per unit floor area and significantly improve the operating rate, enable change or rearrangement of a plurality of cleaning processing chambers to more optimum arrangement in accordance with the cleaning treatment processes and the like, prevent generation of defects in wafers that are in process of, for example, pre-treatment, and simplify the configuration of the apparatus.
In order to achieve the above described object, the present invention provides a cleaning apparatus comprising cleaning lines 2 A and 2 B comprised of lower and upper two levels, each of the levels comprising a plurality of cleaning processing chambers 2 a to 2 d or 2 e to 2 h ; a center transporting means 6 comprising a function of transporting a wafer to be processed into or a function of transporting the processed wafer from each of the cleaning processing chambers 2 a to 2 h in the lower-layer and upper-layer cleaning lines 2 A and 2 B; an inter-chamber transporting means 16 for sequentially transporting the wafer to the adjacent cleaning processing chamber in each of the lower-layer and upper-layer cleaning lines 2 A and 2 B; and an introducing means for introducing pure water used in the cleaning processing chamber, which carries out precision cleaning in the upper-layer cleaning line 2 B, into the cleaning processing chamber, which carries out rough cleaning in the lower-layer cleaning line 2 A, as washing water for the rough cleaning.
| 7
|
The present invention relates to a dock installation and removal apparatus and method which may be used by a single person to install and remove a segmented dock.
BACKGROUND OF THE INVENTION
Removable docks are mainly used in small and medium size lakes and rivers to access boats. Such docks are removable primarily because many lakes and other bodies of water tend to freeze during the winter months. If the docks remain in the water, they may be damaged.
Known dock systems are difficult and time consuming to install, and generally cannot be easily installed by a single person. Known dock installation procedures often require either floating dock segments into place and then securing the floating sections to a support structure, or building the support structure from the lake or sea bed up. This invariably requires at least one of the installers to get in the water or utilize a boat. Since most people who are interested in installing a dock wish to do so in the spring or early summer, water temperatures are often low and not conducive to the type of work necessary to install a pier. Additionally, wind and wave conditions can affect the use of a boat.
Various docks and systems and apparatus have been proposed for installation and removal of docks. Examples are set forth in U.S. Pat. Nos. 3,999,379, 4,126,006, 4,645,380 and 5,108,230. However, these systems do not allow a single person to easily and quickly install and remove a dock and, in particular, a segmented dock. Accordingly, there is a need for an apparatus and method for installing and removing a segmented a dock which may be employed by a single person without requiring the person installing the dock to enter the water, float any dock segment on the water, or utilize a boat.
SUMMARY OF THE INVENTION
The present invention relates to an apparatus for installing and removing a segment of a segmented dock. The apparatus of the present invention is used to install or remove successive dock segments. Each dock segment includes a frame and a removable deck. The frame of each dock segment is supported above the surface of the water by a number of posts resting on the lake or sea bed.
The dock installing or removing apparatus (referred to herein as the dock installing apparatus or apparatus) includes a suspension structure adapted to be mounted on a previously installed dock segment and preferably mounted directly on or to the posts which support the previously installed segment. It should also be appreciated that the apparatus of the present invention could be used to install a first dock segment by attaching the suspension structure to the ground adjacent the desired position of the first dock segment. Two hinges are used to pivotally connect the frame of the dock segment to the frame of the previously installed dock segment. The hinges enable the frame of the segment to be positioned in a first, inverted or folded position on top of the previously installed segment and rotated or pivoted to a second non-inverted, upright, unfolded or extended position wherein the frame of the segment extends horizontally in substantially the same plane as the previously installed segment.
A frame rotator, preferably in the form of a pulley and cable system is connected to the suspension structure. The frame rotator rotates the frame of the segment from the inverted position (on top of the previously installed segment) to the non-inverted position adjacent to said previously installed segment. The suspension structure is adapted to support the segment in the non-inverted position while the installer attaches the removable deck member(s) to the segment being held in the non-inverted position. After installing the deck section or member(s), the person installing the dock may walk out onto the deck members on the suspended segment that is being installed, and sink posts for supporting the suspended segment from the suspended segment itself. Once all of the posts for the suspended segment have been put in place, the apparatus may be removed, and the new segment will be self-supporting. The apparatus may then be moved out to the newly installed segment, and the process repeated to install yet another segment of dock.
In addition to the apparatus outlined above, the present invention thereby further encompasses a method of installing a segment of a segmented dock. The method may be used on segmented docks in which each dock segment includes one or more deck sections supported by a frame, having first and second ends, and supported by a number of posts. The method involves the following steps. First, the suspension structure is mounted on one or more of the support posts associated with a first previously installed segment of dock. The suspension structure supports at least one pulley above a distal end of the first segment of dock, and the pulley in turn supports a cable. The frame associated with a second dock segment is placed upside down on the first dock segment. The pair of hinges are used to pivotally join the first end of the frame associated with the second dock segment to the second end of the first dock segment. Then, a first end of the cable is suitably fastened to the second end of the frame associated with the second dock segment.
Once the cable has been secured to the second end of the frame associated with the second dock segment, the frame is rotated by pulling the second end of the cable to raise the second end of the frame. After the frame associated with the second dock segment has been rotated past the vertical position, it may be lowered into position by releasing the cable in a controlled manner. Once in the desired position, the frame associated with the second dock segment remains suspended from the suspension structure by locking the cable or tying the cable to a fixed support. Suitable deck sections or members placed on the frame associated with the second dock segment and the posts are installed in the second dock segment. The posts are then attached to the frame associated with the second dock segment to support the second dock segment and the cable is released. The suspension structure may then be removed from the previously installed dock segment. The dock removal method of the present invention reverses this procedure.
Other objects, features and advantages of the invention will be apparent from the following detailed disclosure, taken in conjunction with the accompanying sheets of drawings, wherein like numerals refer to like parts, elements, components, steps and processes. It is therefore an advantage of the present invention to provide a dock installation apparatus and method.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a segmented dock and the apparatus of one embodiment of the present invention used to install a segment of a segmented dock;
FIG. 2 is a end view of the segmented dock and the apparatus of FIG. 1;
FIG. 3 is a side elevational view of the apparatus of FIG. 1 showing a frame of the segmented dock in a first inverted position on a previously installed segment of the dock;
FIG. 4 is a side elevational view of the apparatus of FIG. 1 mounted on a previously installed segment of dock, showing the frame in a partially rotated position;
FIG. 5 is a side elevational of the apparatus of FIG. 1 mounted on a previously installed segment of dock, showing the frame in a final horizontal or non-inverted position;
FIG. 6 is a fragmentary detailed view of one embodiment of an offset bracket used in conjunction with one embodiment of the present invention;
FIG. 7 is an enlarged fragmentary detailed view of the joint between frames of adjacent dock segments, with the frames in a first position and showing the hinge of one embodiment of the present invention;
FIG. 8 is an enlarged fragmentary detailed view of the joint between frames of adjacent dock segments, with frames in a second position and showing the hinge of one embodiment of the present invention; and
FIG. 9 is a fragmentary exploded top plan view of a previously installed dock segment and the frame of a dock segment yet to be installed.
DETAILED DESCRIPTION OF THE INVENTION
One embodiment of the apparatus for installing a segment of a segmented dock according to the present invention is shown in FIGS. 1 to 5 and generally indicated by numeral 10 , together with a segmented dock 12 in various stages of the dock installation process. The segmented dock 12 includes a first segment 14 which has been previously installed, and a second segment 16 which is in the process of being installed.
The first dock segment 14 includes a frame 18 mounted atop posts 20 , 22 and 24 . Complementary posts 20 a, 20 b and 20 c which can be partially seen in FIGS. 1 and 2 are also provided adjacent to posts 20 , 22 and 24 on the opposite side of the dock. The posts extend downwardly to the lake or sea bed to support the first dock segment 14 . Brackets 26 attach the posts to the frame 18 . The decking section(s) or member(s) 28 (generally referred to as the decking section) is/are mounted to the top of the frame 18 . The decking section 28 provides a generally flat surface on which a person may stand. The second dock segment 16 is substantially identical to the first dock segment 14 , and includes a frame 32 to be mounted atop posts such as post 34 in the same manner as the first dock segment 14 . Additional posts not shown in the drawings are provided to support the second dock segment 16 when installation of the second dock segment is complete. As with the first dock segment 14 , one or more decking sections or members such as decking sections 36 are mounted on the frame 32 to support a person on the dock 10 as described below. At least one and preferably two or more hinges are employed to join the second frame 32 to the first frame 18 as described in more detail. below. The hinge enables the second frame 32 to rotate vertically through approximately 180° relative to the first dock segment 14 while remaining joined thereto. It should be appreciated that the frame does not need to rotate a full 180°.
The apparatus 10 of the present invention is provided for installing successive dock segments to dock segments that have been previously installed. Thus, as seen in FIGS. 1 to 5 , the dock installation apparatus 10 is mounted to the posts 20 , 20 a, 22 , 22 a, 24 and 24 a of the previously installed dock segment 14 . The installation apparatus 10 includes a suspension structure 40 which is mounted to posts 24 and 24 a, both of which support the distal end of the previously installed dock segment 14 . A pair of offset mounting brackets 42 and 44 connect the posts 24 and 24 a to the suspension structure 40 . The offset mounting brackets 42 and 44 are configured to attach to the upper ends of the posts, extending outwardly so that the suspension structure itself is wider than the dock 12 . First and second vertical risers 46 and 48 extend upwardly from the offset mounting brackets 42 and 44 , respectively. A horizontal cross member 50 joins the upper ends of the vertical risers 46 and 48 , and supports a pair of pulleys 52 and 54 above the distal end of the previously installed dock segment 14 .
The suspension structure 40 may include first and second stabilizing beams 62 and 64 attached at an intermediate point along the length of the vertical risers 46 and 48 , respectively. The opposite ends of the stabilizing beams 62 and 64 are mounted on the top of the posts supporting either the middle or the proximal end of the previously installed dock segment 14 . In the embodiment shown, a first pair of stabilizing beam upper mounting brackets 66 is provided for attaching the stabilizing beams 62 and 64 to the vertical risers 46 and 48 , and a second pair of stabilizing beam lower mounting brackets 68 is provided for attaching the stabilizing beams to the mounting posts 26 and 26 a. Further, as best seen in FIGS. 3, 4 and 5 , the vertical risers 46 and 48 , and/or the horizontal cross member 50 may include outwardly angled projections or extenders 76 . The projections or extenders 76 enable the pulleys 52 and 54 to be mounted outwardly above the distal end of the previously installed dock segment 14 . In the embodiment shown, the projections or extenders 76 extend from the horizontal cross member 50 . In an alternative embodiment, the upper ends of the vertical risers 46 and 48 may be angled outwardly so that the entire horizontal cross member 50 is supported outwardly above the distal end of the previously installed dock segment 14 .
The dock installation apparatus 10 also includes first and second cables 56 and 58 and first and second winches 70 and 72 . The first cable 56 is wound onto the first winch 70 and pulled through the first pulley 52 . The free end of the first cable 56 may then be secured to the distal end of the frame 32 of the second dock segment 16 which is being installed. Similarly, the second cable 58 is wound onto the second winch 72 and pulled through the second pulley 54 . The free end of cable 58 may then also be secured to the distal end of the frame 32 , preferably in an opposite corner from where the first cable 56 is secured. The winches 70 and 72 may be mounted together on a board 74 which itself may be mounted to the tops of the posts supporting the proximal end of the previously installed dock segment such as posts 20 and 20 a as shown in FIG. 1 . Alternatively, the individual winches 70 and 72 could be mounted directly to the tops of the posts 20 and 20 a or could be mounted elsewhere on the previously installed segment of dock. Further, the winches 70 and 72 could be combined as a single winch, or could be omitted altogether and cables 70 and 72 could be manipulated manually. It should be appreciated that other suitable cable actuators and/or cable securing devices may be used in conjunction with the present invention.
A pair of floating leaf hinges 60 connect the frame 32 of the second dock segment 16 to the frame 18 of the previously installed dock segment 14 . The floating leaf hinges 60 are shown in detail in FIGS. 7 to 9 . Each hinge 60 includes first and second leaves 108 and 110 adapted to pivot about a hinge pin 112 as is commonly known in the art. The first leaf 108 may be rigidly affixed to the frame 32 of the second dock segment 16 . A metal bracket 114 defines a pocket or slot 116 along the end of frame 18 of the previously installed dock segment 14 . As can be seen in FIG. 9, two separate hinges 60 are provided between the frames 18 and 32 , and two brackets 114 are attached at the end of frame 18 . The brackets 114 are configured to receive the second leaf 110 of the hinge 60 . This construction enables the second leaf 110 to float vertically within the pocket 116 while remaining secured horizontally to the frame 16 by the bracket 114 . Thus, as shown in FIG. 8, the frame 32 of the second dock segment 16 may be placed in an inverted position above the previously installed dock segment 14 and the second leaves 110 of hinges 60 may be inserted into the pockets 116 defined by the brackets 114 to join frame 32 to frame 18 . The frame 32 may then be rotated vertically in a clockwise direction as seen from FIG. 7, to a non-inverted substantially horizontal position as shown in FIG. 8 . In this position, the second leaf 110 drops further into the pocket 116 to more firmly join the two frames. A bearing plate 118 may be bolted to the underside of the two frames 18 and 32 to further strengthen the joint between the two dock segments 14 and 16 .
One of the offset mounting brackets 42 and 44 and a portion of the previously installed dock segment are shown in detail in FIG. 6 . The dock segment includes the frame 18 which supports the decking section 38 . A spacer 78 is mounted to the frame 18 between the frame and a post mounting bracket 26 , both of which are bolted to the frame. The post mounting bracket forms a sleeve, and the post 24 is inserted through the sleeve. When the post is in the proper position, i.e. when the bottom of the post is resting on the lake or sea bed, and the upper surface of the dock is level, the frame 18 may be secured in place on the post 24 by a clamping screw 82 .
The offset bracket may be assembled from conventional pipe or conduit fittings. For example, in the embodiment depicted in FIG. 6, the offset bracket comprises a first coupler 84 , short nipples 86 , a 90° elbow 88 , a straight fitting 90 , a “T” 94 and couplers 96 . The first coupler 84 is provided for mounting the offset bracket on the end of post 24 . The first nipple 86 connects the first coupler 84 to elbow 88 , and the two horizontal nipples and the straight fitting 90 extend the bracket outwardly away from the post 24 . The “T” fitting joined to the outermost horizontal nipple 86 orients the upper end of the offset bracket in vertical direction to receive the vertical riser 46 . Finally, pipe couplers 96 are provided for securing the vertical riser 46 in place relative to the offset bracket 44 . It should be appreciated that any suitable alternative offset bracket structure, suitable offset mounting structure or the like may be used in connection with the present invention.
Returning to FIGS. 1 to 5 , the process of using the apparatus of the present invention for installing the second dock segment 16 will now be described. The frame 32 of the second dock segment 16 is placed upside down on the deck of the first, previously installed dock segment 14 as shown in FIG. 3 . With the inverted frame 32 lying in the surface of the first dock segment 14 , the two frames 18 and 32 are joined by the floating leaf hinges 60 as described above. Next, the free ends of the cables 56 and 58 are fastened to the distal end of the second frame 32 in opposite corners. Once the cables 56 and 58 are attached to the frame 32 , the cables 56 and 58 are pulled through the pulleys 52 and 54 by winding the winches 70 and 72 . The cables pull the distal end of the frame 32 upward, causing the entire frame 32 to rotate about the hinge 60 .
FIGS. 1, 2 and 4 show the position of the frame 32 when the cables 56 and 58 are fully wound onto the winches 70 and 72 . At that point, the frame 32 has been rotated slightly past vertical due to the fact that the pulleys are suspended outwardly from the distal end of the previously installed dock segment. The frame 32 may then be lowered into position by slowly unwinding the cables 56 and 58 from the winches 70 and 72 . When the frame 32 reaches a substantially horizontal position as shown in FIG. 5, the winches 70 and 72 may be locked, so that the cables 56 and 58 remain taught and support the frame 32 in the horizontal position. A first section of decking 36 of the second dock segment 16 may then be slid into position from the previously installed dock segment 14 . An individual installing the dock may then proceed out onto the deck section 36 supported by the cables 56 and 58 and the suspension structure 40 . From the first section of decking 36 , the individual installing the dock may sink the support post 34 and its counterpart on the other side of the dock at the mid point of the second dock segment 16 . Once the middle posts are in place and the frame 32 secured thereto, additional sections of decking (not shown) may be put into place at the end of the second dock section. Again, the individual installing the dock may then walk out onto the second section of decking and sink the support posts at the end of the frame 32 . It should be appreciated that cross stabilizing bars are preferably used to stabilize each set of posts.
Once the outermost posts have been installed, the entire apparatus 10 may be removed from the posts supporting the previously installed dock segment, and moved out to the posts supporting the newly installed dock segment 16 . The newly installed dock segment 16 then becomes the previously installed dock segment 14 and the process may be repeated. In this manner, any number of additional dock segments may be added to previously installed dock segments. Each successive dock segment may be added from the previously installed segments without the need to float segments of dock, or without requiring the installer of the dock to enter the water or utilize a boat.
It should be appreciated that to remove a segment of a segmented dock, the method of the present invention described above would be reversed. This would allow a single installer to remove a dock without requiring the person to enter the water or utilize a boat or float segments of the dock. It should also be appreciated that the present invention could be used to install different shaped docks. In particular, people desire T-shape or L-shape docks. The same method could be used to install segments necessary for the T-shape or L-shape docks. It should be appreciated that single segments may be used to form intersecting segments.
While the present invention has been described in connection with. what is presently considered to be the most practical and preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but on the contrary is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the claims. It is thus to be understood that modifications and variations in the present invention may be made without departing from the novel aspects of this invention as defined in the claims, and that this application is to be limited only by the scope of the claims.
|
An apparatus and method are provided for installing successive segments of a segmented dock. A suspension structure is connected to a previously installed segment of dock. The suspension structure includes a frame rotator for rotating a dock frame from an inverted position atop the previously installed dock segment to an extended position substantially parallel to the previously installed dock segment. The suspension structure suspends the frame in place while decking is added to the frame. Once the decking is installed, the person installing the dock may move onto the suspended segment in order to sink support poles from the suspended dock segment.
| 4
|
This application is a division of Application Ser. No. 09/289,871, filed Apr. 12, 1999, now U.S. Pat. No. 6,242,047.
BACKGROUND OF THE INVENTION
The present invention relates generally to a coated paper product having high gloss and brightness and the method of manufacturing such a product. In particular, the invention relates to a process for manufacturing a coated paper product with a surface comparable to a cast coated surface, that may be used, for example, as the facing sheet of a pressure sensitive laminate. In addition to this intended use, the product of the present invention is suitable for a variety of other printing and converting operations such as metallizing, foil laminating and printing, security label applications and, specialty packaging as well as upscale gift wrap and labels.
Such paper products have in the past been produced almost exclusively by a cast coating process. During cast coating, gloss development relies on a replication of the mirror-like finish on a dryer roll, as the applied coating is dried. However, production rates for the cast coating process are considerably slower than the production of coated paper on a high speed papermachine. Thus it would be desirable and advantageous to develop a high speed coating process that could be used to produce a cast coated surface on paper Examples of the cast coating process are disclosed in prior U.S. Pat. Nos. 4,241,143 and 4,301,210.
Another method for producing high gloss paper is disclosed in U.S. Pat. No. 5,360,657. In this patent, a process is disclosed in which a thermoplastic polymeric latex having a second order transition temperature of at least 80 degrees C., and an average particle size smaller than 100 microns is applied to paper which is subsequently calendered to produce high gloss. Other methods for producing high gloss paper include the application of a glossy overprint varnish onto a previously coated substrate. However, in the latter case, the glossy surface produced is not generally useful for offset printing because of the excessive ink drying time required.
It is also known, as disclosed for example in PCT published application WO 98/20201, that a printing paper having high brightness and gloss can be manufactured by applying to paper a coating comprising at least 80 parts precipitated calcium carbonate and at least 5 parts of an acrylic styrene copolymer hollow sphere plastic pigment. The published application also notes that a finishing step using a calender is required to achieve the gloss development, but the method of calendering is deemed to be not restrictive. Likewise, in an article entitled “Lightweight Coated Magazin Papers,” published in the Jul. 5, 1976 issue of the magazine PAPER, Vol. 186, No. 1, at pages 35-38, a relationship between calendering and the use of plastic pigments in coatings is disclosed. The article notes that polymers such as polystyrene are thermoplastic and pressure sensitive, and a pigment based on polystyrene will exhibit a high degree of calendering response.
These and other publications including an article entitled “Light Reflectance of Spherical Pigments in Paper Coatings,” by J. Borch and P. Lepoutre, published in TAPPI, February 1978, Vol. 61, No. 2, at pages 45-48; an article entitled “Plastic Pigments in Paper Coatings,” by B. Aluice and P. Lepoutre, published in TAPPI, May 1980, Vol. 63, No. 5, at pages 49-53; and an article entitled “Hollow-Sphere Polymer Pigment in Paper Coating,” by J. E. Young, published in TAPPI, May 1985, Vol. 68, No. 5, at pages 102-105, all recognize the use of polymer pigments in paper coatings, but none of these publications disclose the unique combination of coating formulation and finishing conditions disclosed herein.
SUMMARY OF THE INVENTION
The present invention relates generally to a coated paper product and method of producing it. More particularly, the invention relates to a coated paper product that can be manufactured on a high speed papermachine and still achieve a high gloss, high brightness surface typical of cast coated paper.
The coatings disclosed herein for practicing the present invention include conventional inorganic pigments such as clay and calcium carbonate in conjunction with elevated amounts of thermoplastic polymer latex beads. The beads are either hollow or solid in composition. Upon applying these coatings onto an uncoated but smoothened basestock, or onto a precoated basestock, it is possible to achieve a high gloss and smoothness with good printing properties when the coated surface is finished in a calendar device such as a supercalender containing heated rolls.
Paper produced with the high plastic pigment content coating preferred for the present invention is suitable for printing using conventional printing methods including sheet-fed litho offset, flexography, rotogravure and web offset.
The high gloss coatings of the present invention comprise standard coating pigments such as clay, ground or precipitated calcium carbonate, titanium dioxide and elevated amounts of plastic pigment. While the content of plastic pigment in the coating formulation plays a significant role in achieving high gloss, an equally important factor which contributes to the desired finished paper properties is the surface area of the paper which comprises plastic pigment. SEM micrographs of coated paper surfaces were analyzed for plastic pigment spheres on the surface of the paper. The number of spheres were counted and an approximate percent of the total area of the sheet was calculated. The results showed an effect of coating speed/coating solids on plastic sphere areas as a percent of surface area. It was noted that as coating speed increased, a greater amount of surface area was filled with plastic spheres producing greater gloss development. The reason for this is not clear, but one possible explanation is that at increasingly higher coating speeds, drying is more intense, and as water is driven from the coated surface during drying, the plastic spheres (being of equivalent density when filled with water and of lower density as water is evaporated), are transported through the coating to the surface of the coated paper. Therefore to achieve a target gloss, lower amounts of plastic pigment may be used when the method and speed of the coating application is taken into account.
In addition, the size of the plastic pigment plays a role in the performance of the coating, vis-a-vis gloss development. For example, paper gloss achieved with a 0.45 micron diameter solid sphere plastic pigment is not as good as that obtained with a hollow sphere plastic pigment when the percent of surface area is taken into consideration. It is postulated that this ineffectiveness may be related to the diameter and curvature of the sphere presented to incoming light and subsequent light scattering. For example, five 0.45 micron diameter solid spheres will occupy approximately the same space as a 1.0 micron diameter hollow sphere. However, hollow spheres can flatten upon calendering and create a plurality of multiple flat surfaces for more efficient light reflection and gloss development. Meanwhile the use of a 0.20 micron diameter solid sphere plastic pigment will more closely simulate a flatter surface than the 0.45 micron diameter spheres because approximately twenty five 0.20 micron diameter spheres will occupy the same space as a single 1.0 micron diameter hollow sphere.
In summary, the preferred coating formulation for achieving the results of the present invention comprises from 46-60% calcium carbonate, 0-33% coating clay, 0-5.5% titanium dioxide and from 14-35% plastic pigment. The preferred plastic pigment is a hollow sphere plastic pigment having a particle size of up to 1.0 micron diameter selected from the group consisting of polystyrene, acrylics and methaecrylates. However, solid sphere plastic pigments ranging from 0.20-0.45 micron diameter may be substituted for the hollow sphere pigment or blended with the hollow sphere pigment as desired.
The preferred finishing step in the manufacture of the high gloss coated paper disclosed herein involves a supercalender apparatus operated at speeds ranging from about 800-2800 fpm, and at calender loads of from about 1500-2000 phi, with one or more rolls heated to a temperature of from about 100-240 degrees F. It should be noted, however, that gloss development equivalent to that obtained with a super-calender apparatus may be obtained with a gloss calender or soft roll calender under appropriate operating conditions.
BRIEF DESCRIPTION OF THE DRAWINGS
The FIGURE of drawing is a plot showing the percent surface area containing plastic pigment vs. the percent plastic pigment in the coating.
DETAILED DESCRIPTION
The present invention will be more fully understood by reference to the following Examples.
EXAMPLE 1
Coatings containing from 7% to 35% of a hollow sphere plastic pigment having a diameter of 1.0 micron (Rohm and Haas HP-1055), were applied onto base stock having 10.0 lb/rm precoat and no precoat. Coated paper samples were then supercalendered. Paper gloss and smoothness data are shown in Table 1. The 10.0 lb/rm precoated sample achieved a 75° paper gloss greater than 91 with 14% or more plastic pigment in the coating. 60° gloss was 62 to 75, and 20° gloss was 30 to 37 for the same samples. As the plastic pigment level was increased, higher gloss values could be achieved at lower coat weight. Print gloss also increased with increased levels of plastic pigment in the coating. For the uncoated base stock, 75° paper gloss values of 84-94 were obtained; 60° gloss was 48-58, and 20° gloss was 20-24. Finished smoothness was less than on precoated base stock, which is what would be expected. Compared to the cast coated control, gloss and smoothness values were met or exceeded.
TABLE 1
75°
60°
20°
Parker
% Coating
Paper
Paper
Paper
Print Surf
Coat. Wt.
Condition
Pigment
Gloss
Gloss
Gloss
@ 10 kg
lb/rm
Base Stock: 10.0-lb/rm precoat
1
7
86
56
26
0.48
8.3
2
14
91
62
30
0.44
8.3
3
21
96
73
33
0.49
7.3
4
28
96
75
37
0.57
7.0
5
35
93
67
28
0.51
5.0
Base Stock: no precoat
6
7
84
49
20
0.67
9.6
7
14
89
52
20
0.65
8.5
8
21
89
48
22
0.68
7.0
9
28
93
58
24
0.66
7.1
10
35
94
48
24
0.64
6.5
Cast Coated Example
—
84
53
22
0.53
—
EXAMPLE 2
Laboratory studies were conducted using 1.0 micron diameter hollow sphere pigment and 0.45 micron diameter solid bead plastic pigments. A pilot coater was used to apply the coatings at 800 fpm, supercalendering was done at 800 fpm. Base stock was precoated with either 8.8 lb/rm or 2.0 lb/rm coating prior to high gloss top coat application. Results are found in Tables 2 and 3. Supercalendering was less intense for this trial, resulting in overall lower gloss values than Example 1. For both base stocks, with hollow sphere plastic pigment (conditions 1, 2 and 3) at 15% or 21% total pigment, paper gloss, print gloss, and smoothness were better than or equal to the cast coated example. At weight percent addition levels comparable to the hollow sphere pigment, paper gloss using the 0.45 micron diameter solid bead pigment (conditions 4, 5, and 6) were lower than both the hollow sphere pigment data and cast coated data. However, print gloss and smoothness were equivalent. Using a mixture of hollow sphere and 0.45 micron solid sphere pigments, (conditions 7 and 8), resulted in properties equivalent to hollow sphere pigment alone.
TABLE 2
75°
60°
20°
Parker
% Coating
Paper
Paper
Paper
Print Surf
Coat. Wt.
Condition
Pigment
Gloss
Gloss
Gloss
@ 10 kg
lb/rm
Base Stock: 8.8 lb/rm precoat
Plastic Pigment: 1.0 micron diameter hollow sphere
1
10
80
46
20
0.45
8.4
2
15
84
53
26
0.40
8.1
3
21
89
58
32
0.44
8.0
Plastic Pigment: 0.45 micron diameter solid bead
4
15
79
40
21
0.38
8.4
5
21
77
40
17
0.43
7.2
6
28
81
50
26
0.36
10.6
Plastic Pigment: 1.0 micron diameter hollow sphere and
0.45 micron diameter solid bead, HP:SB
7
15:7
86
55
28
0.42
7.5
8
14:14
86
52
28
0.59
8.1
Cast Coated Example
—
84
53
27
0.53
—
TABLE 3
75°
60°
20°
Parker
% Coating
Paper
Paper
Paper
Print Surf
Coat. Wt.
Condition
Pigment
Gloss
Gloss
Gloss
@ 10 kg
lb/rm
Base Stock: 2.0 lb/rm precoat
Plastic Pigment 1.0 micron diameter hollow sphere
1
10
83
47
26
0.62
9.8
2
15
88
55
27
0.52
9.0
3
21
90
59
30
0.56
9.3
Plastic Pigment: 0.45 micron diameter solid bead
4
15
81
48
27
0.54
10.1
5
21
80
45
23
0.61
9.4
6
28
85
50
31
0.53
10.3
Plastic Pigment: 1.0 micron diameter hollow sphere and
0.45 micron diameter solid bead, HP:SB
7
15:7
89
60
32
0.47
10.3
8
14:14
90
60
35
0.52
10.6
Cast Coated Example
—
84
53
27
0.53
—
EXAMPLE 3
Solid sphere plastic pigments with diameters of 0.20 micron and 0.45 micron diameter were compared. Weight percent of coating pigment was increased to 40% with the intent of improving the effectiveness of the 0.45 micron pigment. Table 4 shows that even at 40%, the 0.45 micron pigment was ineffective for gloss development. However, using the 0.20 micron bead at 40% addition gave a 75° paper gloss of 88 as shown in Table 4.
TABLE 4
Parker
% Coating
75° Paper
60° Paper
Print Surf
Coat Wt.
Condition
Pigment
Gloss
Gloss
@ 10 kg
lb/rm
Base Stock: 2.0 lb/rm precoat
Plastic Pigment: 0.45 micron diameter solid bead, HP:SB
1
40
79
41
0.76
11.1
Plastic Pigment: 0.20 micron diameter solid bead
2
40
88
57
0.60
12.6
EXAMPLE 4
High gloss paper coatings containing about 20% hollow sphere plastic pigment were applied with a high speed commercial coater at 2500 to 2700 fpm. In ten trials, paper was supercalendered over a broad range of conditions. Calendar speed ranged from 1000 to 1400 fpm, heated roll internal temperatures were 100 to 240° F., and calender loads ranged from 1500 to 1900 pli. Typical results are shown in Table 5. Paper gloss and smoothness greater than or comparable to a cast coated sheet were obtained.
TABLE 5
75°
60°
20°
Parker
% Coating
Paper
Paper
Paper
Print Surf
Coat. Wt.
Condition
Pigment
Gloss
Gloss
Gloss
@ 10 kg
lb/rm
Plastic Pigment 1.0 micron diameter hollow sphere
Base Stock: 2.0 lb/rm precoat
1
20.8
97
71
44
0.62
9.0
2
20.8
93
67
34
0.64
9.0
3
20.8
94
67
38
0.66
9.0
4
20.8
96
69
44
0.65
9.0
Cast Coated Example
—
—
84
53
27
0.53
—
It will therefore be seen that the coated paper product of the present invention can be manufactured on existing high speed papermachines using conventional processes. The favorable effect of the plastic pigment to the coating is exhibited within the range of from about 14-35% addition. The most favorable effect is obtained with the use of hollow sphere plastic pigment having a diameter o about 1.0 micron. Gloss development of the product is achieved by the flattening of the plastic pigment particles between existing particles of other pigments during the calendering process.
While the prior art discloses in general the use of plastic pigments in paper coatings, none discloses the use of the elevated amounts required to achieve the results of the present invention. It is speculated that such pigments have only been sparingly used in the past because of cost considerations and the Theological problems encountered with the use of such pigments. Nevertheless, applicants' herein have managed to overcome these problems and create a product that is competitive with conventional cast coated products.
While the preferred forms of the invention have been described in the Examples, variations will be apparent to those skilled in the art. Thus the invention is not limited to the embodiments described and modifications may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
|
A coated paper product having high gloss and brightness is prepared by a process wherein a paper substrate is coated on at least one side with an aqueous coating formulation comprising an effective amount of a plastic pigment, and finished in a supercalender device containing heated rolls to produce a surface which is comparable to a cast coated surface.
| 3
|
This is a continuation, of application Ser. No. 817,106, filed July 19, 1977 now abandoned.
BACKGROUND OF THE INVENTION
This invention relates to a squeegee arrangement, particularly one which is suitable for use in screen printing machines.
Squeegee arrangements must be readily mountable, easily cleanable and, perhaps most importantly, readily adjustable for various circumstances, such as the required ink (the term is used generically herein to designate coloring matter) application angle. This is the angle formed by the ink pool confined between the printing screen and the squeegee blade. This pool is of essentially wedge-shaped cross-section. It is known from fluid dynamics that the flatter a wedge shape into which a flowable substance is forced, the higher will be the pressure in the wedge-shaped area.
It is this pressure, present in all squeegee arrangements of the type under discussion and exerted by the ink as a function of the relative displacement of squeegee and printing screens, which causes the ink (usually of paste-like consistency) to be forced through the screen and onto (or into) the workpiece to be printed. This same pressure of course also exerts a reaction force upon the squeegee blade.
In known squeegee arrangements the reaction force is resisted by, e.g. a supporting block of the squeegee holder. However, whatever means have heretofore been provided for this purpose (to resist the reaction force and thus maintain the squeegee blade against displacement out of its proper operating position), have been unsatisfactory because they tend to also change the spring characteristic of the squeegee blade itself in an undesirable manner, namely by making the blade rigid in the area where it contacts the printing screen.
Thus, the more strongly the blade is supported against the reaction force, the harder will be the contact between it and the screen which has to be accepted as a trade-off for the supporting function. This is, evidently, a negative change in the squeegee-blade spring characteristic. Conversely, of course, the less supported the blade against deflection by the reaction force, the more it is deflected by this force and the more the angle of ink ejection through the screen will be changed. The spring characteristic of the blade is now too soft.
Heretofore it has been the industry practice to use different squeegee blades for different conditions. However, removal of the old and installation of the new blade is always a difficult and time consuming effort, requiring complete machine shut-down.
Proposals made for squeegee arrangements in German published application (DT-OS) 2,405,108 and in German patent (DT-PS) 1,964,182 and German allowed application (DT-AS) 1,121,074, have all been found unsatisfactory for overcoming the problems outlined above.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the invention to avoid the disadvantages of the prior art.
More particularly, it is an object to provide an improved squeegee arrangement (particularly for use in screen printing machines) wherein the spring characteristic of the squeegee blade is such that it increases uniformly over a relatively wide range of variations, i.e. under varying circumstances. The squeegee blade itself is to be elastically deformable to keep its friction with the printing screen low, and in order to avoid energy losses resulting from its contact with the screen.
In pursuance of these and other objects one feature of the invention resides in a squeegee arrangement, particularly for use in screen printing machines. Briefly stated, the arrangement may comprise a squeegee member having a squeegee blade of elastically deformable material, a holder for the squeegee member, a supporting blade on the holder and engaging the squeegee member, and a spring element engaging the squeegee blade and deflecting the same.
The novel features which are considered as characteristic for the invention are set forth in particular in the appended claims. The invention itself, however, both as to its construction and its method of operation, together with additional objects and advantages thereof, will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a fragmentary side view, partly in section, showing an embodiment of the invention in the context of a rotary-screen printing machine;
FIG. 2 is a view analogous to FIG. 1, but with details of that FIGURE omitted, showing another embodiment; and
FIG. 3 is a view similar to FIG. 2 but of still a further embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 illustrates in part a printing screen 1 of a rotary screen printing machine. Such screens are tubular, i.e. of circumferentially endless hollow cylindrical shape. The screen 1 rotates in direction of the arrow A. The invention can, however, also be used with flat printing screens and with endless-belt printing screens.
An ink supply tube 2 extends over the entire axial length of the tubular printing screen 1. It has a cover or hood 20 beneath which ink is forcibly ejected from the tube 2 through opening(s) 21. The ink then runs into an ink sump or pool 22 which is located ahead of (as considered in the direction of rotation A) the squeegee member 5. The cross-sectional shape and size of the pool 22 changes in dependence upon the quantity of ink supplied via tube 2 per unit time and upon the speed of travel of the screen 1 in direction A.
The squeegee arrangement according to the invention is mounted within the space surrounded by the screen 1, by means of a mount 3 which surrounds a gas-filled envelope 30 forming a gas cushion. This cushion bears upon an upper bar 40 of a squeegee holder 4 which is tiltably mounted on shaft 41 and resiliently restrained from such tilting by springs 42. Shaft 41 is mounted on consoles 43 (one shown) which are distributed over the axial length of the tube 2. Cushion 30 exerts downward pressure to urge the squeegee member 5 towards the inner surface of screen 1; the exerted pressure acts upon the free edge region of the blade of the squeegee member 5 above a spring element 6, as will be subsequently described.
At the lower side 44 of the holder 4 there is provided a supporting block 144 against which a retaining element 45 (e.g. a clamping bar) for the squeegee member 5 bears. The squeegee member 5 can be clamped or otherwise secured between the elements 144 and 45.
It is important that in the rear part of the angle α (see FIG. 1) the squeegee member 5 is held rigidly. The projecting part of member 5 (i.e. the squeegee blade), however, is supported in the region of its free edge (and screen-contact line 55) by an elastically yieldable spring element 6. This may be tongue-shaped in form of either a leaf spring or else in form of an elastomeric (i.e. rubber or rubber-like) member. The member 6 engages the rear side of the squeegee blade (i.e. the one facing upwardly away from contact line 55) at an acute angle and extends with its free end to or substantially to the line 55; under stronger pressure the member 6 slides on the rear side of the squeegee blade. The cross section of member 6, especially if the latter is elastomeric as shown, may be T-shaped and the member 6 may be matingly mounted in holder 4.
The arrangement assures that the squeegee blade is elastically supported close to the contact line 55 and even if the ink wedge 22 has an acute angle α and is under high pressure, the squeegee blade cannot flutter. Again, should the liquid pressure be low and the angle α be greater than shown, proper contact along the line 55 is still assured.
FIG. 2 is the same as FIG. 1, although parts have been omitted for simplicity, except that it shows that the angle α of FIG. 1 can be different and the invention will still be effective.
FIG. 3 is also the same as FIG. 1 except to show that the spring element 6' can be in form of a metallic leaf spring. Of course, synthetic plastic material can be used for the element 6' (irrespective of which shape it has); such material can be readily cleaned of adhering ink.
The arrangement according to the invention has a variety of significant advantages. Thus, the squeegee blade 5 may be made of steel (as shown) and will have little friction with respect to the screen 1. Even though the form of blade 5 may change substantially (due to deflection), the force with which it presses against the screen 1 will change only very little. The arrangement will always be properly positioned with reference to the direction of screen movement and any unevenness (e.g. the inner screen surface) will be readily accommodated because the squeegee blade 5 can flex freely and readily.
The blade 5 can adjust itself to different conditions over the widest possible range (e.g. when the blade 5 is urged towards or tends to recede upwardly from the screen under the influence of changes in the relatively variable gas pressure in envelope 30). The elasticity of blade 5 remains substantially unchanged over a wide range of different contact pressures (of blade 5 on screen 1) and the supporting force exerted upon the blade 5 by the element 6 or 6' will become only gradually stronger as the contact pressure of blade 5 on screen 1 increases. As this takes place the angle included between the elements 5 and 6 also changes, in that it becomes smaller.
Also, the arrangement according to the invention is very simple and inexpensive and can be readily cleaned and maintained.
While the invention has been illustrated and described as embodied in a squeegee arrangement for a rotary-screen printing machine, it is not intended to be limited to the details shown, since various modifications and structural changes may be made without departing in any way from the spirit of the present invention.
Without further analysis, the foregoing will so fully reveal the gist of the present invention that others can by applying current knowledge readily adapt it for various applications without omitting features that, from the standpoint of prior art, fairly constitute essential characteristics of the generic or specific aspects of this invention.
|
A squeegee arrangement has a holder which supports a squeegee member having a squeegee blade. A supporting block on the holder engages and supports the squeegee member. A spring element engages the squeegee blade at or in the vicinity of the longitudinally extending free edge thereof.
| 1
|
TECHNICAL FIELD
[0001] The present invention relates generally to dry gas seals for compressors, pumps and, more specifically, to protect the integrity of the primary dry gas seal during standstill conditions.
BACKGROUND
[0002] The application of dry gas seals to centrifugal compressor shaft sealing has dramatically increased in recent years for many reasons. The benefits offered by the use of dry gas seals on a centrifugal compressor include improved compressor reliability and the associated reduction of unscheduled downtime, elimination of seal oil leaking into the compressor and the associated process contamination, elimination of process gas contaminating the seal oil and requiring sour seal oil reclamation through degassing tanks, elimination of costs for replacement and disposal of sour seal oil, reduction of operating costs based on the greater efficiency of a dry gas seal, the reduction of maintenance costs for the simpler dry gas seal system and the reduction of process gas emissions.
[0003] Dry gas seal installation is also adoptable for centrifugal pumps associated with liquefied gas. The many benefits of dry gas seals at the running conditions of centrifugal compressors and pumps mask problems associated with the use of dry gas seals on centrifugal compressors and pumps at other operating conditions such as the transient times of startup, shutdown and low-speed idle. The reason dry gas seals are problematic at these times is based on the requirement of a higher than suction pressure barrier gas to prevent contamination of the dry gas seal with particulate or liquid materials. The contamination can arrive, for example, from the untreated process gas or from bearing lubrication oil.
[0004] A typical centrifugal compressor utilizing a dry gas seal will divert a portion of the process gas from the high-pressure discharge of the compressor then filter, dry and reduce the pressure of the gas. The clean and dry barrier gas is then injected upstream of the primary seal at a pressure slightly greater than the suction pressure of the compressor. The higher pressure barrier gas prevents the untreated process gas from entering the dry gas seal where contaminates can infiltrate the tight tolerances of the rotating dry gas seal surfaces and cause premature dry gas seal ring failure.
[0005] During transient times of operation, the pressure of the process gas from the discharge of the compressor is reduced to the point where it is equal to the suction pressure of the compressor. Consequently, it is no longer possible to use the flow from the discharge of the compressor as a barrier fluid. Upstream of the primary seal, in the seal chamber, there is a pressure very close to the suction pressure of the compressor or pump. Downstream of the primary seal there is a pressure established by a buffer fluid, typically nitrogen or air available at a pressure of four to seven bar. Further, the higher pressure and un-treated process gas permeates the primary dry gas seal, transporting particulate and liquid contamination. This problem is emphasized with carbon dioxide (CO 2 ) as the process flow. The carbon dioxide (CO 2 ) expansion through the tight tolerances of the dry gas seal rings can form ice on the seal rings. Subsequently, when the compressor returns to normal operating conditions, the contamination between the dry gas seal rings results in premature wear and failure of the dry gas seal.
[0006] Prior attempts to resolve this problem have centered on providing a booster for the process fluid to maintain the barrier gas at the conditions provided during normal operation of the compressor or pump. This solution requires the similar treatment of the process fluid with respect to filtering and heating to prevent contamination of the dry gas seal. Accordingly, market pressure is building for a system and method for preventing the backflow of process fluid, and the associated contaminates, through the dry gas seal during transient operating conditions.
SUMMARY
[0007] Systems and methods according to these exemplary embodiment descriptions address the above described needs by providing a small secondary compressor for boosting the pressure of an intermediate buffer gas during operating conditions (i.e., startup, shutdown and low-speed idle) when the fluid pressure from the discharge of the pump is equal to the suction pressure of the area to be sealed by the dry gas seal. A simple control system detects a drop in barrier gas pressure in the dry gas seal (i.e., the trigger signal could be but is not limited to simply the “no running” condition of the turbomachinery) and protects the dry gas seal from icing by closing a valve between the dry gas seal and a flare-safe area and starting the secondary compressor to boost the intermediate buffer gas to a preconfigured pressure based on the pressure of the process fluid in the area to be sealed by the dry gas seal.
[0008] According to an exemplary embodiment of a system for assuring a safe working condition of a dry gas seal during standstill operations, a barrier fluid pressure measuring system detects a drop in barrier fluid pressure. The exemplary embodiment continues with a valve connecting the chamber between primary and secondary seal with the flare. Further, the exemplary embodiment continues with a booster compressor for boosting the pressure of an intermediate buffer gas injected into the chamber between the primary and secondary seal. Next the exemplary embodiment comprises a control system for operating the booster compressor based on the measured pressure between the primary and secondary seal.
[0009] According to another exemplary embodiment, a method for assuring a safe working condition of a dry gas seal installed on a liquefied gas pump when the pump is in a transient operating condition, is presented. Continuing with the first step of the exemplary method embodiment, the method detects the barrier gas pressure below a preconfigured value. In the next step of the exemplary method embodiment, the method closes a valve connected to the dry gas seal. Further in the exemplary method embodiment, starting a booster compressor associated with an intermediate buffer gas and maintaining said chamber pressure at a preconfigured value.
[0010] In a further exemplary embodiment, a liquefied gas pump dry gas seal protection system is described. The exemplary embodiment includes a means to detect when the pressure of the barrier fluid drops below a lower limit. The exemplary embodiment further includes a means to regulate the flow from the dry gas seal to a flare-safe area. Continuing with the exemplary embodiment, included is a means to increase the pressure of an intermediate buffer gas injected into the dry gas seal. Continuing with the exemplary embodiment, included is a means to measure the pressure of the buffer gas. Next in the exemplary embodiment, a means to control the means to regulate flow and means to increase pressure based on the means to measure pressure and a preconfigured pressure value.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The accompanying drawings illustrate exemplary embodiments, wherein:
[0012] FIG. 1 depicts a prior art cross-section view of a dry gas seal and the associated gas support system in an operating condition;
[0013] FIG. 2 depicts a prior art cross-section view of a dry gas seal and the associated gas support system in a standstill condition;
[0014] FIG. 3 depicts an exemplary embodiment cross-section view of a dry gas seal and the associated gas support system in an operating condition;
[0015] FIG. 4 depicts an exemplary embodiment cross-section view of a dry gas seal and the associated gas support system in a standstill condition;
[0016] FIG. 5 depicts an exemplary embodiment pressure-enthalpy diagram illustrating the gas leakage flow through the primary dry gas seal when the pump is in the operating condition;
[0017] FIG. 6 depicts a prior art pressure-enthalpy diagram illustrating the gas leakage flow through the primary dry gas seal when the pump is in the standstill condition;
[0018] FIG. 7 depicts an exemplary embodiment pressure-enthalpy diagram illustrating the gas leakage flow through the primary dry gas seal when the pump is in the standstill condition; and
[0019] FIG. 8 is a flowchart depicting a method for maintaining sufficient pressure in the chamber between the primary and secondary dry gas seal to prevent contamination of the primary dry gas seal.
DETAILED DESCRIPTION
[0020] The following detailed description of exemplary embodiments refers to the accompanying drawings. The same reference numbers in different drawings identify the same or similar elements. Also, the following detailed description does not limit the invention. Instead, the scope of the invention is defined by the appended claims.
[0021] Looking to FIG. 1 , a detailed diagram of a prior art exemplary embodiment of a dry gas seal (DGS) system 100 for a carbon dioxide (CO 2 ) pump is presented. It should be noted in the exemplary embodiment that any fluid in a supercritical state can be used as a barrier fluid in place of the exemplary carbon dioxide (CO 2 ). The exemplary embodiment reflects the behavior of the dry gas seal during operating conditions and includes a CO 2 pump 102 with its associated area to be sealed, a primary (inboard) seal 104 of a dry gas seal, a secondary (outboard) seal 106 of the dry gas seal, a process fluid filter 108 , a process fluid heater 110 , a valve and control element 112 for controlling the flow to a flare-safe area, an intermediate buffer gas filter 114 , intermediate buffer gas 116 , barrier fluid 118 , pressure reduction valve 120 , a primary dry gas seal chamber 122 and a secondary dry gas seal chamber 124 .
[0022] In general, this exemplary prior art embodiment depicts process fluid, e.g. carbon dioxide, from the pump discharge being used as a barrier fluid. The pressure of the barrier fluid is reduced by a valve 120 and heated by a heater 110 . Continuing with the exemplary prior art embodiment, the barrier fluid is filtered by filters 108 and injected into the primary dry gas seal chamber 122 . In the exemplary embodiment, the pressure of the barrier fluid is higher than the suction pressure of the pump and therefore prevents the entry of any untreated process gas into the primary seal 104 .
[0023] Continuing with the exemplary embodiment, the carbon dioxide (CO 2 ) barrier fluid flows partly into the pump through the inner labyrinth and partly to the primary vent through the primary dry gas seal. Next in the exemplary embodiment, the carbon dioxide (CO 2 ) that flows into the pump reaches a suction pressure that is higher than the critical pressure for carbon dioxide (CO 2 ) and accordingly will not experience icing or flushing. Further in the exemplary embodiment, the carbon dioxide (CO 2 ) that flows through the primary seal to the primary vent expands from P1 to a value established by the buffer gas (typically N 2 /air at 4-7 bar). It should be noted in the exemplary embodiment that the temperature of the carbon dioxide (CO 2 ) barrier fluid must be maintained, by a heater, to a value high enough to avoid, during the expansion, the risk of icing or flushing.
[0024] Continuing with the exemplary embodiment, an intermediate buffer gas 116 , e.g. nitrogen or dry air is filtered by filters 114 and injected into the secondary dry gas seal chamber 124 . It should be noted in the exemplary embodiment that gases other than nitrogen or air are usable as a buffer gas. In the exemplary embodiment, the pressure of the intermediate buffer gas 116 is higher than the pressure of the barrier gas passing through the primary seal 104 and prevents the barrier gas from reaching the secondary seal 106 . In the exemplary embodiment, the mixture of barrier gas 118 and intermediate buffer gas 116 in the secondary dry gas seal chamber 124 passes through a valve 112 and flows to a flare-safe area.
[0025] Looking now to FIG. 2 , a detailed diagram of a prior art exemplary embodiment of a dry gas seal (DGS) system 200 for a carbon dioxide (CO 2 ) pump is presented. The prior art exemplary embodiment reflects the behavior of the dry gas seal during a transient, e.g. standstill, condition and includes a CO 2 pump 202 with its associated area to be sealed, a primary (inboard) seal 204 of a dry gas seal, a secondary (outboard) seal 206 of the dry gas seal, a process fluid filter 208 , a process fluid heater 210 , a valve and control element 212 for controlling the flow to a flare-safe area, an intermediate buffer gas filter 214 , intermediate buffer gas 216 , barrier fluid 218 , pressure reduction valve 220 , a primary dry gas seal chamber 222 and a secondary dry gas seal chamber 224 .
[0026] Continuing with the prior art exemplary embodiment, the CO 2 pump is in a standstill condition and accordingly the discharge pressure from the pump is equal to the pressure in the area to be sealed 202 . When the pump is in a standstill condition, the pressure into the pump reaches a uniform value very close to the suction pressure, know as “settle out pressure”. It should be noted in the prior art exemplary embodiment that the result of the standstill condition is the process fluid from the pump discharge can no longer act as a barrier fluid to prevent the flow of untreated process fluid, from the area to be sealed 202 , into the primary seal 204 . Further in the prior art exemplary embodiment, the untreated process fluid is not heated or filtered and therefore contaminates can enter the primary seal 204 and icing can occur in the primary seal 204 . It should also be noted in the prior art exemplary embodiment that the pressure of the untreated process fluid is greater than the pressure of the intermediate buffer gas 216 therefore the intermediate buffer gas 216 cannot prevent the flow of untreated process fluid through the primary gas seal 204 .
[0027] Continuing with FIG. 3 , a detailed diagram of an exemplary embodiment of a dry gas seal (DGS) system 300 for a carbon dioxide (CO 2 ) pump is presented. The exemplary embodiment reflects the behavior of the dry gas seal during a operating, e.g. running, condition and includes a CO 2 pump 302 with its associated area to be sealed, a primary (inboard) seal 304 of a dry gas seal, a secondary (outboard) seal 306 of the dry gas seal, a flare valve 312 , and a control element for controlling the flow to a flare-safe area, an intermediate buffer gas filter 314 , intermediate buffer gas 316 , barrier fluid 318 , a primary dry gas seal chamber 322 , a secondary dry gas seal chamber 324 , a booster compressor 326 and, a booster compressor 326 discharge valve 328 , a booster compressor 326 inlet valve 330 and a booster compressor 326 bypass valve 332 .
[0028] In a non-limiting exemplary embodiment, while the pump is in a running condition, the pressure in the area to be sealed 302 is lower than the pressure of the barrier fluid 318 , provided from the pump discharge, and while the barrier fluid pressure is higher than the pressure of the area to be sealed, flare valve 312 and booster compressor 326 bypass valve 332 are open, booster compressor 326 discharge valve 328 and booster compressor 326 inlet valve 330 are closed and booster compressor 326 is deactivated. Continuing with the exemplary embodiment, the pressure of the barrier fluid does not allow the process fluid to flow through the primary seal 304 and prevents contamination and icing of the primary seal 304 .
[0029] Looking now to FIG. 4 , a detailed diagram of an exemplary embodiment of a dry gas seal (DGS) system 400 for a carbon dioxide (CO 2 ) pump is presented. The exemplary embodiment reflects the behavior of the dry gas seal during a transient, e.g. standstill, condition and includes a CO 2 pump 402 with its associated area to be sealed, a primary (inboard) seal 404 of a dry gas seal, a secondary (outboard) seal 406 of the dry gas seal, a valve 412 , and control element, for controlling the flow to a flare-safe area, an intermediate buffer gas filter 414 , intermediate buffer gas 416 , barrier fluid 418 , a primary dry gas seal chamber 422 , a secondary dry gas seal chamber 424 , a booster compressor 426 , a booster compressor 426 discharge valve 428 , a booster compressor 426 inlet valve 430 and a booster compressor 426 bypass valve 432 .
[0030] In a non-limiting exemplary embodiment, in “no running” conditions of the pump or compressor (trip, shutdown, startup, pressurized standstill, etc.), the pressure into the pump is uniform and is equal to the settle out pressure value and can no longer be used as a barrier fluid. In this exemplary embodiment condition, the flare valve 412 and the booster compressor 426 bypass valve 432 is closed, the booster compressor 426 discharge valve 428 and the booster compressor 426 inlet valve 430 is opened and the booster compressor 426 is activated. It should be noted in the exemplary embodiment that the booster compressor raises the pressure of the intermediate buffer gas 416 , injected into the secondary dry gas seal chamber 424 , to a predetermined pressure (P3) just below the pressure in the area to be sealed 402 . Continuing with the exemplary embodiment, the increased pressure of the intermediate buffer gas reduces the flow of process gas through the primary seal 404 and prevents contamination and icing of the primary seal 404 . The exemplary embodiment booster compressor 426 operates in a discontinuous fashion, performing ON/OFF cycles. Next, the exemplary embodiment booster compressor 426 is turned on and the pressure into the secondary seal chamber 424 rises until it reaches the pressure P3 and the booster compressor 426 is turned off. The exemplary embodiment continues with the pressure in the secondary seal chamber 424 slowly dropping, because of leakage of buffer gas through the secondary seal 406 . Continuing with the exemplary embodiment, when the pressure in the chamber 424 between the primary seal 404 and the secondary seal 406 drops below a predetermined value (P3−dP3), the booster compressor 426 is turned on. Further, it should be noted in the exemplary embodiment that when the pump returns to operating conditions and barrier fluid 418 pressure rises above the pressure in the area to be sealed 402 the booster compressor 426 is finally turned off
[0031] Turning now to FIG. 5 , in a pressure-enthalpy diagram 500 illustrated is the pressure reduction of the barrier fluid through the control valve 120 , the temperature rise of the barrier fluid through the heater 110 and the expansion of the treated leakage flow through the primary seal to the primary vent with the pump in running condition. The temperature in the exemplary embodiment is high enough to avoid flushing and icing during the expansion.
[0032] Continuing now to FIG. 6 , a carbon dioxide pressure-enthalpy diagram 600 of a prior art exemplary embodiment dry gas seal system in a standstill operating condition is presented. The prior art exemplary embodiment illustrates the pressure difference 602 occurring through the primary seal 604 during a standstill condition. In another aspect of the prior art exemplary embodiment, the enthalpy diagram 600 depicts the expansion 604 of the untreated carbon dioxide leakage flow through the primary seal and crossing the triple point 606 and the bi-phase zones of the diagram for carbon dioxide. Accordingly, the prior art exemplary embodiment indicates that icing will occur in and around the primary seal and will lead to premature failure of the primary seal.
[0033] Looking now to FIG. 7 , an exemplary embodiment of a carbon dioxide pressure—enthalpy diagram 700 of a dry gas seal system in a standstill operating condition is presented. The exemplary embodiment illustrates the pressure difference 702 occurring through the primary seal during a standstill condition. In another aspect of the exemplary embodiment, the enthalpy diagram 700 depicts the expansion 704 of the untreated carbon dioxide leakage flow through the primary seal and not crossing the triple point 706 and neither bi-phase zone of the diagram for carbon dioxide. Accordingly, the exemplary embodiment indicates that icing will not occur in and around the primary seal.
[0034] Continuing now to FIG. 8 , an exemplary method embodiment 800 for assuring a safe working condition of the dry gas seal and preventing flushing and/or icing when the pump or compressor is in a standstill condition is depicted. Starting at exemplary method embodiment step 802 , the pressure of the barrier fluid in the chamber upstream of the primary seal is measured. In this exemplary method embodiment, the measured barrier fluid pressure is compared to a preconfigured value and an indication is generated if the measured barrier fluid pressure is below the preconfigured value.
[0035] Next at exemplary method embodiment step 804 , if the indication is presented that the barrier fluid pressure is below the preconfigured value then a valve associated with the dry gas seal and a flare-safe area is closed. In one aspect of the exemplary method embodiment, the valve prevents the exit of any gas from the chamber between the primary seal and the secondary seal except by passing through the secondary seal. In another aspect of the exemplary method embodiment, closing the valve reduces the volume of intermediate buffer gas required to maintain the desired pressure. Further in the exemplary method embodiment, the intermediate buffer gas can be, but is not limited to, Nitrogen or dry air.
[0036] Next at exemplary method embodiment step 806 , a booster compressor is started to boost the pressure of the intermediate buffer gas injected into the chamber between the primary seal and the secondary seal. In another aspect of the exemplary method embodiment, the booster compressor is operated to maintain the pressure based on a preconfigured value for the chamber pressure that is near the value of the pressure of the process fluid in the area to be sealed by the dry gas seal. Continuing with the exemplary method embodiment, the preconfigured value can dynamically change based on changes in the pressure of the process fluid in the area to be sealed by the dry gas seal. It should be noted in the exemplary method embodiment that the process fluid can be, but is not limited to, carbon dioxide.
[0037] Continuing with the exemplary method embodiment, at step 808 the rise in pressure in the chamber between the primary seal and the secondary seal is monitored until the pressure reaches a specified pressure (P3). Next, at step 810 of the exemplary method embodiment, when the pressure reaches pressure P3, the booster compressor is turned off. Further, at step 812 of the exemplary method embodiment, the pressure is monitored until it falls to a lower specified threshold and the method returns to step 806 and restarts the booster compressor. It should be noted that the exemplary method embodiment continues to cycle in this fashion until the pump/compressor returns to a running condition.
[0038] The disclosed exemplary embodiments provide a system and a method for protecting a dry gas seal from at least icing conditions brought on by process fluid expanding through the primary seal of a dry gas seal. It should be understood that this description is not intended to limit the invention. On the contrary, the exemplary embodiments are intended to cover alternatives, modifications and equivalents, which are included in the spirit and scope of the invention as defined by the appended claims. Further, in the detailed description of the exemplary embodiments, numerous specific details are set forth in order to provide a comprehensive understanding of the claimed invention. However, one skilled in the art would understand that various embodiments may be practiced without such specific details.
[0039] Although the features and elements of the present exemplary embodiments are described in the embodiments in particular combinations, each feature or element can be used alone without the other features and elements of the embodiments or in various combinations with or without other features and elements disclosed herein.
[0040] This written description uses examples of the subject matter disclosed to enable any person skilled in the art to practice the same, including making and using any devices or systems and performing any incorporated methods. The patentable scope of the subject matter is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims.
|
Systems and methods for assuring a safe working condition of a dry gas seal when a pump/compressor is in a standstill condition. A small booster compressor is added to boost the pressure of an intermediate buffer gas injected into the chamber between a primary seal and a secondary seal of the dry gas seal. Control components detect when the barrier gas pressure drops below a preconfigured value and when detected, closes a valve in a line to a flare safe area and turns on the compressor. The boosted intermediate buffer gas, Nitrogen or dry air, slows the flow of untreated process gas through the primary seal of the dry gas seal and prevents icing of the primary seal.
| 5
|
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to the field of clamping arrangements for removably securing headers to the windshield frames of sport utility and other vehicles and more particularly to the field of such clamping arrangements for headers of frameless soft tops.
[0003] 2. Discussion of the Background
[0004] Headers are widely used to removably attach tops including soft tops to the windshield frames of sport utility and other vehicles. In most cases, the header is removably secured to the windshield frame by manually operated clamps or latches. A very common way of doing so involves providing a protruding loop member on the windshield frame and hooking an arm of the clamp under the loop member. The base of the clamp is fixed to the header and as the clamp is closed, the header is drawn downwardly into engagement with the top of the windshield frame. In other arrangements such as in U.S. Pat. No. 6,932,423 at its FIGS. 6 and 7 , the arm of the clamp is hooked under an edge of a recess in the windshield frame rather than under a protruding loop member. However, the basic operation is otherwise essentially the same.
[0005] In both such arrangements, the closing action of the clamp draws the header downwardly into engagement with the top of the windshield frame also creates an undesirable rearward rotational force on the header. This rotational force tends to rock or pivot the header rearwardly on the windshield frame, reducing the effectiveness of the weather seal between them. In some cases, the rotational force may actually lift and separate the front of the header from the windshield frame creating a gap into which dust, water, and other elements may penetrate and collect. In addition to these sealing problems, the esthetic look or lines between the header and windshield frame may also be detrimentally affected giving the impression the members are poorly designed or misfit. Further, with soft tops in particular, the fabric of the top may then be looser than desired detracting from the top's overall neat and taut appearance and causing the soft top to flap or otherwise create wind noise.
[0006] The most pronounced problems caused by such prior art clamps and the rearward rotational forces on the header they create are with frameless soft tops. That is, if the soft top has an underlying frame, the frame is normally affixed to the header and pivotally or otherwise mounted to the body of the vehicle. Such mountings to the vehicle body are typically more than strong enough to counter any rearward rotational force on the header by the manual clamps. The header engagement with the top of the windshield frame is then nearly ideal with a strong weather seal and a trim fit. However, with frameless soft tops, the rearward rotational forces created by conventional clamping arrangements remain a problem.
[0007] With these and other drawbacks in mind, the present invention was developed. In it, a clamping arrangement is provided that creates a forward rather than a rearward rotational force on the header. The forward rotational force then actually enhances the weather seal and fit between the header and the windshield frame. This is advantageous for all soft tops whether or not they have a frame. However, it is particularly desirable for frameless soft tops to help maintain the seal of their header against the windshield frame and their overall clean and taut appearance.
SUMMARY OF THE INVENTION
[0008] This invention involves a clamping arrangement for removably securing an elongated header for a vehicle soft top to the windshield frame of a sport utility or other vehicle. The arrangement includes first and second clamp sections. The first section is fixedly attached to the header and the second section is pivotally mounted or otherwise movable relative to the first. The first clamp section includes a downwardly open hook portion that is positionable over a catch member of a footman loop mounted to the main body of the windshield frame. The catch member is spaced from the main body of the windshield frame and preferably extends along a substantially horizontal axis.
[0009] In operation of the preferred embodiment and with the catch member received in the downwardly open hook portion and the hook portion extending over both the catch member and its axis, the second clamp section is manipulated to engage the main body of the windshield frame. This movement of the second clamp section in the preferred embodiment is in a first rotational direction (e.g., clockwise) generally about the axis of the catch member. Once the second clamp section engages the windshield frame, further closing of the arrangement will rotate the first clamp section and attached header in an opposite direction (e.g., counterclockwise) about the axis of the catch member. This will force or drive the header downwardly against the sealing cap on the top of the windshield frame where it will be secured in place.
[0010] In this manner, a forward torque or rotational force is created by the clamping arrangement on the header that presses or biases the header against the windshield frame and its sealing cap. This forward rotational force actually enhances the seal between the header and windshield frame. It also helps to align the header on the windshield as intended for a trim fit as well as giving the attached soft top the desired neat and taut appearance.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a perspective view of a sport utility vehicle with a soft top according to the present invention covering the cabin area.
[0012] FIG. 2 is an exploded view of the soft top and vehicle of FIG. 1 .
[0013] FIG. 3 is a view similar to FIG. 2 with the soft top shown in its secured position on the vehicle.
[0014] FIG. 4 is a view essentially from the driver's seat looking up at the front left corner of the vehicle showing a prior art clamping arrangement used to secure a soft top header to the vehicle windshield.
[0015] FIG. 5 is a view taken along line 5 - 5 of FIG. 4 but showing the prior art clamp in its open position initially engaging the windshield.
[0016] FIG. 6 is a view similar to FIG. 5 showing the undesirable rearward rotation of the header relative to the vehicle windshield that can occur due to the operation of the prior art clamp.
[0017] FIGS. 7-9 illustrate another prior art clamping arrangement in views similar to FIGS. 4-6 .
[0018] FIGS. 10-14 sequentially illustrate how the clamping arrangement of the present invention secures the header to the windshield frame in a manner that creates a forward rotational force on the header rather than a rearward one as in the prior art approaches of FIGS. 4-9 .
[0019] FIGS. 15-18 sequentially illustrate a second embodiment of the clamping arrangement of the present invention that also creates a forward rotational force on the header rather than a rearward one as in the prior art approaches of FIGS. 4-9 .
DETAILED DESCRIPTION OF THE INVENTION
[0020] FIG. 1 illustrates a vehicle 1 with a soft top 2 according to the present invention secured to the vehicle 1 over the cabin area 3 . In use, the soft top 2 can be easily and quickly removed ( FIG. 2 ) or attached ( FIG. 3 ) in place above the cabin area 3 . In the position of FIG. 3 , the illustrated soft top 2 extends from side-to-side between the members 9 of the safety bar arrangement of FIG. 2 and from front-to-back between the windshield frame 11 and the member 23 of the safety bar arrangement. The member 23 in this regard is immediately behind the driver's and passenger's seats 25 and 27 . In mounting the soft top 2 on the vehicle 1 as seen in FIGS. 2 and 3 , the main body 4 of the elongated header 6 attached to the soft top 2 is releasably secured by clamping arrangements 8 to the windshield frame 11 of the vehicle 1 .
[0021] In prior art approaches such as the one illustrated in FIGS. 4-6 , the soft top header 60 to which the fabric 100 (e.g., canvas, vinyl) of the top 20 is attached (e.g., by screws, snaps, or adhesives) is commonly secured to the windshield frame 111 by clamping arrangements such as 80 . The prior art clamping arrangement 80 as shown essentially has a first clamp section 80 , ( FIG. 5 ) fixedly attached to the header 60 and a second clamp section 80 ″ pivotally mounted to the first clamp section 80 ′. In operation, the second clamp section or arm 80 ″ is hooked at 84 under the upper edge 91 of the recess 93 in the windshield frame 111 . The clamp handle 80 ′″ is then manipulated to the lowered position of FIG. 6 to close the clamping arrangement 80 and bring the header 60 into tight engagement with the windshield frame 111 at its seal 111 ′. In doing so, an undesirable rearward rotational problem can occur as illustrated in FIG. 6 .
[0022] More specifically, this illustrated problem of FIG. 6 can develop because the clamp assemblies 80 used to releasably secure the header 60 to the vehicle windshield 111 create a rearward torque or rotational force F (see FIG. 6 ). The rearward rotational force F in turn tends to lift or rotate the main body 40 of the header 60 relative to the windshield 111 and its seal 111 ′. This rotation is generally about an axis or location 118 (see FIG. 6 ) and not only can compromise the seal between the main body 40 of the header 60 and the windshield sealing cap 111 ′ but also may even cause a distinct separation or crack to appear such as 119 in FIG. 6 .
[0023] The resulting drawbacks of such rearward rotation (even if only slight) can be quite significant from both an appearance standpoint and a structural one. As for example, the rotation tends to create an undesirable dip and looseness in the fabric portion 100 of the top 20 ( FIG. 6 ). This can greatly detract from the desired neat and taut appearance of the top 20 . Additionally, this looseness or slack can cause the fabric 100 to flutter when the vehicle 1 is driven creating undesirable cabin noise. Structurally, as previously mentioned, the rotation of the header 60 in FIG. 6 can compromise the normal seal between the main body 40 of the header 60 and the sealing cap 111 ′ of the windshield 111 . This in turn can allow water, dust, and air to actually enter the cabin onto the occupants in the vehicle 1 as well as create whistling noises when the vehicle 1 is driven.
[0024] The same rearward rotation problem occurs in other prior art clamping arrangements such as 90 in FIGS. 7-9 . In contrast to the prior art arrangement 80 of FIGS. 4-6 , the prior art clamping arrangement 90 of FIGS. 7-9 hooks its clamp arm 90 ′ at 94 ( FIG. 8 ) under a catch member 13 of the footman loop 15 (see also FIG. 7 ). The footman loop 15 as shown protrudes from the main body 111 ″ of the windshield 111 . Otherwise, the prior art clamping arrangement 90 operates essentially in the same manner as the arrangement 80 of FIGS. 4-6 , including creating the undesirable rearward torque or rotational force F tending to rock or lift the header 60 as in FIG. 9 .
[0025] To overcome these problems, the clamping arrangement 8 of the present invention was developed. In it as illustrated in FIGS. 10-14 , a clamping arrangement 8 is provided that creates a forward rotational force F′ ( FIGS. 13 and 14 ) on the header 6 rather than a rearward one as in the prior art approaches. The forward rotational force F′ then actually enhances the weather seal and fit of FIG. 14 between the header 6 at its main body 4 and the windshield frame 11 at its sealing member 11 ′. As discussed above, this design is particularly advantageous for frameless soft tops and other tops that do not have a stiff frame or other structure to counter the rearward rotational force created by the prior art clamps.
[0026] More specifically as illustrated in FIGS. 10 and 11 , the clamping arrangement 8 of the present invention has a first clamp section 8 ′ fixedly attached to the header 6 and a second clamp section 8 ″. The second clamp section 8 ″ as shown in FIG. 10 is mounted at 16 to the first clamp section 81 for pivotal movement relative thereto between the open position of FIG. 10 and the closed position of FIG. 14 . The first clamp section 8 ′ ( FIG. 10 ) has a downwardly open hook portion 18 . The hook portion 18 as shown is spaced from the main body 4 of the header 6 that engages the windshield frame 11 including its seal 11 ′ ( FIG. 14 ).
[0027] In operation, the header 6 is first manually manipulated from the position of FIGS. 10 and 11 to the position of FIG. 12 . In the position of FIG. 12 , the downwardly open hook portion 18 extends over the catch member 13 of the footman loop 15 that protrudes from the main body 11 , of the windshield frame 11 . The catch member 13 is then received ( FIG. 12 ) in the downwardly open hook portion 18 with the header portion 4 adjacent the windshield frame 11 . The catch member 13 establishes the substantially horizontal pivotal axis 17 and is preferably an elongated bar extending along the axis 17 . The pivotal axis 17 is fixed relative to the windshield frame 11 and in the position of FIG. 12 , the hook portion 18 extends over both the catch member 13 and the axis 17 . The part 181 of the hook portion 18 as in FIG. 12 is also positioned between the catch member 13 and the main body 11 ″ of the windshield frame 11 . In this manner, the hook portion 18 essentially straddles the catch member 13 in the illustrated embodiment.
[0028] The clamp lever 24 can then be manipulated to move or drive the second clamp section 811 generally about the axis 17 ( FIG. 12 ) to engage the brace member 26 of the second clamp section 811 with the windshield frame 11 ( FIG. 13 ). In doing so, the second clamp section 8 ″ is moved or driven as shown in a rotational direction R (e.g., clockwise in the orientation of FIGS. 12 and 13 ) about the pivotal axis 16 of the clamp 8 to engage the windshield frame 11 . This pivotal movement of the second clamp section 8 ″ is also generally about the pivotal axis 17 of the catch member 13 . In turn, the header 6 is forced or driven in an opposite rotational direction R′ (counterclockwise in FIGS. 12 and 13 ) about the axis 17 of the catch member 13 toward the brace member 26 to engage the header portion 4 with the windshield frame 11 ( FIG. 13 ). The clamp lever 24 can then be further moved to its overcenter position of FIG. 14 to secure the header 6 to the windshield 11 in a fixed relationship. In this fixed or secured position, the header portion 4 is engaged and pressed or biased under a force F′ against the windshield frame 11 including its seal 11 ′ and main body 11 ″.
[0029] It is noted that the fabric 10 of the soft top 2 can be wrapped about the header portion 4 as illustrated or not so wrapped and the windshield frame 11 can be provided with any number of designs of sealing caps at 11 ′ or none at all. The header portion 4 may then engage the main body 11 ″ of the windshield 11 directly in the sense of an abutting relationship or engage in a manner with other structure such as the fabric top 10 or seal 11 ′ pressed or pinched therebetween as in FIGS. 12-14 . The hooking of the first clamp section 8 ′ has also been illustrated in FIGS. 10-14 as being over an elongated catch or bar member 13 of a footman loop 15 . However, it could also hook over the lower edge or catch member 91 ′ of a recess such as 93 in the windshield frame 111 of FIG. 6 or other catch structure including a more circular loop (e.g., eyebolt). Additionally, the soft top 2 could have other designs than those illustrated covering all or other portions of the vehicle 1 . Further, the clamping arrangement of the present invention as discussed above has particular value for frameless soft tops that are essentially or predominately attached to the windshield frame by the clamps 8 . However, the invention also has desirable applications to soft tops with frames and other tops or accessories attachable to the windshield frame to reduce or eliminate the undesirable rearward torque created by prior art approaches.
[0030] FIGS. 15-18 illustrate a second embodiment of the present invention in which the first clamp section 8 ′ is still hooked at 18 over the catch or bar member 13 ( FIGS. 17 and 18 ). However, the second clamp section 8 ″ of this embodiment can be physically separable as in FIG. 15 from the first clamp section 8 ′ if desired. In operation, the threaded bolt 30 of the second clamp section 8 ″ can be passed between the legs 19 of the footman loop 15 (see FIGS. 15 and 16 ) into the threaded nut 32 on the header 6 ( FIG. 17 ). Tightening of the bolt 30 will then engage the plate 34 against the footman loop 15 forcing or drawing the header 6 along the axis 36 toward the second clamp section 8 ″. This action as in the first embodiment will create a forward rotational force F′ ( FIG. 17 ) driving or causing the header 6 and first clamp section 8 ′ affixed thereto to rotate about the catch member 13 and axis 17 to engage the header portion 4 and windshield 11 . Further tightening of the bolt 30 to the position of FIG. 18 will then secure the header portion 4 in a fixed relationship. In this fixed or secured position as in the first embodiment, the header portion 4 is engaged and pressed or biased under a force F′ against the windshield frame 11 including its seal 11 ′ and main body 11 ″.
[0031] The bolt 30 in this second embodiment could be off to one side of the footman loop 15 if desired. Either way, it will still create the rotation and forward force F′ on the header 6 as the header portion 4 is forced or drawn along the axis 36 of the bolt 30 to engage the windshield frame 11 . The bolt axis 36 in this regard as illustrated in FIGS. 17 and 18 is spaced from and substantially perpendicular to the pivotal axis 17 . The axis 36 is also forward of the axis 17 of the catch member 13 and substantially between the pivotal axis 17 and the windshield frame 11 .
[0032] The above disclosure sets forth a number of embodiments of the present invention described in detail with respect to the accompanying drawings. Those skilled in this art will appreciate that various changes, modifications, other structural arrangements, and other embodiments could be practiced under the teachings of the present invention without departing from the scope of this invention as set forth in the following claims.
|
A clamping arrangement for removably securing an elongated header for a vehicle soft top to the windshield frame of a sport utility or other vehicle. The arrangement includes first and second clamp sections. The first section is fixedly attached to the header and the second section is pivotally mounted or otherwise movable relative to the first. The first clamp section includes a downwardly open hook portion that is positionable over a catch member of a footman loop mounted to the main body of the windshield frame. In operation of the preferred embodiment, the second clamp section engages the main body of the windshield wherein the first section and attached header are then rotated forwardly about the axis of the catch member. This forces or drives the header downwardly against the sealing cap on the top of the windshield frame where it is then secured in place.
| 1
|
FIELD OF THE INVENTION
The invention relates to a vehicle headlight, in particular a motor vehicle headlight, comprising a first light source and comprising at least a second light source.
BACKGROUND INFORMATION
DE 10 2004 053 303 A1 discloses a vehicle headlight for generating a light intensity distribution pattern for dipped-beam light by the emission of light from a plurality of luminaire subunits, each of which has a light source with a semiconductor light emitting element, wherein at least one of the luminaire subunits is configured as a luminaire subunit which emits in the forward direction and which sends light in the forward direction of a vehicle, and at least one luminaire subunit is configured as a laterally emitting luminaire subunit which sends light towards the outer side in the direction of the width of the vehicle at an angle relative to the forward direction, and wherein each laterally emitting luminaire subunit has a reflector provided with a reflective surface having a curved surface in the form of a parabolic column, and a focal line running in the horizontal direction, wherein the reflector diffusely forms light from the light source in the horizontal direction.
DE 10 2004 053 320 A1 discloses a vehicle headlight having a main luminaire body, a base luminaire subunit, which is formed in such a way that it emits light for forming a light intensity distribution pattern for dipped-beam light, and an additional luminaire subunit, which is formed in such a way that it emits light for forming an additional light intensity distribution pattern by virtue of the fact that it temporarily shines into the main luminaire body, wherein a light source lamp is used as light source of the base luminaire subunit, and a semiconductor light emitting element is used as light source of the additional luminaire subunit.
Further vehicle headlights are disclosed in DE-10-2004 060 840 A1, DE 10 2004 061 873 A1, DE 198 14 480 A1, DE 100 27 981 A1, DE 195 39 422 C2 and DE-10-2004 062 286 A1.
DE 198 14 480 A1 discloses a headlight for vehicles according to the projection principle comprising a reflector, a light source, a lens through which passes light which is emitted by the light source and reflected by the reflector, and comprising at least one at least partly light-transmissive element which surrounds the lens at least on part of its periphery and which has optical profiles at least in regions and through which light which is emitted by the light source and cannot be picked up by the reflector passes and is collected, wherein the light which has been reflected by the reflector and has passed through the lens has an upper bright-dark boundary, and wherein the headlight has at least one additional light source for generating a side light which is arranged in such a way that light emitted by it at least partly passes through the element.
DE 100 27 981 A1 discloses a headlight with integrated parking light, comprising a housing, at least one light source and a light disc as termination of the headlight towards the outside, wherein the light disc is subdivided into a plurality of segments, wherein at least one segment is arranged opposite the light source for the parking light function and said one segment opposite the light source for the parking light function has an integrated optical system.
A vehicle luminaire disclosed in DE 103 61 303 A1 has a first luminous means for a first light function, a reflector for concentrating the light emitted by an emission location of the first luminous means, at least a second luminous means displaced upstream of the first luminous means for a second light function, and a back-reflector arranged between the first luminous means and the second luminous means. The reflector has a first prism structure having a first prism surface and second prism surface. In this case, the first prism surfaces are arranged for deflecting the light impinging directly on them from the emission location to the light disc.
It is an object of the invention to specify an improved vehicle headlight. It is a further object of the invention to lower the costs for the production of vehicle headlights.
SUMMARY OF THE INVENTION
The aforementioned object is achieved by means of a vehicle headlight or vehicle front headlight, in particular motor vehicle headlight or motor vehicle front headlight, comprising a first light source, comprising at least a second light source and comprising a transparent shaped part configured in one piece, wherein the shaped part comprises a first optical structure for the direction of light emitted by the first light source and at least a second optical structure for the direction of light emitted by the second light source, and wherein the first optical structure and the second optical structure each comprise a continuously curved surface or a continuous, curved surface each having an extent of at least half a centimeter, in particular one centimeter, in two orthogonal directions. A surface has an extent of at least a minimum longitudinal extent in two orthogonal directions in particular when the surface comprises or completely covers at least one circle having a diameter corresponding to the minimum longitudinal extent. A first optical structure within the meaning of the invention is in particular a light-concentrating structure. A continuous surface within the meaning of the invention is in particular a continuously derivable surface. A continuous surface within the meaning of the invention has in particular no jumps within the aforementioned minimum extent.
In a further configuration of the invention, the first light source in conjunction with the first optical structure, and also if appropriate further elements, such as e.g. a reflector, forms a dipped-beam light, a full-beam light and/or a fog light.
In one configuration of the invention, the first light source in conjunction with the first optical structure directs light in a different direction from the second light source in conjunction with the second optical structure.
In a further configuration of the invention, the first light source comprises a lamp, in particular a gas discharge lamp or an incandescent lamp, or is configured as a lamp, in particular a gas discharge lamp or an incandescent lamp. The first light source may be e.g. a halogen lamp or a xenon luminaire. Suitable configurations for the first light source can be gathered e.g. from pages 739 to 753 of the book “Bosch, Kraftfahrtechnisches Taschenbuch” [“Bosch, Automotive Technology Handbook”], 23rd edition, Vieweg, 1999, ISBN 3-528-03876-4. However, it may also be provided that the first light source is an LED or an arrangement of LEDs. In this case, the LED or the arrangement of LEDs is configured in particular in such a way that it can be used to implement a dipped-beam light, a full-beam light and/or a fog light.
In a further configuration of the invention, the second light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode. The use of LEDs for signal luminaires for motor vehicles is disclosed e.g. in DE 102 07 431 A1, DE 102 37 263 A1 and DE 195 07 234 B4.
In a further configuration of the invention, the vehicle headlight comprises at least a third light source, wherein the shaped part has at least a third optical structure for the direction of light emitted by the third light source. In a further configuration of the invention, the third light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode.
In a further configuration of the invention, the first, the second and/or the third optical structure and/or a further optical structure is blank-pressed. In a further configuration of the invention, the shaped part is blank-pressed, in particular on both sides. Blank-pressing is to be understood within the meaning of the invention as, in particular, pressing a lens such that subsequent processing of an optically active surface of the lens after pressing can be obviated.
In a further configuration of the invention, the first optical structure is configured as a lens or as part of a lens. In a further configuration of the invention, the first optical structure is configured as a projection lens or as part of a projection lens. In a further configuration of the invention, the first optical structure is configured as a converging lens or as part of a converging lens. In a further configuration of the invention, an optically active surface of the first optical structure that is remote from the first light source is configured convexly or aspherically.
In a further configuration of the invention, the vehicle headlight comprises a light shield, wherein an edge of the light shield can be imaged as a bright-dark boundary by means of the first optical structure.
In a further configuration of the invention, the transparent shaped part substantially consists of glass or the transparent shaped part comprises glass.
In a further configuration of the invention, the transparent shaped part forms an outer part of the vehicle headlight. That is to say, in particular, that in a configuration of the invention no additional outer disc, such as, for instance, the transparent covering designated by reference symbol 30 in DE 10 2004 061 873 A1, is provided.
In a configuration it may be provided that an optical structure has substantially or virtually a roughness of less than 0.05 μm, in particular in the case of a light transmission at the surface of at least 90%. However, partial regions, in particular of the first optical structure, can have a greater roughness. Such partial regions having a greater roughness are configured in particular in accordance with DE 10 2004 011 084. Roughness within the meaning of the invention is to be defined in particular as R a , in particular according to ISO 4287.
In a further configuration it may be provided that an emblem is embossed in particular on a surface of the transparent shaped part which faces the (first) light source. Said emblem is advantageously arranged on that surface of the transparent shaped part which faces the first light source. The aforementioned emblem is advantageously configured in accordance with an emblem disclosed in DE 10 2004 011 104.
In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source or relative to an optical axis of the transparent shaped part (or e.g. the first optical structure) in such a way that light penetrating into the transparent shaped part through a surface remote from the (first) light source along or parallel to the optical axis of the transparent shaped part (or e.g. the first optical structure) is subjected to total reflection at the basic surface. In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source by an angle of between 25° and 80°, in particular between 35° and 60°, or relative to an optical axis of the transparent shaped part (or e.g. the first optical structure) by an angle of between 10° and 65°, in particular between 30° and 55°.
It may be provided that, on that surface of the first optical structure which faces the first light source or on that surface of the transparent shaped part which faces the light source, in the region of the first optical structure, the arrangement comprises an, in particular blank-pressed, deformation or embossing for deflecting part of the light that can be generated by the first light source into a secondary luminous region outside a main luminous region of the first light source in conjunction with the first optical structure. The deformation or embossing may be configured in accordance with a deformation or embossing disclosed in DE 10 2004 024 107. As an alternative or in addition, by means of a further (e.g. the second) light source in conjunction with a further (e.g. the second) optical structure, light can be directed into said secondary luminous region. In a configuration, at least 95%, in particular at least 97%, of the light which can emerge or emerges from the first optical structure is allotted to the main luminous region. In a further configuration, less than 5%, in particular less than 3%, of the light which can emerge or emerges from the first optical structure, but advantageously at least 0.2%, in particular at least 0.5%, of the light which can emerge or emerges from the first optical structure is allotted to the secondary luminous region. By way of example, traffic signs can be illuminated or lit up by means of the secondary luminous region. Main luminous region and secondary luminous region should be regarded as separate if an unilluminated region lies between them. In said unilluminated region, the light intensity is virtually zero or negligibly small.
In a further configuration, substantially no light from the second light source passes through the first optical structure and substantially no light from the first light source passes through the second optical structure.
In a further configuration, the continuously curved or continuous, curved surface of the first optical structure comprises an extent of at least two centimeters, in particular of at least four centimeters, in two orthogonal directions. In a further configuration, the continuously curved or continuous, curved surface of the first optical structure and the continuously curved or continuous, curved surface of the second optical structure each comprise an extent of at least two centimeters, in particular of at least four centimeters, in two orthogonal directions.
The aforementioned object is additionally achieved by means of a transparent shaped part comprising one or more of the aforementioned features.
The aforementioned object is additionally achieved by means of a motor vehicle comprising a vehicle headlight or vehicle front headlight comprising one or more of the aforementioned features. In a configuration of the invention, in this case the bright-dark boundary can be imaged onto a roadway on which the motor vehicle can be arranged.
The aforementioned object is additionally achieved by means of a vehicle headlight or vehicle front headlight, in particular motor vehicle headlight or motor vehicle front headlight, comprising a first light source, comprising at least a second light source and comprising a transparent shaped part configured in one piece, wherein the shaped part comprises a first convex lens for the direction of light emitted by the first light source and at least a second convex or concave lens for the direction of light emitted by the second light source, and wherein the substantial part of the light which is emitted by the first light source and passes through the transparent shaped part emerges from the first convex lens. A convex lens in this sense is in particular a lens having at least one convex surface. A convex lens in this sense is in particular a lens having two convex surfaces, a lens having one convex surface and having one concave surface or a lens having one convex surface and having one plane surface. If a convex lens in this sense comprises a lens having one convex surface and having one concave surface, these surfaces are configured in particular in such a way that the convex lens is configured in light-concentrating fashion.
Within the meaning of the invention, the substantial part of the light which is emitted by a light source and passes through the transparent shaped part is intended to be or comprise in particular substantially all of the light reduced by scattered light.
In a configuration of the invention, the substantial part of the light which is emitted by the second light source and passes through the transparent shaped part emerges from the second convex or concave lens.
In a further configuration of the invention, the first convex lens and the second convex or concave lens each comprise an extent of at least one centimeter in two orthogonal directions.
In a further configuration of the invention, the first light source in conjunction with the first convex lens, and also if appropriate further elements, such as e.g. a reflector, forms a dipped-beam light, a full-beam light and/or a fog light.
In one configuration of the invention, the first light source in conjunction with the first convex lens directs light in a different direction from the second light source in conjunction with the second convex or concave lens.
In a further configuration of the invention, the first light source comprises a lamp, in particular a gas discharge lamp or an incandescent lamp, or is configured as a lamp, in particular a gas discharge lamp or an incandescent lamp. The first light source may be e.g. a halogen lamp or a xenon luminaire. Suitable configurations for the first light source can be gathered e.g. from pages 739 to 753 of the book “Bosch, Kraftfahrtechnisches Taschenbuch” [“Bosch, Automotive Technology Handbook”], 23rd edition, Vieweg, 1999, ISBN 3-528-03876-4. However, it may also be provided that the first light source is an LED or an arrangement of LEDs. In this case, the LED or the arrangement of LEDs is configured in particular in such a way that it can be used to implement a dipped-beam light, a full-beam light and/or a fog light.
In a further configuration of the invention, the second light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode. The use of LEDs for signal luminaires for motor vehicles is disclosed e.g. in DE 102 07 431 A1, DE 102 37 263 A1 and DE 195 07 234 B4.
In a further configuration of the invention, the vehicle headlight comprises at least a third light source, wherein the shaped part has at least a third convex or concave lens for the direction of light emitted by the third light source. In a further configuration of the invention, the third light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode.
In a further configuration of the invention, the first, the second and/or the third convex or concave lens and/or a further convex or concave lens is blank-pressed. In a further configuration of the invention, the shaped part is blank-pressed, in particular on both sides. Blank-pressing is to be understood within the meaning of the invention as, in particular, moulding a lens such that subsequent processing of an optically active surface of the lens after pressing can be obviated.
In a further configuration of the invention, the first convex lens is configured as a lens or as part of a lens. In a further configuration of the invention, the first convex lens is configured as a projection lens or as part of a projection lens. In a further configuration of the invention, an optically active surface of the first convex lens that is remote from the first light source is configured aspherically.
In a further configuration of the invention, the vehicle headlight comprises a light shield, wherein an edge of the light shield can be imaged as a bright-dark boundary by means of the first convex lens.
In a further configuration of the invention, the transparent shaped part substantially consists of glass or the transparent shaped part comprises glass.
In a further configuration of the invention, the transparent shaped part forms an outer part of the vehicle headlight. That is to say, in particular, that in a configuration of the invention no additional outer disc, such as, for instance, the transparent covering designated by reference symbol 30 in DE 10 2004 061 873 A1, is provided.
In a configuration it may be provided that a convex lens has substantially or virtually a roughness of less than 0.05 μm, in particular in the case of a light transmission at the surface of at least 90%. However, partial regions, in particular of the first convex lens, can have a greater roughness. Such partial regions having a greater roughness are configured in particular in accordance with DE 10 2004 011 084. Roughness within the meaning of the invention is to be defined in particular as R a , in particular according to ISO 4287.
In a further configuration it may be provided that an emblem is embossed in particular on a surface of the transparent shaped part which faces the (first) light source. Said emblem is advantageously arranged on that surface of the transparent shaped part which faces the first light source. The aforementioned emblem is advantageously configured in accordance with an emblem disclosed in DE 10 2004 011 104.
In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source or relative to an optical axis of the transparent shaped part (or e.g. the first convex lens) in such a way that light penetrating into the transparent shaped part through a surface remote from the (first) light source along or parallel to the optical axis of the transparent shaped part (or e.g. the first convex lens) is subjected to total reflection at the basic surface. In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source by an angle of between 25° and 80°, in particular between 35° and 60°, or relative to an optical axis of the transparent shaped part (or e.g. the first convex lens) by an angle of between 10° and 65°, in particular between 30° and 55°.
It may be provided that, on that surface of the first convex lens which faces the first light source or on that surface of the transparent shaped part which faces the light source, in the region of the first convex lens, the arrangement comprises an, in particular blank-pressed, deformation or embossing for deflecting part of the light that can be generated by the first light source into a secondary luminous region outside a main luminous region of the first light source in conjunction with the first convex lens. The deformation or embossing may be configured in accordance with a deformation or embossing disclosed in DE 10 2004 024 107. As an alternative or in addition, by means of a further (e.g. the second) light source in conjunction with a further (e.g. the second) convex lens, light can be directed into said secondary luminous region. In a configuration, at least 95%, in particular at least 97%, of the light which can emerge or emerges from the first convex lens is allotted to the main luminous region. In a further configuration, less than 5%, in particular less than 3%, of the light which can emerge or emerges from the first convex lens, but advantageously at least 0.2%, in particular at least 0.5%, of the light which can emerge or emerges from the first convex lens is allotted to the secondary luminous region. By way of example, traffic signs can be illuminated or lit up by means of the secondary luminous region. Main luminous region and secondary luminous region should be regarded as separate if an unilluminated region lies between them. In said unilluminated region, the light intensity is virtually zero or negligibly small.
The aforementioned object is additionally achieved by means of a transparent shaped part comprising one or more of the aforementioned features.
The aforementioned object is achieved by means of a vehicle headlight or vehicle front headlight, in particular motor vehicle headlight or motor vehicle front headlight, comprising a first light source, comprising at least a second light source, comprising a light shield and comprising a transparent shaped part configured in one piece, wherein the shaped part comprises a first optical structure for imaging an edge of the light shield as a bright-dark boundary with respect to the light emitted by the first light source and at least a second optical structure for the direction of light emitted by the second light source. An optical structure within the meaning of the invention is in particular at least one macrostructure, and not or not just a microstructure. In this case, such a microstructure is intended to be in particular a structure composed of small alterations on a surface, wherein the small alterations on a surface bring about a scattering of light. A macrostructure within the meaning of the invention has in particular an extent of at least half a centimeter.
In a further configuration of the invention, the first light source in conjunction with the first optical structure is part of a dipped-beam light.
In one configuration of the invention, the first light source in conjunction with the first optical structure directs light in a different direction from the second light source in conjunction with the second optical structure.
In a further configuration of the invention, the first light source comprises a lamp, in particular a gas discharge lamp or an incandescent lamp, or is configured as a lamp, in particular a gas discharge lamp or an incandescent lamp. The first light source may be e.g. a halogen lamp or a xenon luminaire. Suitable configurations for the first light source can be gathered e.g. from pages 739 to 753 of the book “Bosch, Kraftfahrtechnisches Taschenbuch” [“Bosch, Automotive Technology Handbook”], 23rd edition, Vieweg, 1999, ISBN 3-528-03876-4. However, it may also be provided that the first light source is an LED or an arrangement of LEDs. In this case, the LED or the arrangement of LEDs is configured in particular in such a way that it can be used to implement a dipped-beam light, a full-beam light and/or a fog light.
In a further configuration of the invention, the second light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode. The use of LEDs for signal luminaires for motor vehicles is disclosed e.g. in DE 102 07 431 A1, DE 102 37 263 A1 and DE 195 07 234 B4.
In a further configuration of the invention, the vehicle headlight comprises at least a third light source, wherein the shaped part has at least a third optical structure for the direction of light emitted by the third light source. In a further configuration of the invention, the third light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode.
In a further configuration of the invention, the first, the second and/or the third optical structure and/or a further optical structure is blank-pressed. In a further configuration of the invention, the shaped part is blank-pressed, in particular on both sides. Blank-pressing is to be understood within the meaning of the invention as, in particular, pressing a lens such that subsequent processing of an optically active surface of the lens after pressing can be obviated.
In a further configuration of the invention, the first optical structure is configured as a lens or as part of a lens. In a further configuration of the invention, the first optical structure is configured as a projection lens or as part of a projection lens. In a further configuration of the invention, the first optical structure is configured as a converging lens or as part of a converging lens. In a further configuration of the invention, an optically active surface of the first optical structure that is remote from the first light source is configured convexly or aspherically.
In a further configuration of the invention, the transparent shaped part substantially consists of glass or the transparent shaped part comprises glass.
In a further configuration of the invention, the transparent shaped part forms an outer part of the vehicle headlight. That is to say, in particular, that in a configuration of the invention no additional outer disc, such as, for instance, the transparent covering designated by reference symbol 30 in DE 10 2004 061 873 A1, is provided.
In a configuration it may be provided that an optical structure has substantially or virtually a roughness of less than 0.05 μm, in particular in the case of a light transmission at the surface of at least 90%. However, partial regions, in particular of the first optical structure, can have a greater roughness. Such partial regions having a greater roughness are configured in particular in accordance with DE 10 2004 011 084. Roughness within the meaning of the invention is to be defined in particular as R a , in particular according to ISO 4287.
In a further configuration it may be provided that an emblem is embossed in particular on a surface of the transparent shaped part which faces the (first) light source. Said emblem is advantageously arranged on that surface of the transparent shaped part which faces the first light source. The aforementioned emblem is advantageously configured in accordance with an emblem disclosed in DE 10 2004 011 104.
In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source or relative to an optical axis of the transparent shaped part (or e.g. the first optical structure) in such a way that light penetrating into the transparent shaped part through a surface remote from the (first) light source along or parallel to the optical axis of the transparent shaped part (or e.g. the first optical structure) is subjected to total reflection at the basic surface. In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source by an angle of between 25° and 80°, in particular between 35° and 60°, or relative to an optical axis of the transparent shaped part (or e.g. the first optical structure) by an angle of between 10° and 65°, in particular between 30° and 55°.
It may be provided that, on that surface of the first optical structure which faces the first light source or on that surface of the transparent shaped part which faces the light source, in the region of the first optical structure, the arrangement comprises an, in particular blank-pressed, deformation or embossing for deflecting part of the light that can be generated by the first light source into a secondary luminous region outside a main luminous region of the first light source in conjunction with the first optical structure.
The deformation or embossing may be configured in accordance with a deformation or embossing disclosed in DE 10 2004 024 107. As an alternative or in addition, by means of a further (e.g. the second) light source in conjunction with a further (e.g. the second) optical structure, light can be directed into said secondary luminous region. In a configuration, at least 95%, in particular at least 97%, of the light which can emerge or emerges from the first optical structure is allotted to the main luminous region. In a further configuration, less than 5%, in particular less than 3%, of the light which can emerge or emerges from the first optical structure, but advantageously at least 0.2%, in particular at least 0.5%, of the light which can emerge or emerges from the first optical structure is allotted to the secondary luminous region. By way of example, traffic signs can be illuminated or lit up by means of the secondary luminous region. Main luminous region and secondary luminous region should be regarded as separate if an unilluminated region lies between them. In said unilluminated region, the light intensity is virtually zero or negligibly small.
The aforementioned object is additionally achieved by means of a vehicle headlight or vehicle front headlight, in particular motor vehicle headlight or motor vehicle front headlight, comprising a first light source, comprising at least a second light source and comprising a transparent shaped part configured in one piece, wherein the shaped part comprises a first, light-concentrating, optical structure for the direction of light emitted by the first light source and at least a second optical structure for the direction of light emitted by the second light source. A first optical structure within the meaning of the invention is in particular a structure.
An optical structure, in particular first optical structure, within the meaning of the invention is in particular at least one macrostructure, and not or not just a microstructure. In this case, such a microstructure is intended to be in particular a structure composed of small alterations on a surface, wherein the small alterations on a surface bring about a scattering of light. A macrostructure within the meaning of the invention has in particular an extent of at least half a centimeter.
In a further configuration of the invention, the first light source in conjunction with the first optical structure, and also if appropriate further elements, such as e.g. a reflector, forms a dipped-beam light, a full-beam light and/or a fog light.
In one configuration of the invention, the first light source in conjunction with the first optical structure directs light in a different direction from the second light source in conjunction with the second optical structure.
In a further configuration of the invention, the first light source comprises a lamp, in particular a gas discharge lamp or an incandescent lamp, or is configured as a lamp, in particular a gas discharge lamp or an incandescent lamp. The first light source may be e.g. a halogen lamp or a xenon luminaire. Suitable configurations for the first light source can be gathered e.g. from pages 739 to 753 of the book “Bosch, Kraftfahrtechnisches Taschenbuch” [“Bosch, Automotive Technology Handbook”], 23rd edition, Vieweg, 1999, ISBN 3-528-03876-4. However, it may also be provided that the first light source is an LED or an arrangement of LEDs. In this case, the LED or the arrangement of LEDs is configured in particular in such a way that it can be used to implement a dipped-beam light, a full-beam light and/or a fog light.
In a further configuration of the invention, the second light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode. The use of LEDs for signal luminaires for motor vehicles is disclosed e.g. in DE 102 07 431 A1, DE 102 37 263 A1 and DE 195 07 234 B4.
In a further configuration of the invention, the vehicle headlight comprises at least a third light source, wherein the shaped part has at least a third optical structure for the direction of light emitted by the third light source. In a further configuration of the invention, the third light source is a semiconductor light emitting element, in particular an LED or light emitting diode, or comprises a semiconductor light emitting element, in particular an LED or light emitting diode.
In a further configuration of the invention, the first, the second and/or the third optical structure and/or a further optical structure is blank-pressed. In a further configuration of the invention, the shaped part is blank-pressed, in particular on both sides. Blank-pressing is to be understood within the meaning of the invention as, in particular, pressing a lens such that subsequent processing of an optically active surface of the lens after pressing can be obviated.
In a further configuration of the invention, the first optical structure is configured as a lens or as part of a lens. In a further configuration of the invention, the first optical structure is configured as a projection lens or as part of a projection lens. In a further configuration of the invention, the first optical structure is configured as a converging lens or as part of a converging lens. In a further configuration of the invention, an optically active surface of the first optical structure that is remote from the first light source is configured convexly or aspherically.
In a further configuration of the invention, the vehicle headlight comprises a light shield, wherein an edge of the light shield can be imaged as a bright-dark boundary by means of the first optical structure.
In a further configuration of the invention, the transparent shaped part substantially consists of glass or the transparent shaped part comprises glass.
In a further configuration of the invention, the transparent shaped part forms an outer part of the vehicle headlight. That is to say, in particular, that in a configuration of the invention no additional outer disc, such as, for instance, the transparent covering designated by reference symbol 30 in DE 10 2004 061 873 A1, is provided.
In a configuration it may be provided that an optical structure has substantially or virtually a roughness of less than 0.05 μm, in particular in the case of a light transmission at the surface of at least 90%. However, partial regions, in particular of the first optical structure, can have a greater roughness. Such partial regions having a greater roughness are configured in particular in accordance with DE 10 2004 011 084. Roughness within the meaning of the invention is to be defined in particular as R a , in particular according to ISO 4287.
In a further configuration it may be provided that an emblem is embossed in particular on a surface of the transparent shaped part which faces the (first) light source. Said emblem is advantageously arranged on that surface of the transparent shaped part which faces the first light source. The aforementioned emblem is advantageously configured in accordance with an emblem disclosed in DE 10 2004 011 104.
In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source or relative to an optical axis of the transparent shaped part (or e.g. the first optical structure) in such a way that light penetrating into the transparent shaped part through a surface remote from the (first) light source along or parallel to the optical axis of the transparent shaped part (or e.g. the first optical structure) is subjected to total reflection at the basic surface. In a configuration the emblem comprises a basic surface which is inclined relative to that surface of the transparent shaped part which faces the (first) light source by an angle of between 25° and 80°, in particular between 35° and 60°, or relative to an optical axis of the transparent shaped part (or e.g. the first optical structure) by an angle of between 10° and 65°, in particular between 30° and 55°.
It may be provided that, on that surface of the first optical structure which faces the first light source or on that surface of the transparent shaped part which faces the light source, in the region of the first optical structure, the arrangement comprises an, in particular blank-pressed, deformation or embossing for deflecting part of the light that can be generated by the first light source into a secondary luminous region outside a main luminous region of the first light source in conjunction with the first optical structure. The deformation or embossing may be configured in accordance with a deformation or embossing disclosed in DE 10 2004 024 107. As an alternative or in addition, by means of a further (e.g. the second) light source in conjunction with a further (e.g. the second) optical structure, light can be directed into said secondary luminous region. In an advantageous configuration, at least 95%, in particular at least 97%, of the light which can emerge or emerges from the first optical structure is allotted to the main luminous region. In a further configuration, less than 5%, in particular less than 3%, of the light which can emerge or emerges from the first optical structure, but advantageously at least 0.2%, in particular at least 0.5%, of the light which can emerge or emerges from the first optical structure is allotted to the secondary luminous region. By way of example, traffic signs can be illuminated or lit up by means of the secondary luminous region. Main luminous region and secondary luminous region should be regarded as separate if an unilluminated region lies between them. In said unilluminated region, the light intensity is virtually zero or negligibly small.
Motor vehicle within the meaning of the invention is in particular a land vehicle which can be used individually in traffic. Motor vehicles within the meaning of the invention are in particular not restricted to land vehicles having an internal combustion engine.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a motor vehicle;
FIG. 2 shows a schematic illustration of an exemplary embodiment of a vehicle headlight in a cross section;
FIG. 3 shows a schematic illustration of the vehicle headlight in accordance with FIG. 2 in a plan view;
FIG. 4 shows an exemplary embodiment of a transparent shaped part;
FIG. 5 shows a two-dimensional intensity distribution of light emitted by means of the vehicle headlight in accordance with FIG. 2 ;
FIG. 6 shows a further exemplary embodiment of a transparent shaped part;
FIG. 7 shows a side view of the transparent shaped part in accordance with FIG. 6 ;
FIG. 8 shows a further exemplary embodiment of a transparent shaped part;
FIG. 9 shows a side view of the transparent shaped part in accordance with FIG. 8 ;
FIG. 10 shows a further exemplary embodiment of a transparent shaped part;
FIG. 11 shows a side view of the transparent shaped part in accordance with FIG. 10 ;
FIG. 12 shows a cross section through a further exemplary embodiment of a transparent shaped part in a basic illustration;
FIG. 13 shows a cross section through a further exemplary embodiment of a transparent shaped part in a basic illustration;
FIG. 14 shows a cross section through a further exemplary embodiment of a transparent shaped part in a basic illustration;
FIG. 15 shows a further exemplary embodiment of a transparent shaped part in a perspective illustration;
FIG. 16 shows a plan view of the transparent shaped part in accordance with FIG. 15 ;
FIG. 17 shows a side view of the transparent shaped part in accordance with FIG. 15 ;
FIG. 18 shows a further exemplary embodiment of a transparent shaped part in a perspective illustration;
FIG. 19 shows a plan view of the transparent shaped part in accordance with FIG. 18 ;
FIG. 20 shows a side view of the transparent shaped part in accordance with FIG. 18 ; and
FIG. 21 shows a view behind the transparent shaped part in accordance with FIG. 18 .
DETAILED DESCRIPTION
FIG. 1 shows a motor vehicle 100 comprising a vehicle headlight 1 (front headlight), which is illustrated schematically in FIG. 2 in a cross section along a section line designated by reference symbol 17 in FIG. 3 . In this case, FIG. 2 shows the vehicle headlight 1 from a viewing direction designated by reference symbol 16 in FIG. 3 . FIG. 3 shows a schematic illustration of the vehicle headlight 1 from a viewing direction designated by reference symbol 15 in FIG. 2 . The vehicle headlight 1 comprises a one-piece transparent shaped part 2 that is blank-pressed, in particular on both sides. FIG. 4 shows the transparent shaped part 2 from a viewing direction designated by reference symbol 18 in FIG. 2 .
The vehicle headlight 1 additionally comprises a light source 10 for generating light, a reflector 12 for reflecting light that can be generated by means of the light source 10 , and a light shield 14 . The light source 10 is one exemplary embodiment of a first light source within the meaning of the claims. The light source 10 advantageously comprises a lamp, in particular a gas discharge lamp or an incandescent lamp, or is configured as a lamp, in particular a gas discharge lamp or an incandescent lamp. The first light source may be e.g. a halogen lamp or a xenon luminaire. Suitable configurations for the first light source can be gathered e.g. from pages 739 to 753 of the book “Bosch, Kraftfahrtechnisches Taschenbuch” [“Bosch, Automotive Technology Handbook”], 23rd edition, Vieweg, 1999, ISBN 3-528-03876-4.
The transparent shaped part 2 comprises an optical structure 3 for the direction of light emitted by the light source 10 . In this case, the optically active surface of the optical structure 3 which is remote from the light source 10 is configured convexly or aspherically in such a way that an edge—designated by reference symbol 13 in FIG. 2 —of the light shield 14 —as illustrated in FIG. 5 —can be imaged as a bright-dark boundary 40 by means of the optical structure 3 . In this case, FIG. 5 shows a two-dimensional intensity distribution of light emitted by means of the vehicle headlight 1 , wherein regions of very low or no light intensity are represented as white, regions of medium light intensity are represented as black and regions of high light intensity are represented as grey. The optical structure 3 is one exemplary embodiment of a first optical structure within the meaning of the claims.
In the vehicle headlight 1 illustrated, a dipped-beam light is implemented by means of the light source 10 in conjunction with the optical structure 3 . A full-beam light or a fog light can also be implemented by means of the light source 10 in conjunction with the optical structure 3 .
The transparent shaped part 2 additionally comprises an optical structure 4 for the direction of light emitted by a light source 24 , an optical structure 5 for the direction of light emitted by a light source 25 , an optical structure 6 for the direction of light emitted by a light source 26 , an optical structure 7 for the direction of light emitted by a light source 27 and an optical structure 8 for the direction of light emitted by a light source that is not illustrated. The light sources 24 , 25 , 26 and 27 and also the light source interacting with the optical structure 8 are exemplary embodiments of a second or third light source within the meaning of the claims. The optical structures 4 , 5 , 6 , 7 and 8 are exemplary embodiments of a second or third optical structure within the meaning of the claims. The light sources 24 , 25 , 26 and 27 and also the light source interacting with the optical structure are configured as semiconductor light emitting elements, in particular LEDs or light emitting diodes.
By means of the light sources 24 , 25 , 26 and 27 and also the light source interacting with the optical structure 8 , in conjunction with the optical structures 4 , 5 , 6 , 7 and/or 8 , it is possible to implement a static cornering light, a fog light, part of a fog light, part of a dipped-beam light, a city light or daytime running light, a signal light, a headlight flasher, an infrared headlight and/or an indicator. In order to implement an infrared headlight, e.g. one (or a plurality) of the light sources 24 , 25 , 26 and 27 is configured as infrared light emitting diode. By means of the light sources 24 , 25 , 26 and 27 and also the light source interacting with the optical structure 8 , in conjunction with the optical structures 4 , 5 , 6 , 7 and/or 8 , it is also possible to implement a specific corporate design.
In a configuration, the vehicle headlight 1 does not comprise an additional outer disc. Rather, the transparent shaped part 2 forms an outer part of the vehicle headlight 1 .
It may be provided that, on that surface of the optical structure 3 which faces the light source 10 or on that surface of the transparent shaped part 2 which faces the light source 10 , in the region of the optical structure 3 , the arrangement comprises a deformation or embossing for deflecting part of the light that can be generated by the first light source 10 into a secondary luminous region outside a main luminous region generated by means of the light source 10 in conjunction with the optical structure 3 . As an alternative or in addition, by means of the light source 5 in conjunction with the optical structure 25 , light can be directed into the aforementioned secondary luminous region. In a configuration, at least 95%, in particular at least 97%, of the light which can emerge or emerges from the first optical structure is allotted to the main luminous region. In a further configuration, less than 5%, in particular less than 3%, of the light which can emerge or emerges from the first optical structure, but advantageously at least 0.2%, in particular at least 0.5%, of the light which can emerge or emerges from the first optical structure is allotted to the secondary luminous region. By way of example, traffic signs can be illuminated or lit up by means of the secondary luminous region. Main luminous region and secondary luminous region should be regarded as separate if an unilluminated region lies between them. In said unilluminated region, the light intensity is virtually zero or negligibly small.
FIG. 6 and FIG. 7 show a further exemplary embodiment of a transparent shaped part 102 that is blank-pressed in one piece, wherein FIG. 7 shows the transparent shaped part 102 in a side view. The transparent shaped part 102 comprises an optical structure 103 corresponding to the optical structure 3 . The transparent shaped part 102 additionally comprises e.g. optical structures 105 , 106 , 107 and 108 corresponding to one or more of the optical structures 4 , 5 , 6 , 7 and 8 .
FIG. 8 and FIG. 9 show a further exemplary embodiment of a transparent shaped part 202 that is blank-pressed in one piece, wherein FIG. 9 shows the transparent shaped part 202 in a side view. The transparent shaped part 202 comprises an optical structure 203 corresponding to the optical structure 3 . The transparent shaped part 202 additionally comprises e.g. optical structures 204 , 205 , 206 , 207 , 208 and 209 corresponding to one or more of the optical structures 4 , 5 , 6 , 7 and 8 .
FIG. 10 and FIG. 11 show a further exemplary embodiment of a transparent shaped part 302 that is blank-pressed in one piece, wherein FIG. 7 shows the transparent shaped part 302 in a side view. The transparent shaped part 302 comprises an optical structure 303 corresponding to the optical structure 3 . The transparent shaped part 302 additionally comprises e.g. optical structures 304 , 305 , 306 , 307 , 308 , 309 , 310 and 311 corresponding to one or more of the optical structures 4 , 5 , 6 , 7 and 8 .
In the exemplary embodiments illustrated, the transparent shaped parts 2 , 102 , 202 and 302 each comprise only one optical structure 3 , 103 , 203 and 303 , respectively, corresponding to an optical structure for implementing a fog light, a dipped-beam light or a full-beam light. However, it is also possible to provide two or more of said optical structures on a transparent shaped part 2 , 102 , 202 and 302 .
FIG. 12 shows a cross section through a further exemplary embodiment of a transparent shaped part 402 in a basic illustration. The transparent shaped part 402 comprises two optical structures 403 and 404 , at least one of which in one configuration corresponds to the optical structure 3 with regard to its function. On its side remote from a light source and also on its side facing a light source, the optical structure 403 comprises a convex, in particular aspherical, curvature 4031 and 4032 , respectively. On its side remote from a light source and also on its side facing a light source, the optical structure 404 likewise comprises a convex, in particular aspherical, curvature 4041 and 4042 , respectively.
FIG. 13 shows a cross section through a further exemplary embodiment of a transparent shaped part 502 in a basic illustration. On its side facing light sources, the transparent shaped part 502 comprises two optical structures 503 and 504 configured as concave depressions.
FIG. 14 shows a cross section through a further exemplary embodiment of a transparent shaped part 602 in a basic illustration. The transparent shaped part 602 comprises two optical structures 603 and 604 , at least one of which in one configuration corresponds to the optical structure 3 with regard to its function. The optical structure 603 comprises a convex, in particular aspherical, curvature 6031 on its side remote from a light source and a concave curvature 6032 on its side facing a light source. The curvatures 6031 and 6032 are coordinated with one another in such a way that the optical structure 603 is a converging lens. The optical structure 604 comprises a convex, in particular aspherical, curvature 6041 on its side remote from a light source and a concave curvature 6042 on its side facing a light source. The curvatures 6041 and 6042 are coordinated with one another in such a way that the optical structure 604 is likewise a converging lens. The optical structures 403 , 404 , 503 , 504 , 603 and 604 can also be used in mixed fashion in a transparent shaped part.
FIG. 15 shows a further exemplary embodiment of a transparent shaped part 702 in a perspective illustration, FIG. 16 shows a plan view of the transparent shaped part 702 , and FIG. 17 shows a side view of the transparent shaped part 702 . The transparent shaped part 702 comprises an optical structure 703 that corresponds to the optical structure 3 . The transparent shaped part 702 additionally comprises two optical structures 704 and 705 corresponding—with regard to their function—e.g. to one or more of the optical structures 4 , 5 , 6 , 7 and 8 .
FIG. 18 shows a further exemplary embodiment of a curved transparent shaped part 802 in a perspective illustration, FIG. 19 shows a plan view of the transparent shaped part 802 , FIG. 20 shows a side view of the transparent shaped part 802 , and FIG. 21 shows a view behind the transparent shaped part 802 . The transparent shaped part 802 comprises two optical structures 804 and 805 , at least one of which in one configuration corresponds to the optical structure 3 . Furthermore, the transparent shaped part 802 comprises two optical structures designated by reference symbols 803 and 806 . The optical structure 803 comprises a convex, in particular aspherical, optical partial structure 8031 on its side remote from a light source and a cylindrical optical partial structure 8032 on its side facing a light source. The optical structure 806 comprises a convex, in particular aspherical, optical partial structure 8061 on its side remote from a light source and a cylindrical optical partial structure 8062 on its side facing a light source.
In a configuration, the transparent shaped parts 2 , 102 , 202 , 302 , 402 , 502 , 602 , 702 and 802 substantially consist of glass or the transparent shaped parts 2 , 102 , 202 , 302 , 402 , 502 , 602 , 702 and 802 comprise glass. However, the transparent shaped parts 2 , 102 , 202 , 302 , 402 , 502 , 602 , 702 and 802 can also substantially consist of transparent plastic or comprise transparent plastic.
The elements and distances in FIGS. 1 to 14 are depicted taking account of simplicity and clarity and not necessarily as true to scale. Thus, e.g. the orders of magnitude of some elements or distances in FIGS. 1 to 14 are represented in an exaggerated manner relative to other elements or distances in order to improve the understanding of the exemplary embodiments of the present invention.
|
A vehicle headlamp includes a first light source, at least one second light source and an integrally designed, transparent shaped part. The shaped part includes a first optical structure for orienting light radiated by the first light source and at least one second optical structure for orienting light radiated by the second light source. The first optical structure and the second optical structure each have a continuously curved surface or a continuous, curved surface with an extent of at least in each case half a centimeter, in particular one centimeter, in two orthogonal directions.
| 5
|
BACKGROUND AND SUMMARY OF THE INVENTION
This invention relates to an arrangement for guiding lubricating oil in an internal-combustion engine comprising a basin which is arranged between an engine crankshaft drive and an oil sump and has at least one drain opening, and an intermediate shaft which rotates in parallel to the crankshaft and is surrounded at least partially by two struts projecting away from the basin.
From German Patent Document DE-42 04 522 C1, an arrangement in an internal-combustion engine is known which has a basin for letting off lubricating oil which covers the crankshaft drive in the direction of the oil sump. Approximately in the center below the crankshaft, the basin which extends partially along the violin-shaped connecting rod contour has an oil drain opening which acts as an oil deflector. This oil drain opening leads into a damping chamber for the gas pulses caused by the piston movement, this damping chamber comprising another drain opening which is arranged below the oil drain opening and is laterally offset with respect to the oil drain opening. The lubricating oil which is thrown off the crankshaft drive flows through this additional drain opening into the oil sump. A differential shaft may rotate in this damping chamber which is enclosed at least partially by two struts projecting away from the basin. It is disadvantageous in this case that the oil is foamed as a result of the contact with the rotating differential shaft and arrives in the oil sump in this condition.
It is an object of the invention to develop an arrangement of this type for guiding lubricating oil in an internal-combustion engine arranged between the crankshaft drive and the oil sump in such a manner that the lubricating oil released by the crankshaft drive reaches the oil tank in a largely unfoamed manner.
This object is achieved by the present invention by providing an arrangement for guiding oil in an internal-combustion engine comprising a basin which is arranged between an engine crankshaft drive and an oil sump and has at least one drain opening, and an intermediate shaft which rotates in parallel to the crankshaft and is surrounded at least partially by two struts projecting away from the basin, wherein the struts form, together with the basin, a profile which receives the intermediate shaft and which is closed with respect to the crankshaft drive.
When, in the case of an internal-combustion engine of the above-mentioned type, the projecting struts of the basin form a profile which accommodates the intermediate shaft and is closed with respect to the crankshaft drive, the intermediate shaft is shut off with respect to the entering of lubricating oil of the crankshaft drive. This lubricating oil therefore reaches the oil sump while bypassing the rotating intermediate shaft and is not foamed by the rotation.
In an advantageous development, the bottom of the basin is provided in the area of the violin-shaped connecting rod contour with curved segments which follow them and which extend, by means of the curvature, closely adjacent to this contour and therefore leave only a small gap in which oil can be mixed with air. An arrangement of two drain openings which are situated in series with respect to one another with respect to the rotating direction of the crankshaft and behind the profile ensures a reliable discharge of the lubricating oil.
The amount of oil taken from the crankshaft drive and therefore not rotating with it can be increased if roof-type shaped-out areas are arranged behind the drain openings which point in the direction of the crankshaft, are provided with scraper lips and extend directly to the violin-shaped connecting rod contour. These may bound drain ducts which contain the drain openings and guide the taken-up lubricating oil into the oil sump.
In order to provide a further improvement by also taking up the lubricating oil thrown off the counterweights arranged adjacent to the connecting rods on the crankshaft, at least adjacent to one shaped-out area, a scraper may be arranged which extends directly to the counterweight contour.
For the complete shutting-off of the intermediate shaft, the ends of the struts which are situated at a distance from the bottom of the basin, provided for example with elastic seals, may rest against wall sections of the internal-combustion engine in such a manner that they form, together with the profile, a closed volume which extends along the intermediate shaft and accommodates it. These wall sections may be lateral walls of a crankcase which extend downward beyond the crankshaft or walls of an oil tank which is flanged to the crankcase and is constructed as an oil sump. In both cases, one wall section may have an outlet opening for lubricating oil. The oil can therefore be drained which has collected in the shaft formed between one strut and the drain ducts as well as this wall section In the former case, when there is dry sump lubrication, the take-in point of the oil pump which delivers the oil into an oil receptacle constructed as a tank may be situated in this outlet opening.
A surrounding flange of the bottom which is situated on the outside may be situated in a horizontal plane arranged between the crankshaft and the intermediate shaft, the flange, which is also provided with elastic seals, being supported on the wall sections. These seals may be placed, for example, as a sealing ring which has a circular cross-section, in corresponding grooves of the flange or of the struts.
In another embodiment, they may be provided with a sealing lip which extends in a curved manner when resting against the corresponding wall section. By means of the sealing lips, positional tolerances of the bottom or of the struts with respect to the wall sections can easily be compensated. An appropriately selected direction of the curvature of the sealing lips provides that, on the one hand, no oil can emerge from the shaft at points which are not provided for this purpose; and, on the other hand, a tunnel which is arranged on the opposite side of the intermediate shaft is secured against an admission of oil from the crankshaft drive, and oil which may be situated in it can flow off in a groove of the volume receiving the intermediate shaft.
Other objects, advantages and novel features of the present invention will become apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a partially broken top schematic view of an arrangement for guiding oil in an internal-combustion engine constructed according to a preferred embodiment of the invention;
FIG. 2 is a sectional view along Line II--II according to FIG. 1;
FIG. 3 is a sectional view along Line III--III according to FIG. 1;
FIG. 4 is a sectional view along Line IV--IV according to FIG. 1;
FIG. 5 is a sectional view along Line V--V according to a variant of FIG. 1;
FIG. 6 is a sectional view along Line VI--VI according to FIG. 1; and
FIG. 7 is a view in the direction of the arrow Y according to FIG. 3.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A two-bank internal-combustion engine with a V-angle of 180°, which is not shown in detail, has a crankshaft drive comprising a crankshaft 1 which can be rotated about an axis A--A in the direction of the shown arrow. In the center below the crankshaft 1, an intermediate shaft 2 rotates about its axis Z--Z. A crankcase is divided into halves perpendicularly in a plane E--E which contains the axes A--A and Z--Z. Below the crankshaft drive the halves of wall sections 3 and 4 extend in a V-shape with respect to one another, and a single drain opening 5 is arranged in section 4.
The crankshaft drive has conventional counterweights which are situated adjacent to connecting rod journals and which, in the case of a rotation, result in a counterweight contour K. The cylinders Z1, Z2, Z3 assigned to a cylinder bank produce by means of their connecting rod on the crankshaft drive a first violin-shaped connecting rod contour 6; the cylinders Z4, Z5 and Z6 assigned to the other cylinder bank produce a second violin-shaped connecting rod contour 7.
Between the axes A--A and Z--Z, a horizontal plane H--H extends perpendicularly to the plane E--E. Essentially along this plane H--H, a basin 8 extends along the whole length of the crankshaft 1 and comprises a bottom 9 and a flange 10 situated on the exterior.
Two struts 11, 12 extend away from the basin 8 symmetrically with respect to plane E--E and form, together with a piece of the bottom 9, a profile 13 which is closed with respect to the crankshaft drive and which encloses the intermediate shaft 2 in a U-shaped manner.
Below the connecting rod journal of the crankshaft 1, the bottom 9 comprises segments 14 and 15 which, with respect to the rotating direction of the crankshaft 1, are situated in front of the plane E--E and which in a curved manner follow the violin-shaped connecting rod contours 6 and 7 in a closely adjacent manner.
Two roof-type shaped-out areas 20 and 21, which are each provided with lateral walls 16, 17 and 18, 19 adjoin the segments 14, 15 and are situated in series in the rotating direction behind the plane E--E. These shaped-out areas 20 and 21 comprise scraper lips 22 and 23 which are each tilted out in the direction of the crankshaft drive, point against the rotating direction of the crankshaft 1 and extend into the direct proximity of the violin-shaped connecting rod contours 6 and 7.
Between the shaped-out area 20 and the strut 12, a drain duct 25 is formed which has a first drain opening 24; between the shaped-out area 21 and the shaped-out area 20, a drain duct 27 is formed which has a second drain opening 26. Below these drain openings 24 and 26, a shaft 28 is formed which is bounded by one strut 12 and wall section 4 and which extends in parallel along the whole length of the crankshaft 1.
On the opposite side of plane E--E, a closed tunnel 29 is formed between the bottom 9 or its segments 14, 15, the other strut 11 and the wall section 3.
Ends 30, 31 of struts 11, 12 situated at a distance from the bottom 9 rest against the wall sections 3, 4 by means of elastic devices. Additional elastic devices are arranged between the flange 10 and these wall sections 3, 4.
According to FIG. 3, these devices are constructed as sealing rings 33, 34 which are placed in grooves 32 and which are constructed in a surrounding manner according to FIG. 7. In this case, the basin 8 is bounded on the end by walls 35, 36 which extend from the bottom 9 to close to the wall sections 3 and 4 and rest against these wall sections 3 and 4 by means of the elastic devices. In the area of the respective end-side bearings of the crankshaft 1, the basin 8 has roofs 37, 38 which extend beyond these walls 35, 36. FIGS. 3 and 4 show that the intermediate shaft 2 rotates in a volume 39 which is closed in the radial direction.
In a variant according to FIG. 5, the elastic devices are formed of seals 40, 41 which are fitted on and which are each provided with a sealing lip 42, 43. In the condition in which they are installed in the internal-combustion engine, these sealing lips 42, 43 rest against the wall sections 3, 4 in such a curved manner that, on the one hand, the shaft 28 is secured against the emerging of oil and, on the other hand, the tunnel 29 is sealed off on the flange 10 against the admission of oil, and on the strut 12, a flowing-off of oil which may be situated in the tunnel 29 may be possible into a groove 44 of the volume 39. FIG. 5 illustrates that in these case the sealing lips 42, 43 of the struts 11, 12 are curved forward in the rotating direction of the crankshaft 1 and those of the flange 10 are curved forward in the corresponding opposite direction.
A scraper 45 is assigned to each counterweight on the crankshaft 1 which is arranged on the lateral walls 18 and 19 of the additional shaped-out area 21 and which extends into the direct proximity of the counterweight contour K.
In the operation of the internal-combustion engine, the lubricating oil released by the crankshaft drive is received in the area of the connecting rods by the scraper lips 22 and 23 and is guided by way of drain ducts 25 and 27 into the shaft 28. In the area of the counterweights, the oil is gripped by the scrapers 45 and is supplied to the shaft 28 by way of the drain duct 27. The lubricating oil released by the bearings of the crankshaft 1 situated between the segments 14, 15 drips onto essentially flatly designed areas 46 of the bottom 9 and flows to the shaft 28 by way of the drain duct 25. In this shaft 28, the oil flows to the drain opening 5 which is situated approximately in the center with respect to the longitudinal course of the basin 8. All lubricating oil coming from the crankshaft drive is therefore discharged while bypassing the intermediate shaft 2. The path to be covered by the oil on the bottom 9, through the drain openings 24, 26 and in the shaft 28 to the outlet opening 5 permits an extensive degasification of the lubricating oil.
Although the invention has been described and illustrated in detail, it is to be clearly understood that the same is by way of illustration and example, and is not to be taken by way of limitation. The spirit and scope of the present invention are to be limited only by the terms of the appended claims.
|
An internal-combustion engine which has an intermediate shaft extending in parallel to the crankshaft, comprises a basin which is arranged between the shafts and which guides lubricating oil released by the crankshaft drive into an oil sump. This basin has struts which project downwardly away and which surround the intermediate shaft in such a manner that it is secured against the admission of lubricating oil of the crankshaft drive. As a result, this lubricating oil arrives in an oil tank in a largely unfoamed state.
| 5
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This non-provisional International Patent Application claims priority from U.S. Provisional Application Ser. No. 60/392,191, filed on Jun. 28, 2002, and entitled “Plasma or Serum Marker and Process for Detection of Cancer”, which is commonly owned with the present application and incorporated herein by reference for all purposes.
FIELD OF THE INVENTION
[0002] The present invention relates to a PCR based process in detection of blood plasma or serum marker for diagnosis, early detection, monitoring and population screening for cancer and, more particularly, detection of β-catenin RNA and DNA in blood plasma or serum for colorectal cancer.
BACKGROUND OF THE INVENTION
[0003] Colorectal cancer (CRC) is one of the most common malignancies worldwide. The number of new cases of CRC has been increasing rapidly since 1975. More than 70% of CRC cases develop from sporadic adenomas or adenomatous polyps. Early detection and surgical removal of polyps is believed to be the most effective way to prevent benign polyps from developing into malignant tumors and thereby reducing mortality caused by CRC.
[0004] Traditional screening methods for colorectal cancer include sigmoidoscopy, fecal occult blood testing, colonscopy and double contrast barium enema. However, these traditional methods suffer from limitations and are invasive, high cost, of low predictive value or result in low detection rates. For example, WO0142504, the teachings of which are incorporated herein by reference, discloses a multi-reaction process for detection of extracellular tumor associated nucleic acid in blood plasma or serum. Further advances are desirable.
[0005] β-catenin protein was initially identified through its interaction with cadherins. Recent evidence shows that it acts as a transcriptional factor and plays a key role in the Wnt-signaling pathway Willert & Nusse, 1998). It has been demonstrated that accumulation of cytoplasmic and nuclear β-catenin signaling is tightly associated with the genesis of a wide variety of tumors. (Morin, 1999).
[0006] It has been discovered that using immunohistochemical staining that levels of nuclear β-catenin are highly correlated with he purported sequential stages in colorectal carcinogenesis with positive staining observed in 0% of normal tissues, 8% of polyps, 92% of adenomas and 100% of carcinomas. It has been further discovered that the nuclear β-catenin signal appears to clearly differentiate the polyps (non-adenomatous polyps) from adenomas (adenomatous polyps). This would be a useful marker for clinical diagnosis, or early detection of CRC, with the adenoma being considered as endpoint for risk factor. However, this diagnostic method based on the evaluation of nuclear β-catenin requires colonscopic procedure, then surgical removal of the suspected tissues.
[0007] Accordingly, there is a need for an effective, less invasive, more accurate test for early detection of cancer. The present invention meets this need.
SUMMARY OF THE INVENTION
[0008] The present invention provides a PCR (Polymerase Chain Reaction) based method or process in the detection of serum or plasma marker RNA and DNA related to β-catenin providing an effective, less evasive and more accurate test for the diagnosis, early detection, monitoring, and population screening of colorectal and other cancer types. It will be appreciated that this method of detection of β-catenin RNA and DNA in blood serum can be applied to other plasma and serum RNA and DNA encoded for β-catenin associated proteins. In one embodiment, the RNA or DNA is derived from genes encoded beta-catenin, alpha-catenin, E-catherin and other beta catenin associated proteins.
[0009] The process of the present invention comprises detecting blood serum or plasma RNA or/and DNA from a human or animal as a tool in the diagnosis, early detection, monitoring, treatment and population screening of neoplastic diseases at various progression and clinical stages. One advantage of the present invention is the non-invasive nature of the method, and a second advantage is improved accessibility of sample collections and sensitivity
[0010] Details of multiple embodiments of the invention are set forth below. These embodiments are for illustrative purposes only and the principle of the invention can be implemented in other embodiments. Other features and advantages of this invention will become apparent from the following description and examples.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] For a more complete understanding, reference is now made to the following detailed description taken in conjunction with the accompanying drawings. It is emphasized that some components may not be illustrated for clarity of discussion. Reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
[0012] FIG. 1 a , FIG. 1 b and FIG. 1 c illustrate detection of β-catenin RNA from plasma of colorectal carcinoma patients using RT-PCR.
[0013] FIG. 2 a and FIG. 2 b illustrate detection of blood β-catenin RNA from patients for colorectal adenoma using RT-PCR.
[0014] FIG. 2 c illustrate detection of blood β-actin RNA from patients for colorectal adenoma using RT-PCR.
[0015] FIG. 3 a , FIG. 3 b , FIG. 3 c , FIG. 3 d , and FIG. 3 e illustrate detection of serum β-catenin DNA from patients with adenomas or carcinomas and normal controls.
DETAILED DESCRIPTION OF THE INVENTION
[0016] The search for sensitive and specific biomarkers for early detection of colorectal cancer has been discovered in the present invention. The advanced understanding of the molecular mechanism underlying the carcinogenesis of colorectal cancer has helped to identify a few oncogenes and tumor suppressors as potential clinical biomarkers of colorectal cancer development and early detection. These include k-ras, APC, p53, MCC, DCC genes. However, none of the candidate markers alone can provide satisfactory detection rate. The recent PCR-based detections of K-ras, APC and p53 mutations of in the blood samples of cancer patients have indeed greatly increased the accessibility of sample collections. However, the rate of detection is generally lower than that observed with primary tumors. For instance, in a study of 14 patients with colorectal cancer, out of seven confirmed k-ras mutations, the same mutation was found in 6 patients' serum. The serum positive rate was 86% (Anker 1997). Another study showed that serum positive rate for loss of heterozygosity (LOH), microsatellite instability, k-ras and p53 mutations were 0, 0, 19, and 70% respectively (Hibi 1998). Similar results have been obtained with other types of cancers, in which the genetic alterations found in serum DNA (deoxyribonucleic acid) tend to be lower than those found in primary tumors (Kopreski 2001; Sozzi 1999; von Knobloch 2001).
[0017] Compared with other related studies, the use of serum β-catenin DNA in the present invention for early detection of colorectal cancer may fulfill the criteria of being a marker for early detection: 1. The marker is differentially present in blood of normal, and premalignant or tumor-bearing patients; 2. The method has the capacity to detect adenomatous polyps as small as 4 mm in diameter; 3. The method is simple with high degree of accuracy; 4. The amount of blood sample required is small (2-5 ml), and sample collection is through non-invasive, normal blood-drawing procedure. Thus, it has been suggested in the present invention that β-catenin DNA levels, along with β-catenin RNA levels, in blood serum or plasma could provide one answer to the quest for an effective, accurate test for colorectal cancer, using equipment and reagents already readily available—hence appropriate for widespread population screening, early detection, and disease monitoring of this increasingly common cancer.
EXAMPLES
[0018] The following examples are intended to illustrate, but not limit the embodiments of the invention described herein. Specifically, in the following discussion, numerous specific details are set forth to provide a thorough understanding of the present disclosure. However, those skilled in the art will appreciate that some of the techniques herein may be practiced without such specific details. In other instances, well-known elements or specific details have been condensed or omitted altogether inasmuch as detail discussions of these features are not considered necessary to obtain a complete understanding of the disclosure, and are considered to be within the understanding of persons of ordinary skill in the relevant field of art.
Example 1
β-Catenin RNA was Detected in all Plasma Samples of Patients with Colorectal Carcinoma
[0019] To detect the presence of plasma β-catenin, RT-PCR (reverse transcription-polymerase chain reactions) were preformed on two blood samples from patients with carcinoma using Primer #1 that would yield a 224 bp of exon 3 region of the gene. An RNA sample extracted from carcinoma tumor expressing high level of β-catenin was included as positive control. Results showed that two plasma and the positive control RNA samples yielded a 224 bp band in the presence, but not in the absence of, reverse transcriptase (RT) in the reaction ( FIG. 1 a ). RT-PCR analysis was preformed on the other 10 plasma RNA samples using the intron spanning primers (Primer #2, Table 2).
[0020] Data showed that a 250 bp fragment was clearly detected in all 10 patient plasma samples ( FIG. 1 a , lanes 1-10), suggesting the presence of β-catenin RNA in the circulating blood of carcinoma patients. The data also showed that the reaction is RT-dependent ( FIG. 1 b , lane 12). A genomic DNA sample was included as a positive control for PCR reaction and a 450 bp band appeared as expected ( FIG. 1 b , lane 11).
[0021] To prove that the 250 bp band was derived from the RNA, instead of DNA templates in the plasma, tests were performed on the three remaining plasma RNA samples without prior treatment with DNase I.
[0022] Two PCR products, a 250 bp band amplified from RNA and a 450 bp band amplified from the DNA contaminating plasma RNA extract, appeared on the gel. All three samples yielded both 250 and 450 bp bands in the presence of RT ( FIG. 1 b , lanes 13-15), and a single 450 bp band was observed from a RNase treated DNA sample in the absence of RT ( FIG. 1 b , lane 1).
[0023] Fifteen patients were tested with carcinoma using three slight different experimental settings described above, and the data showed that 15 in 15 patients were clearly positive for plasma β-catenin.
Example 2
Plasma RNA was Present at High Rates in Patients with Adenomas, but not in Healthy Individuals
[0024] Seventeen plasma samples were screened for β-catenin RNA from individuals with suspected adenomas. Of the 17 plasma samples from individuals with suspected adenomas screened for β-catenin RNA, 11 were plasma positive, indicated by the presence of a 250 bp RT-PCR product; 6 were found negative ( FIG. 2 a , lanes 1-11; FIG. 2 b , lanes 1-6). RT-PCR assays were performed on the 6 negative samples using primers specific for β-actin sequences (Table 2, Primer #3). β-actin RNA was detected in all six plasma samples ( FIG. 2 c , lanes 1-6), indicating the six plasma RNA extracts were in amplifiable quality. Of the 6 patients with negative β-catenin signals (Table 1, Patients #10, 14, & 16), biopsy later confirmed that three were diagnosed with adenoma, two had granulation tissues, and the other had a dilated lymphatic space (Table 1, Patients #1-3). The percentage of detection among adenoma patients was 79% (11 of 14). Parallel RT-PCR analyses were performed on 10 healthy subjects. Nine of the ten healthy controls showed negative plasma β-catenin signals, but all showed positive β-actin RNA signals ( FIG. 2 d & FIG. 2 e , lanes 1-10). Only 1 of them had a rather weak positive signal ( FIG. 2 d , lane 10).
[0025] In summary, the presence of β-catenin was examined in the blood plasma of 32 patients with confirmed carcinoma or adenoma using RT-PCR analysis. Results showed that 100% (15 of 15) of patients with carcinoma, 79% (11 of 14) of patients with adenoma and 10% (1 of 10) healthy volunteers carried β-catenin RNA in their circulating blood. It is worthy to mention that the apparently healthy subject with weak plasma catenin RNA had been suffered from long-standing colorectal discomfort, occasionally with fecal blood and diarrhea, although no abnormality or ulceration colitis was detected in an endoscopic examination. Three patients with suspected adenoma at admission were also tested for plasma β-catenin. All three patients who were later confirmed by biopsy to be free of adenoma were negative for plasma signal.
[0026] It has been shown that free DNA is present in the circulating blood of patients with disorders and cancers, and this DNA can be detected using PCR assay.
[0027] Furthermore, reports have showed that genetic alterations of specific gene sequences can be detected in the serum of cancer patients (Anker P 1997; Hibi K 1998; Kopreski M S 2001; Sozzi G 1999; von Knobloch R 2001). Aside from plasma DNA, sequence-specific RNAs have also been detected in cancerous, but not healthy, individuals using RT-PCR analysis (Kopreski M S 1999; Lo K W, 1999; Chen X Q 2000). Whether the PCR method for the detection of plasma and serum DNA or RNA can be implemented for cancer diagnosis and prognosis will mainly depend on how well the data can validate the status of the tumor or even the pre-cancerous lesions. For instance, carcinoembryonic antigen (CEA) is expressed widely in a variety of cancers and in some normal tissue including colonic tissues. Along with carbohydrate antigen 19-9 (CA 19-9), these are the two most common tumor markers in the management of patients with CRC. In general, CEA marker yields positive detection rates ranging from 40 to 60% by conventional immunochemical assay for protein content. The use of RT-PCR for serum CEA RNA detection have improved the detection rate from 35% to around 70% (Guadagni, 2001), Another recent study has showed that tyrosine mRNA is present in the serum of 60% (4 of 6) patients with malignant melanoma, but not in any normal control serum (Kopreski, 1999). In our current study, the positive rate for CRC detection is 100% for patients with carcinoma and 79% for patients with adenoma. Thus, the plasma β-catenin RNA seems to be an effective serum marker for CRC detection.
[0028] At present, the only non-invasive method for CRC screening is fecal occult blood testing (FOBT). Several studies found that screening with FOBT in average and high-risk patients reduced the mortality rate by 16%. The limitation of the test, however, is the low predictive rate (less than 20%). The other method used for CRC screening, in particular for early detection of adenomas, is flexible sigmoidoscopy, which is claimed to have reduced the mortality rate by 70% in few of the case-control studies (for reviews, see Scotiniotis I, 1999). The test is sensitive and specific; however, it is invasive in nature. In this regard, the RT-PCR-based method for the detection of serum β-catenin may indeed provide an ideal tool for CRC screening of average and high-risk individuals. This method can be applied to monitoring post-operation and chemotherapy patients. Since β-catenin is also known to be involved in other types of cancer, our current invention for detection serum or plasma β-catenin can be extended for the detection, monitoring, screening of cancers with different tissue origins. This is the first time the presence of plasma β-catenin RNA has been reported and been suggested to have diagnostic value.
Example 3
Immunochemical Staining of Nuclear β-catenin Signals of the Adenoma and Carcinoma Tissues
[0029] In more than 200 cases examined, 92% of adenomas and 100% of carcinomas, but none of the normal tissues showed elevated nuclear β-catenin. To determine the nuclear β-catenin signals of the adenomas and carcinomas obtained from patients derived from Examples 1 & 2, paraffin-embedded tissue blocks of adenoma and carcinoma of 32 patients were sectioned and examined for nuclear β-catenin. The immunohistochemical staining was scored based on both the intensity and the percentage positive cells. Table 2 showed that nuclear translocation of β-catenin was observed in all tissue specimens.
Example 4
Quantification of Blood β-Catenin RNA in Healthy Individuals and Patients with Adenoma or Carcinoma Using Real Time RT-PCR Technology
[0030] The quantitative difference in plasma β-catenin signal between adenoma and carcinoma patients was investigated using real-time reverse transcriptase-PCR (RT-PCR). The results showed that the average copy number of β-catenin mRNA was 30 fold higher in adenoma (n=12; 3 negative; 8 positive: mean, 1.1×10 3 ; ranging from 0.69×10 3 to 1.80×10 3 ) and 598 fold higher in carcinoma (n=18; mean, 2.2×10 4 ranging from 0.67×10 4 to 4.4×10 4 ) patients than the normal individuals ((n=14; mean, 36 ranging from 0 to 169). The copy number of β-catenin mRNA in carcinoma patients was 19 fold higher than in adenoma patients. These quantification analysis provide a clear evidence that the plasma β-catenin mRNA are present differentially and can be used as a diagnostic tool to differentiate healthy subject, adenoma and carcinoma patients.
Example 5
Detection of β-Catenin DNA in the Serum of Patients with Colorectal Adenoma and Carcinoma
[0031] PCR analysis was first performed with serum DNA samples extracted from colorectal carcinoma patients. The results showed that a 359 bp band was observed in all 15 serum DNA samples ( FIG. 3 a , lanes 1 to 16). Ten patients were tested with confirmed adenoma ranging from mild to severe dysplasia. Positive band was detected in 9 of 1.0 patients ( FIG. 3 b , lanes 1-11). The detection rate was 90%. The only negative case ( FIG. 3 b , lane 8) was amplifiable as it yielded positive 156 bp band after amplification with ET specific primers ( FIG. 3 d , lower panel, lane 13). PCR amplification of β-catenin was also performed on 10 healthy volunteer controls. None of the serum samples showed positive signals for β-catenin, while positive signals were clearly detected using RET specific primers ( FIG. 3 c , lanes 1 to 10; & 1 D, lanes 1-11). In addition, a known positive carcinoma serum sample was carried out in parallel and showed typical 359 bp band on the agarose gel ( FIG. 3 c , lane 11). Lane 12 of FIG. 3 c & FIG. 3 d are the negative control for PCR reaction.
[0032] The data showed, for the first time, that serum β-catenin DNA is detectable in all patients with colorectal carcinoma and in 9 out of 10 patients with colorectal adenoma, while all 10 healthy individuals were free of serum β-catenin DNA. This result suggests that the presence of β-catenin DNA in the blood is significantly correlated with the existence of cancer at both preneoplastic and malignant stages, which may also suggest that the circulating β-catenin originated from the adenoma or carcinoma tissue of the patients. The ten adenoma patients, the individual (Patient #9, Table 4) negative in serum β-catenin had the smallest adenoma in this example (3.5 mm in diameter, 48 mm 3 )). Patient with the next smallest size of adenoma (63 mm 3 ) showed PCR amplifiable β-catenin DNA in the blood, suggesting that the sensitivity of the current method would allow us to detect premalignant adenomotous polyps at least as small as 63 mm 3 . Quantification of the copy number of β-catenin DNA in the samples using real-time PCR analysis is suggested. The findings indicate that measuring the levels of β-catenin DNA in the blood provides a highly sensitive but noninvasive method for early detection of colorectal cancer. This method may be extended to cancers of different tissue origins.
[0033] Referring now to the drawings, FIG. 1 collectively shows detection of β-catenin RNA from plasma of colorectal carcinoma patients using RT-PCR. More specifically, FIG. 1 a shows RT-PCR amplification of β-catenin using β-catenin exon primers. Lanes 1-4, RT-PCR reactions of blood RNA samples isolated from two carcinoma patients in the presence (Lane 1 & 3) and absence (Lane 2 & 4) of RT enzyme; Lane 5, mRNA extracted from carcinoma specimen expressing β-catenin as a positive control; Lane 6, a buffer control. M: RNA markers. FIG. 1 b shows RT-PCR amplification of β-catenin using β-catenin intron-spanning primers. Lanes 1-10, DNAase-treated plasma RNAs isolated forum ten carcinoma patients; Lane 11 genomic DNA as a positive control for PCR reaction; Lane 12, a buffer control. Lanes 13-17, Samples derived from Lanes 8-12 respectively without prior DNAase treatment. FIG. 1 c shows Lane 1-3, β-catenin RNA (250 bp) isolated from three patients by RT-PCR with intron-spanning primers without DNAase treatment; lane 4, positive DNA control; lane 5, negative buffer control. M: DNA markers.
[0034] FIG. 2 shows detection of blood β-catenin ( FIG. 2 a & FIG. 2 b ) & β-actin ( FIG. 2 c ) RNA from patients suspicious for colorectal adenoma ( FIG. 2 a - 2 c ) using RT-PCR. A. Lanes 1-17, plasma RNAs isolated from 17 patients; Lane 18, positive DNA control; Lane 19, negative control. Detection of blood β-catenin ( FIG. 2 d ) & β-actin ( FIG. 2 e ) RNA from plasma of ten healthy objects (Lanes 1-10). Lane 11, positive DNA control, Lane 12, negative buffer control.
[0035] FIG. 3 shows detection of serum β-catenin DNA from patients with adenomas or carcinomas and normal controls. FIG. 3 a , FIG. 3 b and FIG. 3 c show PCR analyses with β-catenin specific primers were performed with serum samples isolated from patients with colorectal carcinoma: FIG. 3 a , lanes 1-15; with colorectal adenoma: FIG. 3 b , lanes 1-10; from healthy individuals: FIG. 3 c , lanes 1-10. FIG. 3 d : PCR reactions with RET specific primers were performed with serum samples with negative β-catenin signal. Lanes 1-10, same healthy individual serum samples shown in FIG. 3 c ; FIG. 3 d , lane 13: the same serum sample shown in Panel FIG. 3 b , lane 8. Positive control genomic DNA isolated from carcinoma tumor: FIG. 3 a , lane 16; FIG. 3 b , lane 11; FIG. 3 c , lane 11; FIG. 3 d , lane 11. Negative cell free control: FIG. 3 a , lane 17; FIG. 3 b , lane 12; FIG. 3 c , lane 12; FIG. 3 d , lane 12. M: Hae III λ DNA marker.
TECHNIQUES APPLIED
Blood Samples and RNA Extraction
[0036] A 6-ml blood sample was collected from each patient by transcutaneous needle into 8-ml Vacutaniners containing EDTA lithium heparin. Blood samples were centrifuged at 4800 rpm for 8 min. Plasma was aliquoted into polypropylene tubes and stored at −80° C. for later RNA extraction. RNA was extracted from plasma sample using TRIZOL Kit (Life Technologies, USA), then purified with RNeasy column (Qiagen, Germany) according to the manufacturer's manuals. In brief, 2 ml of each plasma sample was mixed with 1.6 ml TPIZOL and 0.4 ml chloroform, centrifuged at 12,000 rpm for 15 min at 4° C. The aqueous phase was collected for RNA extraction using the RNeasy column. The isolated RNA was dissolved in 15 μl of DEPC-treated water. The RNA samples were farther treated with PCR grade of deoxyribonuclease I (DNase I)(Life Technologies). In the reaction, 1 μl each of 10×DNase I reaction buffer and DNase I were added into the 15 μl of RNA sample and incubated at room temperature for 15 min followed by inactivation of DNase I by the addition of 1 μl of 15 mM EDTA and heated at 65° C. for 5 min, then chilled in ice before RT-PCR reaction.
Primers and RT-PCR Reactions of Blood RNA Samples
[0037] The detection of plasma β-catenin was performed using RT-PCR assay with a set of primers including intron sequence spanning between exon 3 and 4 of β-catenin gene (Table 1). For comparison, a separate set of primers sequences within exon 3 of the β-catenin gene was also incorporated in some PCR reactions. The reverse transcription reaction was performed according to the manufacturer's guides (Qiagen, Germany). PCR was carried out using reagents supplied in a GeneAmp DNA Amplification Kit using AmpliTaq Gold as the polymerase (Perkin-Elmer Corp., Foster City, Calif.). The parameters used in PCR were 40 cycles with initial denaturation at 95° C. for 10 min, followed by 94° C. for 1 min 15 s, 59° C. (β-catenin) for 1 min 30 s, 72° C. for 1 min 30 s, with a final extension step of 72° C. for 10 min. PCR products were analyzed by 1.5% agarose gel electrophoresis and ethidium bromide staining. A negative (water) control was included in each RT-PCR assay. All samples with negative results were subjected to RT-PCR assay for β-actin RNA using intron-spanning primers (Table 3) as a control for the amplifiability of plasma-extracted RNA.
DNA Extraction
[0038] Blood sera were removed from the supernatants of clotted blood samples and were centrifuged at 4800 rpm for 8 minutes, followed by gently aliquoting of serum into polypropylene tubes and storage at −20° C. for later DNA extraction. DNA was isolated from 200 μl serum using QIAamp DNA Mini Kit (Qiagen, Hilden Germany) according to the manufacturer's protocol. The DNA samples, were eluted with 50 μl of ddH20.
Primers and PCR Reactions of Blood DNA Samples
[0039] The detection of β-catenin was performed using PCR assay with set of primers franking the 2 nd and the 3 rd introns of β-catenin gene (Table 3). The PCR was carried out using reagents supplied in a GeneAmp DNA Amplification Kit using AmpliTaq Gold as the polymerase (Perkin-Elmer Corp., Foster City, Calif.). The parameters used in PCR were 40 cycles with initial denaturation at 95° C. for 10 min, followed by 94° C. for 1 min and 15 s, 57° C. (β-catenin) and 69° C. (RET) for 1 min 30 s, 72° C. for 1 min 30 s, with a final extension step of 72° C. for 10 min. PCR products were analyzed by 1.5% agarose gel electrophoresis and ethidium bromide staining. PCR products were confirmed by direct DNA sequencing. A negative (water) control was included in each PCR assay. All samples with negative results were subjected to PCR assay for RET gene as a control for the amplifiable quality of the serum DNA samples. The RET gene sequence which encodes receptor tyrosine kinase, is normally present in circulating blood of healthy individuals (Matisa-Guiu 1998).
Immunohistochemical Staining and Evaluation
[0040] Monoclonal antibody to β-catenin (C19220) was purchased from Transduction Laboratories (U.S.A.). The antibody was produced against the C-terminal of a mouse catenin protein (a.a. 571-581), and is reactive to β-catenin of human, rat and mouse species. Tissue sections with 4 μm thickness were placed on silane-coated (Sigma Chemicals, St. Louis, Mo.) glass slides, air dried overnight and rehydrated with xylene and graded alcohol. Antigen retrieval and immunochemical staining was performed in the Ventana-ES automated immunostainer (Ventana, Tucson, Ariz.) as described. The sections were counterstained with Harris haematoxylin and mounted with permount after dehydration in graded alcohol. The negative control was done by replacing β-catenin antibody with TBS. Positive signals were evaluated in 4 fields under a light microscope at 10×40 magnification, without knowledge of the clinical outcome. The results were evaluated by two independent observe manually and the data were expressed as IHC score obtained by multiplying “percentage of positive cells” by “staining intensity” according to Remmele and Schicketanz with slight modification (Remmele & Schicketanz, 1993; Wong et al., 2001). In this study, the IHC scores were presented as follows: “−”=no expression, 1+=weak expression, 2+=moderate expression 3+=strong expression and 4+=very strong expression.
Quantitative Analysis of Plasma β-catenin RNA by Real-Time RT-PCR
[0041] Copy numbers of plasma β-catenin RNA were measured by real-time RT-PCR, using the TagMan detection system (Heid et al., 1996). The amount of fluorescent product at any given cycle within the exponential phase of PCR is proportional to the initial number of template copies. The reactions were recorded and analyzed using an ABI Prism 7700 sequence detector equipped with a 96-well thermal cycler (Perkin-Elmer Applied Biosystems, UK). Briefly, RNA samples (50-100 ng) were incubated with 0.01 units of uracil N-glycosylase (2 min at 50° C.) and reverse-transcribed in a 25-μl oligo(dT)-primed reaction at 60° C. for 30 min. The cDNA templates were then subjected to a 5-min initial denaturation at 92° C. prior to 40 cycles of PCR (92° C. for 20 s and 62° C. for 1 min, per cycle) in the presence of forward and reverse primers, then labeled with the fluorescent quenching group 6-carboxyfluorescein at the 5′ end and the fluorescent quencher molecule at the 3′ end.
TABLE 1 Sequence of primers used in the PCR reactions. Primer Nucleotide sequence pro- size (5′ to 3′) Design duct 1 sense: Within exon 3 of 224 bp ATTTGATGGAGTTGGACATGG β-Catenin gene antisense: AGCTACTTGTTCTTGAGTGAA 2 sense: Intron-spanning DNA: TGATTTGATGGAGTTGGACAT between 450 bp antisense: exon 3 & 4 of β- cDNA: CATTGCATACTGTCCATCAAT Catenin gene 250 bp 3 sense: Intron-spanning DNA: AAATCGTGCGTGACATTAAGG between 324 bp antisense: exon 4 & 5 of β- cDNA: ATGATGGAGTTGAAGGTAGTT actin gene 230 bp
[0042]
TABLE 2
Correlation of plasma β-catenin RNA in colorectal adenoma and
carcinoma patients with nuclear β-catenin expression (IHC scores) in their
respective lesions.
Duke's
Size of
Plasma
IHC of
Patients
Sex
Age
Diagnosis
stage
lesion
β-catenin
β-catenin
1
F
65
granulation tissue
N.A.
N.A.
−
−
2
F
68
granulation tissue
N.A.
N.A.
−
−
3
F
59
dilated lymphatic space
N.A.
N.A.
−
−
4
F
68
adenoma, moderate dys
N.A.
N.A.
+
+
5
F
75
adenoma, mild dys
N.A.
N.A.
+
++
6
M
82
adenoma, mild dys
N.A.
N.A.
+
+
7
F
61
adenoma, moderate dys
N.A.
5 mm
+
+
8
M
68
adenoma, moderate dys
N.A.
4 mm
+
+
9
F
77
adenoma, moderate dys
N.A.
N.A.
+
++
10
M
72
adenoma, moderate dys
N.A.
10 mm
−
++
11
M
51
adenoma, mild dys
N.A.
N.A.
+
+
12
F
81
adenoma, moderate dys
N.A.
N.A.
+
+
13
M
67
adenoma, moderate dys
N.A.
72 mm 3
+
++
14
M
75
adenoma, moderate dys
N.A.
672 mm 3
−
++
15
M
70
adenoma, mild dys
N.A.
N.A.
+
+
16
M
78
adenoma, severe dys
N.A.
1500 mm 3
−
+++
17
F
73
adenoma, severe dys
N.A.
1200 mm 3
+
+++
18
M
59
adenocarcinorna
B
91 cm 3
+
+
19
F
56
adenocarcinoma
C
90 cm 3
+
+
20
F
67
adenocarcinoma
C
108 cm 3
+
+
21
F
75
adenocarcinoma
C
100 cm 3
+
++++
22
F
92
adenocarcinoma
N.A.
N.A.
+
++++
23
F
79
adenocarcinorna
N.A.
N.A.
+
++
24
F
76
adenocarcinoma
B
88 cm 3
+
++
25
M
82
adenocarcinoma
D
115 cm 3
+
+
26
F
77
adenocarcinoina
B
346 cm 3
+
+
27
F
73
adenocarcinoma
A
21 cm 3
+
++++
28
F
82
adenocarcinoma
N.D.
N.D.
+
++++
29
F
80
adenocarcinoma
B
130 cm 3
+
++
30
M
77
adenocarcinoma
B
155 cm 3
+
+++
31
M
62
adenocarcinoma
B
167 cm 3
+
++
32
F
85
adenocarcinoma
B
143 cm 3
+
+++
dys: dysplasia;
N.A.: not applied;
N.D.: not determied.
[0043]
TABLE 3
Primers used in the PCR reactions.
Nucleotide sequence
Product
Primer
(5′ to 3′)
Design
size
1
sense:
In intron 2
359 bp
TCAATGGGTCATATCACAGAT
and 3 of β-
antisense:
Catenin gene
CTGCATTCTGACTTTCAGTAA
2
sense:
Within exon
156 bp
CCTCTGCGGTGCCAAGCCTC
11 of RET
antisense:
gene
TGTGGGCAAACTTGTGGTAGCA
[0044]
TABLE 4
Patients record
Duke's
Size of
Patient
Sex
Age
Diagnosis
stage
lesion
1
M
23
adenoma, severe dys
N.A.
75 mm 3
2
F
48
adenoma, moderate dys
N.A.
N.A.
3
M
67
adenoma, moderate dys
N.A.
168 mm 3
4
M
67
adenoma, severe dys
N.A.
80 mm 3
5
M
76
adenoma, severe dys
N.A.
63 mm 3
6
F
62
adenoma, mild dys
N.A.
N.A.
7
M
85
adenoma, severe dys
N.A.
153 mm 3
8
F
81
adenorna, moderate dys
N.A.
96 mm 3
9
F
58
adenoma, moderate dys
N.A.
48 mm 3
10
F
68
adenoma, moderate dys
N.A.
528 mm 3
11
M
62
adenocarcinoma
B
182 cm 3
12
M
67
adenocarcinoma
B
72 cm 3
13
M
83
adenocarcinoma
B
43 cm 3
14
M
45
adenocarcinoma
C
67 cm 3
15
M
52
adenocarcinoma
C
41 cm 3
16
F
71
adenocarcinoma
C
64 cm 3
17
M
80
adenocarcinoma
C
47 cm 3
18
M
61
adenocarcinoma
N.D.
N.A.
19
F
70
adenocarcinoma
A
13 cm 3
20
M
69
adenocarcinoma
B
120 cm 3
21
M
61
adenocarcinoma
C
384 cm 3
22
F
72
adenocarcinoma
A
9 cm 3
23
M
76
adenocarcinoma
N.D.
N.A.
24
M
76
adenocarcinoma
C
88 cm 3
25
M
70
adenocarcinoma
B
23 cm 3
dys: dysplasia;
N.A.: not applied;
N.D.: not determined
[0045] While various embodiments are disclosed herein, it should be understood that they have been presented by way of example only, and not limitation. Thus, the breadth and scope of the invention(s) should not be limited by any of the above-described exemplary embodiments, but should be defined only in accordance with the following claims and their equivalents. Moreover, the above advantages and features are affected in described embodiments, but shall not limit the application of the claims to processes and structures accomplishing any or all of the above advantages. Furthermore, teachings from the following references are incorporated herein by reference for all purposes:
Anker, P., Lefort, F., Vasioukhin, V., Lyautey, I., Lederrey, C., Chen, X. Q., Stroun, M., Mulcahy, H. E. and Farthing, M. J. K-ras mutations are found in DNA extracted from the plasma of patients with colorectal cancer. Gastroenterology 112:1114-1120, 1997. Chen, X. Q., Bonnefoi, H., Pelte, M-F., Lyautey, J., Lederrey, C., Movarekhi, S., Schaeffer, P., Mulcahy, H. E., Meyer, P., Stroun, M. and Anker, P. Telomerase RNA as a detection marker in the serum of breast cancer patients. Clinical Cancer Research 6: 3823-3826, 2000. Hibi, K., Robinson, C. R., Booker, S., Wu, L., Hamilton, S. R., Sidransky, D. and Jen, J. Molecular detection of genetic alterations in the serum of colorectal cancer patients. 58:1405-1407, 1998. Kopreski, M. S., Benko, F. A., Kwak, L. W. and Gocke, C. D. Detection of tumor suppressor messenger RNA in the serum of patients with malignant melanoma. Clinical Cancer Research 5: 1961-1965, 1999. Kopreski, M. S., Benko, F. A and Gocke, C. D. Circulating RNA as a tumor marker: detection of 5T4 mRNA in breast and lung cancer patient serum Ann. N.Y. Acad. Sci. 945: 172-178, 2001. Lo, K. W., Lo, Y. M. D., Leung, S. F., Tsang, Y. S., Chan, L. Y. S., Johnson, P. J., Hjelm, N. M., Lee, J. C. K. and Huang, D. P. Analysis of cell-free Epstein-Barr virus-associated RNA in the plasma of patients with nasopharyngeal carcinoma. Clinical Chemistry 45: 1292-1294, 1999. Matias-Guiu, X. RET protooncogene analysis in the diagnosis of medullary thyroid carcinoma and multiple endocrine neoplasia type II. Advances in Anatomic Pathology 5: 196-201, 1998. Morin, P. J. β-catenin signaling and cancer. Bioessays, 21: 1021-1030, 1999. Remmele, W., Schicketanz, K. H. Immunohistochemical determination of estrogen and progesterone receptor content in human breast cancer. Computer-assisted image analysis (QIC score) vs subjective grading IRS. Pathol Res Pract 189: 862-866, 1993. Sozzi, G., Musso, K., Ratcliffe, C., Goldstraw, P., Pierotti, M. A. and Pastorino, U. Detection of microsatellite alterations ill plasma DNA of non-small cell lung cancer patients: a prospect for early diagnosis. Clin. Cancer Res. 5: 2689-2692, 1999. von Knobloch, R., Hegele, A., Brandt, H., Olbert, P., Heidenreich, A. and Hofman, R. Serum DNA and urine DNA alterations of urinary transitional cell bladder carcinoma detected by fluorescent microsatellite analysis. Int. J. Cancer 94: 67-72, 2001. Willert, K. and Nusse, R. β-catenin: a key mediator of Wnt signaling. Curr. Opin, Genet. Dev. 8: 95-102, 1998. Wong, S. C., Chan, K. C., Lee, K. C., Hsiao, W. L. Differential expressions of p16/p21/p27 and cyclin D1/D3, and their relationships to cell proliferation, apoptosis and tumor progression in invasive breast ductal carcinoma. J Pathol 194: 35-42, 2001.
[0058] Additionally, the section headings herein are provided for consistency with the suggestions under 37 CFR 1.77 or otherwise to provide organizational cues. These headings shall not limit or characterize the invention(s) set out in any claims that may issue from this disclosure. Specifically and by way of example, although the headings refer to a “Technical Field of the Invention,” the claims should not be limited by the language chosen under this heading to describe the so-called field of the invention. Further, a description of a technology in the “Background of the Invention” is not to be construed as an admission that technology is prior art to any invention(s) in this disclosure. Neither is the “Brief Summary of the Invention” to be considered as a characterization of the invention(s) set forth in the claims set forth herein. Furthermore, the reference in these headings, or elsewhere in this disclosure, to “invention” in the singular should not be used to argue that there is only a single point of novelty claimed in this disclosure. Multiple inventions may be set forth according to the limitations of the multiple claims associated with this disclosure, and the claims, and their equivalents, accordingly define the invention(s) that are protected thereby. In all instances, the scope of the claims shall be considered on their own merits in light of the specification, but should not be constrained by the headings set forth herein.
|
This disclosures provides, in one aspect, a method for detecting non-clinically diagnosed cancer in a patient. In one embodiment, the method includes extracting blood serum or plasma from the patient, and then detecting beta-catenin RNA in the blood serum or plasma. In addition, in this embodiment, the method includes determining the presence of the cancer based on the detected beta-catenin RNA. In another aspect, this disclosure provides another embodiment of a method for detecting non-clinically diagnosed cancer in a patient. In this embodiment, the method includes extracting blood serum or plasma from the patient, and then detecting beta-catenin DNA in the blood serum or plasma. In addition, in this embodiment, the method includes determining the presence of the cancer based on the detected beta-catenin DNA. Related methods for detecting non-clinically diagnosed cancer in a patient comprising detecting beta-catenin-associated gene RNA, and beta-catenin-associated gene DNA, in the blood serum or plasma are also disclosed.
| 2
|
BACKGROUND OF THE INVENTION
In many loading dock areas, as well as in factories, warehouses, and other industrial areas in which moving equipment such as motorized forklifts are used, safety is important for the protection of personnel, equipment, and goods being handled. The danger of accidents increases in the vicinity of doorways or other passageways through which moving vehicles and/or personnel may travel at high rates of speed into other areas where they may collide with other vehicles, personnel, or obstacles.
There are inherent dangers associated with loading dock stations because loading docks typically are raised several feet with respect to the outside roadway and, moreover, trucks and semi-trailers are frequently moving immediately outside of the loading dock area. Because the passageways at loading dock stations involve high traffic situations to enable the loading or unloading of parked vehicles, it is desired to prevent forklifts from accidentally falling off the loading dock when a parked vehicle is not present. Forklifts are capable of traveling at high rates of speed while being difficult to handle and steer, particularly for inexperienced operators. Forklifts are also very heavy, which combined with their speed, results in large amounts of momentum and kinetic energy, making such forklifts difficult to stop.
Commercial and industrial doors are often subject to damage when they are inadvertently hit by forklifts or other large moving objects. Doors can sometimes prevent forklifts from traveling through the passageway, but many doors, particularly those made of fabric, plastic, or lightweight metal, may provide a false sense of security because they are not capable of stopping a forklift, and hence are subject to damage or disruption of the door as well as serious personal injury to the forklift driver and cargo, as well as other personnel, goods, and equipment which may be in the area.
Efforts have been made to provide substantially reinforced doors in an attempt to prevent such accidents, however, such doors are very expensive and the increased size and weight of the door are counterproductive because they result in slower travel of the door making it impossible to move the door either up or down fast enough to avoid accidents, as well as slowing the loading or unloading operation.
While there has been a long-felt need for a safety barrier to prevent accidental ingress or egress through a passageway, until recently such a barrier has been impractical. For example, a standard swinging gate mounted on a vertical post for pivotal movement about the vertical axis defined by the post, e.g., a barnyard gate, has not been practical in many industrial uses because of the time and effort involved in opening and closing such gates and because such gates can obstruct traffic even when in an open position.
Recently, a new safety gate assembly was invented and disclosed in U.S. patent application Ser. No. 07/799,032 (co-pending with this application) and also assigned to Rite-Hite Corporation. The safety gate of the latter application is hingedly mounted to a support member and pivotally movable in a substantially vertical plane. The pivotal safety gate, however, is inherently limited by the ratio of the width of the passageway to the height of the ceiling or other restrictions of the height to which the pivoting safety gate can travel.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a safety barrier which will solve one or more of the problems noted above while avoiding the limitations of the prior art.
Thus, a safety barrier is provided which may be readily installed in existing or new structures, generally for use in proximity to passageways or doorways, such as those found in loading dock areas, factories, warehouses, and the like. The new safety barrier assembly can be operated in a variety of climatic conditions. When properly used, the safety barrier can help to prevent personal injury, damage to moving equipment and cargo, and damage to doors and other equipment.
Further and additional advantages of the improved safety barrier will become apparent from the description, accompanying drawings and appended claims.
In accordance with one embodiment of the invention, a safety barrier assembly is provided with is mounted in proximity to a passageway such as found in a loading dock at a loading/unloading station. The assembly includes a pair of stationary upright support members which can be positioned on opposite sides of the passageway. A vertically traveling barrier is mounted on the support members and includes at least one horizontal member, or elongate segment, which spans the distance between the support members. The safety barrier can be moved between an operative passage blocking mode and an inoperative non-blocking mode. The barrier travels substantially vertically, and preferably, when in the inoperative mode, the barrier is placed in a position above the flow of traffic. Drive means are provided for the safety barrier, in the form of an electric or hydraulic motor, a manual chain fall and sprocket, or one or two hydraulic cylinders.
Preferably, the barrier means includes two horizontal members or elongate segments which will be placed in predetermined positions when in an operative mode, effectively preventing undesired travel through the passageway. It may be desired to offset the upper elongate segment slightly rearwardly, so that a forklift approaching the front of the passageway will first intersect the lower segment, thereby reducing the moment arm through which such force will be transmitted to the loading dock floor. When in the raised or inoperative blocking mode, it is desired to position both segments as high as possible to maximize the head space. Therefore, the invention includes means to provide for a minimal distance between the two segments when they are in the inoperative mode.
One of the advantages of the present invention is that it is well adapted for use in proximity to passageways which are relatively wide with respect to the height of the ceiling or overhead restrictions. For example, the invention is suitable for use with a passageway that is 15 feet wide when the ceiling is 10 feet high. It will be understood that a wide variety of sizes of passageways will be accommodated by the present invention, both as to the width and height of the passageway. One or more stop means are provided which engage the barrier segments only when in the operative mode. The stop means limit the extent to which the elongate segments can travel in a downward direction. Operatively connected to the drive means is a safety means, such as a lower limit switch described below, which is responsive to a person or an object positioned under the safety barrier so as to obstruct downward movement of the lower segment. The optional safety means senses the obstructing object and may automatically interrupt movement of the elongate segments.
DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the invention reference is made to the drawings wherein:
FIG. 1 is an inside front elevational view of the improved barrier assembly shown with the barrier assembly in an operative mode at the bottom of the figure, and with the barrier assembly in an inoperative mode at the top of the figure.
FIG. 2 is a left side elevational view of the improved barrier assembly of FIG. 1.
FIG. 3 is a right side elevational view of the assembly of FIG. 1.
FIG. 4 is an enlarged sectional view taken along line 4--4 of FIG. 1.
FIG. 5 is an enlarged sectional view taken along line 5--5 of FIG. 1.
FIG. 6 is an enlarged sectional view taken along line 6--6 of FIG. 1.
FIG. 7 is an enlarged fragmentary view showing the flanges 23 and drive shaft 63 in the upper left portion of FIG. 1.
FIG. 8 is an enlarged fragmentary view of the drive member 21 and the idler bearing 61 at the upper right of FIG. 1.
FIG. 9 is an enlarged sectional view taken along line 9--9 of FIG. 6.
FIG. 10 is an enlarged sectional view taken along line 10--10 of FIG. 1.
FIG. 11 is a front elevational view of an alternative embodiment of the invention using a manual chain fall and sprocket drive.
FIG. 12 is a left side elevational view of the assembly shown in FIG. 11.
FIG. 13 is a right side elevational view of the assembly shown in FIG. 11.
FIG. 14 is an enlarged sectional view taken along line 14--14 of FIG. 11.
FIG. 15 is an enlarged sectional view taken along line of 15--15 of FIG. 11.
FIG. 16 is a front elevational view of an alternative embodiment of the invention using hydraulic cylinders as the drive means.
FIG. 17 is a left side elevational view of the assembly shown in FIG. 16.
DESCRIPTION
Referring now to the drawings and more particularly to FIG. 1, one embodiment of the improved safety barrier assembly 10 is shown installed on a floor F in proximity to a passageway P. The floor and the passageway may be similar to that shown in U.S. patent application Ser. No. 07/799,032, also assigned to Rite-Hite Corporation. The safety barrier assembly 10, as illustrated, provides a safety barrier to prevent undesired or unintentional travel through passageway P. The safety barrier assembly 10, as illustrated, includes a pair of laterally spaced, upright post-like support members 11 and 13 which may be of like construction. One support member is disposed adjacent each side of the passageway and preferably within the building interior. The support members are laterally spaced apart a greater distance than the width of the passageway, thus not obstructing the use of the passageway during unloading/unloading operation. The support members 11 and 13 may be provided with track means 14 in which horizontal members or elongate segments 15 and 17 may travel a substantially vertical path. The track 14 may be more clearly understood by reference to FIG. 10, which also illustrates structural reinforcement means which may take the form of a support channel 18. The support channel 18 may be connected to the support members 11 and 13 by weld connections 19, see FIGS. 6 and 10. Support channel 18 shown in FIG. 10 may be used on the lower portions of the support members as shown in FIG. 1, or, alternatively, the reinforcement may take other forms and extend to other parts of the support members. The support members are attached to the floor by the use of bolts B, see FIG. 10, which should be of sufficient diameter and length and of satisfactory material, when considered in combination with the structural strength of the floor, to provide adequate anchoring for the support members and the possible forces to be encountered by the safety barrier when in the operative mode. If desired, additional structural reinforcement (not shown) can be provided by the use of rails, I-beams, or the like, which can be extended from the barrier assembly to the floor, walls, or ceiling of the building.
In the embodiment shown in FIG. 1, a header means is shown which may take the form of a drive member 21 which further adds to the structural stability of the safety gate assembly while also providing roller means for raising and lowering the safety barrier. In the alternative, rollers, pulleys, sprockets, or the like, may be used to provide roller means. The drive member 21 is provided with two pairs of strap guide flanges 23 which will be discussed momentarily. In this embodiment, an electrical gear motor drive 25 is shown, which is mounted on one of the upright support members, in this instance, support member 11. The electric gear motor drive 25 provides drive means for drive member 21, but it will be understood that other drive means such as a manual drive or hydraulic drive or the like may be used as alternative drive means.
As shown in FIG. 1, the electric gear motor drive 25 can be operated to rotate the drive member 21 and thereby raise or lower segment 15 and 17, while the straps 27 are being wound or unwound about the drive member 21 in the places provided by the strap guide flanges 23. Each strap 27 may be connected to drive member 21 at flanges 23 by means of a pin 23a inserted through a loop 27a sewn into the top of strap 27. See FIG. 7. It will be understood that alternative strap means may be provided such as a chain, a rope, a wire rope cable, or the like.
Referring now to the bottom segment 15, a pair of feet 31, one at each end of the segment, provide for a resting position of the bottom segment at the bottom of the passageway. See FIGS. 1-4. The height of the bottom segment when in the operative position is a matter of design choice and can be varied easily by varying the length of feet 31 or by using other stop means such as metal brackets welded to support members 11 and 13 so as to intercept the segment when traveling in tracks 14 toward the down position.
A set of wear pads 33 and 35, preferably made of ultrahigh molecular weight polyethylene, is provided for each end of elongate segment 15. A corresponding (but reversed in size) set of wear pads 51 and 53 is provided for each end of elongate segment 17. In the embodiment shown, wear pads 33 and 53 are thick wear pads and pads 35 and 51 are relatively thin by comparison. The thick wear pads may be about one inch thick whereas the thin wear pads preferably are about 0.375 inches thick. The elongate segments 15 and 17 preferably are in the form of 5 inch by 3 inch rectangular tubes made of steel. In the preferred embodiment the upper elongate segment is offset from the lower elongate segment by reversing the wear pads. Thus, FIGS. 1 and 2 show that the bottom segment 15 is provided with a thick wear pad 33 at the rear of the assembly while segment 17 is provided with a thick wear pad 53 at the front of the assembly. The reason for the offset is that an impact such as from a forklift can be expected to occur at the front of the assembly, and it is desired for the maximum force from the impact to be transmitted to the lower segment to shorten the moment arm between the point of impact and the floor.
The lower segment 15 shown in FIGS. 1-4 is also provided with a spacer 37 so that when the lower segment 15 is raised, the spacer 37 will contact the upper segment 17 and raise the upper segment to inoperative position, see FIG. 4. The straps 27 are attached to each end of lower segment 15 through the use of two anchor bars 41 shown on FIG. 1. See also FIGS. 4, 6, and 9. The bolts 43 are provided nuts 44 which can be adjusted to fasten the anchor bar to the bolts while also allowing some degree of adjustment or positioning of the anchor bar with respect to bolts 43 and lower segment 15.
Upper segment 17 is provided with a foot 45 at each end thereof and in the operative position the foot 45 rests on a stop member 47 welded to support members 11 and 13. Upper segment 17 is provided with a set of wear pads at each end thereof, including a thin wear pad 51 and a thick wear pad 53. At each end of upper segment 17 a slot 55 is provided in the top as well as in the bottom of the segment allowing straps 27 to pass through the segment for connection to anchors 41 and to drive member 21.
In operation, the strap 27 is wound by rotating the drive member 21 thereby lifting lower segment 15 until spacer 37 contacts upper segment 17, whereupon the two segments travel together until they reach the inoperative position at the top of he upright support members. An upper limit switch 57 may be provided as shown in FIG. 5 to detect the presence of upper segment 17 at the upper end of a support member, whereupon the switch can then turn off the motor 25.
The process of lowering the elongate segments is accomplished by reversing the direction of drive member 21 thereby unwinding straps 27 which in turn lowers the lower segment 15 to its operative position. Upper segment 17 is carried by lower segment 15 until upper segment 17 comes to rest on stop member 47 whereupon its motion stops and it is in the operative position.
The phenomenon of the present invention whereby the lower segment 15 may be in motion after the upper segment 17 is stopped on the way to the lowermost travel of segment 15 may be described as lost motion. In the preferred embodiment, lost motion means are provided through the use of straps 27 and slots 55 as shown in FIG. 6. A variety of other mechanisms for producing lost motion could be provided as alternatives, through the use of gears, sprockets, clutches, wires, ropes, cables, or the like. Moreover, it may be desired to use control devices such as a programmable array logic (PAL) programmable logic control (PLC) or a microprocessor to effect such lost motion. Regardless of the particular means selected for producing this phenomenon, it can be appreciated that the horizontal elongate segments 15 and 17 are positioned an optimum vertical distance apart while in the operative mode, but are positioned closely together when in the inoperative mode to maximize the amount of head space available in the passageway.
When the lower segment 15 is being lowered to its operative position, at the end of its travel the horizontal segment 15 comes to rest upon its feet 31 at which time lower limit switch 59 is triggered by the slack in strap 27 which results from any continued rotation of drive member 21. See FIG. 5. Accordingly, when the lower segment 15 reaches its operative position, the electric motor 25 is automatically shut off by the lower limit switch 59.
Returning to the drive member 21 shown at the top of FIG. 1, the right side of drive member 21 is mounted at the top of upright support member 13 through the use of a bracket and an idler bearing 61. See FIG. 5. Similarly, the left end of drive member 21 is mounted at the top of upright support member 11. By use of a suitable bracket, the drive member 21 is connected to the electric motor 25 with output shaft 63. See FIGS. 1 and 7. Other suitable drive member connections such as conventional couplings, guide and bearing collars with locking set screws, etc., may be utilized.
An alternative embodiment of the safety barrier assembly of this invention employs a manual operating mechanism such as the chain fall and sprocket shown in FIGS. 11-15. When possible, the element numbers used to identify parts of the alternative embodiment will correspond to numbers used for the electric-drive embodiment except that a 100 series will be used.
The alternative safety gate assembly 110 shown in FIG. 11 includes an upright post-like support member 111 positioned on one side of the passageway, while another upright support member 113 is positioned on the other side of the passageway.
The manually operated safety barrier assembly of FIG. 11 includes a lower elongate segment 115 and an upper elongate segment 117. A header means which is shown in the form of a drive member 121 is provided with two sets of flanges 123. The drive means provided for the drive member 121 includes a manual chain fall 124 which can be used to rotate sprocket 126 and thereby turn drive member 121 to wind or unwind the straps 127. It will be understood that a variety of manual drive means for operating the drive member 121 can be used through various combinations of gears, pulleys, cables, ropes, straps, or the like. The manually operated safety barrier assembly 110 includes wire rope cables 128 which are attached to counterweights 129 and segments 115 and 117. The wire rope cables 128 travel on pulleys 130 to raise or lower the counterweights which balance the respective segments. As shown in FIG. 15, a foot 131 is attached to the bottom of lower segment 115 and a thick wear pad 133 and a thin wear pad 135 are provided on respective sides of lower segment 115.
Similarly, upper elongate segment 117 is provided with a thin wear pad 151 and a thick wear pad 153, the relative positions of the wear pads being reversed from the positions for the lower wear pads. In the manual safety barrier assembly, the drive member 121 is supported at each end by a support bearing 160, see FIGS. 11, 13, and 14.
A further alternative embodiment of the safety barrier assembly provides for hydraulic means to raise and lower the elongate segments, as shown in FIGS. 16 and 17. The hydraulic safety barrier assembly 210 shown in FIG. 16 includes a lower elongate segment 215 and an upper elongate segment 217. No header in the form of drive member 21 or 121 is required for the hydraulic safety barrier assembly, thereby further reducing the potential for interference with dock door or building components to achieve a given inoperative mode. A hydraulic cylinder 281 fitted with a piston 283 is provided for each side of the passageway and a wire rope cable 285 is affixed at the top of each upright support member from which it travels through a pulley 285 and another pulley 288 through slots provided in upper elongate segment 217 and connecting to lower elongate segment 215. In operation, when the piston is raised to its uppermost height, the wire rope cable 285 will allow the elongate segments to descend to their respective operative positions. When the hydraulic piston 283 is fully retracted, the wire rope cable 287 will raise the lower elongate segment 215 until it intersects upper elongate segment 217 and the two elongate segments are then fully raised to their inoperative position. It will be understood that the two cylinders 281 should be operated to achieve synchronized motion on each side of the assembly, through the use of metering pumps, switches, or the like, as known in the art.
Thus an improved safety barrier assembly has been provided which is effective for providing a safety barrier in proximity to a passageway such as commonly found in loading dock stations. The improved safety barrier assembly is adaptable for a wide range of passageways, including passageways which are relatively wide in comparison to the height of the ceiling or other overhead restrictions. Moreover, a variety of drive means may be provided, such as electric, manual, or hydraulic, and through the use of lost motion means, it is possible to optimally position the barrier means in the operative mode while minimizing the amount of space required for the barrier means when in the inoperative mode.
|
A safety barrier assembly is disclosed to provide a movable barrier for an access passageway or doorway. The assembly includes a pair of upright support members and vertically travelling barrier means with at least two horizontally disposed elongate segments being selectively moveable between an operative passage blocking mode and inoperative non-blocking mode. Drive means are provided for moving the segments and lost motion means allow for positioning the segments a predetermined first distance apart when in the operative mode while positioning the segments close together when in the inoperative mode. Stop means may be provided for engaging one of the elongate members when in the operative mode.
| 4
|
BACKGROUND OF THE INVENTION
This invention relates to article display and vending devices which typically are usable in retail stores to display cigarette packages or other similarly packaged, stackable articles, for example, soap, photographic film, etc.
Retail stores and particularly supermarkets display for sale at the check-out counter a variety of items including cigarettes. A number ot types of cigarette display and vending racks have been used. In the most common type of installation, the rack is a simple cabinet having a number of vertical dividers which define a plurality of parallel vertical slots in which the cigarette packages may be stacked. The rack often is placed on the check-out counter facing the customer and facing away from the cashier. Experience has indicated a very high rate of pilferage from these devices. In addition, they are limited in size for a number of reasons, one of which being that if made too large the rack may obstruct the cashier's view. Thus, the typical self-service type of cigarette rack holds relatively few packages of cigarettes and must be replenished often. Also, because of the generally small size of the rack, the variety of cigarette brands often must be limited.
Pilferage is a substantial problem and a number of efforts have been made to locate cigarette racks remotely from the customer, for example, by placing a cigarette rack on top of the cash register where it can only be reached by the cashier. This type of installation also presents some difficulties. For example, a rack so located sometimes is difficult and awkward to refill because it may be difficult to reach. In addition, placement of the cigarette rack over the cash register obstructs a substantial portion of the cashier's view. Also, such racks are quite limited in size, for example, to the width of the register.
In addition to the above, prior racks have presented still further difficulties. For example, it is not uncommon for an entire stack of cigarettes to fall out of its vertical channel. Also, with typical prior art cigarette racks, each vertical channel is dimensioned to receive only one size of cigarette package (e.g., "regular", "king size", or "one hundred millimeter length"). This requires some care in loading the rack to assure that the correct size cigarette package is placed in the proper vertical channel. It is somewhat of a nuisance and is time consuming. Also among the difficulties is that when the bottom package in the stack is withdrawn from the rack it sometimes happens that more than one package is drawn out. This is somewhat inconvenient and, in some instances, the disruption at the bottom end of the stack can cause the entire stack to become unstable and fall out of its vertical channel.
It is among the objects of the invention to provide an improved display and vending device which overcomes the foregoing and other difficulties.
SUMMARY OF THE INVENTION
The device may be formed in one or more sections which may be arranged in a straight line, L-shaped configuration or otherwise as desired. Each section has a generally rectangular frame which is suspended overhead from the ceiling structure. The frame extends generally parallel to the check-out counter and above the inside edge of the counter. The side which faces the customer is closed by a transparent panel to enable the customer to see the articles in the device. The other side of the frame, which faces the cashier is open to enable the device to be filled and to enable easy withdrawal of the articles by the cashier. A plurality of vertical dividers are horizontally spaced within the frame and extend from top to the bottom to define a plurality of vertical article-receptive channels. A supporting shelf rests on the bottom of the frame inside the device and defines a platform for the lowest article in each vertical stack, the remaining articles in each vertical channel being stacked one atop each other. The shelf has inclined surfaces which tilt the lowest aticle and, therefore, the rest of the articles in the stack to retard their falling out or being drawn outwardly with the lowest article in the stack. The shelf also includes a lip having a plurality of spaced cut-outs therein, there being one cut-out associated with each vertical channel. The lip facilitates retention of a variety of sizes of cigarette packages and the cut-outs facilitate easy grasping of the individual bottom package in the stack. Each frame also has associated with it, at the open face thereof, a horizontally extending bar located above the support shelf to insure that the cigarette packages or other articles will be in proper alignment as they gravitate toward the shelf.
It is among the objects of the invention to provide an improved display and vending rack.
A further object of the invention is to provide an improved check-out counter configuration for a retail type of establishment embodying an improved overhead display and vending rack.
Another object of the invention is to reduce pilferage of cigarettes or the like at the check-out region of a retail store.
A further object of the invention is to provide a display and vending rack which has a substantially increased capacity.
Another object of the invention is to provide an article display and vending rack which is easy to load and in which removal of the individual articles is facilitated.
A further object of the invention is to provide a vending rack for stackable articles which displays the articles to the customer but which does not permit the customer to actually reach the articles.
Another object of the invention is to provide a cigarette vending and display rack which can accommodate substantially all commercially available lengths of cigarette packages.
A further object of the invention is to provide a display and vending device for use in the cashier region of a retail establishment which does not obstruct the cashier's view.
Another object of the invention is to provide an improved display and vending rack in which any of the vertical channels can receive substantially any size or brand of commercially available cigarette packages.
Still another object of the invention is to provide an improved display and vending device which results in more usable space at the counter level of a check-out counter.
DESCRIPTION OF THE DRAWINGS
The foregoing and other objects and advantages of the invention will be understood more fully from the following further description thereof, with reference to the accompanying drawings wherein:
FIG. 1 is an illustration of an L-shaped display and vending rack as might be seen by the customer;
FIG. 2 is a segmented plan illustration of the rack shown in FIG. 1;
FIG. 3 is a front elevation of the device as seen from the customer's side;
FIG. 4 is an elevation of the device as seen from the cashier's side;
FIG. 5 is a side elevation of an end portion of the frame of the device as seen along the line 5--5 of FIG. 4;
FIG. 6 is a sectional elevation of the device as seen along line 6--6 of FIG. 4;
FIG. 7 is a partial plan sectioned illustration of the device as seen along line 7--7 of FIG. 5; and
FIG. 8 is a somewhat diagrammatic plan illustration of a typical check-out counter employing the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIGS. 1 and 8 show an embodiment of the invention and the manner in which it may be installed with respect to a typical check-out counter, for example, as in a supermarket. FIG. 1 shows an embodiment in which the device is formed from two sections 10, 12 which are suspended overhead from the ceiling structure by suspension rods 14. The sections 10, 12 are substantially identical in construction except that in the embodiment shown the section 10 is longer than the section 12. As shown, sections 10, 12 may be supported in an L-shaped configuration. FIG. 8 illustrates, diagrammatically, a desired relative location in plan, of the rack with respect to a typical check-out counter as is found in a supermarket. The generally L-shaped check-out counter shown includes the counter portion 16 on which the cash register 18 is placed. The sections 10, 12 of the device similarly are arranged in an L-shaped configuration and are suspended so that they extend along the inside regions of the check-out counter, where the cashier is located. The sections 10, 12 are suspended at an elevation in which the bottom of the sections 10, 12 are well above the cashier's head so that they do not obstruct the cashier's view.
As shown in FIGS. 2, 3 and 4 each of the sections includes a generally rectangular frame defined by an upper frame section 20, a lower frame section 22 and a pair of side frame sections 24, 26, all of which preferably are fabricated from sheet metal. For ease in description, the frame will be considered as having an outwardly or rearwardly facing side (the side facing the customer as seen in FIG. 1) and an inwardly or forwardly facing side (as would be seen by the cashier). The upper and side frame sections 20, 24 and 26 are of generally channel-shaped cross-section having flanges 28 extending longitudinally along their edges. The lower frame section 22 also has a flange 30 extending longitudinally and upwardly along its outwardly disposed edge. The frame sections 20, 22, 24 may be joined together where they meet at the corners by appropriate sheet metal fastening techniques. The outward face of each section is covered by a transparent panel (e.g., plastic) 32 which fits whithin the frame and is retained by the flanges 28, 30. The transparent panel 32 serves as a completely closed rear wall but enables the customer to view articles carried in the section.
The articles to be displayed and sold, such as cigarette packages, are exposed on the cashier's side of the panel 32 and are supported on a transversely extending shelf, indicated generally at 34 in FIGS. 4-6. The shelf 34 extends the full width of the section, from one of the side frame sections 24 to the other 26. The shelf 34 is generally concave, or V-shaped and also is fabricated from sheet metal bent to define (as seen in cross section) a rear leg 36, a downwardly and forwardly inclined rear shelf portion 38, a forwardly and upwardly inclined front shelf portion 40, a reverted forwardly and upwardly inclined lip 42 and a downwardly extending front leg portion 44. The configuration of these parts of the shelf 34 is such that the junction 46 of the rear leg 36 and rear shelf portion 38 is disposed above the other portions of the shelf 34. The rear shelf portion 38 preferably makes an angle with the rear leg portion 36 of no more than approximately 45°, and the front shelf portion 40 and extension defining the lip 42 make an angle with the rear shelf portion of at least more than 90° and, preferably of the order of 120°. The shelf 34 is self supporting in the device and the rear leg 36 bears against the inwardly facing surface of the transparent panel 32 to retain the panel in place. The legs 36, 44 bear directly on the lower frame section 22. Also, the shelf 34 preferably is constructed so that the outermost edge of the lip 42 lies below the height of the juncture 46. As will be described, the configuration of the support shelf 34 serves to present the lowermost pack of cigarettes to the cashier in a manner which facilitates its removal.
The lower frame section 22 may have, at its forward edge, an upwardly extending lip, indicated in phantom at 23 in FIG. 5, to engage the leg portion 44 of the shelf. Alternatively, the lip 23 may be omitted and the forward edge of the lower frame section 22 may have a channel-shaped extension depending therefrom, as defined by panels 25 and 27, shown in solid in FIG. 5. This latter configuration further strengthens the structure.
The interior of the rectangular section 10 is divided into a plurality of vertically extending channels indicated generally by the reference character 48 to separate the vertical stacks of articles from each other. The vertical channels 48 are defined by a plurality of dividers 50 which extend from the upper frame section 20 downwardly to the shelf 34. The dividers 50 may also be fabricated from sheet metal having vertical front and rear edges 52, 54 (FIG. 6) and a lower edge 56 which is inclined downwardly and rearwardly and rests on the front shelf portion 40 of the shelf 34. The dividers are retained in place by means of tabs 58, 60 which extend through forwardly-rearwardly extending slots 62, 64 formed in the upper frame section 20 and front shelf portion 40, respectively. By way of example, a typical section may include 24 vertical channels 48. In the embodiment shown the dividers 50 are evenly spaced and the channels 48 which they define of equal width.
This configuration is suited particularly for use in connection with vending of cigarette packages which, typically, all are of substantially the same width and thickness. Cigarette packages, however, do differ in length and a number of cigarette lengths are commercially available such as "regular size" (approximately 70 millimeters), "king size" (approximately 85 millimeters) and "100 millimeter" size. The invention is able to accommodate any of these sizes in any of the vertical channels 48. The depth of the channel and, particularly, the configuration of the shelf 34 are such that the smallest length package will be easily accessible while the longest length package will not protrude excessively from the device. FIG. 5 illustrates the manner in which the cigarette packages, indicated in phantom at 66, may be stacked within one of the channels 48. The lowermost package, indicated at 66', will protrude well beyond the other packages in the stack sufficiently so that it can be grasped easily by the cashier. This results from the configuration of the shelf 34. As it can be seen from FIG. 5, when the lowest package 66' is removed, the remaining packages in the stack above will fall of their own weight. The rear shelf portion 38 which is inclined forwardly and downwardly will guide the lowest package in the stack forwardly to the position suggested at 66'. The lowest pack 66' which rests on the shelf portion 40 and lip portion 42 is supported so that its forward end is in a forwardly and upwardly inclined attitude which causes the remaining packages stacked above also to assume the inclined attitude suggested in FIG. 5. That attitude tends to preclude the cigarette packages from falling out of the channels 48 in that each of them tends to slide downwardly and rearwardly toward and against the transparent rearward wall 32.
The forward shelf portion 40 and forwardly extending lip 42 are sufficiently deep (as measured from the forward edge 67 of the lip to the juncture 70 of shelf portions 38 and 40) to be able to provide a firm support surface for the full range of package sizes. As illustrated, the depth of the shelf portion 40 and lip 42 is greater than the length of "regular" size cigarette packages but is less than the length of "100 millimeter" size cigarette packages.
In order to be able to easily grasp all of the commercially available sizes of cigarette packages, the lip 42 is provided with a plurality of cut-out regions 68, there being one cut-out associated with each vertical channel 48. The cut-out region 68 is sufficiently deep so that when even the smallest length of cigarette package is supported on the shelf 34 (with its lower rearward corner disposed at the corner 70 of the shelf 34) the forwardmost end of the lowest cigarette package 66' will project forwardly beyond and overlap the cut-out 68 as suggested in phantom at 72' in FIG. 5. The reference character 72 illustrates the location of the forwardmost end of the next adjacent cigarette pack in the stack.
The invention also includes a horizontal aligning bar indicated at 74 mounted to the front side of the device above the shelf 34 and extending transversely across the entire width of the device. The horizontal bar 74 is secured by appropriate means to the side frame sections 24, 26. The bar 74, is employed to urge any of the cigarette packages in the stack which may be protruding too far forwardly, back into the device to maintain the stability of the stack and also to insure that the cigarette packages will engage the shelf 34 and be properly positioned on the shelf 34 for removal. To this end, the horizontal bar 74 includes a downwardly and rearwardly inclined flange 76 which extends from the upper edge of the bar as shown. As indicated at 66", a cigarette package which may have been improperly placed in the device and which extends too far forwardly will engage the bar and will be guided back into the channel as the package 66" slides along the flange 76. The horizontal bar 74 also aids in rigidifying the device. The bar 74 may be secured to the frame, for example, at the side frame sections 24, 26 by bolts 71. The bar 74 may be fabricated from sheet metal and, in the illustrative embodiment, is bent along its length to define a bottom panel 73, a front panel 75, and the downwardly and rearwardly inclined flange 76. The transverse ends of the bottom panel 73 may have an upwardly extending tab 77 which bears against the forwardly facing flange 28 of the side frame sections 24, 26 to facilitate securing the bar 74 in place. The bolts 71 may be passed through aligned holes in the front panel 75 and tabs 77 as shown.
The device may be hung from an appropriate overhead support, such as the ceiling grid or ceiling structure, by brackets 78 secured to the side frame sections which receive suspension rods 14. Where two sections are arranged in an L-shaped configuration as shown it is desirable to connect the adjacent ends of the sections as by an additional bracket 80 connected to the upper ends of each of the sections 10, 12. If desired, an additional L-shaped connector bracket 82 may be passed through the adjacent channels defined by the bars 74 where those bars mate as suggested at 84 in FIG. 1.
The device is capable of handling a large inventory of cigarette packages encompassing the full range of commercially available cigarettes. In this regard, it may be noted that the frame section 10, for example, may be approximately 41 inches wide and 24 inches high and approximately 51/2 inches deep. A section having these dimensions is capable of holding 24 different brands totalling approximately 650 individual packages. The total weight of such a substantial number of cigarette packages is significant and the construction of the device is such that it can hold such a load without deformation which might have an adverse affect on its operation.
While the invention has been described primarily in connection with a device for displaying and vending cigarette packages it should be understood that it is usable to display and vend other types of packages or articles. It will be appreciated that the invention enables a substantial number of articles to be displayed while enabling them to be readily available for sale. Moreover, these objectives are achieved without interfering with the cashier's view and in a manner which also results in increased usable counter space. In addition, losses from pilferage necessarily are significantly reduced.
It should be understood that the foregoing description of the invention is intended merely to be illustrative thereof and that other modifications and embodiments may be apparent to those skilled in the art without departing from its spirit.
|
A display and vending device for stackable articles such as cigarette packages or the like is suspended from overhead supports, for example, at the check-out counter of a retail store. The articles contained in the device are accessible only to the cashier but are visible to the customer. The device includes a frame having a plurality of vertical dividers which separate the stacks of articles and which enable the articles to be gravity fed. Means are provided for displacing the lowest article in each stack so that it projects from the stack and is easily grasped by the cashier.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Continuation of application Ser. No. 12/801,332 filed Jun. 3, 2010, which is a Divisional of application Ser. No. 12/318,844 filed Jan. 9, 2009, which is a Divisional of application Ser. No. 11/826,292 filed Jul. 13, 2007, which is a Continuation of application Ser. No. 11/245,027 filed Oct. 7, 2005, which is a Divisional of application Ser. No. 10/913,485 filed Aug. 9, 2004, which is a Divisional of application Ser. No. 10/093,699 filed Mar. 11, 2002, which is a Continuation of PCT/CH00/00563 filed Oct. 18, 2000, which claims priority from German Patent Application. No. 199 50 204.8 filed Oct. 19, 1999 and German Patent Application. No. 299 19 053.6 filed Nov. 3, 1999.
BACKGROUND OF THE INVENTION
[0002] 1. Field of Invention
[0003] The invention relates to an interdental treatment device that includes an electrically powered vibrating head.
[0004] 2. Description of Related Art
[0005] For teeth-cleaning purposes nowadays use is made either of conventional manual toothbrushes or of electric toothbrushes, in the case of which a movable brush head can be motor-driven from the handle. Electric toothbrushes usually achieve a more intensive cleaning action than the manual toothbrushes, but they have the disadvantage that they are relatively bulky and expensive and may damage the gums and subject the tooth enamel to pronounced abrasion.
SUMMARY OF THE INVENTION
[0006] An object of the present invention is to provide a cost-effective vibrating toothbrush which corresponds, in size, approximately to the conventional manual toothbrushes and nevertheless allows a better cleaning action than the latter.
[0007] This object is achieved according to the invention by a toothbrush including a vibrating head part, a mechanical vibratory device in at least one of the head and a neck, and a power supply, preferably in the handle.
[0008] Since a mechanical vibratory device which causes the head part to vibrate is accommodated in a front head part of the toothbrush, or in a neck-part region adjacent to the head part, the neck part connecting the head part to the handle, and is operatively connected to a power source, preferably accommodated in the handle, via electrical connections running in the neck part, vibration-damping means preferably being provided in order to prevent vibration transmission to the handle, this achieves the situation where the vibrations which effect the improved cleaning action are produced predominantly in the head part and can only be felt to a slight extent in the handle, as a result of which comfortable handling of the toothbrush is achieved. A further advantage of the toothbrush according to the invention is that there is no need for any mechanical drive means to be led through the flexible neck part to the vibratory device. It is merely the electrical connections, designed as wires, cables or electrically conductive plastic tracks, which run through the neck part.
[0009] Preferred developments of the toothbrush according to the invention form the subject matter of the dependent claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The invention will now be explained in more detail with reference to the drawing, in which, purely schematically:
[0011] FIG. 1 shows a side view, partially in section, of a first exemplary embodiment of a toothbrush according to the invention and of a handle-closure part separated from one another (without a battery);
[0012] FIG. 2 shows a bottom view, partially in section, of a second exemplary embodiment of a toothbrush according to the invention in the assembled state;
[0013] FIG. 3 shows a side view, partially in section, of the toothbrush according to FIG. 2 and the closure part separated from one another (without a battery);
[0014] FIG. 4 shows a side view of a third exemplary embodiment of a toothbrush according to the invention in the assembled state;
[0015] FIG. 5A shows a front part of the toothbrush according to FIG. 4 with different embodiments of exchangeable interdental treatment heads; and
[0016] FIGS. 5B-D show different embodiments of exchangeable interdental treatment heads.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0017] Both the toothbrush illustrated in FIG. 1 and that according to FIGS. 2 and 3 each have a handle 1 , a front bristle-carrying head part 3 and a neck part 4 , which connects the head part 3 to the handle 1 . The bristles combined to form clusters of bristles 6 are anchored in a bristle carrier 5 and form a possibly profiled brushing surface with their free ends. In the embodiment illustrated, the bristle carrier 5 with the clusters of bristles 6 is positioned, in a manner which is known per se and thus is not described in any more detail, on a retaining part 2 of the head part 3 such that it can be exchanged.
[0018] The neck part 4 is provided with neck-part zones 7 which are made of an elastically relatively compliant material component and provide for, or additionally increase, the elasticity of the neck part 4 , with the result that, during use of the interdental treatment device, the head part 3 can be forced back resiliently in the case of forces acting in the direction of the brushing surface. If appropriate, the neck-part zones 7 are designed as notches which extend over part of the neck circumference and are filled with elastically compliant material (e.g. with thermoplastic elastomer). Of course, it would also be quite conceivable for the form and number of neck-part zones to be different. It is also conceivable to have a flexible neck zone without using elastic material components, e.g. by providing constrictions or by way of a bellows.
[0019] Integrated in the front head part 3 , or in that region of the neck part 4 which is adjacent to the head part 3 , is a mechanical vibratory device 10 , by means of which vibrations which effect or enhance the teeth-cleaning action may be imparted to the head part 3 . The vibratory device 10 can be connected to an electric power source, accommodated in the handle 1 , via electrical connections running in the neck part 4 , as is described herein below. The already mentioned neck-part zones 7 made of an elastically compliant material act here as means which damp the vibration between the vibrating head part 3 and the handle 1 , with the result that the vibratory action is produced, in particular, in the head part and is only transmitted to the handle 1 to a slight extent. This means that only slight vibrations can be felt in the handle 1 during the teeth-cleaning operation, and the toothbrush is thus comfortable to handle. Conversely, however, it is also advantageous that the vibration produced is not damped by the handle 1 and can act to full effect in the head part 3 . Instead of the neck-part zones 7 consisting of elastically compliant material, however, other vibration-damping means would also be conceivable; it is not absolutely necessary to use an elastic material. The damping may also be achieved, using a basic material, by the neck part being configured in a particular form, for example by the presence of a bellows/accordion part, etc.
[0020] Accommodated in the handle 1 is a sheath or sleeve 20 which extends in the longitudinal direction of said handle and is made of electrically conductive material. Both the handle 1 and the sleeve 20 are open to the rear, this forming a cavity 21 which can be closed from the rear by a closure part 22 and into which it is possible to insert a battery 25 , in the exemplary embodiment illustrated a commercially available, non-rechargeable cylindrical battery, with a defined power (e.g. 1.5 V) as the power source for the vibratory device 10 . It would also be possible, however, for a button cell or for a rechargeable storage battery to be used as the power source.
[0021] A spring contact 29 for the positive pole 30 of the battery 25 (see FIG. 2 ) is fitted in the sleeve 20 , on a transverse wall 28 , and is connected to the vibratory device 10 via an electric line 31 , a switch 32 , which is installed in the sleeve 20 and can be actuated from the outside of the handle 1 , and an electric line 33 running in the neck part 4 . The electrical connection can be interrupted by means of the switch 32 .
[0022] The closure part 22 is provided with a threaded stub 22 a made of an electrically conductive material and can be screwed into the handle 1 and/or into the sleeve 20 by way of said threaded stub. The threaded stub 22 a is provided with a contact surface 22 b which, with the closure part 22 screwed in, comes into abutment against the negative pole 35 of the battery 25 inserted into the sleeve 20 . The negative pole 35 is electrically connected to the vibratory device 10 via the threaded stub 22 a, the sleeve 20 itself and a line 34 , which connects the sleeve 20 to the vibratory device 10 and runs in the neck part 4 .
[0023] Instead of being transmitted via the electrically conductive sleeve 20 , it would also be possible for the power from the negative pole 35 to be transmitted in some other way, for example using wires or an electrically conductive plastic.
[0024] In the exemplary embodiment illustrated in FIG. 1 , the vibratory device 10 comprises a vibratory element 11 ′ which functions preferably in the manner of a vibratory armature, can be electrically connected directly to the power source via the lines 33 , 34 and, with the power source connected, is made to vibrate.
[0025] In the case of the toothbrush variants illustrated in FIGS. 2 and 3 , the vibratory device 10 comprises a vibratory element 11 in the form of an eccentric, which produces mechanical vibrations and can be rotated about an axis located in the longitudinal direction of the toothbrush, and also comprises a drive which is arranged directly adjacent and is designed as a micromotor 15 . The vibratory element 11 is connected to the shaft 15 a of the micromotor 15 , which can be electrically connected to the power source via the lines 33 , 34 . The micromotor 15 and the eccentric may be accommodated as a structural unit in a housing 12 .
[0026] Instead of an eccentric which can be driven in rotation, it would also be possible to have a vibratory element 11 which can be driven in a translatory manner.
[0027] It would be possible, in the case of the toothbrush according to the invention, to arrange the bristle-carrying head part 3 such that it can be moved in relation to the neck part 4 in order for the latter, in the case of vibrations produced by means of the vibratory device 10 , to be made to move in relation to the rest of the toothbrush.
[0028] The electric lines 31 , 33 , 34 could also be realized by electricity-conducting plastic tracks.
[0029] The switch 32 , which connects or interrupts the lines 31 , 33 , may also be, for example, a magnetic switch.
[0030] The preferred configuration of the switch 32 , however, contains a pulse switch arranged on a printed circuit board as well as further electronic components which store the switching state.
[0031] It is also possible, however, for the electrical connection between the battery 25 and the vibratory element 11 ′ ( FIG. 1 ) or the drive 15 ( FIGS. 2 and 3 ) to be produced or interrupted not by the switch 32 , but by the closure part 22 , which can be screwed into the handle 1 and/or into the sleeve 20 or connected to the same in a bayonet-like manner, being turned (i.e. the switch 32 is dispensed with in the case of such a configuration).
[0032] Instead of the rear closure part 22 being screwed to the handle 1 , it would, of course, also be possible to have some other type of releasable connection (e.g. plug-in connection, bayonet connection, etc.) and a corresponding configuration of the contact part interacting with the negative pole 35 .
[0033] It would also be possible for the closure part 22 to be in a form which is quite different to that illustrated in the drawing. For example, the closure part could be provided with a set-down surface or a foot part and thus serve as an element on which the toothbrush can be set down.
[0034] The toothbrush illustrated in FIG. 4 corresponds essentially to that according to FIGS. 2 and 3 ; the same parts, once again, have the same designations. According to FIG. 4 , the vibratory device 10 is arranged directly in the front head part 3 . In this exemplary embodiment, the sleeve 20 is dispensed with; the battery 25 is connected directly to the vibratory device 10 via the lines 33 , 34 . It is also the case with this device that use is preferably made of an exchangeable carrier 5 which can be positioned on a retaining part 2 of the head part 3 , e.g. in the manner of a snap-in connection. The capacity for changing the bristle carrier 5 provided with the clusters of bristles 6 is particularly advantageous since the interdental treatment device provided with the vibratory device 10 can be used irrespective of the service life of the bristles, which is usually even shorter than the service life of the battery 25 .
[0035] As can be seen from FIG. 5 , it is possible, instead of the bristle carrier 5 or 5 a, which forms part of a conventional brush head and is provided with respective clusters of bristles 6 or 6 a, to position other, optionally different carriers or adapters 5 b to 5 d on the retaining part 2 , these being provided with different interdental brushes 6 b, 6 c or interdental treatment parts 6 d for effective cleaning of the spaces between the teeth. The interdental brush 6 b may be designed, for example, as a helical brush made of coated wire with plastic filaments twisted in. The interdental brush 6 c comprises bristles which, together, form a cluster tip. The treatment part 6 d may be designed, for example, as a plastic element which has a tip and may preferably be provided with an abrasive coating for removing plaque and tartar from the spaces between the teeth. Of course, it would also be possible to use any other desired treatment heads.
[0036] It is also the case with the variant according to FIGS. 4 and 5 that the bristle carrier 5 could be configured such that a vibration-induced movement in relation to the retaining part 2 were possible.
[0037] For the introduction of the vibratory device 10 , the connecting lines 33 , 34 and further electronic components, it is possible for the toothbrush according to the invention, or the housing thereof, to be produced in two parts and for the two parts to be welded in a water-tight manner once the abovementioned parts have been positioned therein.
[0038] It is also possible, however, for the toothbrush according to the invention to be produced by injection molding preferably involving two or more components. The abovementioned parts are advantageously positioned as a unit in an injection molding made of a first material component and then encapsulated in the second material component (or in the further material component) by injection molding. It is not necessary here for full encapsulation to take place. Certain parts may be exposed, as a result of which it is possible to achieve an esthetic effect.
[0039] It would also be possible, however, for the abovementioned electronic components to be inserted into a ready molded handle 1 .
[0040] Since it is not only the vibratory element 11 , 11 ′ itself but also the drive, i.e. the micromotor 15 , which are arranged in the front head part 3 , or in the directly adjacent front region of the neck part 4 , it is not necessary for any mechanical drive means to be led through the flexible neck part 4 in order to connect the micromotor to the vibratory element 11 . It is only the electric lines 33 , 34 (wires, cables or electrically conductive plastic tracks) which run through the neck part 4 .
[0041] According to the invention, use is made of a mechanical vibratory device 10 which has a diameter of less than 15 mm, preferably less than 6 mm, and is less than 35 mm, preferably less than 20 mm, in length. This ensures that the toothbrush may be of ergonomic configuration and is easy to handle. The toothbrush according to the invention may correspond, in size, more or less to the conventional manual toothbrushes, which makes them more straightforward to handle in comparison with the commercially available, considerably larger electric toothbrushes, even though this toothbrush achieves a cleaning action which is comparable with that of the known electric toothbrushes, but is gentler than the latter. Moreover, the toothbrush according to the invention is straightforward and cost-effective to produce.
[0042] It is nevertheless also possible for the vibratory device according to the invention to be integrated in conventional electric toothbrushes.
|
An interdental treatment device, such as a toothbrush, includes a handle configured to accommodate an electric power source, a head carrying an interdental treatment tool, and a neck between the handle and the head. The head or neck includes a mechanical motorized vibratory device, including a drive which causes the head to vibrate. Electrical connections are operably connected to the mechanical vibratory device and the electric power source to power the mechanical vibratory device via the electrical connections. In various embodiments, a switch may be operably connected to at least one of the electrical connections to interrupt power from the power source to the mechanical motorized vibratory device. In various embodiments, a vibration-damping structure dampens vibration transmission from the head to the handle.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This patent application is a continuation of Ser. No. 10/308,824 filed Dec. 2, 2002, which claims the benefit of provisional application Ser. No. 60/334,143 filed Nov. 28, 2001.
FIELD OF INVENTION
The present invention generally relates to a pen and/or pencil apparatus having a cosmetic application and, more particularly, to a pen and/or pencil apparatus containing a cosmetic preparation and/or cosmetic applicator.
BACKGROUND OF THE INVENTION
Companies that produce cosmetic products are continually trying to make their products more marketable by making them smaller and more compact thereby allowing them to be conveniently carried in a user's purse or handbag, or even in a student's backpack. Such companies also know that aside from reducing the space required to carry such items, users of cosmetic products value products that are convenient to use yet capable of discreetly being carried.
Accordingly, in an effort to provide compact cosmetic products that can be easily accessed for use while being discreetly carried, the present invention uses small everyday functional items such as pens and pencils to dually function as carriers of cosmetic products.
SUMMARY OF THE INVENTION
The present invention is directed to a pen and/or pencil apparatus comprising a first end containing lead or ink for writing, and at least one second end containing a cosmetic preparation for application to a user. The cosmetic preparation may include one or more of a lipstick, a lipliner, a lip color, an eyeliner, an eyelid color, an eyebrow pencil, a cheek color, a mascara, and any other cosmetic preparation capable of being contained within a tubular shaped opening having a diameter approximately equal to the diameter of a functioning pen and/or pencil. The pencil may be either a regular lead based pencil or a mechanical pencil having a telescoping feature to expose additional lead. The pen may be any type of pen such as, for example, a roller ball, a felt tip, etc., and may also have a telescopic feature for presenting the pen during use and storing the pen when not in use.
In one aspect of the invention, the first and second ends of the pen and/or pencil may have caps to cover the ink, lead, or cosmetic preparation when not in use. In another aspect of the invention, a cap covering the end containing the cosmetic preparation may include an applicator attached thereto for applying the cosmetic preparation. In still another aspect of the invention, the applicator may include a wand and a tip that is flat, rounded or brush shaped for applying the cosmetic.
In yet another aspect of the invention, the end of the pen and/or pencil containing the cosmetic preparation may also include a telescopic feature for presenting non-used portions of the cosmetic preparation when visible portions of the preparation are used up.
The present invention is also directed to a method for making a pen and/or pencil apparatus having a cosmetic application which includes providing a tubular member having first and second ends, installing a writing element Such as a pen or pencil tip and ink(or lead in one end of the tubular member for writing, and installing a cosmetic preparation in the opposite end of the tubular member for application to a user.
BRIEF DESCRIPTION OF THE DRAWINGS
Additional aspects of the present invention will become more evident upon reviewing the non-limiting embodiments described in the specification and claims taken in conjunction with the accompanying figures, wherein like numerals designate like elements, and:
FIGS. 1 and 2 are perspective views of a mechanical pencil and roller ball pen, respectively, each having a rounded lip gloss applicator positioned on their opposite ends;
FIGS. 3 and 4 are perspective views of a mechanical pencil and roller ball pen, respectively, each having screw caps including wand applicators with rounded tips positioned at their opposite ends;
FIGS. 5 and 6 are perspective views of a mechanical pencil and roller ball pen, respectively, each having screw caps including wand applicators with brushes positioned at their opposite ends;
FIGS. 7 and 8 are perspective views of a mechanical pencil and roller ball pen, respectively, each having a lip or eye color pencils positioned at their opposite ends;
FIGS. 9 and 10 are perspective views of a mechanical pencil and roller ball pen, respectively, each having a lipliner or eyeliner pencil positioned at their opposite ends; and
FIGS. 11 and 12 are perspective views of a mechanical pencil and roller ball pen, respectively, each having more than one lip or eye color pencil positioned at their opposite ends.
FIG. 13 is a cross-sectional view of FIG. 5 taken along line 13 - 13 of FIG. 5 to show the telescopic elements for presenting lead or ink at one end of the pen and/or pencil.
DETAILED DESCRIPTION
Preferred exemplary embodiments of the present invention will hereafter be described in conjunction with the description that follows. It will be understood that the detail provided herein is for illustration purposes only and that the subject invention is not so limited.
While specific embodiments of the pen/pencil apparatus having cosmetic application will be described in greater detail below, in general, the apparatus of the present invention includes a pen and/or pencil having a first end containing ink or lead for writing, and a second end containing a cosmetic preparation for application to a user.
FIGS. 1 and 2 show perspective views of a mechanical pencil 10 and roller ball pen 20 , respectively, each having a rounded lip gloss applicator 30 positioned on their opposite ends. Pencil 10 includes first end 12 having lead 14 for writing and second end 16 having applicator 30 for applying lipgloss and the like. Pencil 10 may also include one or more caps 18 for covering lead 14 and applicator 30 when not in use. It will also be understood by those skilled in the art that ends 12 and 16 of pencil 10 may include telescopic members which allow lead 14 and applicator 30 to be alternatively projected and retracted within ends 12 and 16 , respectively.
Pen 20 shown in FIG. 2 includes first end 22 having roller ball tip 24 and second end 26 having applicator 30 for applying lipgloss and the like. Like pencil 10 , pen 20 may also include one or more caps 28 to cover first and second ends 22 and 26 . First and second ends 26 and 28 may also include telescopic members. Applicator 30 may also be replaced with a lipstick which can be projected and retracted within second ends 16 and 26 of pencil 10 and pen 20 , respectively.
Turning now to FIGS. 3 and 4 , perspective views of a mechanical pencil 40 and roller ball pen 50 , respectively, are shown each having screw caps 48 including wand applicators 58 with rounded tips 59 positioned at their opposite ends. Pencil 40 includes first end 42 having lead 44 for writing and second end 46 having threads 60 which mate with screw cap 48 to secure screw cap 48 to second end 46 of pencil 40 . Second end 46 has an opening 47 that is contiguous with a reservoir (see, for example, reference number 85 in FIG. 13 ) which functions to retain a cosmetic preparation. Pen 50 includes first end 52 having roller ball tip 54 and second end 56 having threads 60 which mate with screw cap 48 to secure crew cap 48 to second end 56 of pen 50 . Second end 56 has an opening 57 that is contiguous with a reservoir (see, for example, reference number 85 in FIG. 13 ) which functions to retain a cosmetic preparation. Pencil 40 and pen 50 may also include a cap 61 for covering the first ends 42 and 52 of the pencil 40 and pen 50 , respectively, when not in use.
Any number of cosmetic preparations may be contained within the reservoirs contiguous with openings 47 and 57 of ends 46 and 56 of pencil 40 and pen 50 , respectively, thereby enabling tip 59 of applicator wand 58 to absorb and retain the cosmetic prior to its application to a user. Examples of suitable cosmetic preparations include, but are not limited to, powders, creams and lotions for eyes, cheeks and lips.
FIGS. 5 and 6 show perspective views of a mechanical pencil 70 and roller ball pen 80 , respectively, each having screw caps 78 including wand applicators 88 with spiral brushes 89 positioned at their opposite ends. Pencil 70 includes first end 72 having lead 74 for writing and second end 76 having threads 90 which mate with screw cap 78 to secure crew cap 78 to second end 76 of pencil 70 . Second end 70 has an opening 71 that is contiguous with a reservoir (see, for example, reference number 85 in FIG. 13 ) which functions to retain a cosmetic preparation. Pen 80 includes first end 82 having roller ball tip 84 and second end 86 having threads 90 which mate with screw cap 78 to secure screw cap 78 to second end 86 of pen 80 . Second end 86 has an opening 81 that is contiguous with a reservoir (see, for example, reference number 85 in FIG. 13 ) which functions to retain a cosmetic preparation. Pencil 70 and pen 80 may also include a cap 91 for covering the first ends 72 and 82 of pencil 70 and pen 80 , respectively, when not in use. Mascara is just one example of a suitable cosmetic preparation that might be used with spiral brush 89 of applicator wand 88 .
FIG. 13 shows a cross-sectional view taken along line 13 - 13 of FIG. 5 .
FIG. 13 shows a telescopic element 87 contained within the pen and/or pencil apparatus which enables unused portions of a lead or ink based substrate to be extended from the first end 72 of the apparatus. FIG. 13 also shows a reservoir 85 contiguous with an opening 71 at the second end 76 of pencil 70 .
FIGS. 7 and 8 are perspective views of a mechanical pencil 110 and roller ball pen 120 , respectively, each having a lip or eye color pencils positioned at their opposite ends. Pencil 110 includes first end 112 having lead 114 for writing and second end 116 having cosmetic pencil 130 for applying lip color, eye color, and the like. Pencil 110 may also include one or more caps 118 for covering lead 114 and cosmetic pencil 130 when not in use. It will also be understood by those skilled in the art that ends 112 and 116 of pencil 110 may include telescopic members which allow lead 114 and cosmetic pencil 130 to be alternatively projected and retracted within ends 112 and 116 , respectively.
Pen 120 shown in FIG. 8 includes first end 122 having roller ball tip 124 and second end 126 having cosmetic pencil 130 for applying lip color, cheek color, eye color, and the like. Like pencil 110 , pen 120 may also include one or more caps 128 to cover first and second ends 122 and 126 . First and second ends 122 and 126 may also include telescopic members. Cosmetic pencil 130 may also be replaced with a lipstick which can be projected and retracted within second ends 116 and 126 of pencil 110 and pen 120 , respectively.
FIGS. 9 and 10 are similar to FIGS. 7 and 8 , previously described, with the exception that cosmetic pencil 130 shown in FIGS. 9 and 10 is smaller for cosmetic preparations such as eyeliners, lipliners, and the like.
Finally, FIGS. 11 and 12 show perspective views of a mechanical pencil and roller ball pen, respectively, each having more than one lip or eye color pencil positioned at their opposite ends. For example, cosmetic pencils 130 having different colors 151 and 152 may be stacked on top of one another so that a user may have access to a variety of colors for cosmetic application.
While various principles of the invention have been described in illustrative embodiments, many combinations and modifications of the above described structures, arrangements, proportions, elements, materials and components used in the practice of the invention in addition to those not specifically described may be varied and particularly adapted for specific environments and operating requirements, without departing from the principles of the present invention.
|
A pen and/or pencil having an opening positioned opposite its writing end for retaining or storing a cosmetic preparation which can be applied to a user. Caps may also be included to cover both the writing end and/or the opposite end containing the cosmetic preparation. The cap covering the cosmetic preparation may also include an applicator such as a wand having a flat, round, or brush shaped tip.
| 1
|
BACKGROUND OF THE INVENTION
The present invention relates to a fabric drawing device for a flat knitting machine, comprising a traction roller, an entrainment means for the latter and rollers pressed against the traction roller. The entrainment means comprises pawls coacting with a ratchet wheel mounted on a traction roller, a tensioning spring associated with the pawls to impart spring bias to the traction wheel, and a cam which acts to increase the spring tension as desired.
This type of embodiment already is known from prior art. The drawing device described in the German patent No. 407,853 uses a cam which operates a lever against the force of a traction spring. The lever supports a pawl which coacts with a ratchet wheel fastened on a roller. The cam follower is prevented from contacting the lower portions of the cam by a tension balance between the force of the spring and the tension of the fabric resisting a downward pull. When the cam acts to increase the spring tension, that is, when the follower passes over a raised portion or protuberance on the cam, the pawl is raised and advances by one tooth. During this period of time, the ratchet wheel is held in its position by a non-return pawl. A certain recoil is then inevitable. This basic principle, which underwent several improvements, still is used. Among other matters, the number of pawls was increased, each of which is of different length in order to subdivide the pitch of the ratchet wheel; fastening points of the adjustable spring were introduced in order to make possible an adjustment of the length and a division of the initial force of the spring; torsion bars were introduced betweed the ratchet wheel and the roller to equalize the transmitted torque, etc.
In conventional drawing means there are substantial fluctuations in the spring tension, thus resulting in variations in fabric tension. These fluctuations often necessitate the inclusion of torsion bars which increase the cost of these mechanisms.
The regularity of the stitches and thus the good quality of the knitted goods is a function of the regularity of the traction exerted on the fabric. Thus, it is understandable that the drawing devices are a subject of continuous research.
OBJECTS AND SUMMARY OF THE INVENTION
The objective of the invention is to equalize the traction force, to avoid the recoil and to simplify the design.
In the device for drawing according to the invention, two levers, whose pivoting axes are offset in relation to each other, are pulled against each other by the spring, spaced from each other separately by the cam and each is provided with at least one pawl which coacts with the ratchet wheel.
The attached drawing exemplifies an embodiment of the drawing device according to the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front view.
FIG. 2 is a view from the bottom.
FIG. 3 is a front view of a knitting machine.
FIG. 4 is a front view of the draw down mechanism showing the levers in a spread position.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The wall 1 is fastened on the frame of the knitting machine. It bears a shaft to which the traction roller 3 is fixed. The bearing plate supports a shaft 4 on which roller supports 5 are mounted which support retaining rollers 6 pressed against the traction roller 3 by springs 39. The fabric 7 drops down from the needle beds 8, 9, represented by dots and dashes. The fabric passes between the traction roller 3 and the retaining rollers 6 and is pulled in the direction of the arrow 10 toward the bottom of the machine, by the traction roller 3. The retaining rollers 6 are entrained by the fabric and press the latter against the traction roller 3. It is entrained by an entrainment means which is described below.
A spacing bushing 11 and the ratchet wheel 12 are fastened to the shaft 2. The lever 13 is pivotally mounted on the end of the shaft 2. A stud 14 is chased into a protuberance 13a of the lever. This stud supports three pawls 15a, b and c which can pivot on the stud and which are pressed against the ratchet wheel 12 by the compression spring 16. The three separate pawls 15a, b and c have only been shown in FIG. 4. Alternatively, a single pawl 15 may be utilized as shown in the remainder of these FIGURES.
A stud 17 whose axis is shifted in relation to the axis of the shaft 2 is fastened in the bearing plate 1. The lever 18 is pivotally mounted on it. A stud 19 is chased into this lever 18. This stud 19 supports the three pawls 20a, b and c pawls 20 which can pivot on it and are pressed against the ratchet wheel 12 by the compression springs 21. The three separate pawls 20a, b and c have only been shown in FIG. 4. Alternatively, a single pawl 20 may be utilized as shown in the remainder of these FIGURES.
The two levers 13 and 18 are drawn against each other by the traction spring 22. This spring is hooked by one of its loops to the eyebolt 23, the latter being chased into the end 18a of the lever 18. The other loop of the spring 21 is hooked to an adjustment screw 24. The latter crosses an elbowed support 13b, located at the end of the lever 13. The adjustment screw 24 bears a nut 25 which bears down on the elbowed support 13b. By turning the nut 25, the length of the part of the adjustment screw 24 is changed which crosses the elbowed support, and thereby the length of spring 22 is modified. That way, the force with which both levers are pulled toward each other is changed.
The lever 13 is provided with a lug 26 and lever 18 with a lug 27. The arm 28 of one lever is located between both lugs 26 and 27. During the knitting, this lever continuously carries out an oscillating movement along arrow 29, of the same amplitude, for which it is entrained by a cam 40 (FIG. 3); This arm 28, through the oscillation caused by the cam 40, acts to increase the tension in the spring 22 by separating the lugs 26 and 27 and the levers 13 and 18 connected thereto. This spreading of the levers causes the ends of the spring 22 to become further separated, thus increasing the spring tension.
FIG. 4 depicts the use of three pawls mounted to each of the studs 14 and 19. The pawls 15a, b and c and 20a, b and c are of staggered length to minimize backlash and refine the advance and feeding of the fabric, thereby making the apparatus more operational. The use of multiple pawls also minimizes the stress in any one pawl, and allows sufficient tooth size to ensure sufficient traction force.
The drawing device operates in the following manner: The oscillating arm 28 spreads both levers 13, 18 according to the amplitude of its movement. This spreading causes the lever 13 and its pawl 15 to shift counterclockwise around its pivot 2a (which is the end portion of the shaft 2), and causes lever 18 and its pawl 20 to shift counterclockwise around its pivot (stud 17). Pawls 15 and 20 are allowed to slip over the ratchet wheel due to the configuration of the ratchet teeth. Once the levers are spread, their pawls engage into the teeth of the ratchet wheel. The pawls then hold the levers spread, while exerting a thrusting force on the ratchet wheel. This force is proportional to the preadjusted tension of the spring 22. It creates a torque in the ratchet wheel, said torque being transmitted via shaft 2 to the traction roller 3, where a traction force is created on the fabric. When a row of stitches is produced between the needlebeds 8,9, the fabric drops slightly, thus reducing the resistance offered against the traction roller. The traction roller, urged by spring 22 across the levers 13,18 and their pawls, turns slightly in a clockwise direction as the fabric drops. The spring tension insures that pawls move with the rotation of the traction roller, thus causing levers 13 and 18 to move toward each other, pivoting in a clockwise and counterclockwise direction, respectively. The arm 28 then oscillates to spread the lugs 26 and 27, thus restoring the preadjusted tension and the desired tension on the fabric, and the cycle is repeated.
The length of the fabric produced between two oscillations of the arm 28 being very small, the oscillating movements of both levers 13 and 18 likewise is very small, so that the length of the spring 22 is almost unchanged. Its traction force thus remains practically constant, which is translated into a very constant traction on the fabric.
FIG. 3 shows a knitting machine from which we removed a few parts to show the fabric drawing device more clearly.
This machine is composed of needlebeds 8 and 9 (FIG. 1) held by rear legs 30, 31, 32 and front legs 33, 34, 35, of a knitting carriage 36, coils 37 and a coil or bobbin holder 38. The bearing plate 1 is fastened between the rear leg 31 and the front leg 34. A bearing plate 1 is fastened between the rear leg 32 and the front leg 35.
Shafts 2 and 4 are located in these bearing plates 1 and 1'. The fabric 7 passes between the pulling roller 3 and the retaining rollers 6. The retaining rollers 6, carried by the roller supports 5 are pressed against the traction roller 3 by the springs 39, for example, according to the German Pat. No. 629,840.
The oscillating movement of the arm 28, may, for example, be generated by the rotation of an eccentric cam 40 placed in the plane of the movement of arm 28 and be entrained by an electric motor 41. The arm 28 pivots on a shaft 42, perpendicular to the movement plane and is maintained in contact with the cam 40 by a spring 43, stretched between the rear leg 31 and the end of the arm 28 remote from the lugs 26,27 (FIG. 1). Thus, the eccentric cam 40, which contacts the arm 28 between the pivot shaft 42 and the end of the arm in contact with the levers 13 and 18, acts to oscillate the shaft 28 and thereby regulate the tension on the fabric.
|
A fabric draw down device for a flat knitting machine having a traction roller for tensioning fabric, retaining rollers for pressing against the traction roller and entrainment means for driving the traction roller. The entrainment means includes a pair of opposing levers which are pivotally mounted on offset axes and are drawn together with a spring. The levers each have a pawl which acts on a ratchet wheel mounted on the traction roller. A camming means moves the pair of opposing levers to alternately drive and release the ratchet wheel.
| 3
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a digital communication system comprising at least one primary station arranged for frequency hopping based burst mode communication with a plurality of secondary stations, the primary station comprising a plurality of transceivers and a plurality of transceiver controllers which are coupled to the transceivers via a distribution medium. Such a system can be a digital cellular radio system in which the primary station is a radio base station and the secondary stations are mobile radio stations, or any other frequency hopping based digital communication system.
The present invention further relates to a primary station for use in such a system.
2. Description of the Related Art
A digital communication system and primary station of this kind are known from the International Patent Application WO 90/16122. In this Patent Application a radio base station for use in TDMA (Time Division Multiple Access) digital mobile radio systems is disclosed using frequency hopping techniques. The base station comprises a plurality of transceivers which are coupled to at least one antenna via a so-called combiner, and further a base station controller and a plurality of transceiver controllers. The transceiver controllers comprise channel codecs, speech codecs, and processors for handling signalling data or the like. For efficiently implementing a so-called baseband switching frequency hopping technique, the transceivers and the transceiver controller are coupled to a bus as a common distribution medium, the bus also being coupled to the base station controller. The transceiver comprises a receiver for receiving data such as voice data or other data from mobile stations and a transmitter for transmitting data to the mobile stations on a TDMA basis. Via the bus, when receiving, for particular mobile subscribers time slots e.g. containing bursts of digitally coded speech are directed to the correct transceiver controller as determined by a frequency hopping algorithm comprised in the base station controller, i.e. on a TDMA frame basis, each transceiver is connected with the correct transceiver controller. When transmitting a similar approach is taken. With baseband switching frequency hopping, the transceivers are tuned to fixed frequencies, the TDMA bursts to and from particular mobile subscribers having varying time slot positions within the TDMA frames. Such a bus structure as a common distribution medium is disadvantageous as to fault tolerance of the system. For a fault tolerant system, the bus should be doubled (redundancy).
SUMMARY OF THE INVENTION
It is an object of the present invention to provide digital communication system of the above type which is fault tolerant, and which can easily support said baseband switching type frequency hopping technique, and further a synthesizer hopping technique.
To this end a digital communication system according to the present invention is characterised in that the distribution medium comprises point-to-multipoint links between transceiver receiver sections and the transceiver controllers, and between the transceiver controllers and transceiver transmitter sections. It is achieved that, when a transceiver or a transceiver controller fails, only one line is down. Although, in the case of baseband switching, the traffic processing capacity of the primary or base station is slightly reduced when a transceiver controller goes down, and less frequencies are available when a transceiver goes down, the system is highly fault tolerant. With such failure, most of the current traffic can still be handled. The system can simply be reconfigured to a 100% working system, though with reduced capacity.
In an embodiment of a digital communication system according to the present invention point-to-multipoint links are shared by at least two transmitter receiver sections, and further point-to-multipoint links are shared by at least two transceiver controllers. Although with some reduced fault tolerancy, in this embodiment the number of physical connection lines between the transceivers and the transceiver controllers is reduced.
In an embodiment of a digital communication system according to the present invention the point-to-multipoint links are divided into data links and timing links, whereby the data links are coupled between the transceivers and the transceiver controllers, and the primary station comprises a primary station controller which is coupled to the timing links, the timing links controlling the transceivers and the transceiver controllers. In this way synchronous data transfer is achieved.
In an embodiment of a digital communication system according to the present invention at least the timing links are duplicated. Although the system is also fault tolerant as to the timing links because any of the units coupled to a timing link can take over control as a master in case the actual master goes down, with this redundancy it is achieved that the system is still more reliable.
Further embodiments allow the system to be configured for both baseband switching frequency hopping and synthesizer hopping frequency hopping. In case of synthesizer hopping each transceiver comprises a synthesizer which can quickly be adjusted to each frequency of the so-called hopping cluster, i.e. the group of transceivers which are grouped together using a predetermined set of frequencies for their traffic.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example, with reference to the accompanying drawings, wherein
FIG. 1 schematically shows a digital communication system according to the present invention,
FIG. 2 is a blockdiagram of a first embodiment of a primary station for use in such a system,
FIG. 3 is a blockdiagram of a second embodiment of a primary station,
FIG. 4 shows timing signals on the timing links,
FIG. 5 shows a structure of a SID signal,
FIG. 6 shows a packet structure of a packet on the data links,
FIG. 7 shown an RF-unit, and
FIG. 8 shows a radio codec and control unit.
Throughout the figures, the same reference numerals are used for the same features.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 schematically shows a digital communication system 1 according to the present invention, comprising radio base station transceivers as primary stations BS1, BS2, and BS3 in cells ce1, ce2, and ce3 respectively. The primary stations BS1, BS2, and BS3 are arranged for frequency hopping based burst mode communication with a plurality of secondary stations MS1, MS2, and MS3. The digital communication system can be any frequency hopping based digital communication system. In the example given it will be assumed that the primary stations BS1, BS2, and BS3 are radio base stations transceivers providing radio communication in the respective cells ce1, ce2, and ce3, and that the secondary stations MS1, MS2, and MS3 are mobile radio stations roaming through the cells ce1, ce2, and ce3. An example of such a system is a so-called GSM System (Global System for Mobile Communications, Groupe Special Mobile). In order not to cause interference with neighbouring cells, the radio base stations transceivers, at least in adjacent cells, transmit and receive at different frequencies. In the said GSM system, which is a time division multiple access (TDMA) mobile radio system, each radio base station transceiver BS1, BS2, and BS3 transmits at a number of frequencies, e.g. twelve frequency channels. With eight time slots per frequency channel, 96 logical channels are available for radio communication per base station, then. In principle, the radio base stations transceivers BS1, BS2, and BS3 communicate with the mobile radio stations MS1, MS2, and MS3 when present in their respective cells ce1, ce2, and ce3, in the given example the radio base station transceiver BS1 communicating with the mobile radio stations MS1 and MS2, and the radio base station transceiver BS3 communicating with the mobile radio station MS3. When the mobile radio stations MS1, MS2, and MS3 are roaming through the cells ce1, ce2, and ce3, a so-called handover from one radio base station transceiver to another occurs if the quality of the communication link deteriorates. That is a system control function carried out by a Mobile Switching Centre MSC, which is connected to the radio base stations transceivers BS1, BS2, and BS3 via a base station controller BSC1. Also other clusters of radio base stations are coupled to the MSC via a further base station controller, e.g. BSC2. The MSC is connected to a Public Switched Telephone Network PSTN, in case of Public Mobile Radio. Instead of a PSTN, the MSC can also be connected to an Integrated Services Digital Network as a digital telephony network. For globally averaging fading phenomena in such a digital mobile radio system, so-called frequency hopping techniques are applied which are well-known per se. For implementing such techniques the radio base stations transceivers BS1, BS2, and BS3 each comprise a number of transceivers. In one frequency hopping technique, a so-called baseband switching frequency hopping technique, the transceivers are tuned to different fixed frequencies. Then, frequency hopping is achieved by switching each traffic channel over the various transceivers corresponding to the frequencies included in the frequency hopping scheme or algorithm, such algorithms being well-known per se. In another frequency hopping technique, a so-called synthesizer hopping frequency hopping technique, the transceivers are tuned from one frequency to another before each hop. In principle, baseband switching frequency hopping is a preferred technique, because of delays caused by tuning of synthesizers in the synthesizer hopping technique, and because of the necessity of having fast and complicated synthesizers available. In small cellular networks, however, the base stations do not have enough transceivers to implement a baseband switching frequency hopping technique and so synthesizer hopping is implemented. As will be described hereinafter, the present invention allows for both baseband switching and synthesizer hopping frequency hopping techniques. For a more detailed description of a cellular radio system, and further, a more detailed description of frequency hopping techniques, reference may be made to articles in Conference Proceedings of the Digital Cellular Radio Conference DCRC, Oct. 12-24, 1988, Hagen, Westfalia, FRG, "An Overview of the GSM System", B. J. T. Mallinder, pp. 1a/1-1a/13, "The Base Transceiver Station (BTS) to Base Station Controller Interface A-bis", H. Rosenlund, pp. 5b/1-5b/11, and "Options for the Implementation of Network Infrastructure", G. Mazziotto, pp. 6a/1-6a/11. In Chapter 8, "The GSM System", par. 8.3.4, "Frequency Hopping", pp. 698-700, of the handbook, "Mobile Radio Communications", R. Steele, Pentech Press, London, 1992, a GSM Frequency Hopping Algorithm is disclosed.
In FIG. 1, part of the radio base station transceiver BS3 is shown in more detail. Shown is a transceiver or RF-unit RFU1 comprising an RF-controller RFC1 controlling a transmitter radio part TX1 which modulates and transmits a baseband signal, and a receiver radio part RX1 which receives, demodulates and digitizes a received radio signal. The transmitter part TX1 and the receiver part are coupled to antenna coupling equipment ACE, and further to a cluster link interface CLI1 which is also coupled to the RF-controller RFC1. According to the present invention, the cluster link interface CLI1 is coupled to a point-to-multipoint cluster data link CDL and to a point-to-multipoint cluster timing link CTL, both links being coupled to similar RF-units (not shown). Further coupled to the links CDL and CTL is a radio codec and control unit RCC1, corresponding to the RF-unit RFU1. The radio codec and control unit RCC1 comprises a cluster link interface CLI2 coupled to channel codecs CHC which are coupled to a 64 kbits/sec PCM link PCM via speech codecs SPC. The cluster link interface CLI2 is further coupled to the PCM link PCM via a processor pool PP for carrying out other tasks than coding/decoding, such as monitoring, maintenance and the like. In the present context, cluster means the group of transceivers which are grouped so as to use a single set of frequencies for their traffic on the basis of frequency hopping techniques, i.e. the transceivers form a so-called hopping cluster. In one embodiment all participants of the hopping cluster are within a single rack RCK, the rack RCK being controlled by a rack interface unit RIF comprising a cluster link interface CLI3 coupled to the cluster timing link CTL and to the PCM link PCM via internal PCM hardware IPCM. The rack interface unit RIF further comprises a rack interface controller RIFC. Apart from the data links CDL as cooperating with the RF-units and the radio codec and control units as to the present invention, the base station 3 operates as a GSM base station, well-known in the art. The rack interface unit RIF acts as a master unit and controls the timing on the cluster timing link CTL, to be described subsequently. The data which are transmitted between the RF-units and the radio codec and control units, and vice versa, are basically the transmit data/receive data for/from mobile radio stations, i.e. the traffic, as well as control data for the RF-units with respect to the traffic itself, i.e. frequency offset of the synthesizer, timing offset in the frame, channel information, and the like. In addition to this data, in a single packet, a so-called operations and maintenance packet, an RF-unit may be remotely controlled by a radio codec and control unit, thus allowing direct communication between RF-units and radio codec and control units. Then, the communication medium is the cluster data link CDL. In another embodiment the hopping cluster may be divided over various racks.
FIG. 2 is a blockdiagram of a first embodiment of a base station BS1, BS2, and BS3 as a primary station for use in the system in FIG. 1. Shown are the transceivers RFU1, RFU2, . . . , RFUn, n being a predetermined integer, and further the transceiver controllers RCC1, RCC2, . . . , RCCn. The RF-units RFU1, RFU2, . . . , RFUn are coupled to a combiner COMB with their respective transmitter parts TX1, TX2, . . . , TXn, and to a receiver multi-coupler or splitter SPL with their respective receiver parts RX1, RX2, . . . , RXn. The transceivers comprise synthesizers, a synthesizer SY1 being shown for the transceiver RFU1. The synthesizers are tuned in a known way. The transceiver controllers RCC1, RRC2, . . . , RCCn, comprise codecs and processors as shown in FIG. 1, which are shown in FIG. 2 as radio codec transmit part RCTX1 to indicate a transmit part thereof as being coupled to the transmitter part TX1 of the transceiver RFU1, and as radio codec receive part RCRX1 to indicate a receive part thereof as being coupled to the receiver part RX1 of the transceiver RFU1, and control circuitry RCCT1 to indicate further functionality. In the part RCRX1, channel decoding and speech decoding is carried out, and in part RCTX1, speech coding and channel coding is carried out. The receiver part RX1 is coupled to the receive parts RCRX1, RCRX2, . . . , RCRXn via a point-to-multipoint link RXL1, as are the receiver parts RX2, . . . , RXn via respective point-to-multipoint links RXL2, . . . , RXLn. The radio codec transmit part RCTX1 is coupled to the transmitter parts TX1, TX2, . . . , TXn via a point-to-multipoint link TXL1, as are the radio codec transmit parts RCTX2, . . . , RCTXn via respective point-to-multipoint links TXL2, . . . , TXLn. The links RXL1, RXL2, . . . , RXLn, TXL1, TXL2, . . . , TXLn form the cluster data link CDL. A point-to-multipoint cluster timing link CTL is coupled to the rack interface unit R/F, being the master, to the transceivers RFU1, RFU2, . . . , RFUn, and to the transceiver controllers RCC1, RCC2, . . . , RCCn. For redundancy the timing link CTL may be duplicated.
FIG. 3 is a blockdiagram of a second embodiment of the radio base station transceiver BS1, BS2, and BS3 as a primary station. In this embodiment, being a sub-multiplexing variant, the receiver parts RX1 and RX2 share the link RXL1, to the receiver parts RXn-1 and RXn, sharing the link RXLn/2, and the radio codec and control transmit parts RCTX1 and RCTX2 share the link TXL1, to the radio codec and control transmit parts RCTXn-1 and RCTXn, sharing the link TXLn/2. In this embodiment the number of physical connection lines at one side is reduced by a factor of two. Further reduction factors may be implemented.
FIG. 4 shows timing signals on the timing links CTL, hatched lines showing uncertainty in timing. The cluster timing link CTL is used to ensure that all transceivers and transceiver controllers operate synchronously. Basically a 2.17 MHz clock signal and a synchronisation information data signal SID are transmitted on the timing link CTL, the clock being generated in the master RIF. For redundancy, the clock line is duplicated as CLKA and CLKB. The master can derive its clock signal from the incoming PCM link. The clock is used within the cluster link interfaces CLI1, CLI2, CLI3, . . . , for receiving and transmitting data on the cluster data links CDL. The clock is generated according to GSM Recommendations. The SID signal is a data stream at a data rate of 2.17 MHz, the same as for the cluster data links. The SID signal is updated on a per TDMA frame basis, i.e. with a period of 4.616 msec. With CDATA data on the cluster data links are indicated.
FIG. 5 shows a structure of the SID signal, which comprises a so-called TDMA number TDMA-NR in accordance with GSM Recommendation 05.02, with components T2bis, T3bis, T1, T2, and T3, for synchronisation purposes. The SID signal further comprises a frame sync pattern FSYNC between two guard bands G1 and G2, a CRC, and a bit sync pattern BSYNC. The TDMA number TDMA-NR is updated on a per frame basis, the TDMA number changing at the transition of time slot TS7 to time slot TS0. The TDMA number TDMA-NR is fed to the rest of the system in a frame following the one in which it appears on the timing link CTL. In this way it is guaranteed that everything, concerning synchronisation, has been correctly decoded before the rest of the system receives the TDMA number. The bit sync pattern BSYNC is used as a final sync check. The principle of operation is, once synchronised, the cluster link interfaces maintain their own value for the TDMA number and maintain phase synchronisation independently from the cluster timing link CTL. The cluster links interfaces at all times monitor the SID signal and obtain phase synchronisation and the TDMA number from the bus, only when requested to do so.
FIG. 6 shows a packet structure of a packet PK on the data links. The packet contains 8 bits start-of-packet SOP, 8 bits packet control PCTL, an 8 bits packet address PA at least containing a 4 bits destination address DA, and, optionally, a four bits source address SA, N*8 bits data D0, . . . , DN-1, N being an integer indicating a variable length data section, and a 16 bits packet check sequence PCS. Data on the cluster data links are transferred in packets on a per GSM time slot basis, the relation between the GSM time slots and the frame synchronisation being provided by the SID signal. The start-of-packet SOP is used by packet receivers to determine whether or not a packet exists. A transceiver of radio codec and control unit should send an all zero logic pattern when not transmitting a packet. The SOP signal is generated in the cluster link interfaces. The packet control PCTL, which is generated by an external source, indicates the type of data in the data fields D0, . . . , DN-1, types TX Data, TX Control, RX Control, RF Data, and O&M (Operations and Maintenance), respectively. The source address SA is the address of the transceiver or transceiver controller transmitting data via the data link, and the destination address DA is the address of the receiving transceiver or transceiver controller. So, by proper routing, different packet within corresponding time slots in successive frames may be sent to different destinations. From transceiver controller to transceiver: TX Data is 148 bits; TX Control comprises 3 bits TX Channel Index; RX Control comprises 3 bits RX Channel Index; O&M is 40 bits. From transceiver to transceiver controller: RF Data comprises RX Data; O&M is 40 bits. TX Data, the format of which is defined in GSM Rec. 05.02, is the information to be transmitted on the air interface during the current time slot. The TX Channel Index is used by the transceiver a pointer to a radio frequency channel. The RX Channel Index provides a pointer to a radio frequency channel. The channels corresponding to each pointer value should be available to the transceiver. RF Data is used to transfer a received data burst and associated parameters from the transceiver to the transceiver controller. Data transfer on the cluster data links is synchronised to the start of a time slot. An operation and maintenance channel is provided between transceiver controllers and transceivers in both directions, and is a single packet as described before, i.e. is a single packet per time slot. In the case of GSM control and data packets, the frequency hopping algorithm ensures that two transceivers or transceiver controllers are not transmitting to the same destination simultaneously. The O&M channel is exclusively used between a transceiver controller and its associated transceiver, and the transceiver only puts data on the O&M channel when requested to do so by the transceiver controller. Via the O&M channel the system is configured before being put into operation. When both the source address SA and the destination address DA are present, only a hopping algorithm, which is known per se e.g. from GSM Recommendation 05.02, Chapter 6.2.3, is present in the transceiver controller RCC, because of the fact that a transceiver knows to which transceiver controller it should transmit a received data packet. Such an implementation is a preferred one. When only the destination address DA is present, extra software has to be loaded into the RF-controllers RFC for unambiguous routing of data packets. Then, care has to be taken that the hopping algorithm is consistent with the extra software loaded into the RF-controllers, i.e. when changing the hopping algorithm the software in the RF-controllers has to be adapted accordingly. Via the TX Control field, controlling frequency adjustment of a transceiver, the TX Channel Index being the output of the frequency hopping algorithm. Which of the frequency hopping techniques is implemented, baseband switching frequency hopping or synthesizer hopping frequency hopping depends on the physical hardware of the base station. With a fixed filter/combiner frequency hopping is restricted to baseband switching, whereby the transceivers are adjusted to a fixed frequency, and time slots for a particular subscriber have a varying destination for successive frames. Then, only a single channel is filtered out, whereas all other channels are attenuated. In this implementation transmitters can be combined without giving rise to large output losses, an advantage for larger base stations. With a hybrid combiner without filter, i.e. a broadband combiner, synthesizer hopping can be implemented, whereby the frequency of the transceiver varies with a constant destination address for a particular subscriber from time slot to time slot. In a hybrid combiner transmitter outputs are interconnected via a starpoint having no filtering characteristics. Only two transmitter outputs can be coupled with each other at a starpoint, so, when combining more than two transmitters, the starpoints have to be cascaded, giving rise to relatively high output power losses. The latter hopping technique can be used in relatively small cellular systems where not enough synthesizers are available to implement baseband switching. In case of baseband switching the result of the calculation from the frequency hopping algorithm, the Channel Index, is interpreted and mapped onto a transceiver address using that fixed frequency and data are sent to the respective transceiver via the cluster data link. In case of synthesizer hopping, the Channel Index is sent directly to the transceiver corresponding to a transceiver controller and the transceiver is tuned accordingly. In the above implementations, the combiners are known per se.
FIG. 7 more in detail shows an RF-unit RFU1 in which also an equaliser EQU and a modulator MOD are shown. The cluster link interface CLI1 provides control information to the modulator MOD and the transmit part TX1 such as frequency channel adjustment data, and receives data from the receive path for direction to a selected destination. The RFC provides so-called O&M data (Organisation & Management data) to the cluster link interface CLI1 such as configuration data allowing operation of synthesizer hopping or baseband hopping and general control data for the RF-unit.
FIG. 8 more in detail shows a transceiver controller RCC1 in which a number of signal processor controller SPC1 and SPC2 are coupled to the cluster link interface CLI2 via a cluster output board COB to which further a number of channel codecs CHC are coupled. The channel codecs CHC are coupled to the cluster link interface CLI2 and to the A-bis interface and process received data RX-data and transceive data TX-data.
|
In digital radio communication systems such as FDMA/TDMA digital cellular mobile radio systems, in which a number of radio base stations communicate with a number of mobile radio stations, frequency hopping is used to combat fading. That requires that data bursts be routed between the transceivers (RFU1, RFU2, . . . , RFUn) and the transceiver controllers (RCC1, RCC2, . . . , RCCn) in a radio base station according to a frequency hopping algorithm. Such routing has heretofore been done by transporting the data bursts over a bus which serves as a common distribution medium between the transceivers and the transceiver controllers. In order to achieve a more fault tolerant system, instead of a bus the invention uses as a common distribution medium point-to-multipoint links (RXL1, RXL2, . . . , RXLn; TXL1, TXL2, . . . , TXLn) between the receiver section of each transceiver and the receiver sections of all of the transceiver controllers, and between the transmitter section of each transceiver controller and the transmitter sections of all of the transceivers. In case of failure of a particular transceiver or transceiver controller, most of the existing traffic can still be handled. Also, the system can readily be reconfigured to become fully operative again, though with slightly reduced capacity.
| 7
|
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation-in-part of U.S. patent application Ser. No. 12/889,100 filed Sep. 23, 2010, which claims the benefit of U.S. Provisional Patent Application Ser. No. 61/245,594 filed Sep. 24, 2009. This application also claims the benefit of U.S. Provisional Patent Application Ser. No. 61/586,732 filed Jan. 13, 2012. All of these applications are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to treatment of coal combustion products, and more particularly relates to systems and methods for comminuting coal combustion products for recirculation into coal-fired burners.
BACKGROUND INFORMATION
[0003] Concrete and other hydraulic mixtures used for construction rely primarily on the manufacture of Portland cement clinker as the main binder controlling the rate of development of mechanical properties. The manufacture of Portland cement clinker is energy intensive and releases large amounts of carbon dioxide into the atmosphere. To reduce the environmental impact of cement and concrete manufacture, supplementary materials with lower carbon dioxide footprint are used to partially replace Portland cement clinker as the binder in hydraulic mixtures.
[0004] Large amounts of coal ash and other coal combustion products are generated worldwide from the burning of coal as fuel for electricity generation and other energy intensive applications. A large amount of coal combustion byproducts are disposed of in landfills, at a high economical and environmental cost. Existing methods to beneficiate coal ash so as to make them suitable for other uses, such as in construction, generally do not enable 100 percent usage of coal ashes in beneficial applications. Furthermore, existing treatment methods commonly either use cost ineffective application of chemicals, or require treatment at a separate facility from where the coal combustion takes place, therefore incurring additional transportation costs and capital investments. Currently, most changes made to beneficiate coal combustion products are strictly related to the cleaning or sequestration of harmful chemicals within the coal combustion product.
[0005] Unfortunately, the use of coal ash and other coal combustion products in concrete has many drawbacks. For example, addition of fly ash to concrete results in a product with low air entrainment and low early strength development.
[0006] Most fly ash produced by coal combustion generally contains a significant percentage of fine, unburned carbon particles, sometimes called char, that reduces the ash's usefulness as a byproduct. Before the fly ash produced by the combustion of coal and/or other solid fuels can be used in most building products applications, it must be processed or treated to reduce residual carbon levels therein. Typically, it is necessary for the ash to be cleaned to as low as 1-2 percent by weight carbon content before it can be used as a cement additive and in other building products applications. If the carbon levels of the fly ash are too high, the ash cannot be used in many of the aforementioned applications. For example, although fly ash production in the United States for 1998 was in excess of 55 million tons, less than 20 million tons of fly ash were used in building product materials and other applications. Consequently, carbon content of the ash is a key factor retarding its wider use in current markets and the expansion of its use to other markets.
[0007] In order to lower the residual carbon content of fly ash to appropriate levels, it generally is necessary remove or immobilize excess carbon, for example by the use of a separate combustion system to ignite and combust the carbon. The fly ash particles must be supplied with sufficient temperature, oxygen and residence time in a heated chamber to ignite and burn the carbon within the fly ash particles. Currently, a number of technologies have been explored to try to effect carbon combustion in fly ash to reduce the carbon levels as low as possible. The primary problems that have faced most commercial methods in recent years generally have been the operational complexity of such systems and maintenance issues that have increased the processing costs per ton of processed fly ash, in some cases, to a point where it is not economically feasible to use such methods.
[0008] Such current systems and methods for carbon reduction in fly ash include, for example, a system in which the ash is conveyed in basket conveyors and/or on mesh belts through a carbon burn out system that includes a series of combustion chambers. As the ash is conveyed through the combustion chambers it is heated to burn off the carbon therein. Other known ash feed or conveying systems for transport of the ash through combustion chambers have included screw mechanisms, rotary drums and other mechanical transport devices. At the high temperatures typically required for ash processing, however, such mechanisms often have proved difficult to maintain and operate reliably. In addition, such mechanisms typically limit the exposure of the carbon particles to free oxygen by constraining or retaining the ash within baskets or on mesh belts such that combustion is occasioned by, in effect, diffusion through the ash, thereby retarding the effective throughput through the system. Accordingly, carbon residence times within the furnace also must be on the order of upwards of 30 minutes to effect a good burn out of carbon. These factors generally result in a less effective and costlier process.
[0009] Another approach to generating carbon combustion in fly ash has utilized bubbling fluid bed technology to affect carbon burn out. In this system, the ash is placed in a bubbling fluid bed supplied with high temperature and oxygen so that the carbon is burned or combusted as it bubbles through the bed. This bubbling fluid bed technology generally requires residence times of the carbon particles within a furnace chamber for up to about 20 minutes or more. The rate of contact of the carbon particles with oxidizing gasses in the bubbling fluid bed also is generally limited to regions in which the bubbles of gas contact solids, such that the rate of contact is related to the effective gas voidage in the bubbling bed, which is typically around 55-60 percent (i.e. around 40-45 percent of solids by volume). These systems have, however, been found to have limited through-put of ash due to effective carbon combustion rates with required carbon particle residence times generally being close to those of other conventional systems.
[0010] The present invention has been developed in view of the foregoing and to remedy other deficiencies of the prior art.
SUMMARY OF THE INVENTION
[0011] The present invention provides a method and system for reducing the content of un-burned carbon in coal combustion products. The coal combustion products may be added to cementitious materials to improve the rate of development of mechanical properties in hydraulic mixtures. In accordance with embodiments of the present invention, a coarse, carbon-rich fraction of fly ash is milled or ground with the addition of materials rich in silica, alumina and calcium to form a homogeneous mixture, followed by injection of the mixture into a coal combustion chamber for thermal treatment and incorporation of the mixture with the final coal combustion product. The invention further relates to hydraulic mixtures, e.g., concrete and mortar, that contain coal combustion products that have been modified by the selective separation and cogrinding of coarse fly ash with additions of materials rich in silica, alumina and calcium, optionally with selected colors to form a homogeneous mixture.
[0012] An embodiment of the present invention provides a process where coarse fly ash particles with entrapped un-burned carbon are collected and separated from finer fly ash particles by means of a separator, followed by the addition of performance enhancing additives and comminution of the coarse fly ash with the additives to produce a mixture of the additives and the ground fly ash particles comprising released carbon particles. The mixture may then be injected back into a coal combustion chamber to facilitate improved combustion of residual carbon along with further enhancement of the final coal combustion product through the performance additives. The additives may enhance the performance of the resulting coal combustion product through mechanisms such as thermal activation of the additives, dilution of residual carbon, improved combustion of residual carbon, and surface modification of the amorphous phase in fly ash.
[0013] An aspect of the present invention is to provide a method of processing a coal combustion product comprising separating the coal combustion product into a coarse particle fraction and a fine particle fraction, comminuting the coarse particle fraction to provide comminuted particles, and combusting the comminuted particles with coal to thereby combust un-burned carbon contained in the comminuted particles.
[0014] Another aspect of the present invention is to provide a method of introducing a modified coal combustion product into a coal combustion chamber comprising introducing coal into the combustion chamber, introducing the modified coal combustion product into the combustion chamber, and combusting the coal and the modified coal combustion product, wherein un-burned carbon contained in the modified coal combustion product is combusted.
[0015] A further aspect of the present invention is to provide a system for processing a coal combustion product comprising a separator for separating the coal combustion product into a coarse particle fraction and a fine particle fraction, a comminutor for decreasing the average particle size of the coarse particle fraction to provide comminuted particles, and a combustion chamber for combusting the comminuted particles with coal.
[0016] Another aspect of the present invention is to provide a feed material for a coal combustion system comprising a comminuted mixture of a coal combustion product, and an additive comprising limestone, concrete, kaolin, recycled ground granulated blast furnace slag, recycled crushed glass, recycled crushed aggregate fines, silica fume, cement kiln dust, lime kiln dust, weathered clinker, clinker, aluminum slag, copper slag, granite kiln dust, rice hulls, rice hull ash, zeolites, limestone quarry dust, red mud, ground mine tailings, oil shale fines, bottom ash, dry stored fly ash, landfilled fly ash, ponded flyash, spodumene lithium aluminum silicate materials, lithium-containing ores and other waste or low-cost materials containing calcium oxide, silicon dioxide and aluminum oxide.
[0017] These and other aspects of the present invention will be more apparent from the following description.
BRIEF DESCRIPTION OF THE DRAWING
[0018] The figure is a partially schematic diagram of certain elements of a coal-fired power plant showing a process for comminution of coal combustion products and recirculation of a portion of the comminuted products into the burner of the power plant in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION
[0019] The figure illustrates a coal combustion product processing system 10 in accordance with an embodiment of the present invention. The system may be part of a coal-fired power plant, as more fully described below. Coal combustion products generated from the boiler of the coal-fired power plant are fed to a separator 30 , where the coal combustion product is separated into a coarse particle fraction and a fine particle fraction. The fine particle fraction may be stored in a silo 34 or other storage container, or transported for various types of uses. The coarse particle fraction is transferred in the direction of arrow 36 to a comminutor 42 comprising any known type of mill, grinder or the like that is used to reduce the particle size of the coarse particle fraction. The comminuted particles 43 are transferred to another separator 44 , where coarse particles 45 are removed and recirculated through the comminutor 42 . In the embodiment shown, dust produced in the comminutor 42 may be fed to a dust filter 46 driven by a fan 47 where the fine dust particles are captured and the air in which the dust particles were entrained is exhausted. Comminuted particles of sufficiently small size 60 that pass through the separator 44 , are fed to the boiler of the coal-fired power plant. The comminuted particles 60 may be fed into the boiler 15 at any suitable location, such as shown in the figure.
[0020] The average particle size of the coarse particle fraction 36 is typically at least 10 percent larger than the average particle size of the comminuted particles 43 , for example, 20 or 50 or 100 percent greater. The “average particle size” may be determined by the standard procedure of ASTM B822-10 Standard Test Method for Particle Size Distribution of Metal Powders and Related Compounds by Light Scattering. The coarse particle size fraction 36 may have an average particle size of greater than 50 microns, for example, greater than 100 microns. The comminuted particles 43 may have an average particle size of less than 50 microns, for example, less than 30 or 20 microns.
[0021] Additives 40 may be combined with the coarse particle fraction 36 of the coal combustion product to form a mixture 41 that is fed to the comminutor 42 . The additives may include limestone, concrete including waste concrete such as recycled Portland cement concrete, kaolin, recycled ground granulated blast furnace slag, recycled crushed glass, recycled crushed aggregate fines, silica fume, cement kiln dust, lime kiln dust, weathered clinker, clinker, aluminum slag, copper slag, granite kiln dust, rice hulls, rice hull ash, zeolites, limestone quarry dust, red mud, fine ground mine tailings, oil shale fines, bottom ash, dry stored fly ash, landfilled fly ash, ponded flyash, spodumene lithium aluminum silicate materials, and lithium-containing ores may also be fed to the comminutor. In the embodiment shown, the additives 40 are combined with the coarse particle fraction 36 before being fed to the comminutor 42 . However, the additives 40 and coarse particle fraction 36 may be fed to the comminutor 42 separately, or may be fed to separate comminutors.
[0022] As shown in the figure, boiler slag, bed ash and/or bottom ash 50 from the coal-fired power plant may also be fed to the comminutor 42 . In the embodiment shown, the ash 50 is combined with the mixture 41 to form a mixture 51 comprising the coarse fraction 36 , the additives 40 , and the slag or bottom/bed ash 50 . This mixture 51 is combined with the coarse particles 45 from the separator to form a feed mixture 52 that enters the comminutor 42 .
[0023] The figure also schematically illustrates certain elements of a coal-fired power plant. The power plant includes a combustion chamber 15 such as a conventional tangential firing burner configuration. Pulverized coal is introduced into the combustion chamber 15 via at least one coal inlet line 14 . A coal hopper feeds into a coal pulverizer 16 which comminutes the coal to the desired particle size for introduction into the combustion chamber 15 . The pulverized coal may be mixed with hot air and blown through the inlet(s) 14 into the combustion chamber 15 where the coal is burned. The comminuted particles 60 may be introduced into the combustion chamber 15 via the coal inlet line 14 , or separately through one or more additional inlet lines.
[0024] Water flows through tube-lined walls of the boiler 20 , where it is heated by the combusted coal to form steam that passes to a steam turbine. Combustion products pass from the boiler region to a particulate collection region 22 where the solid combustion products are collected and transferred to the separator 30 . Exhaust gas passes through a scrubber 28 and is vented through a stack 29 .
[0025] Coal fly ash is essentially formed from the combustion gases as they rise from the combustion zone and coalesce above that zone. Typically, when temperatures are in the range of 1,800-2,200° F., these gases form predominantly amorphous hollow spheres. Depending upon the chemistry of the coal being used (using coal as an example), the ash is either an alumina-silicate, from the combustion of bituminous coal, or calcium-alumina-silicate from the combustion of a sub-bituminous coal. While fly ash from sub-bituminous coal may be self-cementing, fly ash from bituminous coal may not be self-cementing.
[0026] An embodiment of the invention provides for the selection and addition of raw materials 40 to be added to the coarse fly ash particles 36 with entrapped carbon to increase the carbon removal rate as well as adjusting the color and reactivity of the resulting coal combustion products without any retarding effects on the alite hydration in Portland cement clinker used together with said coal combustion products in a hydraulic mixture.
[0027] In certain embodiments, the content of un-burned carbon in the coal combustion product may be measured along with other components affecting the color and reactivity of the resulting product, such as silica, alumina, CaO and other reactive and non-reactive elements are the use of X-ray diffraction methods, including Rietvield analysis, X-ray fluorescence or any other methods to identify said components. Both methods can be used in-line or end-of-line. calorimetric methods are particularly suitable to monitor the reactivity at different stages of the early age development of mechanical properties of hydraulic mixtures comprising Portland cement clinker and coal combustion products. Methods to measure strength (early and late), set time and slump can be derived from any methods described in ASTM standards relative to the measurement of said properties, or measures of conductivity, or ultrasonic methods, or any other method that can measure or infer any of the aforementioned properties. Said methods provide insight into the optimum selection of types, amounts and desired thermal cycle for the different additions to the coal combustion chamber for the purpose of optimizing the value and performance of the resulting product.
[0028] The additives 40 may be selected from limestone, waste concrete such as recycled Portland cement concrete, recycled ground granulated blast furnace slag, recycled crushed glass, recycled crushed aggregate fines, silica fume, cement kiln dust, lime kiln dust, weathered clinker, clinker, aluminum slag, copper slag, granite kiln dust, rice hulls, rice hull ash, zeolites, limestone quarry dust, red mud, fine ground mine tailings, oil shale fines, bottom ash, dry stored fly ash, landfilled fly ash, ponded flyash, spodumene lithium aluminum silicate materials, lithium-containing ores and other waste or low-cost materials containing calcium oxide, silicon dioxide and/or aluminum oxide. In accordance with certain embodiments of the present invention, the additives may comprise one or more of the following materials: 7-20 weight percent limestone; 1-5 weight percent ground granulated blast furnace slag; 1-5 weight percent crushed concrete; 0.1-2 weight percent crushed glass; 0.1-5 weight percent kaolin; and 0.01-1 weight percent silica fume. The total amount of the additives may be at least 8 weight percent of the total weight of the comminuted particles, for example, at least 10 weight percent. The additives may be provided in desired particle size ranges and introduced into the combustion chamber in the same region as the coal, or in other regions.
[0029] One embodiment of the present invention uses the coal fired boiler of an electric power plant as a chemical processing vessel to produce the combustion products, in addition to its normal function of generating steam for electrical energy. This approach may be taken without reducing the efficiency of the boiler's output while, at the same time, producing a commodity with a controlled specification and a higher commercial value to the construction market. The resulting ash product is designed to have beneficial pozzolanic properties for use in conjunction with Portland cement, or with different chemical modifications also producing a pozzolan that could also be a direct substitution for Portland cement. In both cases, advantages may be both economic and environmental. Landfill needs are reduced, and cost savings result by avoiding transportation and land filling of the ash. In addition, to the extent that the ash replaces Portland cement, it reduces the amount of carbon dioxide and other toxic emissions generated by the manufacture of Portland cement.
[0030] In accordance with the present invention, chemical additives like those listed can be added directly to the boiler in such a way that an ash from coal can be enhanced for optimum performance. In certain embodiments, additives such as clays, including kaolin, can be added to the boiler. Such materials may not decompose and recombine with the ash, but rather may be thermally activated and intimately mixed through the highly convective flow patterns inherent in the boiler. The result is a uniform ash/additive blend achieved completely through the boiler combustion process, and requiring no secondary processing. Essentially, as the vapor from the combusted products coalesce when they rise from the high temperature zone, glassy calcia-alumina-silicates will form. Vaporized additives dispersed in the plume will become part of the glassy phase, while those that have not vaporized will act as nuclei for the coalescing vapors. Other additives that do not take part with the glassy phase formation may be intimately mixed with the ash, producing a highly reactive pozzolanic mixture. For example, kaolin introduced in the boiler may not take part in the ash formation, but may transform to metakaolin, an otherwise costly additive.
[0031] The intimate blending of the additives directly into a boiler permits the combustion synthesis of the additives together with the coal and relies upon the intimate mixing generated by the convective flow in or near the boiler to produce chemically modified fly ash. This blending may take place in the main combustion zone of the boiler, directly above the main combustion zone in the boiler, or downstream from the boiler. For example, additives such as kaolin, metakaolin, titanium dioxide, silica fume, zeolites, diatomaceous earth, etc. may be added at such downstream locations at other points where the coal combustion products coalesce into amorphous fly-ash particles. In one embodiment, relatively low cost kaolin may be added and converted into metakaolin during the process, thereby resulting in the economical production of metakaolin having desirable strength enhancing properties when added to cement. By virtue of the materials selected as additives to the coal, the resulting ash byproduct can be designed to have a chemical structure that will enable it to act as a cementitious binder together with Portland cement for strength enhancing properties of a cement or a concrete. The particles being injected are, in some cases, much larger than the resulting ash particles, indicating that the intense high-temperature mixing causes particle reduction/attrition both through intense collisions as well as through chemical combustion. For example, the particle size of the combustion product may be such that 90 percent of the particles may be less than 50 microns, typically less than 20 microns, while the particle size of 30 percent or more of the starting additive materials may be greater than 50 or 100 microns.
[0032] In addition to using the intense blending nature of the boiler plume for the combustion synthesis of unique ash products, other beneficial additives can be mixed in the high temperature gas flow simply to achieve intimate mixing in a single processing step. Such additions of non-reactive materials can be accomplished without reducing the efficiency of the coal combustion process.
[0033] In another embodiment geopolymer cements may be added in the combustion process to reduce pollutants in flue gas. Such geopolymer cements may serve as binding agents for mercury, heavy metals, nitrogen oxides and sulfur oxides, and additional silica.
[0034] It is through the injection of these additions that the resultant fly ash formed in the coal combustion process may be modified by the inclusion of the chemical compounds within these additives directly into the coalescing fly ash. In addition, some chemical species added in this manner that do not become chemically bound to the coalescing fly ash are intimately blended with the fly ash through the natural convection in the boiler resulting in a very uniform blending process achieved without the need for secondary, cost intensive, powder blending of the resultant ash product.
[0035] In another embodiment, a method is provided for testing the resulting coal combustion ash after addition of other materials and adjusting the combustion parameters and materials to reach target levels of calcium oxide, silicon dioxide and aluminum oxide in the resulting coal combustion ash. Such testing and adjusting may include measuring contents of calcium oxide, silicon dioxide and aluminum oxide and other reactive and non-reactive elements directly. The method also may include measuring properties of concrete made from the resulting coal combustion ash so as to determine early strength, late strength, slump and setting time of the concrete made of the resulting coal combustion ash. The measurements may be coupled to algorithms to rapidly assess the data and make changes to the feed rates in real time.
[0036] The testing methods may measure components such as calcium oxide, silicon dioxide and aluminum oxide and other reactive and non-reactive elements using x-ray diffraction (XRD) methods, including Rietvield analysis, x-ray fluorescence (XRF) or any other methods to identify said components. Such methods can be used in-line or end-of-line. Methods to measure strength (early and late), set time and slump can be derived from methods provided in ASTM standards relative to the measurement of such properties, or measures of heat of hydration through calorimeters, or measures of conductivity, or ultrasonic methods, or any other method that can measure or infer any of the aforementioned properties.
[0037] In one embodiment, the incorporation of sensors in a boiler that can monitor the in-situ quality/chemistry of an ash product as it is being generated. The sensors can include conventional residual gas analyzers, x-ray fluorescence spectrometers, mass spectrometers, atomic absorption spectrometers, inductively-coupled plasma optical emission spectrometers, Fourier transform infrared spectrometers, and lasers for performing laser induced breakdown spectroscopy, as well as mercury analyzers, NO x detectors and SO x detectors. The levels of gases, etc. measured by such techniques can be linked to the optimum chemistry of an ash product.
[0038] The sensors can provide real-time monitoring feedback to a human controller or an automated analysis system. For example, the sensor(s) may transmit the value of a measured property to a controller which compares the measured value to a reference value and adjusts the flow rate of the strength enhancing material based thereon. The controller may transmit a signal to one or more additive injectors in order to increase or decrease the flow rate of the additive into the combustion zone. The purpose of this feedback system is to link directly to the individual sources of chemical additives and adjust their feed rates to maintain the ash chemistry quality required for optimum concrete performance.
[0039] Using gas analysis equipment during the modified coal combustion process, it is also possible to measure the effluent gases generated by the coal combustion process. Typically, these gases include NO x , SO x , CO 2 , and mercury. Through prior analysis of these gas ranges, taken together with the resulting ash reactivity, it is possible to use gas monitoring processes to optimize the addition of the chemical additives. In this way, an optimum reactive ash chemistry can be adjusted in-situ, that is in real time during the coal combustion process, to optimize the chemistry of the resulting coal ash.
[0040] The combustion products of the present invention may be added to various types of cement, including Portland cement. For example, the combustion products may comprise greater than 10 weight percent of the cementitious material, typically greater than 25 weight percent. In certain embodiments, the additive comprises 30 to 95 weight percent of the cementitious material.
[0041] The present invention provides a method to reduce disposal of coal combustion ashes in landfills by converting them into higher value hydraulic binders, usable as a substitute of cement in quantities in excess of 40% of substitution. Another advantage of the invention is that it provides a cost-effective alternative to other methods to beneficiate coals combustion ashes, by applying the injection of treatment and materials in the combustion boiler, rather than at a separate facility. The method and system enables treatment of the coal combustion ash as a part of the normal process of power generation, thereby reducing the need for transportation to a separate facility, capital outlay for said facility, and also avoiding the application of additional chemicals such as activating agents.
[0042] Whereas particular embodiments of this invention have been described above for purposes of illustration, it will be evident to those skilled in the art that numerous variations of the details of the present invention may be made without departing from the invention as defined in the appended claims.
|
A method and system for reducing the un-burned carbon content in coal combustion products are disclosed. A coal combustion product is separated into a coarse particle fraction and a fine particle fraction, and the coarse particles are comminuted by milling, grinding or the like. Additives may be added of the coarse particles prior to comminution. The comminuted particles are then co-combusted with coal to burn at least a portion of the un-burned carbon contained in the original coal combustion product.
| 8
|
This application is a continuation of now abandoned application, Ser. No. 07/965,689, filed Oct. 22, 1992, which is a continuation of now abandoned application Ser. No. 07/690,255, filed on Apr. 23, 1991.
BACKGROUND OF THE INVENTION
This invention relates to a mixing device which has been devised particularly though not necessarily solely for mixing materials such as cement, mortar, plaster and grout, but it will be apparent that the mixing device could also be used for mixing other materials such as fertilizer stock feeds, seed, soil mixes, paint or other wet or dry ingredients that require combining.
Referring in particular to concrete mixing devices, various approaches to mixing small batches of cement to form concrete have been tried. For example mixing can be achieved by using spades or shovels on a ground surface. Such an approach is disadvantageous in that it is difficult to mix the ingredients in that considerable effort is required and this approach is therefore physically exhausting. If several batches are to be mixed, the person making the mix requires ideally to be a strong and physically fit person. A flat surface is required and often the mixed product has to be transported from the area of mixing to the area of use often in an unsatisfactory manner requiring the use for example of buckets or the like. Consistency between sequential mixes can be difficult to obtain and the mixing can create considerable mess particularly when effected by persons having little experience in making such a mix. In such circumstances the cleaning up after the mixing operations can be difficult.
In an alternative method the mixing can be carried out for example in a wheel barrow. Again there are disadvantages in that the ingredients are difficult to mix and again a strong physically fit person is ideally required because of the physically exhausting nature of the mixing. Again it is difficult to get consistency between sequential mixes and the mixing can be messy and cleaning the utensils again can be difficult.
A standard concrete mixer may be employed but generally this is disadvantageous in that a power source is required and also the concrete mixer is relatively expensive to rent or to buy. Concrete mixers are also difficult to transport and again they are such as to ideally require a strong physically fit person to use because again considerable effort is required to fill and empty the mixer. Again transportation to the place of use from the mixing point may prove difficult and difficulties are met in the cleaning of utensils. When not in use the standard concrete mixer is difficult to store.
In an effort to overcome these disadvantages Australian patent specification 584592 describes a construction which can be rolled along the ground. The construction takes the form of a truncated cone and a flange is provided at each end to provide the basis for the rolling action. An aperture is provided at the narrow end of the cone through which the mixer can be filled or emptied.
The construction is again disadvantageous however in that the quantity of mix that can be contained is small otherwise leakage will occur through the opening and also the mixing protrusions or blades will provide an inadequate mixing rate.
Because of this a substantial mixing period is required and again substantial effort must be expended to satisfactorily mix the contents and also a large number of mixes will need to be made to achieve any satisfactory quantity of cement.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide a mixer which will obviate or minimize the foregoing disadvantages in a simple yet effective manner or which will at least provide the public with a useful choice.
Accordingly, the invention consists in a mixing device comprising a hollow cylinder having an opening at one end, a lid engagable with the cylinder to close the opening, and at least one baffle extending inwardly from the cylindrical wall of the drum. The baffle is constructed so that upon rotation of the drum about its longitudinal axis and with the longitudinal axis substantially horizontal in use, the baffle or baffles will cause material within the drum to be tumbled and moved in a direction generally towards an end of the cylinder. The cylinder is sized so as to be manually rotatable about the longitudinal axis.
To those skilled in the art to which the invention relates, many changes in construction and widely differing embodiments and applications of the invention will suggest themselves without departing from the scope of the invention as defined in the appended claims. The disclosures and the descriptions herein are purely illustrative and are not intended to be in any sense limiting.
BRIEF DESCRIPTION OF THE DRAWINGS
One preferred form of the invention will now be described with reference to the accompanying drawings in which:
FIG. 1 is a side elevation of a mixing device according to one preferred form of the invention;
FIG. 2 is a detail view partly in cross section showing the engagement between a lid and cylindrical container part of a mixing device according to the invention;
FIG. 3 is a cross section view taken along line 3--3 in FIG. 1;
FIG. 4 is a cross section view taken along line 4--4 in FIG. 1;
FIG. 5 is a side elevation of a lid for use in the mixing device of the invention;
FIG. 6 is a plan view of the lid in FIG. 5;
FIG. 7 is a cross section view taken along line 7--7 in FIG. 6;
FIG. 8 is a cross section view taken along line 8--8 in FIG. 6;
FIG. 9 is a diagrammatic perspective view of a mixing device according to the invention with the lid and container part separated;
FIG. 10 shows material being inserted into the container part of the mixing device according to the invention;
FIG. 11 shows liquid being placed into the container part of the mixing device according to the invention;
FIG. 12 shows the mixing device of the invention with the lid placed on the container;
FIG. 13 shows a method of manually causing the contents of the mixing device to be mixed; and
FIG. 14 shows the directions of movement of the contents of the mixing device during use.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings, a mixing device such as a concrete mixer is provided in the form of a hollow cylinder or drum 1 closed at end 2 which forms the bottom of the construction during filling and open at the end 3 through which the mixing device can be filled in use.
Engagable over the opening at end 3 is a lid 4 and engagement between the lid 4 and the cylindrical drum 1 may be by means of co-operating threads 5 on the cylindrical drum 1 and 6 on the lid 4.
The lid 4 can be formed from any desirable material and any desirable method but is for example injection moulded from high density polyethylene.
Similarly the drum 1 may be formed in any desired manner from any desirable material but desirably is blow moulded from high density polyethylene.
Whilst the precise dimensions of the drum are not crucial to the invention the construction is of a size such that it is readily moveable by manual operation, that is to say by the hands or feet of the user and to this end it has been designed to mix for example 25 kg of cement.
A suitable size for the drum would give a height of about 440 mm with a diameter of about 320 mm and the base end 2 may be slightly concave.
At least one and preferably a pair of baffles 10 are provided. In the preferred embodiment described herein the baffles are oppositly positioned and extend from the base 2 to a point within about 50 mm from the shoulder 11 where an inward step is provided to the threaded part 12 which receives the lid 4.
The baffles are shaped so that the contents during mixing will not only be tumbled but also moved in a direction towards the ends 2 and 3 of the drum 1. This can be achieved by providing the baffles in the form a helix and in a preferred embodiment of the invention the included angle between the side walls 13 and 14 of each baffle 10 may be about 45°.
The angle between the centre line of the baffle and the extremity of the baffle 10 being angle A in FIG. 4 may be about 151/2° at the line 4--4 in FIG. 1 and towards its inner most end the angle B may have increased to about 221/2°.
Because of the helical shape it will be found that the general axis of the baffle 10 at the cylindrical wall (i.e. an axis disposed between and parallel to radially outermost portions of sidewalls of the baffle 10) will form an angle with the general (or apex) at the inward extremity of the baffle 10 and this angle can be visualized by reference to the line 16 in FIG. 1 which indicates the direction of the innermost extremity (or apex) of the baffle 10. Thus, as shown in FIG. 1, the line 16 (representing the apex of the baffle 10) is substantially non-parallel to lines extending along the radially outermost portions of the sidewalls of the baffle 10.
Thus it can be seen that although the baffles 10 are provided on a helix the amount of turn of the helix over the length of the drum 1 is relatively small.
The external surfaces of the baffle 10 can be gripped so as to assist in rotation of the drum and also provides a convenient hand grip for ease of pouring.
The lid 4 provides a cylindrical wall 25 which in use becomes positioned about the inset portion (or reduced diameter portion) 26 of the drum 1 formed by the shoulder at 11.
The cylindrical wall leads to an upper surface (or raised portion) 27 which in the preferred embodiment includes a concavity 28 in its central portions. This concavity 28 can be used to provide a water measure to assist with recipe proportions and to this end can be marked with markings indicating water levels.
Spanning opposite sides of the raised portion 27 is a handle 29 which may be strengthened by a connection between the handle 29 and the bottom of the concavity 28 if needed or desired.
An annular cavity 30 is provided on the underside of the lid into which may be positioned a seal such as an O-ring 31 which may be retained in place by a rib 32 which extends inwardly relative to the groove or channel 30 from downwardly depending rib 33.
The use of the invention is as follows.
In use the lid 4 is removed from the drum 1 for example by pressure on the handle 29 which may also be used to carry the construction when the lid 4 is in position on the contained drum 1.
Ingredients 40 to be mixed are then inserted into the interior of the drum 1 and, if required, water or other liquid 41 is also inserted thereon for example by pouring from the lid 4 as above outlined.
The lid 4 is then engaged with the drum 1 as shown in FIG. 12 and the construction tipped onto its side as shown in FIG. 13.
The drum 1 may then be rolled in a to and fro manner or in one direction as desired for example by use of the hands as shown in FIG. 13 or alternatively the feet can be used.
The baffles 10 create a tumbling action whereby the ingredients are lifted, relocated within the length of the mixer, dropped and redistributed. In particular the ingredients are tumbled and also moved towards the ends of the container as shown by the arrows in FIG. 14.
It is found that a high quality mix of ingredients can be obtained in a time span of as little as 30 to 60 seconds in normal use.
The mixing can take place on substantially any surface whether it is rough, smooth or even sloping and can be performed both indoors, outdoors and in restricted space areas. Once the rolling or mixing has been completed the drum 1 is stood upright and the lid 4 unscrewed. The mixed product can either be trowelled out or simply poured from the drum 1. Cleaning can be effected by a simple hosing operation of the drum 1 and lid 4.
Thus it can be seen that a mixing device has been provided which at least in the preferred form of the invention has the advantage that where standard recipes are followed a good level of batch consistency is achieved. The construction also requires minimal physical effort in use and therefore the mixer can be used by most people. For a construction of about the size described it is found that the total weight is approximately 3.4 kg and the construction is therefore easy to carry and also because of its relatively small size can readily stored.
|
A mixing device such as a concrete mixer is provided in the form of a hollow cylindrical drum with an opening at one end. A lid is engageable with the drum to close the opening. At least one and preferably two baffles are provided within the drum and these are shaped so as to cause an end to end as well as tumbling movement of the contents of the drum when the drum is rolled along a ground surface.
| 1
|
BACKGROUND OF THE INVENTION
The substitution of pulverized coal for coke in an iron-making blast furnace is well known in the art. Efficient operation of the blast furnace requires that the coal be uniformly distributed in the furnace to prevent channeling of the blast air, as well as other problems. The coal is, normally, injected into the tuyeres which communicate with the furnace. The tuyeres are also used for supplying the high temperature blast air which supports the iron-making reduction of the ore. The tuyeres are generally arranged equiangularly circumferentially around the furnace above the hearth and, consequently, the injected coal is similarly injected at equiangularly located positions around the furnace.
The coal which is injected into the furnace through the tuyeres is, generally, finely ground or pulverized and has a very low, on the order of about 0.5%, moisture. Due to the fine grind of the coal, it is generally transported to the tuyeres by means of a pneumatic system conveying the coal through a system of pipes from the coal preparation facility to the blast furnace. In order to simplify the numbers and the complexity of the pipe system, it is preferred that the ground coal be transported to a coal distributor located adjacent the furnace. The coal distributor preferably provides a suitable number of outlets communicating with the tuyeres. Ideally, the coal distributor should be constructed so that each of the lines feeding a tuyere receives an air/coal suspension of a quantity substantially equal to the amount received by the other lines feeding the other tuyeres. In this way, uniform distribution of the pulverized coal in the furnace can be assured with the result that efficient operation of the blast furnace can be maintained.
Matthys, et al, U.S. Pat. No. 3,204,942, discloses a distributor for pneumatically transporting particulate material, preferably coal. Matthys discloses an upstanding cylinder having a centrally located inlet coal/air supply line and a plurality of equiangularly disposed outlets positioned on a common horizontal plane. The distributor of Matthys discloses an inverted cone disposed in the bottom of the cylinder and having a downwardly diminishing diameter in order to prevent coal accumulation. Experience has shown, however, that the Matthys distributor results in unequal distribution of the coal/air suspension to the lines communicating with the tuyeres. Consequently, the Matthys distributor is not capable of providing sufficient uniformity of coal distribution which would permit greater efficiency in the operation of the blast furnace. While Matthys discloses that flow restrictors may be placed in the lines to effect equality of pressure drop, the actual use of such restrictors has proven to be extremly complicated and that the insertion of one restrictor has an effect on other lines in the system.
Wennerstrom, U.S. Pat. No. 4,027,920, discloses a distributor similar to Matthys' and in which a hollow cylinder is suspended in the distributor aligned with the central opening in order to maintain central orientation of the oncoming stream. Wennerstrom, the assignee of which is also the assignee of the Matthys patent, in commenting on the Matthys patent states "Recent experience has shown the deviation of the incoming stream from its central orientation results in pulsation and non-uniform distribution of the effluent streams." Consequently, there is an appreciation in Wennerstrom by the owner of the Matthys' patent that the Matthys' distributor does not provide optimum distribution to each of the tuyeres. Unfortunately, experience has also shown that the Wennerstrom solution to the Matthys problem results in a similarly non-uniform distribution to each of the tuyere lines.
The present invention discloses a method for controlling the substantially uniform distribution of the coal/air suspension from a multi-outlet distributor which is in communication with the tuyeres of a blast furnace. The method of the invention permits the blast furnace operator to select that level of distributor deviation which can either be tolerated by the blast furnace or which is the best obtainable in view of practical physical limitations. The present method permits a blast furnace operator to contstruct a distributor bottle taking into account the velocity of the coal particles and the diameter of the bottle as well as the distance from the top plane of the cone to a plane coincident with the central axes of the outlet tuyere pipes. Consequently, the present method permits the construction of a distributor bottle in which the distributor deviation may be controlled from zero deviation to that amount of deviation which the furnace operator is willing to tolerate. The present method provides, therefore, a novel and unique means for controlling the distribution of coal to a blast furnace in order to premit optimum efficient operation of the furnace.
OBJECTS OF THE INVENTION
It is a primary object of the disclosed invention to provide a method for overcoming the above-noted disadvantages and problems of prior art distributors.
It is an additional object of the disclosed invention to provide a system which permits the furnace operator to control the deviation from the mean of the coal injected into a blast furnace.
It is a further object of the disclosed invention to provide a means for providing a distributor constructed so as to have the optimum dimensions for attaining the preselected distributor deviation.
Yet another object of the disclosed invention is to provide a means for providing a distributor which has the minimum volume necessary for attaining the pre-selected deviation level.
Still a further object of the disclosed invention is to provide a means for providing a distributor bottle the size of which may deviate from the optimum size yet which will still attain the pre-selected deviation level.
Yet still a further object of the disclosed invention is to provide a distributor bottle having dimensions sufficient to attain the pre-selected deviation level after the velocity of the particle-moving gas stream has been selected.
Yet still a further object of the disclosed invention is to provide a distributor bottle which is capable of attaining substantially uniform distribution of particulates from a multi-outlet distributor.
These and other objects and advantages and novel features of the present invention will be readily apparent in view of the following description and drawings of the above-described invention.
DESCRIPTION OF THE DRAWINGS
The above and other objects and advantages and novel features of the present invention will become apparent from the following detailed description of the preferred embodiment of the invention illustrated in the accompanying drawings, wherein:
FIG. 1 is a side elevational view, with portions broken away, showing the distributor bottle of the method;
FIG. 2 is a schematic view of the distributor bottle of the system in communication with a supply of particulates and a blast furnace, and
FIG. 3 is a graph of the diameter D of the distributor versus the height H above the cone to a plane coincident with the distributor outlets and disclosing the isodistribution lines resulting from use of the equation for deriving the dimensions of the distributor.
DESCRIPTION OF THE INVENTION
A particulate distributor or distributor bottle 10, as best shown in FIG. 1, includes a generally vertically disposed right cylinder 12. Cylinder 12 is closed at its top 14 and its bottom 16. Bottom 16 includes a central opening or aperture 18 which is connected to a particulate supply line 20. An inverted right circular conical insert 22 is disposed in cylinder 12 adjacent bottom 16 and includes an opening 24 aligned with opening 18 in bottom 16. The opening 24 of conical insert 22 opens gradually outwardly as the distance from bottom 16 increases and, therefore, yields the conical slope of insert 22. Insert 22 has a top 26 which represents a horizontally disposed plane which is parallel to bottom 16.
Cylinder 12 includes a plurality of openings or outlets 28, four of which are shown in FIG. 1, although a greater or fewer number may be employed as circumstances warrant, and which are disposed equiangularly around cylinder 12, although equiangularly positioning is not necessary for functioning of the invention. Each of the outlets 28 is horizontally disposed such that a longitudinal centrally disposed axis, such as axis 30, is coincident with a horizontal plane 32 passing through each of the axes 30. The plane 32 coincident with the axes 30 is generally horizontally disposed and is parallel to the plane 34 aligned with the top 26 of conical insert 22.
As best shown in FIG. 2, distributor bottle 10 is in communication with particulates 36, which preferably includes coal particles which are ground so that 80% or more of the particles are less than 200 mesh, and are contained in a coal preparation receiver 38. Inlet supply line 20 is in fluid communication with coal receiver 38 and acts to pneumatically convey the coal particles 36 to distributor 10. Preferably, the coal particles 36 have been dried so that the moisture of the particles 36 does not exceed 0.5%. The coal particles 36 are preferably maintained at a temperature of between 120° F. to 150° F. in order to prevent volatilization of the particles 36 in order to prevent, therefore, the eventual plugging of supply line 20. The coal particles 36 are pneumatically conveyed along supply line 20 by dried heated air, whose temperature does not exceed 150° F.
Distributor 10 includes a plurality of tuyere outlet supply lines 40 which are coaxially aligned with and have a diameter at least equal to the diameter of openings 28. Tuyere outlet supply lines 40 are in fluid communication with tuyeres 42 which feed blast furnace 44, in a manner well known in the art. Although only one of tuyere outlet supply lines 40 is shown in communication with a tuyere 42, one skilled in the art will appreciate that a plurality of tuyeres 42 are circumferentially arranged about furnace 44 and that each tuyere 42 is in communication with one of tuyere outlet supply lines 40. In this way, coal particulates 36 in receiver 38 may be pneumatically conveyed through supply line 20 to distributor 10 and hence along tuyere outlet supply lines 40 to tuyeres 42 and ultimately injected along with the blast air into the blast furnace 44.
Matthys, U.S. Pat. No. 3,204,942, describes how the coal particulates 36 move upwardly through opening 18 and mushroom along top 14 and ultimately distribute through outlets 28 and tuyere outlet supply lines 40 and, further elucidation on the operation of the distributor 10 is not necessary.
In order to efficiently operate a blast furnace, such as blast furnace 44, it is necessary that the wind rate, that is the amount of hot blast air injected into the furnace, be known. Additionally, the length of the run of each of the tuyere outlet supply lines 40, as well as the number of tuyeres and the top pressure of the furnace 44 must be known. Once these values have been determined, the available oxygen per tuyere is determined and it is the available oxygen per tuyere which determines the maximum coal flow rate to each tuyere. One skilled in the art will appreciate that coal is an amorphous mixture of a number of carbon containing molecules and that it is the combustion of these molecules which help to heat the furnace. There are many and various grades of coal, each with its own particular volatility and free carbon available for combustion, and the present invention is not limited to any particular type or grade of coal. After the amount of coal to be fed to each tuyere has been determined, the line size, or the internal diameter, of the tuyere outlet supply lines 40 can be determined. Preferably, the tuyere outlet supply lines 40 have an internal diameter ranging from approximately 3/4 inches to approximately 2 inches.
Calculation of the size of the tuyere outlet supply lines 40 may be accomplished in a manner which is well known to one skilled in the art. It is necessary, however, that the velocity of the moving air/coal suspension be maintained at least equal to, and preferably slightly greater than, the saltation velocity of the mixture. The saltation velocity is that velocity at which none of the entrained particulates 36 will settle out or separate from the air/particulate suspension. The saltation velocity is a function of the line size, the density of the mixture and the velocity of the conveying fluid, as is well known in the art.
One skilled in the art will appreciate that because the coal particulates 36 are ground to a size such that 80% or more will pass through a 200 mesh sieve, the particulates 36 are extremely small. Due to the extremely small size of the particulate 36, they behave essentially, as part of the gas stream. Consequently, the total gas flow through the tuyeres is the sum of the gas flow, which is preferably dried, heated air, through the tuyeres plus the particulates entrained in the flowing gas/coal suspension. Consequently, the size of the distributor 10 is not directly proportional to the quantity of coal 36 being injected into the furnace 44.
After the total gas flow and the saltation velocity have been determined, sizing of the distributor 10 may proceed in a relatively straightforward manner, as will hereafter be explained. The furnace operator (not shown) may either decide to select that size bottle which will provide the optimum, that is equal, distirbution to each of the outlet supply lines 40 or, due to physical plant limitations, may select that distributor 10 which provides a distributor deviation which is acceptable and a bottle size which may be utilized. Distributor deviation or DMAX equals that amount expressed as a percentage by which the flow through a tuyere exceeds or is less than the mean flow available for each of the tuyeres. Consequently, DMAX is the maximum deviation and represents that tuyere through which the greatest or the least amount of coal/air suspension passes. The mean flow rate through each of the outlet supply lines 40 is merly the total flow rate divided by the number of outlet supply lines 40.
The following equation permits the furnace operator to determine the optimum sizing for the distributor 10 taking into account DMAX. The equation is a function of the distance from the outlet center lines 32 to the top of the conical section 34, as designated H in FIG. 1 and with H expressed in inches. The equation is also a function of the internal diameter D of the distributor 10, as best shown in FIG. 1, with the internal diameter D expressed in inches. Finally, the equation is a function of the gas velocity V of the moving air/coal suspension with the velocity expressed in feet per seconds.
The equation for calculating the size of the distribution 10 or permitting the optimization of the distributor deviation is: ##EQU1## The V used for calculating the Z to be applied in the equation for DMAX must be at least equal to the saltation velocity.
One skilled in the art will appreciate that X, Y and Z are all dimensionless numbers and therefore they permit universal application of the equation for DMAX with the effect that that equation can be applied to any right cylindrical distributor 10, as above described.
In order to obtain the optimally sized distributor 10 having the minimum value for DMAX, then calculation of Z permits one skilled in the art to determine X and Y by means of differential equations as is well known in the art. The volume of the bottle 10 may then be calculated according to the equation: ##EQU2## This equation for the volume of the distributor 10 is applicable when the angle beta, as best shown in FIG. 1, is equal to 60°. The equation may be adjusted depending on the angle Beta. It can be appreciated from the above, that the calculation of the optimum or minimum DMAX results in a minimum volume Vo for the distributor 10 for the DMAX value.
Due to physical plant limitations, the furnace operator may not be capable of utilizing a distributor 10 having the minimum DMAX attainable due to size considerations of the bottle. The furnace operator may, however, also not require the minimum deviation from the mean distribution with the result that a differently sized distributor 10 may be effectively utilized. One skilled in the art will appreciate that the equation for DMAX results in an infinite number of values for D and H for any given DMAX in excess of the minimum DMAX value, for a constant velocity V.
FIG. 3 discloses isodistribution lines 46, 48, 50, 52, 54, 56, 58 and 60 calculated for one distributor 10 with V=75 fps. It will be appreciated that the isodistribution lines each represent a curve which at any point on the curve will yield an equal value for DMAX. The legend associated with the isodistribution lines 46-60 is given below FIG. 3.
The minimum DMAX 62, as shown in FIG. 3, may result in a distributor 10 which is too large to be accommodated by the furnace operator. Should the furnace operator feel that a DMAX equal to 8%, as best shown by isodistribution line 46, is sufficient, then by appropriately selecting values for D and H along isodistribution line 46 the furnace operator may choose a bottle 10 which may be utilized in his situation. Similarly, the furnace operator may utilize any of other isodistribution lines 48-60 where situations warrant. It should also be appreciated that in FIG. 3 only a limited number of isodistribution lines 46-60 have been shown but that an infinite number could have been derived depending upon the levels of DMAX chosen.
One skilled in the art will appreciate that it is possible to minimize DMAX as a function of X, Y and Z with the result that the minimized value for DMAX may not be equal to zero but may exceed a threshold level. In one study, DMAX was minimized and equaled 3.51% with a gas velocity V equal to 50.12 feet per second with a diameter D equal to 38.39 inches and a height H equal to 62.78 inches. The results obtained were, however, not physically possible as the saltation velocity for the coal/air suspension was approximately 60.0 feet per second with a consequence that the gas velocity V was not sufficient for maintaining the ground coal entrained in the mixture. Consequently, the results obtained whenever the equation for DMAX is utilized must be physically correlated in order to prevent non-physical sizing of the distributor 10.
In a working embodiment of the system, the saltation velocity or V was determined to be 75 feet per second. DMAX was then minimized and resulted in a height H equal to 46.4 inches and a diameter D equal to 32.6 inches and the value of DMAX was equal to 5.18%. Consequently, for the velocity chosen the minimum deviation from the mean could only be controlled to 5.18%. Consequently, a gas flow velocity of 75 feet per second with a minimum DMAX value of 5.18% represents the optimum control available for that given velocity. Other control levels, as shown by the isodistribution lines 46-60 in FIG. 3, were also attainable for the gas flow velocity V equal 75 feet per second and, consequently, infinite control over DMAX and the diameter D and the height H of the distributor 10 is attainable by means of use of the equation for DMAX.
While this invention has been described as having a preferred design, it is understood that it is capable of further modifications, uses and/or adaptations of the invention following in general the principle of the invention and including such departures from the present disclosure as come within know or customary practice in the art to which the invention pertains, and as may be applied to the essential features hereinbefore set forth, and fall within the scope of the invention of the limits of the appended claims.
|
A method for controlling substantially equal distribution of particulates from a multi-outlet distributor in a conveying system conveying a supply of particulates to at least a first receiver is disclosed wherein a relationship between the velocity of the moving particles and the internal diameter and the heighth above a cone in the distributor is utilized to control distributor deviation.
| 2
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to failure prevention of a hard disk recording apparatus for storing and reproducing content data.
2. Description of the Related Art
Generally, an information processing apparatus, such as a personal computer, is provided with a hard disk drive (hereinafter, referred to as a HDD), which is a magnetic storage device serving as a data storage device. The HDD is precision equipment for recording information on a compact disk in a high-density state while rotating the compact disk at a high speed, and also often fails by vibration or impulsion. If the HDD fails, all recorded information cannot be read. Also, when data recorded in the HDD is not backed up, all information is lost, thereby causing a problem.
Therefore, generally, a HDD has been proposed, in which it executes the self-diagnosis on the basis of SMART (Self-Monitoring Analysis and Reporting Technology) information which is condition managing information of the HDD such as the number of damaged sectors, sector numbers of the damaged sector, sector numbers of alternative sectors, a read error ratio, an ON/OFF frequency of a power supply or the like, and has the SMART function for detecting expectable interferences.
When there are abnormalities in SMART information, the HDD having the SMART function outputs SMART errors. Since the SMART errors are outputted when there is a possibility that interferences occur in the HDD, the HDD normally operates at this time. For this reason, when the SMART error is generated, it is possible to prevent the data from being lost by backing up necessary data and replacing the HDD. Therefore, it is possible to protect the data.
In addition, generally, in order to monitor a magnetic storage device of a slave station installed at a remote location, there is provided a condition managing system of a magnetic storage device in which a master station can monitor detailed operating conditions of the magnetic storage device in a slave station by collecting self-analysis information (SMART information) of the slave station and take prevention measures before abnormalities occur in the magnetic storage device (For example, see JP-A-2003-233511).
A hard disk recorder (HDD video recorder), and a hard disk recorder complex machine having a record-typed DVD drive or a video tape recorder have come into wide use as household appliances having a HDD.
These appliances only display error messages when abnormalities are generated on the HDDs during use, and they don't have effective self-diagnosis functions. For this reason, users cannot understand conditions of the appliances until the messages are displayed. Since the appliances are not operated due to the sudden failure of the HDDs, it is not possible to notify the user of the possibilities that interferences occur in advance, and they have disadvantages.
SUMMARY OF THE INVENTION
The present invention has been made to solve the above-mentioned problems and it is an object of the present invention to provide a hard disk recording apparatus capable of managing conditions of a HDD and detecting the failure in advance.
In order to achieve the above-mentioned objects, according to a first aspect of the invention, there is provided a hard disk recording apparatus including: a receiving unit for receiving programs on the air; a reservation data receiving unit for accepting input of reservation recording data including a reservation recording starting time; a reservation data storing unit for storing the reservation recording data received by the reservation data receiving unit; a recording unit for recording the programs received by the receiving unit on a hard disk on the basis of the reservation recording data stored by the reservation data storing unit, and having a self-diagnosis function for detecting the presence or absence of abnormalities of the hard disk; and a control unit for executing the self-diagnosis in the recording unit if the main body is in the standby state and there is a spare time more than a time required for the self-diagnosis by a next reservation recording starting time, when the current time timed by a timer built in the main body becomes the self-diagnosis starting time, and not executing the self-diagnosis in the recording unit if the main body is not in the standby state or there is not a spare time more than a time required for the self-diagnosis by the next reservation recording starting time.
In this construction, when the current time timed by a timer built in the main body becomes the self-diagnosis starting time, a hard disk recording apparatus executes the self-diagnosis in the recording unit if the main body is in the standby state and there is a spare time more than a time taken for the self-diagnosis by the next reservation recording starting time, and doesn't execute the self-diagnosis in the recording unit if the main body is not in the standby state or there is not a spare time more than a time taken for the self-diagnosis by the next reservation recording starting time. Therefore, when there is not a spare time more than the time taken for the self-diagnosis of the hard disk, the reservation recording is performed without executing the self-diagnosis, so that it is possible to execute the recording without causing problems. In addition, when there is a spare time required for the self-diagnosis of the hard disk, the self-diagnosis is surely executed, so that it is possible to understand whether the abnormalities occur on the had disk.
According to a second aspect of the invention, the hard disk recording apparatus further includes a standby state setting unit for setting and canceling the standby state of the main body. Also, when canceling the standby state of the main body during the self-diagnosis of the recording unit, the control unit stops the self-diagnosis.
In this construction, if the standby state of the main body is cancelled during the self-diagnosis of the recording unit, the self-diagnosis of the hard disk is stopped, so that users can immediately use the hard disk recording apparatus in the case of use.
According to a third aspect of the invention, the hard disk recording apparatus further includes a standby time storing unit for storing data of a period of time for which the main body is in the standby state by an amount of data corresponding to a predetermined period, and the control unit sets the self-diagnosis starting time on the basis of the data stored by the standby time storing unit.
In this construction, the hard disk recording apparatus sets the self-diagnosis starting time on the basis of the data corresponding to a predetermined period in a period of time for which the main body is in the standby state, stored by the standby time storing unit. Therefore, users can set executing the self-diagnosis of the hard disk in the period of time in which users doesn't use the hard disk recording apparatus, and use the hard disk recording apparatus without paying attention to executing the self-diagnosis of the hard disk.
According to a fourth aspect of the invention, the control unit stops the self-diagnosis if the standby state of the main body is cancelled during the self-diagnosis of the recording unit, and resets the self-diagnosis starting time on the basis of the data stored by the standby time storing unit.
In this construction, if the standby state is cancelled during the self-diagnosis of the recording unit, the control unit resets the self-diagnosis starting time on the basis of the data stored by the standby time storing unit. Therefore, users can use the hard disk recording apparatus without paying attention to executing the self-diagnosis of the hard disk.
According to the hard disk recording apparatus of the present invention, since the user understands a condition of the HDD by executing the self-diagnosis of the HDD on a regular interval, it is possible to notify the user of the possibilities that interferences occur in advance and take prevention measures before the failure of the HDD. Furthermore, since the hard disk recording apparatus according to the present invention can select the time when users doesn't use the apparatus to set executing the self-diagnosis, the hard disk recording apparatus can automatically execute the self-diagnosis without setting the self-diagnosis of the hard disk recording apparatus by users.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other objects and advantages of this invention will become more fully apparent from the following detailed description taken with the accompanying drawings in which:
FIG. 1 is a block diagram schematically showing the structure of an optical disk recording apparatus according to an embodiment of the present invention; and
FIG. 2 is a flow chart illustrating a process at the time of self-diagnosis of the optical disk recording apparatus.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 is a block diagram schematically showing the structure of an optical disk recording apparatus according to an embodiment of the present invention. A hard disk recorder 1 , which is a hard disk recording apparatus having a built-in DVD drive, includes a DVD record reproducing unit 11 , a HDD (hard disk drive) 12 , a tuner 14 connected to an antenna 13 , a data processing unit 15 , an input terminal 16 , output terminals 17 and 18 , a control unit 19 , a storage unit 20 , a display unit 21 , and an operating unit 22 . The DVD record reproducing unit 11 includes an optical pickup element having a laser element, an actuator, a servo circuit, and the like, which are not shown. The DVD record reproducing unit 11 records data on a writable DVD 10 called DVD-R or DVD-RW, and reads the data recorded on the regenerating or writable DVD 10 . The HDD 12 stores a television program received by the tuner 14 , and video data and audio data which is the content outputted from other video output devices through the input terminal 16 .
The tuner 14 receives broadcasting of a channel selected by the operating unit 22 through the antenna 13 , and outputs video and audio data of the currently broadcasted program to the data processing unit 15 .
The data processing unit 15 outputs content data including the video and audio data transmitted from the tuner 14 or the input terminal 16 to the HDD 12 . In addition, the data processing unit 15 outputs content data outputted from the DVD record reproducing unit 11 and content data read from the HDD 12 to the DVD record reproducing unit 11 or the output terminals 17 and 18 . The input terminal 16 is a terminal which is connected to another video output device and which inputs the video data and audio data of the content outputted from another video output device to the data processing unit 15 . FIG. 1 shows an example in which a video deck 3 is connected to the input terminal 16 .
The output terminal 17 is a terminal for outputting the image data and the audio data outputted from the data processing unit 15 to a monitor 2 having one end connected to the output terminal 17 .
The output terminal 18 is a terminal for outputting the image data and the audio data outputted from the data processing unit 15 to the video recording device having one end connected to the output terminal 18 . FIG. 1 shows an example in which a hard disk recorder 4 is connected to the input terminal 16 .
The control unit 19 controls each unit of the hard disk recorder 1 . Further, the control unit 19 has a timer 23 for timing current date and time, a day of the week, and time.
The storage unit 20 stores a program or the like to be executed in the firmware and the hard disk recorder 1 . The display unit 21 displays messages to be transmitted to a user using letters or images. The operating unit 22 accepts the operations such as, setting of the program to be stored on the HDD 12 , setting at the time of recording the data to the DVD-R 10 from the HDD 12 , setting of the channel to be received at the tuner 14 or the like, and outputs the signals according to the operation to the control unit 19 .
Next, a normal function of the hard disk recorder 1 will be described. The hard disk recorder 1 can store the data, which includes a television program received at the tuner 14 and a content outputted from the video reproducing device connected to the input terminal 16 , on the HDD 12 . In addition, the hard disk recorder 1 can record the data of the content, such as a television program stored on the HDD 12 , on the writable DVD 10 . Furthermore, the hard disk recorder 1 can display the content such as a television program stored on the HDD 12 , the content recorded on the writable DVD 10 , and the content such as the television program received at the tuner 14 , on the monitor 17 connected to the output terminal 17 . In addition, the hard disk recorder 1 can execute the reservation recording of the program on the basis of EPG received at the tuner 14 .
Next, a self-diagnosis function of the HDD 12 of the hard disk recorder 1 will be described. The hard disk recorder 1 has a function for executing the self-diagnosis of the HDD 12 on a regular interval.
Here, the HDD 12 may be a HDD having the self-diagnosis function, and may be, for example, an HDD having an SMART function. In addition, in this case, the HDD 12 may be set such that it executes an “SMART execute Offline immediate” command as a self-diagnosis command. When executing the self-diagnosis according to “the SMART execute Offline immediate” command, the HDD 12 checks up the entire region of the disk. For this reason, the checking time required for performing the self-diagnosis is different depending on the capacity of the disk. For example, it takes about fifty minutes to check up the entire region of an HDD having the capacity of 80 gigabytes.
The hard disk recorder 1 may be set such that it automatically determinates when is a time the user desires or when is the time the frequency of user's use is the least and executes the self-diagnosis on a regular interval. When the hard disk recorder 1 is set to execute the self-diagnosis on a regular interval at the time when the user desires, the user may operate the operating unit 22 to input the desired time and a self-diagnosis executing cycle. In this way, the hard disk recorder 1 executes the self-diagnosis of the HDD 12 on a regular interval. In the hard disk recorder 1 , it is possible to set any period as the self-diagnosis executing cycle. However, for example, when the usage frequency of the hard disk recorder 1 is high, that is, the hard disk recorder 1 is used every day, it may be set to execute the self-diagnosis every one or two weeks. In addition, when the usage frequency of the hard disk recorder 1 is low, that is, the hard disk recorder 1 is used once or twice a week, it may be set to execute the self-diagnosis every one or two months. In this way, it is possible to notify the user of whether there is a possibility in which a failure occurs at the HDD 12 in accordance with the frequency of use of the hard disk recorder 1 .
Further, the hard disk recorder 1 has a function for counting data for the user's usage, and records the time when the user executes the reservation recording, and the period of time for which the HDD 12 or the DVD record reproducing unit 11 is used. When the user doesn't set the self-diagnosis starting time, the hard disk recorder 1 has an automatic setting function to execute the self-diagnosis of the HDD 12 on a regular interval during the period of time for which the frequency of user's usage is the least on the basis of counted data for the user's usage.
When the user doesn't set the self-diagnosis starting time, first the hard disk recorder 1 counts the data for the user's usage for one week from the beginning of the usage, and sets executing the self-diagnosis of the HDD 12 every week at the time for which the frequency of user's usage is the least on the basis of counted data for the user's usage. In addition, the hard disk recorder 1 additionally counts the data for the user's use, and sets the self-diagnosis executing cycle and time on the basis of the data for the user's usage for one month from the beginning of the use. For example, when the usage frequency of the hard disk recorder 1 is high, for example, the hard disk recorder 1 is used every day, it is set to execute the self-diagnosis every week Also, the hard disk recorder 1 is set to execute the self-diagnosis at the period of time for which the user doesn't use the hard disk recorder 1 , such as the period of time for which the user executes the reservation recording of the program, the period of time for which the program recorded on the HDD 12 is reproduced, and the period of time for which the program is recorded or reproduced on the DVD.
Moreover, the hard disk recorder 1 continuously counts the data for the user's usage and conducts a review of the self-diagnosis executing cycle and time on a regular interval (for example, every month). Accordingly, the hard disk recorder 1 is set to execute the self-diagnosis at a day of week and the period of time for the frequency of use is the least.
The hard disk recorder 1 is set to become automatically a standby state when the self-diagnosis is finished. When the abnormality is not detected by the self-diagnosis (a normal case), the hard disk recorder 1 stores the result of the self-diagnosis together with information related to the checking date and time on the storage unit 20 , and enters into the standby state. Meanwhile, when the abnormality is detected by the self-diagnosis, the hard disk recorder 1 enters into the standby state in a state in which the result of the self-diagnosis is stored on the storage unit 20 together with the information related to the checking date and time, similar to a normal case. When a power switch of the operating unit 22 is operated, the control unit 19 displays the result of the self-diagnosis on the display unit 21 and allows the result of the self-diagnosis to be displayed on the monitor 2 by outputting the signal to the output terminal 17 from the data processing unit 15 . In this step, since the HDD 12 is normally operated even if there is a possibility in which a failure occurs on the HDD 12 , as shown in FIG. 1 , the backup of the HDD 12 is executed by connecting an input terminal of the hard disk recorder 4 to the output terminal 18 . As a result, it can be prevented in advance that having access to the data recorded on the HDD 12 is not possible due to the failure of the HDD 12 .
Even though the hard disk recorder 1 executes the self-diagnosis at the time when the user desires or the period of time for which the frequency of use is the least as described above, the time when the user reserves the recording of the program and the time when the self-diagnosis is executed can overlap each other. Further, the period of time for which the hard disk recorder 1 executes the self-diagnosis and the period of time for which the user uses the hard disk recorder 1 can overlap each other. In this case, the control unit 19 of the hard disk recorder 1 stops executing the self-diagnosis and changes the self-diagnosis executing time to another time just before the self-diagnosis is executed or during the self-diagnosis.
In a case in which the self-diagnosis executing time period is changed, when the user sets the reservation time or operates the power switch of the operating unit 22 , the control unit 19 displays display for urging setting the self-diagnosis executing time on the display unit 21 and the monitor 2 by the outputting the signal to the output terminal 17 from the display unit 21 and the data processing unit 15 . If the new self-diagnosis executing time is set by operating the operating unit 22 , the control unit 19 executes the self-diagnosis in the new self-diagnosis executing time period.
Furthermore, in a case in which the recording is reserved or the power switch is operated for the self-diagnosis executing time period, if being set previously such that the self-diagnosis executing time period is automatically set again, the control unit 19 sets the self-diagnosis executing time again on the basis of the counted data for the user's usage. That is, if the reservation recording is executed, the control unit 19 confirms the self-diagnosis executing time period. In this case, when the reservation recording time and the self-diagnosis executing time period overlap each other, the control unit 19 selects a day of the week and the time period the closest to the self-diagnosis executing time period for which the frequency of user's use is the least on the basis of the counted data for the user's usage, and then the control unit 19 sets executing the self-diagnosis in the selected time period. In this way, it is possible to early detect the abnormality of the HDD 12 even if the self-diagnosis of the HDD 12 is suspended.
Since the hard disk recorder 1 has the above-mentioned functions, it is possible to execute the self-diagnosis of the HDD 12 in the time desired by the user. In addition, when the user doesn't set the self-diagnosis executing time, the hard disk recorder 1 executes the time setting to execute the self-diagnosis in the period of time for which the frequency of user's use is the least by counting the data for the user's usage. Therefore, even if the user forgets executing the self-diagnosis of the HDD 12 , it is possible to execute the self-diagnosis.
Further, when the reservation recording time overlaps the self-diagnosis executing time period and a power is applied in the self-diagnosis executing time period, the hard disk recorder 1 changes the self-diagnosis executing time period. Therefore, the user can freely use the hard disk recorder 1 without paying attention to the self-diagnosis of the HDD 12 .
Next, a process at the time of the self-diagnosis of the hard disk recorder 1 will be described with reference to a flow chart. FIG. 2 is a flow chart illustrating the process at the time of the self-diagnosis of the optical disk recording apparatus.
In the hard disk recorder 1 , the self-diagnosis starting time is set by a user in advance or is automatically set on the basis of the data for the user's usage. Furthermore, the self-diagnosis executing time of the HDD 12 is set as fifty minutes.
When becoming the self-diagnosis starting time (s 1 ), first, the control unit 19 of the hard disk recorder 1 confirms the state of the main body. In other words, the control unit 19 confirms'whether it is the standby state or not (s 2 ), and whether there is a spare time more than fifty minutes by the reservation recording starting time (s 3 ). In addition, when the control unit 19 is not in the standby state and when there is not a spare time more than fifty minutes by the reservation recording starting time, the control unit 19 stops the self-diagnosis (s 11 ) and automatically resets the self-diagnosis starting time on the basis of the data for the user's usage (s 12 ). Then, the self-diagnosis is finished.
Meanwhile, when the main body is in the standby state and when there is a spare time more than fifty minutes by the reservation recording starting time, the control unit 19 allows the self-diagnosis of the HDD 12 to be started (s 4 ).
When it is detected that the power switch of the operation unit 22 is operated during the self-diagnosis (s 5 ), the control unit 19 executes processes subsequent to a step s 11 . In addition, when the power switch of the operation unit 22 is not operated during the self-diagnosis, the control unit 19 performs the process continuously by the check (self-diagnosis) for the entire region of the HDD 12 is finished (s 4 to s 6 ).
If the self-diagnosis of the HDD 12 is finished, in a case in which the abnormality is not detected during the self-diagnosis (normal case), the control unit 19 stores the result of the self-diagnosis together with the information related to the checking date and time on the storage unit 20 and enters into the standby state (s 8 ), and then the process is finished. Meanwhile, when the abnormality is detected during the self-diagnosis in the step s 19 , the control unit 19 stores the result of the self-diagnosis together with the information related to the checking date and time on the storage unit 20 , similar to the normal case. Further, when the power switch of the operation unit 22 is activated by the operation, the control unit 19 allows the result of the self-diagnosis to be displayed on the display unit 21 and sets displaying the result of the self-diagnosis on the monitor 2 by outputting the signal to the output terminal 17 from the data processing unit 15 . Then, the control unit 19 enters into the standby state (s 9 ) and the process is finished.
As described above, the hard disk recorder 1 according to the embodiment of the present invention can execute the self-diagnosis of the HDD 12 at the time desired by the user. Furthermore, when the user doesn't set the self-diagnosis starting time, the hard disk recorder 1 sets the time so as to execute the self-diagnosis at the time when which the frequency of user's use is the least by counting the data for the user's usage. Therefore, even if the user forgets executing the self-diagnosis of the HDD 12 , it is possible to execute the self-diagnosis. Additionally, when the reservation recording time overlaps the self-diagnosis executing time period and a power is applied in the self-diagnosis executing time period, the hard disk recorder 1 changes the self-diagnosis executing time period. Therefore, the user can freely use the hard disk recorder 1 without paying attention to the self-diagnosis of the HDD 12 .
[ FIG. 1 ]
1 : HARD DISK RECORDER
2 : MONITOR
3 : VIDEO DECK
4 : HARD DISK RECORDER
11 : DVD RECORD REPRODUCING UNIT
12 : HDD
14 : TUNER
15 : DATA PROCESSING UNIT
19 : CONTROL UNIT
20 : STORAGE UNIT
21 : DISPLAY UNIT
22 : OPERATING UNIT
23 : TIMER
[ FIG. 2 ]
S 1 : SELF-DIAGNOSIS STARTING TIME
S 2 : STANDBY STATE?
S 3 : IS THERE SPARE TIME MORE THAN FIFTY MINUTES BY RESERVATION RECORDING STARTING TIME
S 4 : EXECUTE SELF-DIAGNOSIS OF HDD
S 5 : IS POWER SWITCH OPERATED?
S 6 : IS SELF-DIAGNOSIS FINISHED?
S 7 : IS THERE ABNORMALITY ON HDD
S 8 : RECORD RESULT OF SELF-DIAGNOSIS ON STORAGE UNIT
S 9 : SET NOTIFYING WHETHER THERE IS ABNORMALITY OR NOT AT THE TIME OF NEXT POWER SWITCH OPERATION
S 11 : STOP SELF-DIAGNOSIS
S 12 : RESET SELF-DIAGNOSIS TIME
|
A hard disk recording apparatus including: a receiving unit for receiving programs; a reservation data receiving unit for accepting input of reservation recording data including reservation recording starting time; a reservation data storing unit for storing the reservation recording data; a recording unit for recording the programs on a hard disk based on the reservation recording data, and having a self-diagnosis function for detecting the presence or absence of abnormalities of the hard disk; and a control unit for executing the self-diagnosis if the main body is in the standby state and there is a spare time a spare time more than a time required for the self-diagnosis by a next reservation recording starting time, and not executing the self-diagnosis if the main body is not in the standby state or there is not a spare time more than a time required for the self-diagnosis.
| 7
|
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a toothbrush which may have one of a variety of heads, a massage structure or the like, with bristles mounted thereon secured in either a straightline and/or adjustable angular orientation to the handle.
2. Description of the Prior Art
Toothbrushes, of course, have been used in modern day society for many years. Accordingly, the prior art is replete with various design configurations, structures, materials, etc. incorporated in the basic toothbrush. These design changes and alterations have been made for the purpose of better facilitating the cleaning of the teeth. One problem generally associated with the manufacture of an efficient toothbrush is achieving the proper angle of the head and, of course, the bristles mounted thereon relative to the teeth being cleaned. In order to solve this problem, a relatively recent development has been a fixed one piece handle and head wherein the head portion was arranged at a predetermined allegedly "most efficient" angle for cleaning.
It should be obvious to even the most casual observer that the best or most appropriate angle of the handle to the head depends upon which of the plurality of teeth in the user's mouth are being cleaned. As an obvious example, the back teeth are best reached when the head is mounted on the handle at a different angle than if the front teeth were being brushed. In such a situation, it is clear that a fixed angle toothbrush does not always achieve the most efficient angle for bristle contact with the teeth being cleaned.
In order to overcome all of the above se t forth problems, the prior art has developed numerous structural designs incorporating what may be referred to as a "adjustable" head having bristles mounted thereon wherein the head is selectively disposable at various orientations to the handle portion of the toothbrush. The following U.S. Patents disclose structures which are generally representative of this type of adjustable head toothbrush.
Hyman, U.S. Pat. No. 4,488,328, discloses a floating head toothbrush having an elongated handle and a brush head supported at one end which is capable of somewhat limited pivotal movement between opposed arms of a supporting yoke like structure. Hyman does not necessitate the removal and reorientation of the head bu t rather, relies on a certain amount of permissible movement of the head when the bristles thereon engage the teeth to be cleaned.
Stevens, U.S. Pat. No. 4,575,894, discloses a vertical action toothbrush designed for brushing along the major axis of the teeth and incorporating a tongue-in-groove means so that the head can easily be removed and replaced on the same handle and also incorporating a resilient means for automatically promoting a wiping action of the bristles and a reorientation of the head and bristles.
Del Rosario, U.S. Pat. No. 4,333,199, discloses an improved toothbrush which includes an elongated handle and a brush with a base and a mounting in the form of a coil spring connecting the brush base to the distal end of the handle which enables the head to swing, rotate or tilt for an allegedly more efficient orientation of the brush relative to the teeth being cleaned.
Bortman, U.S. Pat. No. 4,796,325, discloses a swivel type, angularly adjustable, double headed toothbrush capable of brushing oppositely disposed surfaces of the same tooth at the same time and further wherein the head is specifically adjustable relative to the supporting handle.
Other patents exist which while not specifically directed to a toothbrush structure do show a head having bristles mounted thereon and selectively positionable at various angular orientations relative to a supporting handle. These structures are represented in Booharin, U.S. Pat. No. 2,395,245 and Johnson, U.S. Pat. No. 3,604,044.
The patent to Borea, U.S. Pat. No. 4,592,109, discloses a toothbrush device having a handle or grip portion which is anatomically formed to fit the hand of the user and wherein a head portion is relatively attachable to the handle in a variety of different positions. The position or orientation of the grip or handle in the hand of the user cooperates with the position of the head attached to the handle to allegedly accomplish the proper angle of attack of the bristles to the teeth being cleaned.
Even in light of the structures as set forth above, there is still a need in this industry for a toothbrush structure which includes a head capable of assuming a plurality of operative positions which are defined by a straightline orientation of the head and handle as well as a plurality of different angular orientations of the head relative to the handle. The user may therefore selectively orient the head as well as the bristles thereon to a "preferred" angular orientation best suited. In addition, such a preferred structure should also include a handle capable of being used with a variety of heads wherein each head may, for example, include a bristle structure of different flexibility, softness, rigidity, design configuration, etc.
SUMMARY OF THE INVENTION
The present invention relates to a toothbrush structure of the type wherein a head having the cleaning bristles attached thereto is mounted on a supporting and gripping handle at a plurality of operative positions defined individually by at least one substantially coaxial or straightline position and a plurality of angularly oriented positions. The orientation may be at a plurality of different angles to best accomplish reaching the various teeth in the mouth of the user.
The structure of the present invention comprises an elongated handle of sufficient dimension and configuration to facilitate gripping by the hand of the user as well as manipulation of the brush during the cleaning process. The structure includes at least one head having bristles extending outwardly from at least one side thereof and further including a somewhat elongated connecting stem terminating at a free end. A free end of the head portion is dimensioned and structured to mate in confronting engagement with a corresponding free end of the handle when the attached head is connected to the handle in any one of its plurality of operative positions.
A mounting means is secured both to the handle as well as being at least partially formed on the head and comprises an elongated mounting rod fixed to the aforementioned free end of the handle and extending outwardly therefrom at an angular orientation which is not parallel to or colinear with the central longitudinal axis of the handle. Similarly, an elongated receiving channel is integrally formed in the handle in an orientation which is not colinear or parallel to the central longitudinal axis of the head. The outer surface of the mounting rod and the inner surface of the receiving channel are respectively configured so as to prevent relative rotation of the head and handle. However, the head can be removed by pulling longitudinally away from the mounting rod and replaced at a different angular orientation to dispose the head and the bristles thereon in one of the aforementioned plurality of operative positions.
It should be readily apparent therefore that a user may have one head which he may attach at any of the aforementioned straightline or angularly oriented, operative positions or alternately, one or more users may utilize the structure by having one handle attachable to any number of heads. In this latter embodiment, each of the bristles on the various heads may have a different configuration, degree of flexibility, strength, size, etc.
BRIEF DESCRIPTION OF THE DRAWINGS
For a fuller understanding of the nature of the present invention, reference should be had to the following detailed description taken in connection with the accompanying drawings in which:
FIG. 1 is a side view of the tooth brush of the subject invention in assembled form.
FIG. 2 is a side view in unassembled form.
FIG. 3 is a side view of ne embodiment of the present invention also in unassembled position.
FIG. 4 is a sectional view along line 4--4 of FIG. 2.
FIG. 5 is a sectional view along line 5--5 of FIG. 3.
FIG. 6 is a sectional view along line 6--6 of FIG. 3.
FIG. 7 is a separated view in partial cutaway.
FIGS. 8, 9 and 10 are respectively side views of the toothbrush assembly of the present invention representing different angular orientations of the head relative to the handle.
Like reference numerals refer to like parts throughout the several views of the drawings.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The toothbrush assembly of the present invention is generally indicated as 10 and comprises a handle 12 and a head portion generally indicated as 14. The handle has an elongated configuration of sufficient length and overall external configuration to facilitate gripping thereof by the hand of the user. The handle 12 terminates at oppositely disposed free distal end 18 and proximal end 16.
The head 14 comprises a bristle attachment area as at 20 to which a plurality of bristles may be mounted so as to extend outwardly therefrom as at 22. It should be emphasized that while the structure of the present invention is demonstrated with the aforementioned bristle structure 20, other elements such as a rubber tip or like massage device could be substituted and still be within the scope of the present invention. The configuration and position of the bristles 22 may vary and still be within the intended scope of the present invention. An elongated stem as at 24 is also an integral part of the head 14 and serves to interconnect the bristle and the bristle mounting portion 22 and 20, respectively, to the handle 12. More specifically, one corresponding free end as at 26 is designed to confrontingly engage the distal end 18 of the handle 12. The free end 26 is formed in somewhat of a receiving socket which corresponds to and receives therein an outward somewhat tapered protuberance defining the distal end 18 as shown.
An important feature of the present invention is the mounting means generally indicated as 30. The mounting means comprises an elongated rigid material substantially high strength mounting rod 32 affixed to and extending outwardly from the distal end 18. In one embodiment, the mounting rod 32 may have a sufficient length to have one inner most end 34 embedded in somewhat of an integral formation into the interior of the handle 12 as shown such that the remainder thereof extends outwardly from the free end at an angular orientation. More specifically, the elongated mounting rod 32 is mounted on or attached to the handle 12 in a location where it is not colinear with or parallel to the central longitudinal axis of the handle 12. To the contrary, it is arranged at a predetermined specific angular orientation as shown.
The mounting means 30 further comprises-an elongated receiving channel 36 formed on the interior of the head 14 and includes an open end as at 38 which is adjacent or contiguous with the free end 26. Both the dimension of the open end 38 and the interior of the channel 36 are such as to allow the mounting rod to be placed therein. Further, at least a portion of the length of both the mounting rod 32 and the channel 36 may be correspondingly configured to prevent relative rotation between the handle 12 and the head 14. This can be accomplished by having a multi-sided configuration formed on at least one exterior portion of a length of the mounting rod 32 and a corresponding multi-sided configuration disposed along at least a portion of the length of the interior of the channel 36. It should be noted, of course, that the elongated channel 36 is also disposed at an angular orientation relative to the central longitudinal axis of the head 14 so as to not be colinear therewith or parallel thereto. The cooperative angular orientations of the rod 32 and the channel 36 therefore allow the mounting of the head in any one of a plurality of operative positions. This is accomplished by separating the head 14 from the handle 12 by removing the mounting rod 32 from the channel 36 and then rotating the head 14 to a desired position relative to the handle 12. The mounting rod 32 may then be reinserted into the channel 36 with the multi-sided configuration on the mounting rod 32 in mating alignment with the corresponding multi-sided configuration within the channel 36. One such operative position may be a straightline substantially linear relative orientation between the head and the handle wherein the mounting rod 32 and channel are in alignment with the length of the attached handle 12 and head 14, as shown in FIGS. 1 and 2. Alternately, the head may be arranged at any of a plurality of different angular orientations relative to the handle so as to give the user thereof a choice of angles to accomplish the best results in cleaning. The number of operative positions which the head 14 may assume relative to the handle 12 may in fact be determined by the number of faces or sides. on the multi-sided configuration along an external surface of the rod 32 and an internal surface of the channel 36 as set forth above.
Further, an attachment means is provided in the form of an enlarged attachment member or head 40 extending radially outward from at least a portion of the remainder of the rod 32. This attachment member is mounted for receiving engagement within a receiving portion or pocket 42 formed on the interior of the channel 36 along a portion of the length thereof. The material from which the portion of the handle 14 and more particularly, the stem 24 substantially surrounding the receiving portion or pocket 42 has sufficient flexibility to allow at least some outward expansion thereof to accommodate for the enlarged head or attachment member 40 as it passes into the receiving pocket 42. Such flexibility will prevent inadvertent dislodgment or displacement of the head 14 from the handle 12 but will allow its removal and replacement at a different operative position, if such is desired, when sufficient pulling force is applied to the head 14 against the handle 12.
In operation, the head is merely pulled from the handle, realigned at a different operative position, either straightline or angular orientation, and then replaced back in its attached position. Because the mounting rod 32 extends from the distal end 18 at an angular orientation to the handle 12, and the channel 36 is also disposed at an angular orientation relative to the longitudinal axis of the head 14, the achieved operative position depends upon the rotated position of the head relative to the handle.
It should also be emphasized that the handle 12 can be used with a great number of different heads 14 each of which may have a different bristle configuration, strength, etc.
|
A toothbrush structure having a head which may be removably attached to a handle at any one of a plurality of operative positions wherein such operative positions are defined by a first, substantially straightline orientation between the handle and the head and a remainder of said operative positions are defined by various angular orientations of said head and handle to accomplish the best angle of approach of the bristles mounted on the head to the teeth being cleaned by the brush in the user's mouth.
| 0
|
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of provisional patent application (PPA) Ser. No. 61/933,336, filed Jan. 30, 2014 by the present inventors, which is incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention generally relates to computer communication, and in particular, it concerns computer access to remote data.
BACKGROUND OF THE INVENTION
[0003] Currently, network access is done by writing a descriptor to system memory and informing the IO device that work is ready. Typical implementations include a computer's central processing unit (CPU) writing to the computer's local memory, and then informing a locally attached IO device. The IO device then will fetch the work descriptor (command buffer), perform an actual IO operation (for example, reading a remote memory location over the network), and report completion of the command. The CPU needs to be aware of completion of the written command, typically by either the CPU polling on a completion status or the CPU being interrupted using an interrupt message (for example MSI-X).
[0004] This conventional process for network IO access, where network access is done in an asynchronous manner, is beneficial were latency can be tolerated. In this case, the CPU can continue working while the network access is done in the background.
[0005] In some cases network IO access (the network phase) cannot overlap the compute phase. In other words, the CPU cannot continue working until the CPU receives (or transmits) the subject data. In these cases, the inherent asynchronous nature of operation adds latency to processing but does not provide any benefit.
SUMMARY
[0006] In cases where network IO access (a network phase) cannot overlap a compute phase, a direct network access from the instruction stream decreases latency in CPU processing. At a high level, the general approach to the current embodiments are to treat the network as yet another memory that can be directly read from, or written to, by the CPU. Network access can be done directly from the instruction stream using loads and stores. Example scenarios where synchronous network access can be beneficial are SHMEM (symmetric hierarchical memory access) usages (where the program directly reads/writes remote memory), and scenarios where part of system memory (for example DDR) can reside over a network and made accessible by demand to different CPUs.
[0007] According to the teachings of the present embodiment there is provided a method for accessing data including the steps of
(a) issuing, by a CPU, a LOAD command including a virtual address; (b) deriving network access information based on the virtual address, the network access information including one or more references to a remote memory; (c) checking, using the one or more references to the remote memory, if access is allowed to the remote memory; (d) if access is denied to the remote memory:
(i) then
(A) notifying the CPU the LOAD command failed; and (B) invoking management software to handle the failure of the LOAD command,
(ii) else attempt to load data from the remote memory;
(e) if the attempt is successful:
(i) then returning the data to the CPU; (ii) else
(A) notifying the CPU the LOAD command failed; and (B) invoking management software to handle the failure of the LOAD command.
[0021] In another optional embodiment, further including after the step of issuing: setting a load timer; and if the load timer expires before the data is returned to the CPU then notifying the CPU the LOAD command failed; and invoking management software to handle the failure of the LOAD command.
[0022] In another optional embodiment, the step of deriving network access information includes:
(a) translating the virtual address to a physical address; (b) parsing the physical address for a network address index; and (c) retrieving at least a portion of the network access information based on the network address index.
[0026] In another optional embodiment, the step of retrieving is from a network connection table.
[0027] In another optional embodiment, further including parsing the physical address for a remote virtual address portion of the network access information.
[0028] In another optional embodiment, the step of deriving network access information includes:
(a) translating the virtual address to a physical address; (b) parsing the physical address for at least a portion of the network access information.
[0031] In another optional embodiment, further including after the step of deriving network access information: waiting for any previously issued STORE commands to the remote memory to be completed prior to continuing with the step of checking.
[0032] In another optional embodiment, wherein after the attempt fails further including prior to the step of notifying the CPU: repeating attempt to load data from the remote memory.
[0033] According to the teachings of the present embodiment there is provided a method for accessing data including the steps of
(a) issuing, by a CPU, a STORE command including a virtual address; (b) deriving network access information based on the virtual address, the network access information including one or more references to a remote memory; (c) checking, using the one or more references to the remote memory, if access is allowed to the remote memory; (d) if access is denied to the remote memory:
(i) then
(A) notifying the CPU the STORE command failed; and (B) invoking management software to handle the failure of the STORE command,
(ii) else attempt to store data to the remote memory;
(e) if the attempt is successful:
(i) then continue with normal operation of the CPU; (ii) else
(A) notifying the CPU the STORE command failed; and (B) invoking management software to handle the failure of the STORE command.
[0047] In another optional embodiment, the step of deriving network access information includes:
(a) translating the virtual address to a physical address; (b) parsing the physical address for a network address index; and (c) retrieving at least a portion of the network access information based on the network address index.
[0051] In another optional embodiment, the step of retrieving is from a network connection table.
[0052] In another optional embodiment, further including: parsing the physical address for a remote virtual address portion of the network access information.
[0053] In another optional embodiment, the step of deriving network access information includes:
(a) translating the virtual address to a physical address; (b) parsing the physical address for at least a portion of the network access information.
[0056] In another optional embodiment, further including after the step of deriving network access information: if the remote memory is strongly ordered then waiting for any previously issued STORE commands to the remote memory to be completed prior to continuing with the step of checking.
[0057] In another optional embodiment, wherein after the attempt fails further including prior to the step of notifying the CPU: repeating attempt to store data to the remote memory.
[0058] According to the teachings of the present embodiment there is provided a system for accessing data including:
(a) a processing system containing one or more processors, the processing system being configured to:
(i) issue a LOAD command including a virtual address; (ii) derive network access information based on the virtual address, the network access information including one or more references to a remote memory; (iii) check, using the one or more references to the remote memory, if access is allowed to the remote memory; (iv) if access is denied to the remote memory:
(A) then
(I) send a notification that the LOAD command failed; and (II) invoke management software to handle the failure of the LOAD command,
(B) else attempt to load data from the remote memory;
(v) if the attempt is successful:
(A) then return the data; (B) else
(I) send a notification that the LOAD command failed; and (II) invoke management software to handle the failure of the LOAD command.
[0073] According to the teachings of the present embodiment there is provided a system for accessing data including:
(a) a CPU (central processing unit) configured to:
(i) issue a LOAD command including a virtual address; and (ii) receive a notification the LOAD command failed and responsive to the notification invoke management software to handle the failure of the LOAD command,
(b) a local NIC (network interface card) configured to:
(i) derive network access information based on the virtual address, the network access information including one or more references to a remote memory; and (ii) receive a notification that the LOAD failed and responsive to the notification notify the CPU that the LOAD command failed; and
(c) a remote NIC configured to
(i) check, using the one or more references to the remote memory, if access is allowed to the remote memory; (ii) if access is denied to the remote memory:
(A) then send a notification to the local NIC that the load failed; (B) else attempt to load data from the remote memory;
(iii) if the attempt is successful:
(A) then return the data; (B) else notify the local NIC that the load failed.
[0088] According to the teachings of the present embodiment there is provided a system for accessing data including:
(a) a processing system containing one or more processors, the processing system being configured to:
(i) issue a STORE command including a virtual address; (ii) derive network access information based on the virtual address, the network access information including one or more references to a remote memory; (iii) check, using the one or more references to the remote memory, if access is allowed to the remote memory; (iv) if access is denied to the remote memory:
(A) then
(I) send a notification that the STORE command failed; and (II) invoke management software to handle the failure of the STORE command,
(B) else attempt to store data to the remote memory;
(v) if the attempt is successful:
(A) then continue with normal operation of the system; (B) else
(I) send a notification that the STORE command failed; and (II) invoke management software to handle failure of the attempt.
[0103] According to the teachings of the present embodiment there is provided a system for accessing data including:
(a) a CPU (central processing unit) configured to:
(i) issue a STORE command including a virtual address; and (ii) receive a notification the STORE command failed and responsive to the notification invoke management software to handle the failure of the STORE command,
(b) a local NIC (network interface card) configured to:
(i) derive network access information based on the virtual address, the network access information including one or more references to a remote memory; and (ii) receive a notification that the STORE failed and responsive to the notification notify the CPU that the STORE command failed; and
(c) a remote NIC configured to:
(i) check, using the one or more references to the remote memory, if access is allowed to the remote memory; (ii) if access is denied to the remote memory:
(A) then send a notification to the CPU that the STORE command failed; (B) else attempt to store data to the remote memory;
(iii) if the attempt is successful:
(A) then continue with normal operation of the CPU; (B) else notify the local NIC that the store failed.
[0118] According to the teachings of the present embodiment there is provided a non-transitory computer-readable storage medium having embedded thereon computer-readable code for accessing data, the computer-readable code including program code for:
(a) issuing, by a CPU, a LOAD command including a virtual address; (b) deriving network access information based on the virtual address, the network access information including one or more references to a remote memory; (c) checking, using the one or more references to the remote memory, if access is allowed to the remote memory; (d) if access is denied to the remote memory:
(i) then
(A) notifying the CPU the LOAD command failed; and (B) invoking management software to handle the failure of the LOAD command,
(ii) else attempt to load data from the remote memory;
(e) if the attempt is successful:
(i) then returning the data to the CPU; (ii) else
(A) notifying the CPU the LOAD command failed; and (B) invoking management software to handle the failure of the LOAD command.
[0132] According to the teachings of the present embodiment there is provided a non-transitory computer-readable storage medium having embedded thereon computer-readable code for accessing data, the computer-readable code including program code for:
(a) issuing, by a CPU, a STORE command including a virtual address; (b) deriving network access information based on the virtual address, the network access information including one or more references to a remote memory; (c) checking, using the one or more references to the remote memory, if access is allowed to the remote memory; (d) if access is denied to the remote memory:
(i) then
(A) notifying the CPU the STORE command failed; and (B) invoking management software to handle the failure of the STORE command,
(ii) else attempt to store data to the remote memory;
(e) if the attempt is successful:
(i) then continue with normal operation of the CPU; (ii) else
(A) notifying the CPU the STORE command failed; and (B) invoking management software to handle the failure of the STORE command.
BRIEF DESCRIPTION OF FIGURES
[0146] The embodiment is herein described, by way of example only, with reference to the accompanying drawings, wherein:
[0147] FIG. 1 is a high-level diagram of network access of remote memory.
[0148] FIG. 2 is a simplified diagram of memories and usage.
[0149] FIG. 3 is a sketch of an exemplary network connection table.
[0150] FIG. 4 is a flowchart of a method of loading data.
[0151] FIG. 5 is a flowchart of a method of storing data.
[0152] FIG. 6 is a high-level partial block diagram of an exemplary system configured to implement a method of the present invention.
ABBREVIATIONS AND DEFINITIONS
[0153] For convenience of reference, this section contains a brief list of abbreviations, acronyms, and short definitions used in this document. This section should not be considered limiting. Fuller descriptions can be found below, and in the applicable Standards.
[0154] ACK—Acknowledgment.
[0155] BAR—Base Address Register. To address a PCI device, the PCI device must be enabled by being mapped into a system's IO port address space or memory-mapped address space. The system's firmware, device drivers or the operating system program the BARs to inform the PCI device of address mapping by writing configuration commands to the PCI controller.
[0156] Command—A task to be accomplished, such as LOAD and STORE. Commands are implemented at least in part by one or more innovations of the current description.
[0157] CPU—Central processing unit. Also referred to as a processor.
[0158] Credits—Used in PCIe to expose the internal buffer. A component (for example a CPU) that desires to talk to a PCIe internal device (for example, a NIC) needs credits. The component uses the component's credits each time the component wants to talk to the device. For example, when the CPU wants to talk to the NIC to do a LOAD or STORE.
[0159] Descriptor—Used to implement high-level commands such as LOAD and STORE. Descriptors are written to memory and include various information depending on the specifics of the command, for example: read, write, send, destination (network address), actual location in the remote memory (for RDMA), and data or a pointer to data.
[0160] DDR—Double data rate. A class of memory integrated circuits used in computers. In the context of this document, the term “DDR” is generally used as a general term to refer to system memory (local or remote), typically local RAM used by the CPU.
[0161] GID—Global Identifier. A 128-bit identifier similar to an IPv6 address (technically, a GID is a valid IPv6 identifier with restrictions). The GID consists of the 64-bit GUID plus an additional 64-bit EUI-64 identifier, for a total of 128 bits. The GID is used for routing between subnets. The default GID prefix is 0xfe80::0.
[0162] GUID—Global Unique Identifiers (also known as Direct Address). Every host on an InfiniBand fabric has three identifiers: GUID, GID, and LID. A GUID is similar in concept to a MAC address because the GUID consists of a 24-bit manufacturer's prefix and a 40-bit device identifier (64 bits total).
[0163] HCA—Host Channel Adapter.
[0164] HW—Hardware.
[0165] IB—InfiniBand. An industry standard, channel-based, switched fabric interconnect architecture for server and storage connectivity. A computer network communications link typically used in high-performance computing featuring very high throughput and very low latency, as compared to conventional network communications. Information can be found in the IB specification available from the InfiniBand Trade Association Administration (3855 SW 153rd Drive, Beaverton, Oreg. 97006, USA) or on the Internet at http://www.InfiniBandta.org/.
[0166] IO—Input/output.
[0167] ISA—Instruction set architecture.
[0168] LID—Local Identifier. The local identifier (LID) is assigned by the subnet manager. The LID is a 16-bit identifier that is unique within a subnet. Hosts have an LID between 0 and 48,000, usually expressed in hexadecimal notation (such as 0xb1). Routing within a subnet is managed by LID.
[0169] LOAD—Operation in which data is requested (and if successful, received), typically as a CPU loads data from memory. For simplicity in the current description, the term LOAD is generally used to refer to accessing remote data (data from a remote location, that is, a location other than local storage/memory).
[0170] Memory region—A collection of memory pages within a local HCA's memory.
[0171] NACK or NAK—Negative-Acknowledgment.
[0172] Network access—In the context of this document, general term referring to LOAD and/or STORE operations. Can also refer to conventional accesses such as InfiniBand RDMA-Read, RDMA-Write, RDMA-Write-With-Immediate, and Send.
[0173] Network address information—information required and/or sufficient for a local element to access a remote element. Examples include remote virtual address, destination local identifier (LID), destination GID, destination queue pair, and memory key (memory region).
[0174] NIC—Network interface card. Currently, most NICs are PCI-based.
[0175] NP credits—Non-posted credits.
[0176] Network access information—Information used for network access, such as which network node to access, which memory region within the node to access, an offset within the memory region, and a length (of the memory to be accessed).
[0177] OOO—Out-of-order execution. Also known as dynamic execution, an implementation where a processor executes instructions in an order other than the instructions original order in a program, for example based on availability of input data.
[0178] PCI—Peripheral Component Interconnect. A high-speed serial computer expansion bus standard.
[0179] PCIe—Peripheral Component Interconnect Express. A high-speed serial computer expansion bus standard.
[0180] QoS—Quality of service.
[0181] RDMA—Remote dynamic memory access.
[0182] RF—Register file
[0183] SHMEM—Symmetric Hierarchical Memory access. A family of parallel programming libraries, initially providing remote memory access for big-shared memory supercomputers using one-sided communications. Later expanded to distributed memory parallel computer clusters, and is used as parallel programming interface or as low-level interface.
[0184] SM—Subnet manager.
[0185] STORE—Operation in which data is sent (and if successful, stored in a destination), typically as a CPU stores data to memory. For simplicity in the current description, the term STORE is generally used to refer to sending or writing data to a remote location (location other than local storage/memory).
[0186] Strongly-ordered memory systems (models)—Systems in which memory requests (load and store operations) are not allowed to be reordered, that is, values are accessed in the same order in which the values were written.
[0187] SW—Software.
[0188] TCA—Target channel adapter.
[0189] VC—Virtual channel.
[0190] Weakly-ordered memory systems (models)—Systems that are allowed to reorder memory requests. Any load or store operation can effectively be reordered with any other load or store operation, as long as the store would never modify the behavior of a single, isolated thread.
DETAILED DESCRIPTION
First Embodiment
FIGS. 1 to 6
[0191] The principles and operation of the system according to a present embodiment may be better understood with reference to the drawings and the accompanying description. A present invention is a system for network access of remote memory directly from a local instruction stream using conventional loads and stores.
[0192] Referring now to the drawings, FIG. 1 is a high-level diagram of network access of remote memory. A local computer 100 includes a local CPU 102 with associated local DDR 104 and a local NIC 106 . The local NIC 106 includes an internal NIC command buffer 108 . Local computer 100 is connected via a network 110 to at least one other computer, such as remote computer 120 . Similar to local computer 100 , remote computer 120 includes a remote CPU 122 with associated remote DDR 124 and a remote NIC 126 . Additional computers such as second remote computer 130 , similar to local computer 100 may also be in operational connection, typically via network 110 . In this document, connection and operation of the local and remote computers ( 100 , 120 ) may also be referred to as connection between the local and remote CPUs ( 102 , 122 ). Local and remote computers are also referred to in the field as nodes. The NICs may be integrated with the associated CPUs, or as shown in the current figure, separate and operationally connected. Typically, connection of CPUs and NICs are via a PCIe bus, and this non-limiting implementation is used in the current description. However, one skilled in the art will realize that other connections and element, module, and component configurations are possible.
[0193] The current embodiment can be implemented for a variety of architectures. For simplicity in the current description, the current embodiment will be described using a non-limiting implementation with InfiniBand (IB). IB is a known high-performance networking standard.
[0194] Conventional network access is done by the local CPU 102 writing a descriptor (command, command buffer) to local system memory (local DDR 104 ). Then the local CPU 102 informs the local NIC 106 (generally any IO device) that the descriptor is ready (work is ready for the local NIC 106 ). The local NIC 106 then will fetch the descriptor from local DDR 104 , perform an actual IO operation (for example, reading a remote memory location over the network, such as from remote DDR 124 ), and report completion of the descriptor. After the local NIC 106 has completed the task associated with the descriptor, the CPU needs to be aware of completion of the written descriptor. Typically, either the local CPU 102 polls on a completion status or the local CPU 102 is interrupted using an interrupt message. As described above, in this conventional process for network IO access, network access is done in an asynchronous manner and the local CPU 102 can continue working while the network access is done in the background.
[0195] The present embodiment facilitates network access of remote memory directly from a local instruction stream using conventional loads and stores. In other words, using existing, normal, default commands (such as LOAD and STORE) that have not been altered (unaltered, native commands) for additional and/or alternate operations. Analysis and research to implement embodiments of the present invention for accessing the network directly from the instruction stream (and specifically accessing remote memory), developed the following points that should be addressed for successful implementation:
How to convert a store to network write? How to convert a load to network read? If to allow speculative OOO access to the network, and how to handle? How to treat network errors if the operation (command) does not complete successfully (both loads and stores)? How to convert memory addressing to network addressing? How to handle memory ordering?
[0202] When considering the current problem, the above points are not obvious points to form a set of issues that need to be addressed. Additionally, there are detailed interrelations between some of the points. Thus, independent solutions cannot be combined to solve this problem. Conventional solutions for address decoding, tunneling a command over a network, handling OOO execution, and memory are not sufficient without additional innovative synergy described in the current description.
[0203] In the context of this description, the phrase “invoke management software” is used for simplicity to refer to a CPU transferring execution (flow control) from the current thread (software or application, of the local CPU) to a different (other, alternate, and/or new) thread (management software, other software, or application), thereby continuing with normal operation of the CPU. In other words, the CPU does not crash, instead possibly informing a user or a currently running software application of the event, rolling execution back to a recent checkpoint, stopping execution of the current thread, continuing execution of the current thread at a different point, and/or gracefully terminating operation of the system. Flow control can be transferred using conventional techniques such as a “Fault” or an “Interrupt”.
[0204] 1. Speculative OOO Access to the Network (Overlapping Reads from the Network)
[0205] Modern CPU architectures typically implement a deep pipeline, where instructions are executed out of order (OOO) and speculatively. A major benefit of this architecture is the fact that loads are executing speculatively such that misses to main memory are being overlapped. In conventional computers OOO (speculative access) for network access is not done. In other words, (well-written) conventional software will only try to access areas (such as memory) that the software has access to, that is, are pre-authorized for the software to access. In this conventional implementation, the software will not try to access an area that the software cannot reach, so this situation does not need to be handled by the software.
[0206] Viewing a network as yet another data source (similar to memory), allows for executing loads from the network OOO thereby pipelining network accesses, which can result in huge latency reduction, as compared to conventional network loads. This OOO implementation also implies that branch prediction while executing a sequence of commands can try to access areas that are not authorized (the software does not have access to). In other words, the micro-architecture may be performing actions that the user (software) does not want, possibly never wanted nor planned to authorize.
[0207] Due to branch miss-prediction, load accesses from the network may execute without the programmers intent. Speculative network loading can be made resilient to this branch miss-predication using the following implementation:
[0208] A. Loads from areas that the remote host has made available (accessible or permitted to be accessed) to the network will happen without any side effect. For example, on remote computer 120 , memory regions of remote DDR 124 that have been made available to other computers, such as local computer 100 .
[0209] B. Loads from areas that the remote host did not make available will be identified by paging tables in a remote NIC and will be dropped. For example, on remote computer 120 , memory regions of remote DDR 124 that have not been made available are identified by paging tables in remote NIC 126 . In conventional implementations, attempts to load from memory regions that are not available result in the LOAD request being dropped and notifying the originator of the LOAD request to not allow subsequent LOAD requests for this memory region. In contrast to this conventional operation, an innovative NACK response will be sent (from the remote NIC 126 ) to the requesting NIC (local NIC 106 ), and the network will continue operating unhindered. In other words, while the current LOAD request is dropped, the originator of the LOAD request may re-issue a LOAD request. This NACK is the result of branch mis-prediction and can be implemented in hardware (without invoking management software).
[0210] Stores do not execute speculatively, so an attempt to store to a remote memory that is not authorized (attempt for unauthorized access) results in a fatal error (for the network connection). In this case, a NACK will result in “Connection Termination” and invocation of management software (transfer of control of execution).
[0211] 2. Required Support from the CPU (how to Treat Network Errors if the Operation (Command) does not Complete Successfully)
[0212] Conventional LOADs and STOREs are executed by a CPU to local attached memory, for example by local CPU 102 to local DDR 104 . In modern computers, access to this local memory is reliable—so much so that unrecoverable errors are typically not handled, and typically results in an unrecoverable exception (such as known in the vernacular as the “blue screen of death”). For example, if a memory access returns data with an unrecoverable parity error.
[0213] In the current embodiment, a CPU can execute a LOAD command for remote memory—via a network that is unreliable in comparison to conventional access to local memory. For example, the local CPU 102 executing a LOAD via the network 110 for data stored on the remote DDR 124 . In this case, a network error can result in a load fault (failure to load the requested data/from remote DDR 124 ). In other words, the previously reliable local loading and storing is relatively unreliable for remote loading and storing Remote memory access using conventional loads and stores can be made resilient to network errors using implementations based on the following method:
[0214] A. Let a LOAD fault in case of network error.
In case of network error, the IO device (for example, the local NIC 106 ) will inform the CPU (for example, local CPU 102 ) that the LOAD will not complete. Informing can be done using known methods, for example, by using PCIe's completer abort encoding (assuming the typical modern connection of the NIC to the CPU via PCIe). Then the CPU will invoke management software to handle this event (LOAD fault). Additionally, faulting can be invoked implicitly by the CPU, for example by setting a timer every time a LOAD is executed, and if the timer expires before the LOAD completes, faulting (informing the CPU that the LOAD will not complete).
[0217] B. Stores need to be completed once entering the internal PCIe controller.
Typically, a CPU core 102 A is connected via an internal fabric 102 B to a PCIe internal controller 102 C in the CPU 102 . When the CPU core 102 A sends a STORE to the PCIe internal controller 102 C, the CPU core 102 A considers the STORE successful (due to the high reliability of internal connections). With the implementation of remote memory access, stores cannot be assumed to be successful, due to the relatively lower reliability of the network 110 . An asynchronous fault in case of a network error on store can be implemented. This STORE fault can notify the CPU core via a known technique such as using an interrupt or a mailbox. Similar to the above-described handling of LOAD faults, the CPU can invoke management software to handle the STORE fault, thus avoiding an unrecoverable exception that would stop CPU operation. The management software can, for example, continue operation of the CPU at an earlier checkpoint.
[0220] In a case where the CPU needs to wait for the STORE to complete, or operation would be improved by waiting for the success or failure of the STORE before continuing, after a STORE is executed a LOAD can be executed. Thus, before continuing the CPU core will wait for the LOAD to complete—which implies that the previous STORE has completed. Refer to the section elsewhere in this description on memory ordering and flushing stores.
[0221] C. Generate a network address, as described below.
[0222] 3. Implementation in the NIC
[0223] Modern computers typically use some sort of credit scheme to handle (throttle) access from the CPU to devices. For example from local CPU 102 via a PCIe bus (not shown) to local NIC 106 . PCIe flow control manages accesses to the NIC using posted credits (to throttle writes to the NIC) that will become network access) and non-posted (NP) credits (to throttle reading data from the NIC that will become a network access).
[0224] In the current implementation, an association from physical address to network address is implemented in the NIC. See the below section on generating a network address for more details. Responses can be handled using implementations based on the following method:
Read response:
Successful—The NIC can return a read response as a regular PCIe device (PCIe completion with the correct tag identifying the request). Failure—The NIC can return a response using the “Completer Abort” encoding indicating the device (local NIC on behalf of the remote NIC) is unable to send a response.
Write response:
Successful—no further actions required. Failure—Inform the CPU, for example by sending an interrupt o the CPU or writing to a specific mailbox.
[0231] Based on this description, one skilled in the art will be able to implement NIC communications with the CPU (bus communications).
[0232] 4. Generating a Network Address (Converting Memory Addressing to Network Addressing)
[0233] When performing a network access (for example, using conventional (normal, unaltered) commands such as LOAD or STORE), multiple addressing components are required, including:
[0234] A. The network location of the remote node (for example, IP address or InfiniBand's GID).
[0235] B. The memory/protection domain within the network address (for example, InfiniBand's memory region).
[0236] C. The actual address that needs to be accessed.
[0237] D. The length of the access (size/amount of memory to access).
[0238] In the context of this description, a NIC associated with a DDR from which data is requested is also referred to as a target NIC. In the current non-limiting example, local computer 100 with local NIC 106 sends a request to remote computer 120 where the request is received by remote NIC 126 , the target NIC. Using a protocol such as RDMA, when a target NIC receives a request for data, the NIC can access associated memory without CPU interaction. For example, a request is received at remote NIC 126 which accesses remote DDR 124 independently of (without interaction with) remote CPU 122 . In the InfiniBand specification a “memory region” is defined in the DDR that is accessible to remote users, while other portions of DDR memory, that are not in the memory region, are accessible only via the CPU (not directly accessible to remote users).
[0239] In conventional network access, a CPU uses multiple writes of data to local memory including some writes for network address information and some writes for the information to be transmitted. After the multiple writes are completed, then the CPU notifies the NIC that the data is ready (for pickup/transmission by the NIC). Then the NIC reads the data from local memory (comes to get the data), and then transmits (writes) the data to a target remote memory (remote location).
[0240] Refer now also to FIG. 2 , a simplified diagram of memories and usage. In the current figure, the number of bits used in an address is shown horizontally with wider boxes indicating more bits in the address. The number of addresses is shown vertically, with higher boxes indicating more addresses. For a clarifying example, refer to virtual address space 200 . Each address 200 A is M-bits, where M is an integer, for example 64, shown as width number of virtual address bits 200 B. The number of virtual addresses is shown as height 200 W. The number of addresses 200 W is determined by the number of bits 200 B in each address 200 A. In the current example using the number of virtual address bits 200 B=64 the number of addresses 200 W=2̂M, or 2̂64. Similarly shown is the number of physical address bits 204 B (for example 51 bits) and the number of actual DDR address bits (DDR size) 202 B (for example 39 bits).
[0241] A virtual memory has a virtual address space 200 . The size of the virtual memory is referred to in the field as the size of the virtual address space, virtual address size, or virtual address space. One skilled in the field will understand the usage of terms from the context of the discussion. Space for virtual addressing is typically limited by the architecture to the system. For example, in x86 and ARMv8 the virtual address space is limited to 64 bits (2̂64 addresses). Physical DDR (such as local DDR 104 ) has a DDR size 202 that is typically smaller than the size of the virtual address space 200 . Dashed horizontal line 202 S corresponds to the DDR size 202 . Addresses below the dashed line 202 S are below, or within the DDR size 202 . Addresses above, or on top of the dashed line 202 S are more than, out of, or beyond the range of the DDR size 202 . Physical address space 204 is the physical space on the CPU's bus for accessing actual DDR. The physical address space 204 that is above the DDR size 202 is shown as forwarded region 214 . Typically, the virtual address space is larger than the DDR size and larger than the physical address space 204 . Typically, the physical address space 204 is larger than the DDR size 202 . Forwarded region 214 is interpreted 206 by the NIC to provide network address information. The forwarded region has two parts: a network address index 226 , and a remote virtual address 216 . There is a configurable division (dotted vertical line) 236 between the network address index 226 and the remote virtual address 216 . For example, if physical address space 204 has 51 physical address bits ( 204 B=51) and access is desired for (up to) 2̂10 different network locations, the configurable division 236 will be at bit 41 . Bits 51 : 42 will denote the network address index 226 and the remaining 41 bits 41 : 0 can be used for the remote virtual address 216 .
[0242] In the current embodiment, descriptors, corresponding to commands, are first written to memory, later fetched, and used by a NIC. For example, written by the local CPU 102 to the local DDR 104 to be used by the local NIC 106 . This first writing is to virtual memory having a virtual address space 200 . However, the physical address space 204 used with the NIC is smaller than the virtual address space 200 ( 204 B< 200 B).
[0243] The current embodiment features a single store of data from the CPU for the NIC, in contrast to conventional network access that requires multiple writes of data to local memory. One issue that needs to be handled for the current embodiment is: how can the address bits (physical address bits 204 B) be used to relay all of the data required for network access (transmission and receipt)? To handle this issue, the data can be written to a memory location, but now a memory location directly in the NIC. Then the NIC uses the remote address location to copy the data from the NIC to the remote address location (remote memory location). This is shown by the DDR size 202 being smaller than the size of the virtual address space 200 . For example, modern computers might implement 64 bits of virtual memory, but only can use about 39 bits for actual DDR physical addresses.
[0244] In addition, when converting memory addressing to network addressing, additional information is required, such as described in the above list (memory domain, actual address, length, etc.). A solution to passing the required information using a limited number of bits is based on using the following method:
[0245] A. An existing paging mechanism (for example TLB) can be used to map a region of the virtual address space 200 to the network (via physical address space 204 ). This region of the virtual address space is shown as forwarded region 214 . In other words, the TLB in the local CPU 102 converts a virtual address specified by the command to a physical address, and then the physical address is transferred to the local NIC 106 . An access to the forwarded region 214 will result in a physical address which is beyond the DDR size 202 (above the top of the DDR address space 202 S) on the system.
[0246] B. When the NIC sees an access request with a pre-determined physical address bit set (corresponding to an address in forwarded region 214 ), the NIC re-interprets 206 the bits of the address (from the forwarded region 214 , not as a single address but) as two parts (pieces of information):
I. a network address index 226 , and II. a remote virtual address 216 .
[0249] In RDMA, a network access requires the following information:
Which network node to access, Which memory region within the node, and An offset within the memory region.
[0253] The first two values are extracted from the table accessed using the network address index (entries 326 ). The network address index 226 is used to access entries 302 in a network connection table 300 , described below to provide at least a portion of network access information such as which network node to access and which memory region within the node. The remote virtual address 216 can be used as the offset within the memory region of the remote memory. A length (of the memory to be accessed) can be given as part of the request on the PCIe bus from the local CPU to the local NIC.
[0254] A division between the network address index 226 and the remote virtual address index 216 is preferably configurable (shown as the configurable division 236 ). In other words, how many bits should be used for the network address index 226 and how many bits should be used for the remote virtual address index 216 . For example, if 51 bits are used for each physical address and local computer 100 needs to communicate with less than 1023 remote computers ( 120 , 130 , etc.), then 10 bits can be used for the network address index 226 and the remaining 41 bits can be used for the remote virtual address 216 .
[0255] C. Refer now also to FIG. 3 , a sketch of an exemplary network connection table. The NIC will use the network address index 226 (determined as described above) to access a network connection table 300 . The network connection table 300 is typically prepared ahead of time (before operational use) and contains information needed for the local computer 100 (local CPU 102 ) to communicate with remote computers. The network connection table can live in the computer's main memory and be cached in the NIC, or can reside in the NIC's internal storage. Each network address index 226 refers to an entry in the network connection table 300 . For example, network address index “INDEX A” 326 A 1 corresponds to entry “ENTRY A” 326 A 2 . Similarly, network address index “INDEX B” 326 B 1 corresponds to entry “ENTRY B” 326 B 2 , and in general, network address index “INDEX N” 326 N 1 corresponds to entry “ENTRY N” 326 N 2 . Each entry includes information and/or pointers sufficient for the local computer 100 to communicate with remote computers. Obviously, the size of network connection table 300 will be determined by the number of network address indexes and amount of information (size/number of bits) needed for each entry 302 . Each entry 302 describes the network connection for one target (remote computer). For example, an entry can include:
[0256] Destination local identifier (LID)
[0257] Destination GID
[0258] Destination Queue Pair
[0259] Memory Key (memory region)
[0260] The NIC can send a network packet to the network destination using the remote virtual address 216 extracted from the address bits, and the entry 302 information based on the network address index 226 as was originally requested by the CPU. For example, the local NIC 106 accesses the network connection table 300 based on INDEX A 326 A 1 and uses corresponding ENTRY A 326 A 2 information to communicate with a memory region on remote DDR 124 . Optionally, the process of network address generation can be virtualized by a hypervisor.
[0261] Since the division between network address and virtual address is configurable (the configurable division 236 ) the current architecture can support multiple configurations. For example:
Fewer remote machines (less bits needed for the network address indexes 226 ), each with high amount of memory (relatively more bits used for the remote virtual address 216 ). More remote machines (more bits needed for the network address indexes 226 ), each with less memory (relatively fewer bits used for the remote virtual address 216 ) attached to each of the remote machines.
[0264] Alternatively, if the forwarding region 214 includes enough bits (number of physical address bits 204 B) to encode all of the required data for network access, then instead of extracting the network access fields from the network connection table 300 the data can be directly encoded in the address bits of the forwarded region 214 . For example, the InfiniBand “Send” operation does not require a remote virtual address 216 (functions without explicitly specifying a remote virtual address 216 ) so the remote virtual address 216 field is not required and all of the physical address bits 204 B can be used to encode network access information, such as:
[0265] Destination LID,
[0266] Destination QP, and
[0267] Solicited event.
[0268] Alternatively, if the target NIC (for example remote NIC 126 ) handles the remote virtual address 216 then the remote virtual address 216 is not needed in the address interpretation 206 and all of the physical address bits 204 B can be used as the network address index 226 to reference the network connection table 300 . In this case, the configurable division 236 can be considered to be 0 (zero).
[0269] 5. Memory Ordering:
[0270] A memory ordering suitable for implementing the current embodiment is now described. In general, memory ordering can be considered a definition of use from a system to a user of the system. In other words, an architecture (micro-architecture) defining how a user sees memory access. General definitions and use of strongly ordered and weakly ordered memory implementations are known in the art, and will not be further discussed. In order to support the current embodiment of network access of remote memory directly from a local instruction stream using conventional loads and stores, several variations of memory ordering semantics can be implemented. A non-limiting example of a preferred implementation includes the following semantics:
[0271] A. Loads are weakly ordered (as implied from the InfiniBand specification).
[0272] B. Stores to a single network destination may be either weakly or strongly ordered (thus an implementation may choose to reorder stores internally)—both options can be supported.
[0273] C. Stores to different (at least two) network destinations are weakly ordered.
[0274] D. Loads from a given network destination will guarantee all pending stores to the given network destination memory are completed, as in the current InfiniB and memory ordering definition. In PCI terms, loads will keep flushing stores. In other words, a LOAD command is a barrier to all STORE commands—when a LOAD command is issued, all previously issued STORE commands are completed prior to the LOAD command executing.
[0275] Refer now to FIG. 4 , a flowchart of a method of loading data and FIG. 5 , a flowchart of a method of storing data. In general, the current methods can be performed by a processing system containing one or more processors configured to execute steps of the current methods. In particular, processors such as CPUs (local CPU 102 ) and NICs (local NIC 106 ) can perform network access of data in remote memories (remote DDR 124 ). The use of specific elements for simplicity and clarity does not limit the scope of the methods of this invention.
[0276] A method for accessing data, in particular for loading data from the remote DDR 124 to the local CPU 102 (or to the local DDR 104 ), begins with the local CPU 102 issuing (block 402 ) a LOAD command. The LOAD command includes at least a virtual address on the local computer 100 . The local NIC 106 derives (block 410 ) network access information based on a physical address converted from the virtual address. The network access information includes one or more references to the remote memory (remote DDR). The one or more references to the remote memory are used to check (block 422 ) if access is allowed to the remote memory 124 . Typically the remote NIC 126 implements the check (block 422 ) if access to remote memory is allowed.
[0277] If access is denied (not allowed) to the remote memory 124 then a NACK (block 436 ) is used to notify the local CPU 102 the LOAD command failed and the local CPU 102 invokes management software (block 438 ). If access is allowed to the remote memory 124 then the remote NIC 126 attempts (block 424 ) to load data from the remote memory 124 .
[0278] If (block 426 ) the attempt to load data (block 424 ) is successful (does not fail), the data is loaded from the remote memory 124 and then returned (block 428 ) to the local CPU 102 (to the originator of the load request). If the attempt is not successful (fails), then the local CPU 102 is notified (block 434 ) the LOAD command failed, and management software is invoked (block 438 ) to handle failure of the attempt. Optionally, after the local CPU 102 issues (block 402 ) a LOAD command, a load timer can be set (block 404 ). If the load timer expires before the data is returned to the local CPU 102 then the local CPU 102 is notified (block 434 ) the LOAD command failed, and management software is invoked (block 438 ) to handle failure (timeout) of the LOAD command.
[0279] Network access information can be derived by various methods as described elsewhere in this document. Optionally, deriving (block 410 ) network access information includes translating (block 412 ) the virtual address 200 to a physical address 204 . If (block 414 ) a network connection table 300 is being used, the physical address 204 is parsed for a network address index 226 . The network address index 226 is then used to access (block 418 ) an entry 302 in the network connection table 300 and retrieve at least a portion of the network access information (based on the network address index). The physical address 204 can also be parsed for (to provide) a remote virtual address 216 portion of the network access information.
[0280] Optionally, deriving (block 410 ) network access information includes translating (block 412 ) the virtual address 200 to a physical address 204 . If (block 414 ) a network connection table 300 is not being used, the forwarded region can be used (block 416 ) to provide at least a portion of the network access information. Optionally, the physical address can be used to provide all of the network access information required for the current command. In other words, network access information can be derived and/or provided without (independent of) the network connection table 300 . For example, the physical address 204 can be parsed for at least a portion of the network access information.
[0281] Optionally, after the step of deriving (block 410 ) network access information the method waits (block 420 ) for any previously issued STORE commands to the remote memory 124 to be completed prior to continuing with the step of checking (block 422 ). Waiting (block 420 ) can be done either on the local NIC 106 or the remote NIC 126 . Typically waiting (block 420 ) is done on the remote NIC 126 . In general, blocks 402 through 418 are implemented in the local computer 100 , and blocks 420 through 430 are implemented in the remote computer 120 . Optionally, prior to the step of invoking (block 434 ) management software the method (local NIC 106 ) can repeat the attempt (block 424 ) to load data from the remote memory 124 .
[0282] Refer again to FIG. 5 . Similar to the above-described method for loading data, a method for storing data to the remote DDR 124 from the local CPU 102 (or from local DDR 104 ), begins with the local CPU 102 issuing (block 502 ) a STORE command. The STORE command includes at least a virtual address on the local computer 100 . The local NIC 106 derives (block 510 ) network access information based on a physical address converted from the virtual address. The one or more references to the remote memory are used to check (block 522 ) if access is allowed to the remote memory 124 . Typically the remote NIC 126 implements the check (block 522 ) if access to remote memory is allowed.
[0283] As described above, if access is denied (not allowed) to the remote memory 124 then a NACK (block 536 ) is used to notify the local CPU 102 the STORE command failed. Then management software will be invoked (block 538 ) to handle the connection termination and transfer of control of execution. If access is allowed to the remote memory 124 then the remote NIC 126 attempts (block 524 ) to store data to the remote memory 124 .
[0284] If (block 526 ) the attempt to store data (block 524 ) is successful (does not fail), the data is stored to the remote memory 124 and then the local CPU 102 continues (block 528 ) with normal operation (execution of the next instruction). If the attempt is not successful (fails), then the local CPU 102 is notified (block 534 ) the STORE command failed and management software is invoked (block 538 ) to handle failure of the attempt,
[0285] Similar to block 410 , network access information can be derived by various methods as described elsewhere in this document. Optionally, deriving (block 510 ) network access information includes translating (block 512 ) the virtual address 200 to a physical address 204 . If (block 514 ) a network connection table 300 is being used, the physical address 204 is parsed for a network address index 226 . The network address index 226 is then used to access (block 518 ) an entry 302 in the network connection table 300 and retrieve at least a portion of the network access information (based on the network address index). The physical address 204 can also be parsed for (to provide) a remote virtual address 216 portion of the network access information.
[0286] Optionally, deriving (block 510 ) network access information includes translating (block 512 ) the virtual address 200 to a physical address 204 . If (block 514 ) a network connection table 300 is not being used, the physical address 204 can be parsed for at least a portion of the network access information.
[0287] Optionally, after the step of deriving (block 510 ) network access information, if the remote memory 124 is strongly ordered, then the NIC (preferably the remote NIC 126 but optionally the local NIC 106 ) waits for any previously issued STORE commands to the remote memory 124 to be completed, prior to continuing with the step of checking (block 522 ) if access is allowed to the remote memory 124 .
[0288] Optionally, prior to the step of notifying (block 534 ) the method (the local NIC 106 or the remote NIC 126 ) can repeat the attempt (block 532 ) to store data to the remote memory 124 .
[0289] FIG. 6 is a high-level partial block diagram of an exemplary system 600 configured to implement a method of the present invention. System (processing system) 600 includes a processor 602 (one or more) and four exemplary memory devices: a RAM 604 , a boot ROM 606 , a mass storage device (hard disk) 608 , and a flash memory 610 , all communicating via a common bus 612 . As is known in the art, processing and memory can include any computer readable medium storing software and/or firmware and/or any hardware element(s) including but not limited to field programmable logic array (FPLA) element(s), hard-wired logic element(s), field programmable gate array (FPGA) element(s), and application-specific integrated circuit (ASIC) element(s). Any instruction set architecture may be used in processor 602 including but not limited to reduced instruction set computer (RISC) architecture and/or complex instruction set computer (CISC) architecture. A module (processing module) 614 is shown on mass storage 608 , but as will be obvious to one skilled in the art, could be located on any of the memory devices.
[0290] Mass storage device 608 is a non-limiting example of a computer-readable storage medium bearing computer-readable code for implementing the data storage and retrieval (descriptor execution, LOAD and STORE) methodology described herein. Other examples of such computer-readable storage media include read-only memories such as CDs bearing such code.
[0291] System 600 may have an operating system stored on the memory devices, the ROM may include boot code for the system, and the processor may be configured for executing the boot code to load the operating system to RAM 604 , executing the operating system to copy computer-readable code to RAM 604 and execute the code.
[0292] Network connection 620 provides communications to and from system 600 . Typically, a single network connection provides one or more links, including virtual connections, to other devices on local and/or remote networks. Alternatively, system 600 can include more than one network connection (not shown), each network connection providing one or more links to other devices and/or networks.
[0293] System 600 can be implemented as a server or client respectively connected through a network to a client or server.
[0294] Referring again to FIG. 1 , system 600 can implement a computer such as local computer 100 , processor 602 can implement a CPU such as local CPU 102 , RAM 604 can implement DDR such as local DDR 104 , and network connection 620 can implement NICs such as local NIC 106 .
[0295] Note that a variety of implementations for modules and processing are possible, depending on the application. Modules are preferably implemented in software, but can also be implemented in hardware and firmware, on a single processor or distributed processors, at one or more locations. The above-described module functions can be combined and implemented as fewer modules or separated into sub-functions and implemented as a larger number of modules. Based on the above description, one skilled in the art will be able to design an implementation for a specific application.
[0296] Note that the above-described examples, numbers used, and exemplary calculations are to assist in the description of this embodiment. Inadvertent typographical errors, mathematical errors, and/or the use of simplified calculations do not detract from the utility and basic advantages of the invention.
[0297] To the extent that the appended claims have been drafted without multiple dependencies, this has been done only to accommodate formal requirements in jurisdictions that do not allow such multiple dependencies. Note that all possible combinations of features that would be implied by rendering the claims multiply dependent are explicitly envisaged and should be considered part of the invention.
[0298] It will be appreciated that the above descriptions are intended only to serve as examples, and that many other embodiments are possible within the scope of the present invention as defined in the appended claims.
|
A method for network access of remote memory directly from a local instruction stream using conventional loads and stores. In cases where network IO access (a network phase) cannot overlap a compute phase, a direct network access from the instruction stream greatly decreases latency in CPU processing. The network is treated as yet another memory that can be directly read from, or written to, by the CPU. Network access can be done directly from the instruction stream using regular loads and stores. Example scenarios where synchronous network access can be beneficial are SHMEM (symmetric hierarchical memory access) usages (where the program directly reads/writes remote memory), and scenarios where part of system memory (for example DDR) can reside over a network and made accessible by demand to different CPUs.
| 6
|
CROSS REFERENCE TO RELATED APPLICATIONS
This is a continuation of U.S. patent application Ser. No. 09/384,451, filed Aug. 27, 1999, now U.S. Pat. No. 6,754,490 and incorporated herein in its entirety.
FIELD OF THE INVENTION
This invention relates to the accessing of different and distinct cellular/wireless (C/W) telephone network/systems with a particular cellular/wireless (C/W) telephone instrument not necessarily adapted to operation in any one of the particular systems. Access is consummated by means of adapting an interface with the system requirements through adaptation of processing procedures of the cellular/wireless network/system alone. In particular the network adaptation process granting access and functionality is attuned for a C/W telephone instrument in response to entries transmitted to the network system from the C/W telephone instrument.
BACKGROUND OF THE INVENTION
A normal cellular/wireless (C/W) telephone instrument is designed to operate only with a particular cellular/wireless (C/W) communication network/system and as such is designed in accord with interface requirements specific to the network/system sought to be accessed. Such requirements include modulation schemes, format, signal structure, link protocols, signal waveforms and signal frequencies. These are all unique to each network/system and a cellular/wireless telephone instrument designed to work in one cellular/wireless network/system will not function in another C/W network/system having a different operating environment.
Traveling subscribers, particularly international travelers are impacted by inoperability of cellular/wireless telephone instruments in a different C/W system, particularly in international travel. In some instances a cellular/wireless telephone instrument is designed to be operative in more than one cellular/wireless/network/system. An example is cellular/cordless telephone instruments which operate in either a cellular or cordless medium. Such a telephone instrument however carries a large overhead of redundant design and feature amenities. As a result such a telephone instrument is expensive and may even be unwieldy in size in order to support all the various features so that the user may properly interact with the different systems.
Several prior efforts have been made to accommodate the various dilemma of the traveling telephone user. A common dilemma is the different operating parameters and operating characteristics of C/W telephone instruments associated with different C/W networks. One solution to these dilemma has been to provide a “universal” telephone instrument associated with a network/system that accepts a database encoded on a card (e.g., a smartcard) to control and/or modify telephone instrument operations. This causes the telephone instrument to operate in a manner identical with operations that the user is used to in his home network/system.
Universal telephone instruments, for example, are associated with a particular network but can be programmed to mimic responses of a telephone instrument associated with a different telephone network. They often include a smartcard reader to provide a database for such purpose. The foreign user inserts a smartcard into the telephone instrument. It includes all the data as to how the telephone instrument should appear to the user, what language to use, how it should respond and how it is operated in order to make it conform to a telephone instrument that the user is accustomed to. A database of this operational information may be contained solely on the smartcard or it may be included in a database located in the universal telephone instrument. Such a technique is disclosed in U.S. Pat. No. 5,878,124, which also provides an overlay device to the telephone instrument to provide the home appearance and functions that the user is accustomed to. In this arrangement the universal telephone instrument is a specialized telephone instrument which must be provided by the system the user is attempting to access. It does not concern a cellular/wireless telephone instrument, which within the cellular/wireless network/system is personally assigned to the user and likely to be used in another system.
Personalized features of a home base network/system are provided to the traveling telephone user in using a telephone instrument in another network/system with a different exchange in which the user enters a code and a personal identification number (PIN) to any telephone instrument of a foreign system. The personalized features are retrieved from a national database, as described in U.S. Pat. No. 4,899,373, and used to provide the telephone user with his specialized features. In another aspect the features are encoded on a card which features are conveyed to the network database. Unfortunately from the point of view of a cellular/wireless telephone instrument the process does not make a C/W telephone instrument operative in a foreign network/system as opposed to providing familiar home type features to the user of a telephone instrument of a different system from the home system.
Various approaches have been proposed for making a foreign telephone user feel familiar with local telephone operations by providing features and functions such as they are accustomed to at home, but all have involved using a special “universal” telephone instrument or are limited to providing system features such as are available to a user in his home network/system. Yet to be addressed is the ability of the visitor to the system to use his own C/W telephone instrument in a new different C/W network/system. This is particularly critical in the instance of cellular/wireless, since the user prefers to use his/her own C/W telephone instrument, which he/she is accustomed to.
SUMMARY OF THE INVENTION
A cellular/wireless (C/W) foreign subscriber/user, when roaming beyond a local cellular/wireless (C/W) network/system, compatible with his/her telephone instrument, is enabled to use her/his own cellular/wireless telephone instrument by entry of a code and a PIN into the foreign network/system desired to be used. The local serving C/W network/system algorithmically responds to the code and PIN by changing signal processing characteristics of the radio equipment of the network/system to accommodate operation of the subscriber's cellular/wireless telephone instrument with the foreign network/system desired to be used.
In a particular embodiment of the invention, the foreign user has been assigned an InterSystem Roamer Access Code Number (IRACN) and Personal Identification Number (PIN). This permits use of the C/W network/system upon application, followed by validation, to a C/W network/system designed to accommodate foreign subscriber telephone instruments. The radio communication system responds to the transmitted IRACN and PIN by adjusting its interfacing and signal processing equipment to interact with the cellular/wireless telephone instrument of the subscriber.
In operation the local C/W network/system receives the IRACN and PIN and upon validation detects and characterizes the signals transmitted by the subscriber's C/W telephone instrument and adjusts the receiver of the radio system to change the received signal to a format and character adjusted to the network/system operation requirements. Once identity and authentication is established the call may proceed normally. Reply downlink signals are changed to a format and character acceptable to the C/W telephone instrument prior to transmission.
In a specific embodiment, a foreign C/W subscriber requests service in the local C/W network/system, by using the cellular/wireless access channel and transmits the PIN and the IRACN to the central office (CO) of the local C/W network/system. The received signal is detected and characterized. A determination is made if it is a foreign or US (local) C/W service request, depending upon the C/W telephone instrument used. For US based C/W telephone instrument calls the process of registration and authentication proceeds as normal. For calls made using a foreign C/W telephone instrument, the received signal is characterized to determine if it is a GSM, TDMA, FDMA, PCS, etc. The signal is channeled to the appropriate radio system for that particular modulation and processing scheme. The uplink signal is frequency translated, and demodulated; it is decrypted and decoded, protocol converted, and deframed; it is subsequently structured and framed, modulated, frequency translated and adapted to NA (North American)-digital or analog radio system requirements in the local Central Office (CO).
Registration and authentication is initially performed to validate the subscriber PIN, IRACN and his/her identity. Transmitters of Invalid PIN and IRACN numbers are asked to check the numbers and try again. Valid subscriber entries are given a request acknowledgement to access the network and start transmitting. For a US based call, with a C/W telephone instrument designed for the local C/W network/system, registration and authentication follows normal operating procedure.
DESCRIPTION OF THE DRAWING
FIG. 1 is a block diagram illustrating the process of adapting the local cellular/wireless network/system to process signals supplied from a foreign non-system cellular/wireless telephone instrument;
FIG. 2 is a block diagram illustrating an algorithmic framing process in adapting radio signals to allow the local network/system to provide service to a foreign cellular/wireless telephone instrument;
FIG. 3 is a schematic portrayal of frames structured by the process of FIG. 2 ;
FIG. 4 is a block schematic of a radio system of a cellular/wireless telephone network/system incorporating the principles of the invention; and
FIG. 5 is a schematic of a signal processor used in the circuitry of FIG. 4 .
DETAILED DESCRIPTION
An algorithmic process for adapting a foreign cellular/wireless telephone instrument for operation with a new/local cellular/wireless telephone network/system is shown in the flow chart of FIG. 1 . A subscriber traveling within an area other than his/her home/foreign area wishes to use a cellular/wireless telephone instrument in a new area serviced by a local cellular/wireless telephone network/system different in operation and location from his/her normal home/foreign area. The process is initiated with a service request as indicated in block 101 . The service request is transmitted over the access channel used by cellular/wireless network/systems for this purpose. The receiving network/system accepts/detects the signal and as indicated in the block 103 detects and characterizes the request signal as to its format, frequency, modulation, framing, etc. Whether the request for service is from a local or foreign cellular/wireless telephone instrument (i.e., foreign vs. US) is determined as indicated by decision block 105 . If the request is from a US/local C/W telephone instrument the flow proceeds to process registration, authentication for US/local processing as indicated in decision block 107 .
If the request is from a foreign cellular/wireless telephone instrument, as determined by the instructions of decision block 105 , the flow proceeds to determine the type of modulation, as per decision block 111 , that the requesting foreign cellular/wireless telephone instrument is using. For illustrative purposes three types of modulation are illustrated although it is to be understood that the invention is not limited to the three designated modulation types. If the detected modulation scheme is time division modulation (i.e., TDMA,GSM) the flow process proceeds all the way through blocks 113 a , 115 a , 117 a and 119 a . The system processing frequency is adjusted to the signal frequency and the demodulation scheme of the transmitting telephone instrument, as per block 113 a . The protocol of conversion is adjusted as per block 115 a to accommodate the transmitting telephone instrument. Appropriate formatting and structuring is performed in accord with the instructions of block 117 a and frequency translation of the signal to the network/system values is performed as per block 119 a . A Mux/Demux process 121 (multiplexer and demultiplexer) provides bi-directional connection between the appropriate processing circuitry and the requesting telephone instrument.
The Mux/Demux process 121 is coupled to a decision block 107 concerned with registration and authentication. If the codes (IIRACN and PIN) entered are approved the flow proceeds to call processing as shown in the block 109 . The requesting telephone instrument may now communicate through the network/system. The process flow (b and c) for amps and PCS is similar to that for TDMA/GSM and hence it is not necessary to discuss.
If the origin of the calling telephone instrument is unknown to the network/system. The decision process of block 105 the flow returns to the state of block 101 .
When, as discussed above with reference to FIG. 1 , an International Roamers Access Radio System (IRARS) participant requests service, the received signal frequency is determined, and the IRACN and PIN are verified for validity. The signal undergoes frequency adjustment, demodulation and carrier recovery, decoded and de-interleaved. It is deframed; the deframing process removes all the overhead bits by the Decision circuitry and stores it in the RAM. Only the information bits remain. Protocol conversion takes place, after bandwidth/time slot adjustment, channel spacing, and rate adjustment are made in the processor. The outputs of the protocol converter, as discussed below, are looped back to the modulator where signal is modulated with pi/4DQPSK, to adapt to NA-TDMA type modulation. The processor sends the modulated signal to the framer where the information is structured and adapted to NA-TDMA. It is encoded and interleaved such that the final bit count and the bit pattern is equal to 1944 bits (972 symbols) per frame and is similar to the NA-TDMA frame structure.
FIG. 2 shows the framing algorithm to accomplish this structuring, and the bit patterns for the framing transformation are shown in the diagram of FIG. 3 . For example, if the GSM system is chosen for processing, FIG. 2 shows the transformation algorithm for this modulation scheme. The invention is not limited to GSM framing and framing for other modulation schemes is included within the scope of the invention.
Framing processing starts with the number of bits N of the incoming frame being determined as indicated in block 201 . If the number of bits N is less than 1944, as per decision block 203 , the process proceeds to a block 205 whose instruction is to add the difference between the number of bits and 1944. If the number of bits now equals 1944 as per decision block 209 the process proceeds to the framing process of block 217 from whence the frame is transmitted to an encoder.
If the number of bits N is not less than 1944 as per decision block 204 a subsequent decision (decision block 207 ) determines if the value of N exceeds 1944. If it doesn't then at this point in the process N should equal 1944, which is what decision block 211 , determines. If n=1944 the process proceeds to framing step of block 217 and if not the process returns to the start block 201 .
If the decision of block 207 determines that N exceeds 1944 a subsequent instruction of block 213 subtracts the difference from N. N should now equal 1944 and this is checked in decision block 215 . If N=1944 the process proceeds to the framing of block 217 and if not the process returns to block 213 to repeat the subtraction step of block 213 .
The results of the framing process are detailed graphically in the FIG. 3 diagram. The GSM frame 301 is shown comprising a total of 1248 bits with 8 slots each slot including 156 bits and a time duration of 4.615 ms. The content of each GSM slot 303 includes three tail bits 303 a ; fifty eight information bits 303 c ; a training sequence 303 e of twenty six bits; fifty eight more information bits 303 g ; three tail bits 303 h and a guard section 303 j of eight bits. Each slot 303 has a total of 156 bits for a duration of 0.577 ms.
The frame 305 in process has a bit pattern in each slot in which all the overhead bits except the tail bits have been removed. This leaves 120 bits in each slot or a total of 960 bits per frame. The in-process frame is now adjusted to adapt the signal to the NA-TDMA format and structure to be ready for encoding and interleaving.
The NA-TDMA frame 307 has 1944 bits or 972 symbols in which each slot 309 had 324 bits at a rate of 48.6 kbps or 6.67 ms/slot. This is the NA-TDMA frame and down link structure processed by the network/system.
When the subscriber is receiving signals the bit pattern is adapted to GSM standards, shown by frame 309 , which the subscriber's cellular/wireless telephone instrument is able to receive. While GSM NA-TDMA transition is shown the invention is not so limited. Other transitions fall within the purview of the invention.
A radio transceiver used in the network/system, which illustrates the invention, is shown in the FIG. 4 and includes a RF front end; an IF section and a Baseband section. Uplink signals are received at a receiving antenna 401 and are coupled to a bandpass filter (BPF) 403 .
A frequency detector is coupled to the input of BPF 403 and detects the frequency of the uplink signal as well as the type of system in use (i.e., GSM, PCS, FDMA, etc.) and IRARS and PIN validity. This frequency determination and other information determined is coupled to the IRARS processor 501 discussed below with reference to FIG. 4 .
The filtered signal output of BPF 403 is amplified in amplifier 405 and mixed in mixer 407 with the reference signal frequency of local oscillator 409 to achieve the IF signal. After further filtering and amplification the signal is bifurcated to form I (In-phase) and Q (Quadrature-phase) signals. The I and Q signals are applied to mixers 413 and 415 for demodulation and referencing by a second reference signal (by local oscillator 417 ) to achieve baseband frequency, respectively. The signal is further processed, to recover original signal information, in both paths by an A/D converter 419 to recover a digital signal format and in various processes the carrier is recovered 421 , and de-interleaved 423 , decoded 425 (to recover original information) and deframed 427 (to remove overhead bits). These signals are applied to the processor 501 discussed in reference to FIG. 5 . These signals are also processed in path 451 to adjust to signal characteristics of the local C/W network/system connected to lead 453 .
Downlink I and Q signals, as processed in processor 501 , are framed 431 , encoded 433 , interleaved 435 and converted from digital to analog format in D/A converter 437 . Framing reinserts the overhead bits and structures the packet into a suitable format. The signal is modulated in mixer 439 and upped to IF frequency in mixer 441 to produce a modulated IF signal for the front end. After filtering and amplification the signal is converted to RF, suitable for the foreign subscriber's telephone instrument, in mixer 443 amplified in amplifier 445 filtered by BPF 447 , for spectrum control, and applied to a transmitting antenna 449 .
Processing to adjust the various uplink and downlink signals to the requirements of the cellular/wireless network/system processing the calls to the requirements of the subscriber's instrument are performed by the processing circuitry 501 . Processor 501 accepts both I and Q incoming signals from the subscriber, on leads 502 and 503 , and in a pair of switches 504 and 505 selects subsequent circuit connections to (in the example) enable processing of GSM or NA-TDMA processing. Time slot control GBW (Gaussian Modulation Shift Keying BW) 541 applies a control signal to a GSM channel 514 or 516 and changes the time slots and framing of the GSM incoming signal. The I and Q signal has the rate appropriately adjusted in mixers 518 and 520 , respectively, in response to control signals provided by a variable rate generator 526 which is controlled by a processor 530 .
The same type process is used for NA-TDMA and other modulation schemes. This process is known to those skilled in the art and its implementation is not discussed.
A second channel is included to provide North American TDMA (NABW) control to a NA-TDMA channel 524 and 526 also under control of processor 530 , through time slot control 543 .
Outgoing signals (downlink) intended for the C/W telephone instrument of the foreign user are modulated to its operating requirements in mixers 551 and 552 and output on leads 561 and 562 to the radio output circuitry shown in the FIG. 4 .
Signals for C/W network/system processing are output on leads 571 and 572 .
|
A cellular/wireless foreign subscriber is enabled to use her/his own cellular/wireless telephone instrument in a local cellular/wireless (C/W) network/system by entry of a code and a PIN into the local network/system desired to be used. The local C/W network/system algorithmically responds to the code and PIN by changing characteristics of the radio equipment of the local C/W network/system to accommodate operation of the subscriber's cellular/wireless telephone instrument with the network/system desired to be used.
| 7
|
BACKGROUND OF THE INVENTION
1. Technical Field
This invention relates to an improved rope clamp of the smallest possible size and one in which the holding strength or efficiency is not dependent upon the skill of fabricating personnel, and, more particularly, to a rope clamp for the terminating end of a composite rope having a metallic core and an outer sheath of fibrous plastic material, or made from multi-layered plastic materials. Such composite rope normally has a multi-strand metallic core surrounded by one or more outer sheaths of fibrous plastic material comprising a lightweight line capable of carrying heavy loads, which rope is widely used by rescue workers, firemen and in various safety applications. The rope is also frequently used in certain military and marine applications, the rope being resistant to severing, chemicals, shock and the like, and is also resistant to destruction by high temperatures such as may be encountered in fires or explosions. The subject rope clamp may also be used with a rope comprised of several separately-braided layers of fibrous plastic materials without the multi-strand metallic core.
A primary purpose of this invention is to meet the military and commercial requirements for a rope end clamp, and which satisfies all of the following requirements for the termination of fibrous synthetic and composite synthetic ropes:
(1) The outer diameter being as near as possible to that of the rope.
(2) A rope clamp that will hold the full strength of the rope.
(3) A rope clamp whose holding strength is consistent and does not vary in large amount from one clamp to another.
(4) A rope clamp whose holding strength is not dependent upon the ability of assembly personnel.
The herein-disclosed embodiments of the subject rope clamp utilize a unique combination of wedging elements and proven assembly techniques for a new and unique design of outer swagged-type of rope end clamp.
2. Background Information
Previously, composite ropes fabricated of both metallic and plastic materials into multi-layered flexible lines have been well-known for use in survival-type situations as well as in mountaineering and other hazardous conditions. Their use in such hazardous conditions has been limited by their inherent nature such as in the event of fire or high-temperature applications. The nylon, polyester or other synthetic materials used in the manufacture of such ropes may melt or burn, or may be so severely weakened by heating that the rope becomes unsafe for further use. Such composite ropes having a metallic core are not easily knotted around stable fixtures and require an improved terminating end clamp to join the rope to a suitable fitting such as a clevis or other connecting member. U.S. Pat. No. 1,855,227 to Fiege discloses a single wedging plug employed in an inner conical recess to clamp a metallic cable to a clevis or turnbuckle. Such clamp is not applicable to use with a composite rope formed of different layered materials, such as one having a metallic core surrounded by plastic sheaths.
Composite ropes which are subjected to applications where they come into contact with rock outcropping or other sharp objects, such as in mountaineering or fire fighting, may be severed or partially severed since the synthetic plastic materials utilized in their outer construction are not highly resistant to chafing and severing. Further, if the outer plastic sheath be severed or partially severed, the multi-layer construction allows the individual outer layers to slip along the inner metallic core or move axially relative to one another making the line difficult to grasp or properly handle.
It is also known that exposure to chemicals can also degrade the rope and ultimately cause its failure. Ropes which have been subjected to such exposure are frequently discarded and not used further as a precautionary measure if subjected to any corrosive chemicals. This may be true where chemicals are found on the ground where the rope has been lying and been exposed to such chemicals.
A further disadvantage of conventional multi-layer composite rope, particularly when used in rescue and safety applications, is its elasticity. While a conventional rope experiences a certain degree of stretch when under load, undue elasticity of a composite rope may adversely affect various rescue and safety operations. The use of a metal cable core avoids the problem of line loss due to heat, fire and severing problems. Composite ropes or cables, due to their elasticity, are difficult to tie and otherwise manipulate due to their flexible but unwieldy nature. In most cases a knot cannot be safely tied in the cable which will cinch tightly enough on itself to hold and provide safe connection of the line and it is normally difficult to increase the diameter of the cable by doubling it to facilitate grasping of the cable due to weight and other considerations. When a metal cable is employed, its outer surface is frequently too slippery to be securely grasped presenting an unsafe condition and is sometimes too abrasive to be handled safely depending upon the used condition of the cable. Various types of knotting of the cable at its end to various metallic fittings has not been satisfactory since the metallic core and outer sheaths may slide axially with respect to one another resulting in an unsafe condition.
Previously, the fastening of cable ends together or the securing of a single composite cable end to a support has encountered considerable difficulty. Where a strong joint is required at the line end, where the rope is fully fabricated having a metallic core, the line in some cases has been welded to connecting members requiring the use of heating apparatus which is destructive of the sheath of plastic material. Various clamping devices have been utilized but such devices have been found to withstand only very limited strain and do not clamp both the metallic core and the outer plastic sheath by separate clamping elements.
Previously the most efficient method of terminating textile ropes has been the "hand splice". Such method relies on the ability and experience of the assembly personnel, has a large variation of holding efficiencies from one clamp to another, and does not provide a satisfactory termination for a synthetic fibrous rope having an internal metallic wire core. A chemically potted termination has a high holding efficiency but is dependent upon the assembly technique and is very large in size. The internal wedge of "Fiege" type clamp is strong, does not rely on assembly proficiency of the fabricating personnel, but is still relatively large in size. The "swagged" type of end clamp can not normally be employed on synthetic textile-type ropes as it can on wire ropes, since the textile or fibrous nature of the rope reduces in diameter with tensile loading and pulls out of a termination that relies on compressive loading alone to hold the rope.
Another type of end clamp for a composite rope has been disclosed in pending U.S. patent application Ser. No. 07/518,572 filed May 3, 1990 now U.S. Pat. No. 5,022,780 entitled "End Clamp for Textile Rope With a Metallic Core", which application is owned by the same common assignee as the present application.
SUMMARY OF THE INVENTION
It is an object of this invention to provide an improved end clamp for a lightweight, manipulatable readily-grasped composite line of relatively high strength for use by personnel such as firemen, rescue workers, mountaineers and others involved in hazardous, rescue or safety conditions. The clamp and its method of attachment may be used with a multi-layered composite rope comprised of several combined sheaths of plastic materials with or without a multi-strand central metallic core. The clamp is particularly useful with a static composite rope having very little stretch and which will withstand exposure to elevated temperatures, sharp objects, chemicals, sunlight or shock which do not produce failure in the rope or require its premature disposal. The clamp is relatively simple in construction and provides a pair of interlocking tapered metallic elements which may be quickly attached to a rope end to withstand an unusual amount of strain or loading equal to or greater than the actual breaking strength of the rope itself.
It is another object of this invention to provide a composite rope end clamp which is capable of securely retaining both the exterior braided or woven layers of plastic material as well as a multi-strand metallic core, both of which are separately restrained in permanently clamped durable relation and which are resistant to relative axial movement of the sheaths along the core and with respect to each other.
A more specific object of this invention is to provide an improved rope end clamp for a flexible composite line of several different types and a unique method of attachment to such lines which clamp employs a solid or hollow tapered plug member which is fitted within the interior of a hollow metallic sleeve, the latter of which is swagged into reformed tapered condition overlying the plug member. The hollow sleeve is capable of being joined to various types of conventional end fittings such as a clevis or hook and which end clamp is capable of withstanding substantial loads. The outer plastic sheaths and the metallic core are separately clamped by the plug member fitted within a cylindrical opening of the hollow metallic sleeve for separate retention of the outer sheaths and the central core, when present, to positively retain the different plastic and metallic materials and to prevent relative axial movement of the diverse materials which comprise the composite rope.
The present invention relates to a durable end clamp for a composite line and method of connection wherein the core is preferably formed of a heat-resistant substantially inelastic metallic cable core preferably having two separately interwoven fibrous plastic sheaths fitted tightly thereabout. The subject clamp is particularly useful in terminating the end of a composite line having an inner fiber sheath braided tightly about the core and an outer fiber sheath braided tightly about and adhered to the inner sheath. The core has a tensile strength sufficient to separately support the desired rate of loading of the rope. The inner and outer sheaths have a combined tensile strength frequently exceeding the tensile strength of the core and contain the core therewithin in such manner that upon breakage of the core under excessive loading, the sheath elements substantially eliminate backlash of the rope and still retain the load. The core has sufficient weight and strength to minimize backlash of the inner and outer sheaths upon subsequent breakage thereof. The composite rope with which the subject clamp is particularly useful is one which will support the rated load even if the inner and outer sheaths are melted or severed by fire, heat or contact with sharp objects, the subject clamp preventing separation of the line at or near its retained end regardless of the adverse conditions encountered.
The end clamp may also be employed with a composite rope comprised of only the two inner and outer sheath members both consisting of separately interwoven multi-strand synthetic fibers, as well as a composite rope having a heat-resistant metallic multi-strand cable core surrounded by the said inner and outer sheath members. The clamp has either a solid or hollow tapered plug member, the latter being used with rope having the metallic cable core for its positive retention therewithin. The plug member is inserted into unfrayed fibers of the inner sheath with frayed fibers of both sheath members extending therearound which are thermally fused into a ball-like mass behind the plug exterior end. The purpose of fusing the fibers behind the plug is to prevent the fibers from slipping past the plug when tension is applied to the rope. A hollow sleeve member is placed over the plug member and the fused ball-like mass and then swagged around the plug member to form complementally tapering concentric surfaces, which permit the tapered plug to wedge the fibers against the tapered inner surface of the sleeve with increasing holding compression as the rope tension increases, the sleeve member then being connected to a rigid metallic conventional cable end fitting.
BRIEF DESCRIPTION OF THE DRAWINGS
A preferred embodiment of the invention, illustrative of the best mode in which the inventor has contemplated applying the principles: set forth in the following description, is set forth in the drawings, and is particularly and distinctly pointed out and set forth in the appended claims.
FIG. 1 is an exploded view of one type of composite rope comprised of only inner and outer sheaths of braided synthetic plastic fibers, and the several elements which comprise the rope end clamp;
FIG. 2 is a vertical sectional view of a solid tapered plug member utilized in a first embodiment of the rope end clamp and method;
FIG. 2A is a view similar to FIG. 2 of a hollow tapered plug member utilized in a second embodiment of the rope end clamp and method;
FIG. 3 is a vertical sectional view of a hollow sleeve member for use in combination with both types of plug members shown in FIGS. 2 and 2A;
FIG. 4 is a side elevational view of the composite rope of the type shown in FIG. 1 with the several sheaths of plastic fibers in frayed condition and with the solid plug member as shown in FIG. 2 inserted therewithin;
FIG. 5 is a view similar to FIG. 4 with the frayed fibers thermally fused around said solid plug member;
FIG. 6 is a view similar to FIG. 5 partially in vertical section showing a hollow sleeve member initially placed over and around said solid plug member and the fused fibers;
FIG. 7 is a view similar to FIG. 6 after the hollow sleeve member is swagged around said plug member and the fused fibers;
FIG. 8 is an exploded view similar to FIG. 1 of a second type of composite rope having a metallic cable core, a hollow tapered plug member and hollow sleeve member adapted to attachment to the end of said composite rope;
FIG. 9 is a side elevational view similar to FIG. 4 with the plastic fibers in frayed condition and the hollow plug member engaging the metallic cable core;
FIG. 10 is a view similar to FIG. 6 partially in vertical section showing the hollow tapered plug member engaging the metallic core and the hollow sleeve member initially placed over and around said hollow plug member and the fused fibers; and
FIG. 11 is a view similar to FIG. 10 after the hollow sleeve member is swagged around said hollow plug member and the fused fibers.
Similar numerals refer to similar parts and elements throughout the drawings.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A common first type of composite rope with which the subject invention is associated is one in which the rope is comprised of multiple sheaths of similar or dissimilar plastic materials. A most common type of all-plastic composite rope is one comprised of an inner nylon sheath and an outer polyester sheath. Both sheaths are comprised of interwoven and braided layers of heat-resistant fibrous multi-strand components constituting a multi-layer plastic rope. The outer polyester sheath shields the inner nylon sheath from exposure to sunlight and abrasion against which the polyester is particularly effective, the polyester thereby protecting the nylon sheath from both adverse conditions and prolonging the life and increasing the durability of the composite rope. The inner and outer sheaths are braided separately into diamond-like braids and are normally adhered to one another by an adhesive material to prevent their relative movement with respect to one another. The outer sheath may be securely adhered to the inner sheath by an adhesive material such as rubber cement having good adhesion to both materials and preventing relative slippage of one with respect to the other.
The inner sheath is normally comprised of a cylindrical braid of continuous nylon filaments or fibers such as 60 fibers braided to a standard well known eight-carrier braid construction. In the manufacture of such plastic composite rope, the inner core is interwoven into braided form. It is then normally passed upwardly through the center of an eight-carrier braiding apparatus and the outer sheath of polyester is tightly braided around the inner sheath in the form of conventional diamond braids.
The outer sheath is formed in a manner similar to that of the inner sheath but is preferably comprised of polyester fibers. The outer sheath is normally comprised of a cylindrical braid of polyester fibers such as 60 fibers braided to a standard eight-carrier braid construction over the inner sheath. As is well known in the art, the plastic fibers and braid configurations may be formed of other known plastic fibers and braid patterns to form the combined inner and outer sheaths having a substantial tensile strength which is resistant to water and most common chemicals.
The subject rope end clamp and method of application to a composite rope are useful for a wide variety of multiple sheath composite ropes as well as those having a metallic multi-strand core which are useful for more demanding use applications.
The first embodiment of the present invention as described hereinafter is for the method of attaching the end clamp to a multi-sheath composite rope comprised of different plastic materials in fibrous form intended for multi-purpose use without a metallic core. The separately braided multi-layers of the all-plastic rope reduce its elasticity and increase its strength, the layers being selected to utilize their individual properties to an optimum degree.
Several sheaths of different materials having different melting and softening point temperatures are used depending upon the chemical and physical properties of the prescribed compositions. A substantial tensile strength is obtained of the order of about 1,000 to 2,000 pounds per square inch in tension depending upon the thickness of the individual sheaths and overall diameter of the composite rope.
In a preferred embodiment of the present invention as utilized with a all-plastic composite rope, FIG. 1 shows in an exploded view such rope designated by the numeral 10 comprised of an inner sheath 11 and outer sheath 12. The end clamp is comprised of several elements including a tapered elongated solid metal plug 15 having an essentially smooth tapered exterior surface 16 and essentially right-cylindrical end surfaces 17 and 18 at its smaller and larger ends respectively. An elongated hollow sleeve member 20 having an overall length greater than plug member 15 is utilized as the second component of the clamp. One end portion of the sleeve 20 is hollow having an exteriorly tapering smooth surface 21, the taper extending from a central region to the open end extremity where the taper is larger in diameter. The interior surface 22 of the sleeve hollow portion has an essentially right-cylindrical contour, its diameter and length being greater than solid plug member 15. The hollow portion of sleeve member 20 terminates in a right-cylindrical open end surface 23, its hollow portion being adapted to enclose and completely surround the plug member 15. The other end portion 24 of the sleeve member 20 has an essentially solid right-cylindrical exterior surface 24 and a right-angled end surface 25 with a relatively large transverse aperture 26 extending through such solid end portion. Aperture 26 is adapted to receive a pin element of a connecting cable end fitting (not shown), which may be of a conventional nature, after the several components of the clamp are fitted to and positively engage the various elements of the all-plastic rope.
In practicing the method of the first embodiment of the present invention, as shown in FIG. 4, a short length of adhesive tape 28 is placed around the exterior of the plastic composite rope being located at an intermediate area adjacent one end of the rope. The interwoven fibers of inner and outer sheaths 11 and 12 are frayed or individually separated at the end area extending beyond the encircling tape 28. The solid plug member 15 is inserted forcefully into the unfrayed fibrous inner sheath 11 in concentric alignment therewith. The plug is then further driven into the unfrayed portions of both sheath members as shown in FIG. 5. The frayed fibers of both sheath members 11 and 12 are collected and brought together extending over and around the large end of plug member 15, the fibers being retained in an essentially tightly gathered bundle around the plug.
A heating element 30 such as a small torch having an open flame 31 as shown in FIG. 5 is brought into close proximity with the gathered fibers of both sheath members 11 and 12 to heat the fibers extending beyond the tape into a thermally-fused molten mass 32 surrounding and encompassing the larger end 18 of the plug member 15. The fused mass is tooled while in molten condition such as by a paddle so that its exterior diameter does not exceed the internal diameter of hollow sleeve member 20. The tape 28 is removed upon cooling of the fused fibers. The plug member 15 and its surrounding thermally-fused mass 32 are then placed into the hollow end portion of sleeve member 20 and seated therewithin closely adjacent the termination of the hollow portion. The sleeve may have a conical seat 27 at its hollow termination to receive the fused mass 32.
After seating the plug and its surrounding fused mass within sleeve member 20, its tapered exterior surface 21 of sleeve 20 is swagged by a suitable tooling mechanism (not shown) into an essentially right-cylindrical exterior configuration, the outer diameter of the sleeve member 20 then being as little as 40 percent larger than the exterior diameter of the unfrayed all-plastic composite rope 10. The tapered plug member and tapered sleeve member have an original taper of about 3 degrees. After swagging, the right-cylindrical interior surface of the sleeve member 20 is then tapered into closely complemental contour with the exterior surface of plug member 15, the degree of taper of both surfaces preferably being about three (3) degrees. Thus, the hollow sleeve member is converted by the swagging operation from being exteriorly tapered to interiorly tapered to provide a surface against which the plug member 20 wedges the fibrous strands of the rope to ensure positive retention of the fused and unfused fibrous elements of the several sheaths which are then permanently restrained between the metallic components of the clamp.
The subject end clamp as formed by the aforesaid method has been found to have a tensile strength closely similar to that of the all-plastic rope and in most cases exceeding such strength for varied connection operations. The aperture 26 in the essentially solid end portion of the sleeve member is adapted to interconnection with a wide variety of cable end fittings such as a clevis, hook or other such cable fittings having a pin type component for passage through the aperture in the sleeve. The subject end clamp may be interconnected to similar or dissimilar ropes or cables also having the same or other types of end clamps for their positive and durable interconnection, the end clamp having a strength which is substantially greater than that of the rope per se. FIG. 7 shows the end clamp in final swagged condition with the exterior surface of the sleeve member having a substantially uniform diameter which is right-cylindrical in configuration closely complemental to the body portion of rope 10 for its interconnection to separate fittings. The fused mass of plastic materials encompassing the plug member, as well as the fused and unfused fibers captured between the co-tapering surfaces of plug and sleeve, serve to restrain the several sheaths in firmly engaged durable relation.
In a second embodiment of the invention as shown in FIG. 8, the composite rope 10A has a multi-strand twisted metallic core 13 surrounded by an inner plastic sheath 11 and an outer plastic sheath 12 as described hereinabove. The metallic core 13 is preferably comprised of interwoven or rotatably twisted small strands of stainless steel wire, for example. The core is comprised of multi-strand metallic elements such as one prefabricated of 10 to 20 strands of high-tensile strength steel, the core having a tensile strength of the order of about 7,000 psi. The core may also include high-tensile strength polymer fibers. The core may also have an elastic memory which causes the line to assume a coiled configuration whenever tension on the line is eliminated or released. The core may be woven or braided from a plurality of metal strands to provide a non-rotating cable core and therefore constitute a primary component of a non-rotating or non-rotatable rope.
The core may be comprised of multi-strand stainless steel elements alone or it may also include an interior core of polyaramid fibers sold under the trademark KEVLAR. One example of such cable is manufactured under U.S. Pat. No. 4,034,547 and sold by Loss & Company, Inc. under the trademarks K-KORE and K-FLEX. The exterior of the core may be coated with ah adhesive material (not shown) such as rubber cement having proper adhesion to the exterior of the cable and the interior of the inner sheath 11 of the composite rope 10A. Inner and outer sheaths 11 and 12 are similarly formed and comprised of different selected materials as disclosed hereinabove. The several sheaths are normally comprised of interwoven braided plastic materials having different chemical and physical properties.
In the second embodiment of the present invention, as shown in FIGS. 8 and 9, metallic plug member 15A has a hollow interior 19a which is slightly larger than metallic core 13. In practicing the second method of attachment of the modified end clamp to the rope 10A, a short length of adhesive tape 28a is attached to an intermediate area of the rope adjacent one end thereof as shown in FIG. 9, the central metallic core 13 projecting for some distance beyond the plastic sheaths. The hollow plug member 15A is placed over and around the metallic core, the plug having an enlarged recess 19b at its larger end. A metallic tubular button element 34 is placed over and crimped around the terminating end of the metallic core 13 which is then drawn into the end cavity of the plug member in firmly seated relation. The several plastic sheaths 11A and 12A are frayed for a distance beyond the encircling tape member. As shown in FIG. 9, the hollow plug member 15a retaining the central metallic core 13 is driven into the unfrayed portion of inner sheath 11A. The frayed fibers of both sheaths 11 and 12 are collected together as described hereinabove with regard to FIG. 5, and the frayed fibers being then heated by the heating element 30.
The frayed fibers are thermally-fused into molten condition to form a fused mass 29a surrounding the large end extremity of the plug member 15a. The fused mass then encloses the crimped button 34 and metallic core end. The fused mass is formed having an exterior diameter lesser than the interior diameter of hollow sleeve member 20 as shown in FIG. 3. Hollow sleeve member 20 is then placed over and around the plug member and fused mass of the plastic fibers as shown in FIG. 10, the plug and fused mass being seated firmly within the extremity of the hollow cavity 22 in the sleeve member. Hollow sleeve member 20 at that time has an essentially right-cylindrical uniform diameter on its interior surface and a tapered surface on its exterior surface having a degree of taper of about three (3) degrees. The exterior surface of the hollow portion of sleeve member 20 is then swagged into an essentially right-cylindrical exterior surface and a tapered interior surface as described hereinabove. The interior surface of the sleeve is then formed with an inside taper closely complemental to that of the tapered hollow plug 15A. The exterior surface of the sleeve member is then essentially right-cylindrical in contour having a diameter as little as 40 percent larger than the composite rope 10a having the metallic core.
In each of the several forms of the subject rope clamp, a separate cable end fitting such as a clevis, eye, oval eye, or the like having a pin type component may be utilized to make a durable connection between the line and the fitting, and to another similar or dissimilar rope clamp depending upon the desired applications. The end clamp fabricated in accordance with the several illustrated embodiments of this invention exhibits great strength in tension comparable to the composite rope itself whether it be comprised of all plastic components or one having a metallic core.
The individual clamping of the different line materials serves to prevent any relative axial movement between the twin sheaths and the central core, or between the twin sheaths without the central core. In the event that any loosening of the diverse materials does occur, the remaining clamped portions prevent sudden release or separation of the clamp from the rope end with the double clamping action of the fused mass of the plastic materials and the mechanical grasping of the fused and unfused portions of the plastic sheaths. A double clamping action is obtained wherein the twin sheaths are not fully dependent one upon the other and its seat is essentially capable of carrying the rated load of the line.
Both the solid and hollow plug members of the several different embodiments are preferably comprised of lightweight aluminum or aluminum alloy, and the hollow sleeve member is also comprised of a similar material. The softer nature of the several metallic components, with the outer metallic member being swagged into firm engagement with the inner, ensures a positive solid seating of the rope components and especially where the wire core strands are employed.
Accordingly, the improved rope end clamp and method of attachment of this invention are simplified, provide a reliable, safe, inexpensive and efficient device which achieves all the enumerated objectives, provides for eliminating difficulties encountered with prior art devices, solves unique problems, and obtains new results in the art.
In the foregoing description, certain terms have been used for brevity, clearness and understanding; but no unnecessary limitations are to be implied therefrom beyond the requirements of the prior art, because such terms are used for descriptive purposes and are intended to be broadly construed.
Moreover, the description and illustration of the invention is by way of example, and the scope of the invention is not limited to the exact details shown or described.
Having now described the features, discoveries and principles of the invention, the manner in which the improved end clamp for a composite rope is constructed and used in several forms, the characteristics of the construction, and the advantageous, new and useful results obtained; the new and useful structures, devices, elements, arrangements, parts and combinations, are set forth in the appended claims.
|
An improved end clamp and method for attachment to a light-weight, manipulatable readily-grasped composite line of relatively high strength for use by personnel involved in hazardous rescue or safety conditions. The clamp and its method of attachment may be used with a multi-layered composite rope comprised of several combined sheaths of plastic materials with or without a multi-strand central metallic core. The clamp is particularly useful with a static composite rope having very little stretch and which will withstand exposure to elevated temperatures, sharp objects, chemicals, sunlight or shock which do not produce failure in the rope or require its premature disposal. The clamp is relatively simple in construction and provides a pair of interlocking tapered metallic elements which may be quickly attached to the rope end to withstand an unusual amount of strain or loading equal to or greater than the actual breaking strength of the rope itself.
| 5
|
U.S. GOVERNMENT RIGHTS
The United States Government has certain rights to this invention under government contract number DAAE30-97-C-1006.
FIELD OF THE INVENTION
The present invention is generally related to sabots, and more particularly to a composite sabot with an anti-splitting ring integral therewith.
BACKGROUND OF THE INVENTION
In military ordnance arts, carriers for projectiles, known as sabots, have been used to facilitate the use of a variety of munitions while engaging in military operations.
In general, a sabot is a lightweight carrier for a projectile that permits the firing of a variety of projectiles of a smaller caliber within a larger caliber weapon. The word sabot is derived form the French word cabot, which means, “shoe.” Because a sabot fits around the projectile in a manner similar to the way a cabot, or “shoe,” slips onto a persons foot, the name has been applied to all such projectile carriers.
A sabot provides structured support to a flight projectile within a gun tube under extremely high loads. Without adequate support from a sabot, a projectile may break up into many pieces when fired.
A sabot fills the bore of the gun tube while encasing the projectile to permit uniform and smooth firing of the weapon. The projectile is centrally located within the sabot that is generally radially symmetrical. After firing, the sabot and projectile clear the bore of the gun tube and the sabot is normally discarded some distance from the gun tube while the projectile continues toward the target.
One method for discarding a sabot is to form a scoop onto the sabot. After the sabot and projectile clear the weapon bore, the scoop gathers, or “scoops,” air particles as it is moving forward. The air pressure on the front scoop lifts the sabot from the projectile and thus the sabot is removed from the projectile in flight, allowing the projectile to continue towards its target.
Additionally, sabots are generally made in three symmetrical segments to facilitate smooth discard upon exit from the gun. Typically, each segment, or petal, spans 120 degrees of the front circumference of the intact sabot. Each petal's scoop portion is still expansive enough, at 120-degrees, to serve its purpose of driving the petal away from the projectile. The three segment design allows sabot petals to discard from the projectile quickly, as opposed to, for example, a design where an intact sabot gradually slips off of the projectile. The overall advantage of a three petal sabot design is that the sabot is released more quickly, thereby reducing parasitic weight and increasing accuracy.
It is desirable to make sabots lightweight to increase the muzzle velocity of projectile at exit. At the same time, the sabot must maintain its rigidity during operation. For example, inside the bore of the weapon the sabot must stay rigid to allow smooth firing and accurate targeting. Further, once outside the bore of the weapon, the sabot must maintain rigidity in order to scoop air particles efficiently, discard its three petals, and allow acceptable projectile dispersion on the target.
The weight of sabots has been reduced considerably through the use of continuous fiber composite material. Generally, such composite sabots are mixtures of fibers and epoxy combined in a chemical molding process. The weight reductions are made possible by aligning the fibers in the longitudinal/radial plane of the sabot which matches the load directions generated during the projectile travel down the weapon bore.
Unfortunately, during sabot discard, significant circumferential, or hoop, tensile loads are created. Since no fibers are oriented in the circumferential, or hoop, direction in known lightweight sabot designs, the sabot splits along the longitudinal/radial plane typically near the middle of the sabot scoop. Compounding the problem, a faulty molding process may leave air voids in the structure of the sabot, which increases the probability that a sabot petal of conventional design will split into more than two pieces.
Consequently, composite sabot petals of conventional design usually split in the middle from the high hoop stresses generated during discard. Thus, a 120-degree petal may split into two 60-degree segments due to the lack of strength in the circumferential direction of the sabot. This could result in asymmetric discard, where the petals are released at different times, and poor projectile dispersion on the target. It also has been found that a 60-degree segment of split sabot petal is more likely to fail in the scoop or break in the saddle compared to 120-degree intact sabot petal. Further, such splits occur with considerable variation in the location and time of splitting. Thus, compensation for the sabot failure using targeting adjustments is very difficult.
Previous attempts to stop the splitting of composite sabots involved filament wrapping. In this process, the entire assembled projectiles are wrapped with filaments, and then the filament wrap is slit along the seams between the sabot petals. However, this process is unwieldy and expensive from a manufacturing standpoint. Further, filament wrapping is known to be ineffective for preventing all sabot splitting problems.
SUMMARY OF THE INVENTION
The present invention overcomes the deficiencies of the prior art by, for the first time, providing a lightweight, reliable, and inexpensive method of eliminating splitting of a composite sabots during discard using an anti-splitting ring within a composite sabot. The present invention provides a composite sabot that discards more uniformly thereby allowing increased accuracy and dispersion of projectiles fired with composite sabots. Further, the present invention provides a composite sabot design that decreases the drag on and increases velocity of a projectile fired with composite sabots.
The invention provides, for the first time, a composite sabot having an anti-splitting ring mounted to the sabot to prevent the composite sabot from splitting during discard.
In one example embodiment of the invention, a composite sabot includes sabot petals with fibers oriented in the radial direction and a front scoop for gathering air particles. An anti-splitting ring is mounted to the front scoop portion of the composite sabot where splitting initiates. The anti-splitting ring may be a variety of shapes and materials and attaches easily and inexpensively to any sabot.
Other objects, features and advantages of the present invention will become apparent to those skilled in the art through the description of the preferred embodiment, claims and drawings wherein like numerals refer to like elements.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a three dimensional perspective view of one example of the apparatus of the invention employed on a composite sabot.
FIG. 2A is a front view of one example of the apparatus of the invention employed on a composite sabot.
FIG. 2B is a partial view of one example of the apparatus of the invention as depicted in FIG. 2 A.
FIG. 3A is a cross-sectional side view of one example of the apparatus of the invention employed on a composite sabot.
FIG. 3B is a partial view of one example of the apparatus of the invention as depicted in FIG. 3 A.
FIG. 4A is a partial cross-sectional side view of an alternative example of the apparatus of the invention employed on a composite sabot.
FIG. 4B is a partial cross-sectional side view of an alternative example of the apparatus of the invention employed on a composite sabot.
FIG. 4C is a partial cross-sectional side view of an alternative example of the apparatus of the invention employed on a composite sabot.
DETAILED DESCRIPTION OF THE INVENTION
Illustrated in FIG. 1 is a three dimensional perspective view of a composite sabot 10 in accordance with the present invention. The composite sabot 10 has a sabot body 20 , an anti-splitting ring 50 , and a penetrator 60 .
The sabot body 20 has a front scoop 30 for trapping air particles. The front scoop has a front edge 40 for mounting the anti-splitting ring 50 . In this example of the present invention, the sabot body 20 is nominally radially divided along three petal divisions 24 into three 120-degree sabot petals 22 . Each sabot petal 22 has a front scoop segment 32 . Each front scoop segment 32 has a front edge segment 42 . Accordingly, the anti-splitting ring 50 is also nominally divided along three ring divisions 54 into three 120-degree anti-splitting ring segments 52 (shown in FIG. 2 B). In one useful embodiment, the petal divisions 24 and the ring divisions 54 are advantageously aligned so that one ring segment 52 substantially covers a mating front edge segment 42 . Fully assembled, the sabot petals 22 and the anti-splitting ring segments 52 encompass the penetrator 60 .
When fired, and after the composite sabot 10 exits from a gun tube, the sabot body 20 releases the penetrator 60 . Release occurs as the front scoop 30 traps or “scoops” air particles. The air particles create lift forces 70 that separate the sabot body 20 , along the petal divisions 24 , into its corresponding sabot petals 22 . Accordingly, as the sabot body 20 separates, the anti-splitting ring 50 also separates along the ring divisions 54 . As the sabot petals 22 are separating, the front scoop segments 32 provide enough surface area to allow total separation from and release of the penetrator 60 . This release process is called discard.
Illustrated in FIG. 2A is a front view of the front scoop 30 of a composite sabot of the present invention taken generally along the line 2 A— 2 A of FIG. 1 . This view shows the front scoop 30 with the front edge 40 . The anti-splitting ring 50 is mounted on the front edge 40 , and thus, hides the front edge 40 from view. The anti-splitting ring 50 may be integrally connected to the front edge 40 or mounted using a wide variety of known structural adhesives. This view more clearly shows that the ring divisions 54 are aligned with the petal divisions 24 and that the fully assembled sabot petals encompass the penetrator 60 .
Further, FIG. 2A shows the high hoop stresses 220 that are generated on the front scoop segments 32 during discard. The anti-splitting ring 50 prevents the hoop stresses 220 from splitting the front edge segments 42 (shown in FIG. 1 and 2B) of the sabot petals 22 throughout the entire discard process.
Illustrated in FIG. 2B is a detailed partial view of the front scoop segment 32 of FIG. 2 A. Front scoop segment 32 has wedges 210 aligned in the radial direction. Each wedge 210 is comprised of wedge fibers 212 aligned in the same direction as the wedges 210 . The radial alignment of the wedges 210 matches loads created during the firing of the composite sabot 10 .
However, during discard, the high hoop stresses 220 generate loads in the circumferential direction; thus, the wedges 210 are not oriented in the proper direction to withstand the hoop stresses 220 . Consequently, the wedges 210 begin to split. In other mechanisms built without the benefit of the anti-splitting ring of the invention, splitting would initiate in the middle of a front edge segment 42 at split point 230 and travel down the length of the sabot petal 22 as the wedges 210 progressively fail.
Further, in such other devices, when splitting occurs, it also has been found that the front scoop segment 32 will fail to provide sufficient trapping of air particles after the sabot petals 22 have begun to separate. Consequently, discard could be asymmetric or the sabot petals 22 could break.
As mentioned hereinabove, the anti-splitting ring 50 of the invention advantageously prevents the hoop stresses 220 from splitting the front edge segments 42 . The anti-splitting ring 50 prevents splitting because it is oriented in the same direction as the hoop stresses 220 and provides the wedge fibers 212 with sufficient circumferential strength to withstand splitting. The anti-splitting ring segments 52 also prevent the front scoop segments 32 from splitting, to allow for proper release of the penetrator 60 throughout the discard process.
Illustrated in FIG. 3A is a cross-sectional view of the composite sabot 10 of the present invention taken generally along the line 3 A— 3 A of FIG. 2 A. This view shows a portion of sabot body 20 , anti-splitting ring 50 , and a portion of penetrator 60 . The anti-splitting ring 50 is mounted to the front edge 40 of front scoop 30 .
Illustrated in FIG. 3B is a detailed partial view of the front scoop 30 of FIG. 3 . This view shows front scoop 30 with front edge 40 . The anti-splitting ring 50 is mounted to front edge 40 . In this example of the present invention, the anti-splitting ring 50 has a U-shaped cross-section 310 .
The anti-splitting ring 50 of FIG. 3A has a first bottom wall 320 , a first front wall 322 , and a top wall 324 that combine to form the U-shape cross-section 310 of this example of the anti-splitting ring 50 . The U-shape cross-section 310 allows the anti-splitting ring 50 to easily mate with the front edge 40 providing circumferential strength to front scoop 30 and the wedge fibers 212 (as shown in FIG. 2 B). The anti-splitting ring 50 with the U-shape cross-section 310 also reinforces and encloses the split point 230 .
Illustrated in FIG. 4A is an alternate embodiment of the present invention with a detailed partial view of the front scoop 30 with a second anti-splitting ring 408 . This view shows front scoop 30 with front edge 40 . A second anti-splitting ring 408 is mounted to front edge 40 . In this example of the present invention, the second anti-splitting ring 408 has an L-shaped cross-section 410 .
The second anti-splitting ring 408 of FIG. 4A has a second bottom wall 412 and a second front wall 414 that combine to form the L-shape cross-section 410 of the second anti-splitting ring 408 . The L-shape cross-section 410 allows the second anti-splitting ring 408 to easily couple with the front edge 40 providing circumferential strength to front scoop 30 and the wedge fibers 212 (as shown in FIG. 2 B). The second anti-splitting ring 408 with the L-shape cross-section 410 also reinforces and encloses the split point 230 .
Illustrated in FIG. 4B is an alternate embodiment of the present invention with a detailed partial view of the front scoop 30 with a third anti-splitting ring 418 . This view shows front scoop 30 with front edge 40 . The third anti-splitting ring 418 is mounted to front edge 40 . In this example of the present invention, the third anti-splitting ring 418 has a curved cross-section 420 .
The third anti-splitting ring 418 of FIG. 4B has a first single wall 422 that forms the curved cross-section 420 of this example of the third anti-splitting ring 418 . The curved cross-section 420 allows the third anti-splitting ring 418 to connect with the front edge 40 providing circumferential strength to front scoop 30 and the wedge fibers 212 (as shown in FIG. 2 B). The third anti-splitting ring 418 with the curved cross-section 420 also reinforces the split point 230 .
Illustrated in FIG. 4C is an alternate embodiment of the present invention with a detailed partial view of the front scoop 30 with a fourth anti-splitting ring 428 . This view shows front scoop 30 with front edge 40 . The fourth anti-splitting ring 428 is mounted to front edge 40 . In this example of the present invention, the fourth anti-splitting ring 428 has a rectangular cross-section 430 .
The fourth anti-splitting ring 428 of FIG. 4C has a second single wall 432 that forms the rectangular cross-section 430 of this example of the fourth anti-splitting ring 428 . The rectangular cross-section 430 allows the fourth anti-splitting ring 428 to connect with the front edge 40 providing circumferential strength to front scoop 30 and the wedge fibers 212 (as shown in FIG. 2 B). The fourth anti-splitting ring 428 with the rectangular cross-section 430 also reinforces the split point 230 .
The invention has been described herein in considerable detail in order to comply with the Patent Statutes and to provide those skilled in the art with the information needed to apply the novel principles of the present invention, and to construct and use such exemplary and specialized components as are required. However, it is to be understood that the invention may be carried out by specifically different equipment and devices, and that various modifications, both as to the equipment details and operating procedures, may be accomplished without departing from the true spirit and scope of the present invention.
More specifically, materials for anti-splitting ring 50 may be chosen from a wide array of materials to serve the intended purpose. The material may be selected from a wide array of metallic materials and alloys, as well as, composite fiber, thermoset or thermoplastic resins and epoxies to serve the intended function and accommodate manufacturing processing to achieve the integral structure as indicated herein. Other resins known to one skilled in the art may be employed as appropriate,
For example, the anti-splitting ring of the invention may advantageously be comprised of material selected from the group consisting of metal, a continuous fiber/epoxy system, a chopped fiber/epoxy system, a thermoset fiber/epoxy system, a thermoplastic fiber/epoxy system, a continuous thermoset fiber/epoxy system, a chopped thermoset fiber/epoxy system, a continuous thermoplastic fiber/epoxy system, a chopped thermoplastic fiber/epoxy system, a thermoset fiber/resin system, a thermoplastic fiber/resin system, a continuous thermoset fiber/resin system, a chopped thermoset fiber/resin system, a continuous thermoplastic fiber/resin system, and a chopped thermoplastic fiber/resin system.
As a further example, fibers employed for making the anti-splitting ring may advantageously include glass fibers, graphite fibers, carbon fibers, boron fibers or any other fibrous materials suitable for making lightweight anti-splitting rings. Suitable metals include aluminum, and any other suitable metal or metal alloys. The anti-splitting ring may be shaped and manufactured using any well known machining or other fabrication techniques from the metal arts or the composite fiber arts as the case may be.
Lastly, the anti-splitting ring 50 may have many possible configurations in addition to those configurations shown in FIGS. 3 B and FIGS. 4A-4C. These and other modifications are all intended to be within the true spirit and scope of the present invention.
|
A composite sabot including an anti-splitting ring connected to the composite sabot body, to prevent the sabot from splitting during discard. The composite sabot includes sabot petals with fibers oriented in the radial direction and a front scoop for gathering air particles. The anti-splitting ring is mounted to the front scoop portion of the composite sabot where splitting initiates. The anti-splitting ring may be a variety of shapes and materials and attaches easily and inexpensively to any sabot.
| 5
|
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority under 35 USC 119 of provisional application No. 60/156,742 filed Sep. 30, 1999 and of Danish application nos. PA 1999 01277 and PA 2000 01069 filed Sep. 10, 1999 and Jul. 7, 2000, the contents of which are fully incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to novel compounds, to methods for their preparation, to compositions comprising the compounds, to the use of these compounds as medicaments and their use in therapy, where such compounds of Formula 1 are pharmacologically useful inhibitors of Protein Tyrosine Phosphatases (PTPases) such as PTP1B, CD45, SHP-1, SHP-2, PTPα, LAR and HePTP or the like,
wherein n, m, X, Y, R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are defined more fully below. It has been found that PTPases plays a major role in the intracellular modulation and regulation of fundamental cellular signaling mechanisms involved in metabolism, growth, proliferation and differentiation (Hunter, Phil. Trans. R. Soc. Lond . B 353: 583-605 (1998); Chan et al., Annu. Rev. Immunol. 12: 555-592 (1994); Zhang, Curr. Top. Cell. Reg. 35: 21-68 (1997); Matozaki and Kasuga, Cell. Signal. 8: 113-19 (1996); Flint et al., The EMBO J. 12:1937-46 (1993); Fischer et al, Science 253:401-6 (1991)). Overexpression or altered activity of tyrosine phosphatases can also contribute to the symptoms and progression of various diseases (Wiener, et al., J. Natl. cancer Inst. 86:372-8 (1994); Hunter and Cooper, Ann. Rev. Biochem, 54:897-930 (1985)). Furthermore, there is increasing evidence which suggests that inhibition of these PTPases may help treat certain types of diseases such as diabetes type I and II , autoimmune disease, acute and chronic inflammation, osteoporosis and various forms of cancer.
BACKGROUND OF THE INVENTION
Protein phosphorylation is now well recognized as an important mechanism utilized by cells to transduce and regulate signals during different stages of cellular function (Hunter, Phil. Trans. R. Soc. Lond. B 353: 583-605 (1998); Chan et al., Annu. Rev. Immunol. 12: 555-592 (1994); Zhang, Curr. Top. Cell. Reg. 35: 21-68 (1997); Matozaki and Kasuga, Cell. Signal. 8: 113-19 (1996); Fischer et al, Science 253:401-6 (1991); Flint et al., EMBO J. 12:1937-46 (1993)). There are at least two major classes of phosphatases: (1) those that dephosphorylate proteins (or peptides) that contain a phosphate group(s) on a serine or threonine moiety (termed Ser/Thr phosphatases) and (2) those that remove a phosphate group(s) from the amino acid tyrosine (termed protein tyrosine phosphatases or PTPases or PTPs).
The PTPases are a family of enzymes that can be classified into two groups: a) intracellular or nontransmembrane PTPases and b) receptor-type or transmembrane PTPases.
Intracellular PTPases
Most known intracellular type PTPases contain a single conserved catalytic phosphatase domain consisting of 220-240 amino acid residues. The regions outside the PTPase domains are believed to play important roles in localizing the intracellular PTPases subcellularly (Mauro, L. J. and Dixon, J. E. TIBS 19: 151-155 (1994)). The first intracellular PTPase to be purified and characterized was PTP1B, which was isolated from human placenta (Tonks et al., J. Biol. Chem. 263: 6722-6730 (1988)). Shortly after, PTP1B was cloned (Charbonneau et al., Proc. Natl. Acad. Sci. USA 86: 5252-5256 (1989); Chernoff et al., Proc. Natl. Acad. Sci. USA 87: 2735-2789 (1989)). Other examples of intracellular PTPases include (1) T-cell PTPase/TC-PTP (Cool et al. Proc. Natl. Acad. Sci. USA 86: 5257-5261 (1989)), (2) rat brain PTPase (Guan et al., Proc. Natl. Acad. Sci. USA 87:1501-1502 (1990)), (3) neuronal phosphatase STEP (Lombroso et al., Proc. Natl. Acad. Sci. USA 88: 7242-7246 (1991)), (4) ezrin-domain containing PTPases: PTPMEG1 (Guet al., Proc. Natl. Acad. Sci. USA 88: 5867-57871 (1991)), PTPH1 (Yang and Tonks, Proc. Natl. Acad. Sci. USA 88: 5949-5953 (1991)), PTPD1 and PTPD2 (Møller et al., Proc. Natl. Acad. Sci. USA 91: 7477-7481 (1994)), FAP-1/BAS (Sato et al., Science 268: 411-415 (1995); Banville et al., J. Biol. Chem. 269: 22320-22327 (1994); Maekawa et al., FEBS Letters 337: 200-206 (1994)), and SH2 domain containing PTPases: PTP1C/SH-PTP1/SHP-1 (Plutzky et al., Proc. Natl. Acad. Sci. USA 89: 1123-1127 (1992); Shen et al., Nature Lond. 352: 736-739 (1991)) and PTP1D/Syp/SH-PTP2/SHP-2 (Vogel et al., Science 259: 1611-1614 (1993); Feng et al., Science 259: 1607-1611 (1993); Bastein et al., Biochem. Biophys. Res. Comm. 196: 124-133 (1993)).
Receptor-type PTPases consist of a) a putative ligand-binding extracellular domain, b) a transmembrane segment, and c) an intracellular catalytic region. The structures and sizes of the putative ligand-binding extracellular domains of receptor-type PTPases are quite divergent. In contrast, the intracellular catalytic regions of receptor-type PTPases are very homologous to each other and to the intracellular PTPases. Most receptor-type PTPases have two tandemly duplicated catalytic PTPase domains.
The first receptor-type PTPases to be identified were (1) CD45/LCA (Ralph, S. J., EMBO J. 6: 1251-1257 (1987)) and (2) LAR (Streuli et al., J. Exp. Med. 168: 1523-1530 (1988)) that were recognized to belong to this class of enzymes based on homology to PTP1B (Charbonneau et al., Proc. Natl. Acad. Sci. USA 86: 5252-5256 (1989)). CD45 is a family of high molecular weight glycoproteins and is one of the most abundant leukocyte cell surface glycoproteins and appears to be exclusively expressed upon cells of the hematopoietic system (Trowbridge and Thomas, Ann. Rev. Immunol. 12: 85-116 (1994)).
The identification of CD45 and LAR as members of the PTPase family was quickly followed by identification and cloning of several different members of the receptor-type PTPase group. Thus, 5 different PTPases, (3) PTPα, (4) PTPβ, (5) PTPδ, (6) PTPε, and (7) PTPζ, were identified in one early study (Krueger et al., EMBO J. 9: 3241-3252 (1990)). Other examples of receptor-type PTPases include (8) PTPγ (Barnea et al., Mol. Cell. Biol. 13: 1497-1506 (1995)) which, like PTPζ (Krueger and Saito, Proc. Natl. Acad. Sci. USA 89: 7417-7421 (1992)) contains a carbonic anhydrase-like domain in the extracellular region, (9) PTPμ (Gebbink et al., FEBS Letters 290: 123-130 (1991)), (10) PTPκ (Jiang et al., Mol. Cell. Biol. 13: 2942-2951 (1993)). Based on structural differences the receptor-type PTPases may be classified into subtypes (Fischer et al., Science 253: 401-406 (1991)): (I) CD45; (II) LAR, PTPδ, (11) PTPσ; (III) PTP, (12) SAP-1 (Matozaki et al., J. Biol. Chem. 269: 2075-2081 (1994)), (13) PTP-U2/GLEPP1 (Seimiya et al., Oncogene 10: 1731-1738 (1995); Thomas et al., J. Biol. Chem. 269: 19953-19962 (1994)), and (14) DEP-1; (IV) PTPα, PTPε. All receptor-type PTPases except Type III contain two PTPase domains. Novel PTPases are continuously identified. In the early days of PTPase research, it was believed that the number of PTPs would match that of protein tyrosine kinases (PTKs) (Hanks and Hunter, FASEB J. 9: 576-596 (1995)). However, although about 90 open reading frames in C. elegans contain the hallmark motif of PTPs, it now seems that the estimate of ‘classical’ PTPases must be downsized, perhaps to between 100 and 200 in humans.
PTPases are the biological counterparts to protein tyrosine kinases Therefore, one important function of PTPases is to control, down-regulate, the activity of PTKs. However, a more complex picture of the function of PTPases has emerged. Thus, several studies have shown that some PTPases may actually act as positive mediators of cellular signaling. As an example, the SH2 domain-containing SHP-2 seems to act as a positive mediator in insulin-stimulated Ras activation (Noguchi et al., Mol. Cell. Biol. 14: 6674-6682 (1994)) and of growth factor-induced mitogenic signal transduction (Xiao et al., J. Biol. Chem. 269: 21244-21248 (1994)), whereas the homologous SHP-1 seems to act as a negative regulator of growth factor-stimulated proliferation (Bignon and Siminovitch, Clin.Immunol. Immunopathol. 73: 168-179 (1994)). Another example of PTPases as positive regulators has been provided by studies designed to define the activation of the Src-family of tyrosine kinases. In particular, several lines of evidence indicate that CD45 is positively regulating the activation of hematopoietic cells, possibly through dephosphorylation of the C-terminal tyrosine of Fyn and Lck (Chan et al., Annu. Rev. Immunol. 12: 555-592 (1994)).
PTPases were originally identified and purified from cell and tissue lysates using a variety of artificial substrates and, therefore, their natural function of dephosphorylation was not well known. Since tyrosine phosphorylation by tyrosine kinases is usually associated with cell proliferation, cell transformation and cell differentiation, it was assumed that PTPases were also associated with these events. This association has now been proven to be the case with many PTPases. PTP1 B, a phosphatase whose structure was the first PTPase to be elucidated (Barford et al., Science 263:1397-1404 (1994)) has been shown to be involved in insulin-induced oocyte maturation (Flint et al., The EMBO J. 12:1937-46 (1993)) and it has been suggested that the overexpression of this enzyme may be involved in p185 c-erb B2 -associated breast and ovarian cancers (Wiener, et al., J. Natl. cancer Inst. 86:372-8 (1994); Weiner et al., Am. J. Obstet. Gynecol. 170:1177-883 (1994)). The association with cancer is recent evidence which suggests that overexpression of PTP1B is statistically correlated with increased levels of p185 c-erb B2 in ovarian and breast cancer. The role of PTP1B in the etiology and progression of the disease has not yet been elucidated. Inhibitors of PTP1B may therefore help clarify the role of PTP1B in cancer and in some cases provide therapeutic treatment for certain forms of cancer.
PTPases: The Insulin Receptor Signaling Pathway/diabetes
Insulin is an important regulator of different metabolic processes and plays a key role in the control of blood glucose. Defects related to its synthesis or signaling lead to diabetes mellitus. Binding of insulin to the insulin receptor (IR) causes rapid (auto)phosphorylation of several tyrosine residues in the intracellular part of the β-subunit. Three closely positioned tyrosine residues (the tyrosine-1150 domain) must all be phosphorylated to obtain full activity of the insulin receptor tyrosine kinase (IRTK) which transmits the signal further downstream by tyrosine phosphorylation of other cellular substrates, including insulin receptor substrate-1 (IRS-1) (Wilden et al., J. Biol. Chem. 267: 16660-16668 (1992); Myers and White, Diabetes 42: 643-650 (1993); Lee and Pilch, Am. J. Physiol. 266: C319-C334 (1994); White et al., J. Biol. Chem. 263: 2969-2980 (1988)). The structural basis for the function of the tyrosine-triplet has been provided by X-ray crystallographic studies of IRTK that showed tyrosine-1150 to be autoinhibitory in its unphosphorylated state (Hubbard et al., Nature 372: 746-754 (1994)) and of the activated IRTK (Hubbard, EMBO J. 16:5572-5581 (1997)).
Several studies clearly indicate that the activity of the auto-phosphorylated IRTK can be reversed by dephosphorylation in vitro (reviewed in Goldstein, Receptor 3: 1-15 (1993); Mooney and Anderson, J. Biol. Chem. 264: 6850-6857 (1989)), with the tri-phosphorylated tyrosine-1150 domain being the most sensitive target for protein-tyrosine phosphatases (PTPases) as compared to the di- and mono-phosphorylated forms (King et al., Biochem. J. 275: 413-418 (1991)). This tyrosine-triplet functions as a control switch of IRTK activity and the IRTK appears to be tightly regulated by PTP-mediated dephosphorylation in vivo (Khan et al., J. Biol. Chem. 264: 12931-12940 (1989); Faure et al., J. Biol. Chem. 267: 11215-11221 (1992); Rothenberg et al., J. Biol. Chem. 266: 8302-8311 (1991)). The intimate coupling of PTPases to the insulin signaling pathway is further evidenced by the finding that insulin differentially regulates PTPase activity in rat hepatoma cells (Meyerovitch et al., Biochemistry 31: 10338-10344 (1992)) and in livers from alloxan diabetic rats (Boylan et al., J. Clin. Invest. 90: 174-179 (1992)).
Until recently, relatively little was known about the identity of the PTPases involved in IRTK regulation. However, the existence of PTPases with activity towards the insulin receptor can be demonstrated as indicated above. Further, when the strong PTPase-inhibitor pervanadate is added to whole cells an almost full insulin response can be obtained in adipocytes (Fantus et al., Biochemistry 28: 8864-8871 (1989); Eriksson et al., Diabetologia 39: 235-242 (1995)) and skeletal muscle (Leighton et al., Biochem. J. 276: 289-292 (1991)). In addition, other studies show that a new class of peroxovanadium compounds act as potent hypoglycemic compounds in vivo (Posner et al.,supra). Two of these compounds were demonstrated to be more potent inhibitors of dephosphorylation of the insulin receptor than of the EGF-receptor, thus indicating that even such relatively unselective inhibitors may convey some specificity in regulating different signal transduction pathways.
It was recently found by Montreal-based research groups that mice lacking the protein tyrosine phosphatase-1B gene (PTP1B) (Elchebly et al., Science 283: 1544-1548 (1999)) yielded healthy mice that showed increased insulin sensitivity and resistance to diet-induced obesity. Importantly, these results have been confirmed and extended independently by another research team from Boston (Klaman et al., Mol. Cell. Biol. 20: 5479-5489 (2000)). The enhanced insulin sensitivity of the PTP −/− mice was also evident in glucose and insulin tolerance tests. The PTP-1B knock-out mouse showed many characteristics which would be highly desirable to have for an anti-diabetes treatment. Most importantly, the knock-out mice grew normally and were fertile and have exhibited no increased incidence of cancer, as obviously there could have been concerns when one considers the mitogenic properties of insulin. From the diabetes perspective, the first notable features of the knock-out animals were that blood glucose and insulin levels were lowered, and the consequent marked increase in insulin sensitivity in the knock-out animals. Moreover, the insulin-stimulated tyrosine phosphorylation levels of IR and IRS-1 were found to be increased/prolonged in muscle and liver—but not in fat tissue. Thus, the main target tissues for this type of approach would appear to be insulin action in liver and muscle. This is in contrast to the main target tissue for the PPARγ agonist class of insulin sensitizers (the “-diones”), which is adipose tissue (Murphy & Nolan, Exp. Opin. Invest. Drugs 9: 1347-1361 (2000)). Several other “diabetic” parameters were also improved, such as plasma triglycerides being decreased in the knock-out mice. However, perhaps even more remarkably and unexpectedly, the knock-out animals also exhibited a resistance to weight gain when placed on a high-fat diet. This is again in contrast to the action of the PPARγ agonist class of insulin sensitizers, which rather induce weight gain (Murphy & Nolan, supra), and would suggest that inhibition of PTP-1B could be a particularly attractive option for treatment of obese Type II diabetics. This is also supported by the fact that the heterozygous mice from this study showed many of these desirable features. In the Montreal study, there appeared to be no gender differences, whereas in the Boston study in general the male animals had larger responses to PTP-1B being knocked out. In both studies, the reduction in weight gain of the knock-out animals on the high fat diet was found to be due to a decreased fat cell mass, although differences were observed with respect to fat cell number. Leptin levels were also lower in the knock-out mice, presumably as a reflection of the decreased fat mass. Significantly, the Boston group also found that the knock-out animals had an increased energy expenditure of around 20% and an increased respiratory quotient compared to the wild-type; again, heterozygote animals displayed an intermediate level of energy expenditure. Whether this increase in metabolic rate is a reflection of the effects of PTP-1B on insulin-signaling or on other cellular components remains to be established, but the bottom-line message that inhibition of this enzyme may be an effective anti-diabetic and perhaps also anti-obesity therapy is clear.
It should also be noted that in the PTP-1B knock-out mice the basal tyrosine phosphorylation level of the insulin receptor tyrosine kinase does not appear to be increased, which is in contrast to the situation after insulin treatment where there is an increased or prolonged phosphorylation. This might indicate that other PTPs are controlling the basic phosphorylation state of the insulin receptor in the knock-out mice—and perhaps in man.
Previous findings are in accordance with the results reported by Elchebly et al. (supra) (recently reviewed in Kennedy, Biomed. Pharmacother. 53: 466-470 (1999)). Thus, it has been found that high glucose concentration induce insulin resistance and increase the expression of PTP1B in rat (fibroblasts expressing the human insulin receptor (Maegawa et al., J. Biol. Chem. 270: 7724-7730 (1995)). In rat L6 cells, insulin and insulin-like growth factor I (IGF-I) were found to induce increased PTPase activity, including increased PTP1B expression (Kenner et al. J. Biol. Chem. 266: 25455-25462 (1993)). In addition, the same group has shown that PTP1B may interact directly with the activated IR (Seely et al. Diabetes 45: 1379-1385 (1996)) and act directly as a negative regulator of insulin and IGF-I-stimulated signaling (Kenner et al. J. Biol. Chem. 271: 19810-19816 (1996)). Osmotic loading of rat KRC-7 hepatoma cells with neutralizing anti-PTP1B antibodies also indicated a role for PTP1B in negative regulating of the insulin signaling pathway (Akmad et al. J. Biol. Chem. 270: 20503-20508 (1995)).
Also other PTPases have been implicated as regulators of the insulin signaling pathway. Thus, it was found that the ubiquitously expressed SH2 domain containing PTPase, PTP1D/SHP-2 (Vogel et al., 1993, supra), associates with and dephosphorylates IRS-1, but apparently not the IR itself (Kuhné et al., J. Biol. Chem. 268: 11479-11481 (1993); (Kuhné et al., J. Biol. Chem. 269: 15833-15837 (1994)).
Other studies suggest that receptor-type or membrane-associated PTPases are involved in IRTK regulation (Faure et al., J. Biol. Chem. 267: 11215-11221 (1992), (Häring et al., Biochemistry 23: 3298-3306 (1984); Sale, Adv. Prot. Phosphatases 6: 159-186 (1991)). Hashimoto et al. have proposed that LAR might play a role in the physiological regulation of insulin receptors in intact cells (Hashimoto et al., J. Biol. Chem. 267: 13811-13814 (1992)). Their conclusion was reached by comparing the rate of dephosphorylation/inactivation of purified IR using recombinant PTP1B as well as the cytoplasmic domains of LAR and PTPα. Antisense inhibition was used to study the effect of LAR on insulin signaling in a rat hepatoma cell line (Kulas et al., J. Biol. Chem. 270: 2435-2438 (1995)). A suppression of LAR protein levels by about 60 percent was paralleled by an approximately 150 percent increase in insulin-induced auto-phosphorylation. However, only a modest 35 percent increase in IRTK activity was observed, whereas the insulin-dependent phosphatidylinositol 3-kinase (PI 3-kinase) activity was significantly increased by 350 percent. Reduced LAR levels did not alter the basal level of IRTK tyrosine phosphorylation or activity. The authors speculate that LAR could specifically dephosphorylate tyrosine residues that are critical for PI 3-kinase activation either on the insulin receptor itself or on a downstream substrate. Conflicting results have been reported for PTP-LAR knock-out mice. Thus, Goldstein and coworkers reported that transgenic mice deficient in PTP-LAR exhibit profound defects in glucose-homeostasis (Ren et al., Diabetes 47: 493-497 (1998)). However, it is difficult to fully assess the contribution of LAR deficiency to the glucose homeostasis in these mice due to the fact that the control mice were of a different genetic background than the knock-out mice. Moreover, normal glucose homeostasis was reported in a different strain of PTP-LAR knock-out mice (Sorensen et al., Diabetologia 40: A143 (1997)).
While previous reports indicate a role of PTPα in signal transduction through src activation (Zheng et al., Nature 359: 336-339 (1992); den Hertog et al., EMBO J. 12: 3789-3798 (1993)) and interaction with GRB-2 (den Hertog et al., EMBO J. 13: 3020-3032 (1994); Su et al., J. Biol. Chem. 269: 18731-18734 (1994)), Møller, Lammers and coworkers provided results that suggest a function for this phosphatase and its close relative PTP as negative regulators of the insulin receptor signal (Møller et al, 1995 supra;
Lammers, et al., FEBS Lett. 404:37-40 (1997). These studies also indicated that receptor-like PTPases might play a significant role in regulating the IRTK.
Other studies have shown that PTP1B and TC-PTP are likely to be involved in the regulation of several other cellular processes in addition to the described regulatory roles in insulin signaling. Therefore, PTP1B and/or TC-PTP as well as other PTPases showing key structural features with PTP1B and TC-PTP are likely to be important therapeutic targets in a variety of human and animal diseases. The compounds of the present invention are useful for modulating or inhibiting PTP1B and/or TC-PTP and/or other PTPases showing key structural features with said PTPases and for treating diseases in which said modulation or inhibition is indicated. A few examples that are not intended in any way to limit the scope of the invention of substrates that may be regulated by PTP1B will be given below.
Tonks and coworkers have developed an elegant ‘substrate trapping’ technique that has allowed identification of the epidermal growth factor receptor (EGF-R) as a major substrate of PTP1B in COS cells (Flint et al. Proc. Natl. Acad. Sci. USA 94: 1680-1685 (1997)). In addition, three other as yet unidentified substrates of PTP1B were isolated. As an example of these studies, it has been found—using the above substrate-trapping technique—that PTP1B in addition to the EGF-R associates with activated platelet-derived growth factor receptor (PDGF-R), but not with colony-stimulating factor 1 receptor (CSF-1R) (Liu & Chernoff, Biochem. J. 327: 139-145 (1997)).
Early studies have shown that the subcellular localization as well as the enzyme activity of PTP1B may be regulated by agonist-induced calpain-catalyzed cleavage in human platelets (Frangioni et al. EMBO J. 12: 4843-4856 (1993)). Moreover, PTP1B cleavage correlated with the transaction from reversible to irreversible platelet aggregation. Thus, as a non-limiting example compounds of the present invention might be used to prevent or induce irreversible platelet aggregation in individuals in need thereof. It was proposed that the cleavage-induced change in the subcellular localization of PTP1B (from membrane to cytosol) results in different substrate specificity not only in platelet but also in other cell types (Frangioni et al., supra).
The above substrate trapping method has further been used to identify the protein tyrosine kinase p210 bcr-abl as a substrate for PTP1B (LaMontagne, Jr. et al. Mol. Cell. Biol. 18: 2965-2975 (1998)). These studies suggest that PTP1B might function as a negative regulator of p210 bcr-abl signaling in vivo. In addition, PTP1B was recently found to bind to and dephosphorylate the docking protein p130 Cas in rat fibroblasts and thereby suppress transformation by v-crk, v-src, and v-ras, but not by v-raf (Liu et al. Mol. Cell. Biol. 18: 250-259 (1998)).
The transmembrane PTPase CD45, which is believed to be hematopoietic cell-specific, was found to negatively regulate the insulin receptor tyrosine kinase in the human multiple myeloma cell line U266 (Kulas et al., J. Biol. Chem. 271: 755-760 (1996)).
Further, PTPases influences the following hormones or diseases or disease states: somatostatin, the immune system/autoimmunity, cell-cell interactions/cancer, platelet aggregation, osteoporosis, and microorganisms, as disclosed in PCT Publication WO 99/15529.
Somatostatin inhibits several biological functions including cellular proliferation (Lamberts et al., Molec. Endocrinol. 8: 1289-1297 (1994)). While part of the antiproliferative activities of somatostatin are secondary to its inhibition of hormone and growth factor secretion (e.g. growth hormone and epidermal growth factor), other antiproliferative effects of somatostatin are due to a direct effect on the target cells. As an example, somatostatin analogs inhibit the growth of pancreatic cancer presumably via stimulation of a single PTPase, or a subset of PTPases, rather than a general activation of PTPase levels in the cells (Liebow et al., Proc. Natl. Acad. Sci. USA 86: 2003-2007 (1989); Colas et al., Eur. J. Biochem. 207:1017-1024 (1992)).
PTPases: The Immune System/autoimmunity
Several studies suggest that the receptor-type PTPase CD45 plays a critical role not only for initiation of T cell activation, but also for maintaining the T cell receptor-mediated signaling cascade. These studies are reviewed in: (Weiss A., Ann. Rev. Genet. 25: 487-510 (1991); Chan et al., Annu. Rev. Immunol. 12: 555-592 (1994); Trowbridge and Thomas, Annu. Rev. Immunol. 12: 85-116 (1994)).
CD45 is one of the most abundant of the cell surface glycoproteins and is expressed exclusively on hemopoetic cells. In T cells, it has been shown that CD45 is one of the critical components of the signal transduction machinery of lymphocytes. In particular, evidence has suggested that CD45 phosphatase plays a pivotal role in antigen-stimulated proliferation of T lymphocytes after an antigen has bound to the T cell receptor (Trowbridge, Ann. Rev. Immunol, 12: 85-116 (1994)). Several studies suggest that the PTPase activity of CD45 plays a role in the activation of Lck, a lymphocyte-specific member of the Src family protein-tyrosine kinase (Mustelin et al., Proc. Natl. Acad. Sci. USA 86: 6302-6306 (1989); Ostergaard et al., Proc. Natl. Acad. Sci. USA 86: 8959-8963 (1989)). These authors hypothesized that the phosphatase activity of CD45 activates Lck by dephosphorylation of a C-terminal tyrosine residue, which may, in turn, be related to T-cell activation. Thus, it was found that recombinant p56lck specifically associates with recombinant CD45 cytoplasmic domain protein, but not to the cytoplasmic domain of the related PTPα (Ng et al., J. Biol. Chem. 271: 1295-1300 (1996)). The p56lck-CD45 interaction seems to be mediated via a nonconventional SH2 domain interaction not requiring phosphotyrosine. In immature B cells, another member of the Src family protein-tyrosine kinases, Fyn, seems to be a selective substrate for CD45 compared to Lck and Syk (Katagiri et al., J. Biol. Chem. 270: 27987-27990 (1995)).
Studies using transgenic mice with a mutation for the CD45-exon6 exhibited lacked mature T cells. These mice did not respond to an antigenic challenge with the typical T cell mediated response (Kishihara et al., Cell 74:143-56 (1993)). Inhibitors of CD45 phosphatase would therefore be very effective therapeutic agents in conditions that are associated with autoimmune diseases with rheumatoid arthritis, systemic lupus erythematosus, type I diabetes, and inflammatory bowel disease as non-limiting examples. Another important use of CD45 inhibitors is for immunosuppression in connection with tissue or cell transplantation and other condtions with need for immunosuppressive treatment.
CD45 has also been shown to be essential for the antibody mediated degranulation of mast cells (Berger et al., J. Exp. Med. 180:471-6 (1994)). These studies were also done with mice that were CD45-deficient. In this case, an IgE-mediated degranulation was demonstrated in wild type but not CD45-deficient T cells from mice. These data suggest that CD45 inhibitors could also play a role in the symptomatic or therapeutic treatment of allergic disorders with asthma, allergic rhinitis, food allergy, eczema, urticaria and anaphylaxis as non-limiting examples.
Another PTPase, an inducible lymphoid-specific protein tyrosine phosphatase (HePTP) has also been implicated in the immune response. This phosphatase is expressed in both resting T and B lymphocytes, but not non-hemopoetic cells. Upon stimulation of these cells, mRNA levels from the HePTP gene increase 10-15 fold (Zanke et al., Eur. J. Immunol. 22: 235-239 (1992)). In both T and B cells HePTP may function during sustained stimulation to modulate the immune response through dephosphorylation of specific residues. Its exact role, however remains to be defined.
Likewise, the hematopoietic cell specific SHP-1 seems to act as a negative regulator and play an essential role in immune cell development. In accordance with the above-mentioned important function of CD45, HePTP and SHP-1, selective PTPase inhibitors may be attractive drug candidates both as immunosuppressors and as immunostimulants. Recent studies illustrate the potential of PTPase inhibitors as immunmodulators by demonstrating the capacity of the non-selective vanadium-based PTPase inhibitor, BMLOV, to induce apparent B cell selective apoptosis compared to T cells (Dawson et al., FEBS Lett. 478: 233-236; Schieven et al., J. Biol. Chem. 270: 20824-20831 (1995)).
PTPases: Cell-cell Interactions/cancer
Focal adhesion plaques, an in vitro phenomenon in which specific contact points are formed when fibroblasts grow on appropriate substrates, seem to mimic, at least in part, cells and their natural surroundings. Several focal adhesion proteins are phosphorylated on tyrosine residues when fibroblasts adhere to and spread on extracellular matrix (Gumbiner, Neuron 11: 551-564 (1993)). However, aberrant tyrosine phosphorylation of these proteins can lead to cellular transformation. The intimate association between PTPases and focal adhesions is supported by the finding of several intracellular PTPases with ezrin-like N-terminal domains, e.g. PTPMEG1 (Gu et al., Proc. Natl. Acad. Sci. USA 88: 5867-5871 (1991), PTPH1 (Yang and Tonks, Proc. Natl. Acad. Sci. USA 88: 5949-5953 (1991)) and PTPD1 (Møller et al., Proc. Natl. Acad. Sci. USA 91: 7477-7481 (1994)). The ezrin-like domain shows similarity to several proteins that are believed to act as links between the cell membrane and the cytoskeleton. PTPD1 was found to be phosphorylated by and associated with c-src in vitro and is hypothesized to be involved in the regulation of phosphorylation of focal adhesions (Møller et al., supra).
PTPases may oppose the action of tyrosine kinases, including those responsible for phosphorylation of focal adhesion proteins, and may therefore function as natural inhibitors of transformation. TC-PTP, and especially the truncated form of this enzyme (Cool et al., Proc. Natl. Acad. Sci. USA 87: 7280-7284 (1990)), can inhibit the transforming activity of v-erb and v-fms (Lammers et al., J. Biol. Chem. 268: 22456-22462 (1993), Zander et al., Oncogene 8: 1175-1182 (1993)). Moreover, it was found that transformation by the oncogenic form of the HER2/neu gene was suppressed in NIH 3T3 fribroblasts overexpressing PTP1B (Brown-Shimer et al., Cancer Res. 52: 478-482 (1992)).
The expression level of PTP1B was found to be increased in a mammary cell line transformed with neu (Zhay et al., Cancer Res. 53: 2272-2278 (1993)). The intimate relationship between tyrosine kinases and PTPases in the development of cancer is further evidenced by the finding that PTPε is highly expressed in murine mammary tumors in transgenic mice over-expressing c-neu and v-Ha-ras, but not c-myc or int-2 (Elson and Leder, J. Biol. Chem. 270: 26116-26122 (1995)). Further, the human gene encoding PTPγ was mapped to 3p21, a chromosomal region, which is frequently deleted in renal and lung carcinomas (LaForgia et al., Proc. Natl. Acad. Sci. USA 88: 5036-5040 (1991)).
In this context, it seems significant that PTPases appear to be involved in controlling the growth of fibroblasts. Thus, it was found that Swiss 3T3 cells harvested at high density contain a membrane-associated PTPase whose activity on an average is 8-fold higher than that of cells harvested at low or medium density (Pallen and Tong, Proc. Natl. Acad. Sci. USA 88: 6996-7000 (1991)). It was hypothesized by the authors that density-dependent inhibition of cell growth involves the regulated elevation of the activity of the PTPase(s) in question. In accordance with this view, a membrane-bound, receptor-type PTPase, DEP-1, showed enhanced (>=10-fold) expression levels with increasing cell density of WI-38 human embryonic lung fibroblasts and in the AG1518 fibroblast cell line (Östman et al., Proc. Natl. Acad. Sci. USA 91: 9680-9684 (1994)).
Two closely related receptor-type PTPases, PTPκ and PTPμ, can mediate homophilic cell-cell interaction when expressed in non-adherent insect cells, suggesting that these PTPases might have a normal physiological function in cell-to-cell signalling (Gebbink et al., J. Biol. Chem. 268: 16101-16104 (1993), Brady-Kalnay et al., J. Cell Biol. 122: 961-972 (1993); Sap et al., Mol. Cell. Biol. 14: 1-9 (1994)). Interestingly, PTPκ and PTPμ do not interact with each other, despite their structural similarity (Zondag et al., J. Biol. Chem. 270: 14247-14250 (1995)). From the studies described above it is apparent that PTPases may play an important role in regulating normal cell growth. However, as pointed out above, other studies indicate that PTPases may also function as positive mediators of intracellular signaling and thereby induce or enhance mitogenic responses. Increased activity of certain PTPases might therefore result in cellular transformation and tumor formation. Indeed, in one study over-expression of PTPα was found to lead to transformation of rat embryo fibroblasts (Zheng, supra). In addition, SAP-1 was found to be highly expressed in pancreatic and colorectal cancer cells. SAP-1 is mapped to chromosome 19 region q13.4 and might be related to carcinoembryonic antigen mapped to 19q13.2 (Uchida et al., J. Biol. Chem. 269: 12220-12228 (1994)). Further, the dsPTPase, cdc25, dephosphorylates cdc2 at Thr14/Tyr-15 and thereby functions as positive regulator of mitosis (reviewed by Hunter, Cell 80: 225-236 (1995)). Inhibitors of specific PTPases are therefore likely to be of significant therapeutic value in the treatment of certain forms of cancer.
PTPases: Platelet Aggregation
PTPases seem to be centrally involved in platelet aggregation. Thus, agonist-induced platelet activation results in calpain-catalyzed cleavage of PTP1B with a concomitant 2-fold stimulation of PTPase activity (Frangioni et al., EMBO J. 12: 4843-4856 (1993)). The cleavage of PTP1B leads to subcellular relocation of the enzyme and correlates with the transition from reversible to irreversible platelet aggregation in platelet-rich plasma. In addition, the SH2 domain containing PTPase, SHP-1, was found to translocate to the cytoskeleton in platelets after thrombin stimulation in an aggregation-dependent manner (Li et al., FEBS Lett. 343: 89-93 (1994)).
Although some details in the above two studies have been questioned, there is over-all agreement that PTP1B and SHP-1 play significant functional roles in platelet aggregation (Ezumi et al., J. Biol. Chem. 270: 11927-11934 (1995)). In accordance with these observations, treatment of platelets with the PTPase inhibitor pervanadate leads to significant increase in tyrosine phosphorylation, secretion and aggregation (Pumiglia et al., Biochem. J. 286: 441-449 (1992)).
PTPases: Osteoporosis
The rate of bone formation is determined by the number and the activity of osteoblasts, which in term are determined by the rate of proliferation and differentiation of osteoblast progenitor cells, respectively. Histomorphometric studies indicate that the osteoblast number is the primary determinant of the rate of bone formation in humans (Gruber et al., Mineral Electrolyte Metab. 12: 246-254 (1987), reviewed in Lau et al., Biochem. J. 257: 23-36 (1989)). Acid phosphatases/PTPases may be involved in negative regulation of osteoblast proliferation. Thus, fluoride, which has phosphatase inhibitory activity, has been found to increase spinal bone density in osteoporotics by increasing osteoblast proliferation (Lau et al., supra). Consistent with this observation, an osteoblastic acid phosphatase with PTPase activity was found to be highly sensitive to mitogenic concentrations of fluoride (Lau et al., J. Biol. Chem. 260: 4653-4660 (1985), Lau et al., J. Biol. Chem. 262: 1389-1397 (1987), Lau et al., Adv. Protein Phosphatases 4: 165-198 (1987)). Interestingly, the level of membrane-bound PTPase activity was increased dramatically when the osteoblast-like cell line UMR 106.06 was grown on collagen type-I matrix compared to uncoated tissue culture plates. Since a significant increase in PTPase activity was observed in density-dependent growth arrested fibroblasts (Pallen and Tong, Proc. Natl. Acad. Sci. 88: 6996-7000 (1991)), it might be speculated that the increased PTPase activity directly inhibits cell growth. The mitogenic action of fluoride and other phosphatase inhibitors (molybdate and vanadate) may thus be explained by their inhibition of acid phosphatases/PTPases that negatively regulate the cell proliferation of osteoblasts. The complex nature of the involvement of PTPases in bone formation is further suggested by the identification of a novel parathyroid regulated, receptor-like PTPase, OST-PTP, expressed in bone and testis (Mauro et al., J. Biol. Chem. 269: 30659-30667 (1994)). OST-PTP is up-regulated following differentiation and matrix formation of primary osteoblasts and subsequently down-regulated in the osteoblasts which are actively mineralizing bone in culture. It may be hypothesized that PTPase inhibitors may prevent differentiation via inhibition of OST-PTP or other PTPases thereby leading to continued proliferation. This would be in agreement with the above-mentioned effects of fluoride and the observation that the tyrosine phosphatase inhibitor orthovanadate appears to enhance osteoblast proliferation and matrix formation (Lau et al., Endocrinology 116: 2463-2468 (1988)). In addition, it was observed that vanadate, vanadyl and pervanadate all increased the growth of the osteoblast-like cell line UMR106. Vanadyl and pervanadate were stronger stimulators of cell growth than vanadate. Only vanadate was able to regulate the cell differentiation as measured by cell alkaline phosphatase activity (Cortizo et al., Mol. Cell. Biochem. 145: 97-102 (1995)). It is of particular interest to the current invention that several studies have shown that bisphosphonates, such as alendronate and tiludronate, inhibit the PTPase activity in osteoclasts, and that the inhibition of PTPase activity correlated with the inhibition of in vitro osteoclast formation and boneresorption (Schmidt et al., Proc. Natl. Acad. Sci. U.S.A. 93: 3068-3073 (1996); Murakami et al., Bone 20: 399-404 (1997); Opas et al., Biochem. Pharmacol. 54: 721-727 (1997); Skorey et al., J. Biol. Chem. 272: 22472-22480 (1997)). Thus, PTPase inhibitors—other than bisphophonates—can potentially be effective for prevention and/or treatment of osteoporosis.
PTPases: Microorganisms
Dixon and coworkers have called attention to the fact that PTPases may be a key element in the pathogenic properties of Yersinia (reviewed in Clemens et al. Molecular Microbiology 5: 2617-2620 (1991)). This finding was rather surprising since tyrosine phosphate is thought to be absent in bacteria. The genus Yersinia comprises 3 species: Y. pestis (responsible for the bubonic plague), Y. pseudoturberculosis and Y. enterocolitica (causing enteritis and mesenteric lymphadenitis). Interestingly, a dual-specificity phosphatase, VH1, has been identified in Vaccinia virus (Guan et al., Nature 350: 359-263 (1991)). These observations indicate that PTPases may play critical roles in microbial and parasitic infections, and they further point to PTPase inhibitors as a novel, putative treatment principle of infectious diseases.
WO 99/46267 discloses compounds which are pharmacologically useful inhibitors of PTPases. However, the present invention which represents a novel selection under WO 99/46267, discloses a class of compounds which surprisingly are more potent against protein tyrosine phosphatases (e.g. PTP1B) than those disclosed in WO 99/46267.
DESCRIPTION OF THE INVENTION
The present invention relates to Compounds of the Formula 1 wherein n, m, X, R 1 , R 2 , R 3 , R 4 , R 5 and R 6 are defined below;
In the above Formula 1
n is 0, 1 or 2;
m is 1 or 2;
X is S or O;
R 1 is hydrogen, COOR 3 , or R 1 is selected from the group consisting of the following 5-membered heterocycles:
R 2 is hydrogen, C 1 -C 6 alkyl, hydroxy or NR 8 R 9 ;
R 3 is hydrogen, C 1 -C 6 alkyl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyloxyC 1 -C 6 alkyl or C 1 -C 6 alkylcarbonyloxyarylC 1 -C 6 alkyl;
R 4 , R 5 and R 6 are independently hydrogen, trihalomethyl, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, oxo, carboxy, carboxyC 1 -C 6 alkyl, C 1 -C 6 alkyloxy-carbonyl, aryloxycarbonyl, arylC 1 -C 6 alkyloxycarbonyl, C 1 -C 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, aryloxy, arylC 1 -C 6 alkyloxy, arylC 1 -C 6 alkyloxyC 1 -C 6 alkyl, thio, C 1 -C 6 alkylthio, C 1 -C 6 alkylthioC 1 -C 6 alkyl, arylthio, arylC 1 -C 6 alkylthio, arylC 1 -C 6 alkylthioC 1 -C 6 alkyl, NR 8 R 9 , R 8 R 9 NC 1 -C 6 alkyl, C 1 -C 6 alkylaminoC 1 -C 6 alkyl, arylaminoC 1 -C 6 alkyl, arylC 1 -C 6 alkylaminoC 1 -C 6 alkyl, di(arylC 1 -C 6 aminoC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkyl-carbonylC 1 -C 6 alkyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkylcarbonylC 1 -C 6 alkyl, C 1 -C 6 alkylcarboxy, C 1 -C 6 alkylcarboxyC 1 -C 6 -alkyl, arylcarboxy, arylcarboxyC 1 -C 6 alkyl, arylC 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkylcarboxyC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonylamino, C 1 -C 6 alkylcarbonylaminoC 1 -C 6 alkyl, arylcarbonylaminoC 1 -C 6 alkyl, -carbonyINR 8 C 1 -C 6 alkylCOR 12 , arylC 1 -C 6 alkylcarbonylamino, arylC 1 -C 6 alkylcarbonylaminoC 1 -C 6 alkyl, CONR 8 R 9 , or C 1 -C 6 alkylCONR 8 R 9 wherein the alkyl and aryl groups are optionally substituted and R 12 is NR 8 R 9 , or C 1 -C 6 alkylNR 8 R 9 ;
R 7 is hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkoxycarbonyl, arylcarbonyl, aryloxocarbonyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkoxycarbonyl, C 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkylcarboxy, R 10 R 11 NcarbonylC 1 -C 6 alkyl wherein R 10 and R 11 are independently selected from hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, arylcarbonyl, arylC 1 -C 6 alkylcarbonyl, C 1 -C 6 alkylcarboxy or arylC 1 -C 6 alkyl-carboxy; wherein the alkyl and aryl groups are optionally substituted;
R 8 and R 9 are independently selected from hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkoxycarbonyl, arylcarbonyl, aryloxocarbonyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkoxycarbonyl, C 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkylcarboxy, R 10 R 11 NcarbonylC 1 -C 6 alkyl wherein the alkyl and aryl groups are optionally substituted; or R 8 and R 9 are together with the nitrogen to which they are attached forming a saturated, partially saturated or aromatic cyclic, bicyclic or tricyclic ring system containing from 3 to 14 carbon atoms and from 0 to 3 additional heteroatoms selected from nitrogen, oxygen or sulphur, the ring system can optionally be substituted with at least one C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, oxo, C 1 -C 6 alkyloxy, arylC 1 -C 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, NR 10 R 11 or C 1 -C 6 alkylaminoC 1 -C 6 alkyl, wherein R 10 and R 11 are independently selected from hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, arylcarbonyl, arylC 1 -C 6 alkylcarbonyl, C 1 -C 6 alkylcarboxy or arylC 1 -C 6 alkylcarboxy; wherein the alkyl and aryl groups are optionally substituted; or
R 8 and R 9 are independently a saturated or partial saturated cyclic 5, 6 or 7 membered amine, imide or lactam;
or a salt thereof with a pharmaceutically acceptable acid or base, or any optical isomer or mixture of optical isomers, including a racemic mixture, or any tautomeric form, or prodrug thereof.
The compounds of the invention can be further modified to act as prodrugs.
It is a well known problem in drug discovery that compounds, such as enzyme inhibitors, may be very potent and selective in biochemical assays, yet be inactive in vivo. This lack of so-called bioavailability may be ascribed to a number of different factors such as lack of or poor absorption in the gut, first pass metabolism in the liver, poor uptake in cells. Although the factors determining bioavailability are not completely understood, there are many examples in the scientific literature—well known to those skilled in the art—of how to modify compounds, which are potent and selective in biochemical assays but show low or no activity in vivo, into drugs that are biologically active. It is within the scope of the invention to modify the compounds of the invention, termed the ‘original compound’, by attaching chemical groups that will improve the bioavailability of said compounds in such a way that the uptake in cells or mammals is facilitated. Examples of said modifications, which are not intended in any way to limit the scope of the invention, include changing of one or more carboxy groups to esters (for instance methyl esters, ethyl esters, acetoxymethyl esters or other acyloxymethyl esters). Compounds of the invention, original compounds, such modified by attaching chemical groups are termed ‘modified compounds’. Said chemical groups may or may not be apparent in the claims of this invention. Other examples of modified compounds, which are not intended in any way to limit the scope of the invention, are compounds that have been cyclized at specific positions—socalled ‘cyclic compounds’—which upon uptake in cells or mammals become hydrolyzed at the same specific position(s) in the molecule to yield the compounds of the invention, the original compounds, which are then said to be ‘non-cyclic’. For the avoidance of doubt, it is understood that the latter original compounds in most cases will contain other cyclic or heterocyclic structures that will not be hydrolyzed after uptake in cells or mammals. Generally, said modified compounds will not show a behaviour in bio-chemical assays similar to that of the original compound, i.e. the corresponding compounds of the invention without the attached chemical groups or said modifications. Said modified compounds may even be inactive in biochemical assays. However, after uptake in cells or mammals these attached chemical groups of the modified compounds may in turn be removed spontaneously or by endogenous enzymes or enzyme systems to yield compounds of the invention, original compounds. ‘Uptake’ is defined as any process that will lead to a substantial concentration of the compound inside cells or in mammals. After uptake in cells or mammals and after removal of said attached chemical group or hydrolysis of said cyclic compound, the compounds may have the same structure as the original compounds and thereby regain their activity and hence become active in cells and/or in vivo after uptake. A number of procedures, well known to those skilled in the art, may be used to verify that the attached chemical groups have been removed or that the cyclic compound has been hydrolyzed after uptake in cells or mammals. An example, which is not intended in any way to limit the scope of the invention, is given in the following. A mammalian cell line, which can be obtained from the American Tissue Type Collection or other similar governmental or commercial sources, is incubated with said modified compound. After incubation at conditions well known to those skilled in the art, the cells are washed appropriately, lysed and the lysate is isolated. Appropriate controls, well known to those skilled in the art, must be included. A number of different procedures, well known to those skilled in the art, may in turn be used to extract and purify said compound from said lysate. Said compound may or may not retain the attached chemical group or said cyclic compound may or may not have been hydrolyzed. Similarly, a number of different procedures—well known to those skilled in the art—may be used to structurally and chemically characterize said purified compound. Since said purified compound has been isolated from said cell lysate and hence has been taken up by said cell line, a comparison of said structurally and chemically characterized compound with that of the original unmodified compound (i.e. without said attached chemical group or said non-cyclic compound) will immediately provide those skilled in the art information on whether the attached chemical group as been removed in the cell or if the cyclic compound has been hydrolyzed. As a further analysis, said purified compound may be subjected to enzyme kinetic analysis as described in detail in the present invention. If the kinetic profile is similar to that of the original compound without said attached chemical group, but different from said modified compound, this confirms that said chemical group has been removed or said cyclic compounds has been hydrolyzed. Similar techniques may be used to analyze compounds of the invention in whole animals and mammals.
A preferred prodrug is acetoxymethyl esters of the compounds of the present invention which may be prepared by the following general procedure (C. Schultz et al, The Journal of Biological Chemistry, 1993, 268, 6316-6322.):
A carboxylic acid (1 equivalent) is suspended in dry acetonitrile (2 ml per 0.1 mmol). Diisopropyl amine (3.0 equivalents) is added followed by bromomethyl acetate (1.5 equivalents). The mixture is stirred under nitrogen overnight at room temperature. Acetonitrile is removed under reduced pressure to yield an oil which is diluted in ethylacetate and washed with water (3×). The organic layer is dried over anhydrous magnesium sulfate. Filtration followed by solvent removal under reduced pressure afford a crude oil. The product is purified by column chromatography on silica gel, using an appropriate solvent system.
DEFINITIONS
As used herein, the term “attached” or “—” (e.g. —COR 11 which indicates the carbonyl attachment point to the scaffold) signifies a stable covalent bond, certain preferred points of attachment points being apparent to those skilled in the art.
The terms “halogen” or “halo” include fluorine, chlorine, bromine, and iodine.
The term “alkyl” includes C 1 -C 6 straight chain saturated, methylene and C 2 -C 6 unsaturated aliphatic hydrocarbon groups, C 1 -C 6 branched saturated and C 2 -C 6 unsaturated aliphatic hydrocarbon groups, C 3 -C 6 cyclic saturated and C 5 -C 6 unsaturated aliphatic hydrocarbon groups, and C 1 -C 6 straight chain or branched saturated and C 2 -C 6 straight chain or branched unsaturated aliphatic hydrocarbon groups substituted with C 3 -C 6 cyclic saturated and unsaturated aliphatic hydrocarbon groups having the specified number of carbon atoms. For example, this definition shall include but is not limited to methyl (Me), ethyl (Et), propyl (Pr), butyl (Bu), pentyl, hexyl, heptyl, ethenyl, propenyl, butenyl, penentyl, hexenyl, isopropyl (i-Pr), isobutyl (i-Bu), tert-butyl (t-Bu), sec-butyl (s-Bu), isopentyl, neopentyl, cyclopropyl, cyclobutyl, cyclopentyl, cyclohexyl, cyclopentenyl, cyclohexenyl, methylcyclopropyl, ethylcyclohexenyl, butenylcyclopentyl, and the like.
The term “substituted alkyl” or “optionally substituted alkyl” represents an alkyl group as defined above wherein the substitutents are independently selected from halo, cyano, nitro, trihalomethyl, carbamoyl, hydroxy, oxo, COOR 3 , CONR 8 R 9 , C 1 -C 6 alkyl, C 1 -C 6 alkyloxy, aryloxy, arylC 1 -C 6 alkyloxy, thio, C 1 -C 6 alkylthio, arylthio, arylC 1 -C 6 alkylthio, NR 8 R 9 , C 1 -C 6 alkylamino, arylamino, arylC 1 -C 6 alkylamino, di(arylC 1 -C 6 alkyl)amino, C 1 -C 6 alkylcarbonyl, arylC 1 -C 6 -alkylcarbonyl, C 1 -C 6 alkylcarboxy, arylcarboxy, arylC 1 -C 6 alkylcarboxy, C 1 -C 6 alkylcarbonylamino, -C 1 -C 6 alkylaminoCOR 12 , arylC 1 -C 6 alkylcarbonylamino, tetrahydrofuranyl, morpholinyl, piperazinyl, —CONR 8 R 9 , —C 1 -C 6 alkylCONR 8 R 9 , or a saturated or partial saturated cyclic 5, 6 or 7 membered amine, imide or lactam; wherein R 11 is hydroxy, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkyloxy, aryloxy, arylC 1 -C 6 alkyloxy and R 3 is defined as above or NR8R9, wherein R 8 , R 9 are defined as above.
The term “saturated, partially saturated or aromatic cyclic, bicyclic or tricyclic ring system” represents but are not limit to aziridinyl, pyrrolyl, pyrrolinyl, pyrrolidinyl, imidazolyl, 2-imidazolinyl, imidazolidinyl, pyrazolyl, 2-pyrazolinyl, 1,2,3-triazolyl, 1,2,4-triazolyl, morpholinyl, piperidinyl, thiomorpholinyl, piperazinyl, indolyl, isoindolyl, 1,2,3,4-tetrahydro-quinolinyl, 1 ,2,3,4-tetrahydro-isoquinolinyl, 1,2,3,4-tetrahydro-quinoxalinyl, indolinyl, indazolyl, benzimidazolyl, benzotriazolyl, purinyl, carbazolyl, acridinyl, phenothiazinyl, phenoxazinyl, iminodibenzyl, iminostilbenyl.
The term “alkyloxy” (e.g. methoxy, ethoxy, propyloxy, allyloxy, cyclohexyloxy) represents an “alkyl” group as defined above having the indicated number of carbon atoms attached through an oxygen bridge.
The term “alkyloxyalkyl” represents an “alkyloxy” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “alkyloxyalkyloxy” represents an “alkyloxyalkyl” group attached through an oxygen atom as defined above having the indicated number of carbon atoms.
The term “aryloxy” (e.g. phenoxy, naphthyloxy and the like) represents an aryl group as defined below attached through an oxygen bridge.
The term “arylalkyloxy” (e.g. phenethyloxy, naphthylmethyloxy and the like) represents an “arylalkyl” group as defined below attached through an oxygen bridge.
The term “arylalkyloxyalkyl” represents an “arylalkyloxy” group as defined above attached through an “alkyl” group defined above having the indicated number of carbon atoms.
The term “arylthio” (e.g. phenylthio, naphthylthio and the like) represents an “aryl” group as defined below attached through an sulfur bridge.
The term “alkyloxycarbonyl” (e.g. methylformiat, ethylformiat and the like) represents an “alkyloxy” group as defined above attached through a carbonyl group.
The term “aryloxycarbonyl” (e.g. phenylformiat, 2-thiazolylformiat and the like) represents an “aryloxy” group as defined above attached through a carbonyl group.
The term “arylalkyloxycarbonyl” (e.g. benzylformiat, phenyletylformiat and the like) represents an “arylalkyloxy” group as defined above attached through a carbonyl group.
The term “alkyloxycarbonylalkyl” represents an “alkyloxycarbonyl” group as defined above attached through an “alkyl” group as defined above having the indicated number of carbon atoms.
The term “arylalkyloxycarbonylalkyl” represents an “arylalkyloxycarbonyl” group as defined above attached through an “alkyl” group as defined above having the indicated number of carbon atoms.
The term “alkylthio” (e.g. methylthio, ethylthio, propylthio, cyclohexenylthio and the like) represents an “alkyl” group as defined above having the indicated number of carbon atoms attached through a sulfur bridge.
The term “arylalkylthio” (e.g. phenylmethylthio, phenylethylthio, and the like) represents an “arylalkyl” group as defined above having the indicated number of carbon atoms attached through a sulfur bridge.
The term “alkylthioalkyl” represents an “alkylthio” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “arylalkylthioalkyl” represents an “arylalkylthio” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “alkylamino” (e.g. methylamino, diethylamino, butylamino, N-propyl-N-hexylamino, (2-cyclopentyl)propylamino, hexenylamino, pyrrolidinyl, piperidinyl and the like) represents one or two “alkyl” groups as defined above having the indicated number of carbon atoms attached through an amine bridge. The two alkyl groups may be taken together with the nitrogen to which they are attached forming a saturated, partially saturated or aromatic cyclic, bicyclic or tricyclic ring system containing 3 to 14 carbon atoms and 0 to 3 additional heteroatoms selected from nitrogen, oxygen or sulfur, the ring system can optionally be substituted with at least one C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, oxo, C 1 - 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, NR 8 R 9 , C 1 -C 6 alkylaminoC 1 -C 6 alkyl substituent wherein the alkyl and aryl groups are optionally substituted as defined in the definition section and R 8 and R 9 are defined as above.
The term “arylalkylamino” (e.g. benzylamino, diphenylethylamino and the like) represents one or two “arylalkyl” groups as defined above having the indicated number of carbon atoms attached through an amine bridge. The two “arylalkyl” groups may be taken together with the nitrogen to which they are attached forming a saturated, partially saturated or aromatic cyclic, bicyclic or tricyclic ring system containing 3 to 14 carbon atoms and 0 to 3 additional heteroatoms selected from nitrogen, oxygen or sulfur, the ring system can optionally be substituted with at least one C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, oxo, C 1 -C 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, NR 8 R 9 , C 1 -C 6 alkylaminoC 1 -C 6 alkyl substituent wherein the alkyl and aryl groups are optionally substituted as defined in the definition section and R 8 and R 9 are defined as above.
The term “alkylaminoalkyl” represents an “alkylamino” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “arylalkylaminoalkyl” represents an “arylalkylamino” group attached through an alkyl group as defined above having the indicated number of carbon atoms. 10 The term “arylamino” represents an “aryl” group as defined below attached through an amino group.
The term “arylaminoalkyl” represents an “arylamino” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “arylalkyl” (e.g. benzyl, phenylethyl) represents an “aryl” group as defined below attached through an alkyl having the indicated number of carbon atoms or substituted alkyl group as defined above.
The term “alkylcarbonyl” (e.g. cyclooctylcarbonyl, pentylcarbonyl, 3-hexenylcarbonyl) represents an “alkyl” group as defined above having the indicated number of carbon atoms attached through a carbonyl group.
The term “arylcarbonyl” (benzoyl) represents an “aryl” group as defined above attached through a carbonyl group.
The term “arylalkylcarbonyl” (e.g. phenylcyclopropylcarbonyl, phenylethylcarbonyl and the like) represents an “arylalkyl” group as defined above having the indicated number of carbon atoms attached through a carbonyl group.
The term “alkylcarbonylalkyl” represents an “alkylcarbonyl” group attached through an “alkyl” group as defined above having the indicated number of carbon atoms.
The term “arylalkylcarbonylalkyl” represents an “arylalkylcarbonyl” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “arylcarbonylamino” represents an “arylcarbonyl” group as defined above attached through an amino group.
The term “arylcarbonylaminoalkyl” represents an “arylcarbonylamino” group attached through an alkyl group as defined above having the indicated number of carbon atoms.
The term “alkylcarboxy” (e.g. heptylcarboxy, cyclopropylcarboxy, 3-pentenylcarboxy) represents an “alkylcarbonyl” group as defined above wherein the carbonyl is in turn attached through an oxygen bridge.
The term “arylcarboxyalkyl” (e.g. phenylcarboxymethyl) represents an “arylcarbonyl” group defined above wherein the carbonyl is in turn attached through an oxygen bridge to an alkyl chain having the indicated number of carbon atoms.
The term “arylalkylcarboxy” (e.g. benzylcarboxy, phenylcyclopropylcarboxy and the like) represents an “arylalkylcarbonyl” group as defined above wherein the carbonyl is in turn attached through an oxygen bridge.
The term “alkylcarboxyalkyl” represents an “alkylcarboxy” group attached through an “alkyl” group as defined above having the indicated number of carbon atoms.
The term “arylalkylcarboxyalkyl” represents an “arylalkylcarboxy” group attached through an “alkyl” group as defined above having the indicated number of carbon atoms.
The term “alkylcarbonylamino” (e.g. hexylcarbonylamino, cyclopentylcarbonyl- aminomethyl, methylcarbonylaminophenyl) represents an “alkylcarbonyl” group as defined above wherein the carbonyl is in turn attached through the nitrogen atom of an amino group. The nitrogen atom may itself be substituted with an alkyl or aryl group.
The term “arylalkylcarbonylamino” (e.g. benzylcarbonylamino and the like) represents an “arylalkylcarbonyl” group as defined above wherein the carbonyl is in turn attached through the nitrogen atom of an amino group. The nitrogen atom may itself be substituted with an alkyl or aryl group.
The term “alkylcarbonylaminoalkyl” represents an “alkylcarbonylamino” group attached through an “alkyl” group as defined above having the indicated number of carbon atoms. The nitrogen atom may itself be substituted with an alkyl or aryl group.
The term “arylalkylcarbonylaminoalkyl” represents an “arylalkylcarbonylamino” group attached through an “alkyl” group as defined above having the indicated number of carbon atoms. The nitrogen atom may itself be substituted with an alkyl or aryl group.
The term “alkylcarbonylaminoalkylcarbonyl” represents an alkylcarbonylaminoalkyl group attached through a carbonyl group. The nitrogen atom may be further substituted with an “alkyl” or “aryl” group.
The term “aryl” represents an unsubstituted, monocyclic, polycyclic, biaryl and heterocyclic aromatic groups covalently attached at any ring position capable of forming a stable covalent bond, certain preferred points of attachment being apparent to those skilled in the art (e.g., 3-indolyl, 4(5)-imidazolyl).
The definition of aryl includes but is not limited to phenyl, biphenyl, indenyl, fluorenyl, naphthyl (1-naphthyl, 2-naphthyl), pyrrolyl (2-pyrrolyl), pyrazolyl (3-pyrazolyl), imidazolyl (1-imidazolyl, 2-imidazolyl, 4-imidazolyl, 5-imidazolyl), triazolyl (1,2,3-triazol-1-yl, 1,2,3-triazol-2-yl 1,2,3-triazol4-yl, 1,2,4-triazol-3-yl), oxazolyl (2-oxazolyl, 4-oxazolyl, 5-oxazolyl), isoxazolyl (3-isoxazolyl, 4-isoxazolyl, 5-isoxazolyl), thiazolyl (2-thiazolyl, 4-thiazolyl, 5-thiazolyl), thiophenyl (2-thiophenyl, 3-thiophenyl, 4-thiophenyl, 5-thiophenyl), furanyl (2-furanyl, 3-furanyl, 4-furanyl, 5-furanyl), pyridyl (2-pyridyl, 3-pyridyl, 4-pyridyl, 5-pyridyl), 5-tetrazolyl, pyrimidiny (2-pyrimidinyl, 4-pyrimidinyl, 5-pyrimidinyl, 6-pyrimidinyl), pyrazinyl, pyridazinyl (3-pyridazinyl, 4-pyridazinyl, 5-pyridazinyl), quinolyl (2-quinolyl, 3-quinolyl, 4-quinolyl, 5-quinolyl, 6-quinolyl, 7-quinolyl, 8-quinolyl), isoquinolyl (1-isoquinolyl, 3-isoquinolyl, 4-isoquinolyl, 5-isoquinolyl, 6-isoquinolyl, 7-isoquinolyl, 8-isoquinolyl), benzo[b]furanyl (2-benzo[b]furanyl, 3-benzo[b]furanyl, 4-benzo[b]furanyl, 5-benzo[b]furanyl, 6-benzo[b]furanyl, 7-benzo[b]furanyl), 2,3-dihydro-benzo[b]furanyl (2-(2,3-dihydro-benzo[b]furanyl), 3-(2,3-dihydro-benzo[b]furanyl), 4-(2,3-dihydro-benzo[b]furanyl), 5-(2,3-dihydro-benzo-[b]furanyl), 6-(2,3-dihydro-benzo-[b]furanyl) 7-(2,3-dihydro-benzo[b]furanyl)), benzo[b]thiophenyl (2-benzo[b]thiophenyl, 3-benzo[b]thiophenyl, 4-benzo[b]thiophenyl, 5-benzo[b]thiophenyl, 6-benzo[b]thiophenyl, 7-benzo[b]thiophenyl), 2,3-dihydro-benzo[b]-thiophenyl (2-(2,3-dihydro-benzo[b]thiophenyl), 3-(2,3-dihydro-benzo[b]-thiophenyl), 4-(2,3-dihydro-benzo[b]thiophenyl), 5-(2,3-dihydro-benzo[b ]-thiophenyl), 6-(2,3-dihydro-benzo[b]thiophenyl), 7-(2, 3-dihydro-benzo[b]-thiophenyl)), 4,5,6,7-tetrahydro-benzo[b]thiophenyl (2-(4,-5,6,7=tetrahydro-benzo-[b]thiophenyl), 3-(4,5,6,7-tetrahydro-benzo-[b]thiophenyl), 4-(4,5,6,7-tetrahydro-benzo[b]thiophenyl), 5-(4,5,6,7-tetrahydro-benzo-[b]thiophenyl), 6-(4, 5,6,7tetrahydro-benzo-[b]thiophenyl), 7-(4,5,6,7-tetrahydro-benzo[b]thiophenyl)), 4-,5,6,7-tetrahydro-thieno[2,3-c]pyridyl (4-(4,5,6,7-tetrahydro-thieno[2,3-c]pyridyl), 5-4,5,6,7-tetrahydro-thieno[2,3-c]pyridyl) 6-(4,5,6,7-tetrahydro-thieno[2,3-c]pyridyl), 7-(4,5,6,7-tetrahydro-thieno[2,3-c]pyridyl)), indolyl (1-indolyl, 2-indolyl, 3-indolyl, 4-indolyl, 5-indolyl, 6-indolyl, 7-indolyl), isoindolyl (1-isoindolyl, 2-isoindolyl, 3-isoindolyl, 4-isoindolyl, 5-isoindolyl, 6-isoindolyl, 7-isoindolyl), 1,3-dihydro -isoindolyl (1-(1,3-dihydro-isoindolyl), 2-(1,3-dihydro-isoindolyl), 3-(1,3-dihydro-isoindolyl), 4-(1,3-dihydro-isoindolyl), 5-(1,3-dihydro-isoindolyl), 6-(1,3-dihydro-isoindolyl), 7-(1,3-dihydro -isoindolyl)), indazole (1-indazolyl, 3-indazolyl, 4-indazolyl, 5-indazolyl, 6-indazolyl, 7-indazolyl), benzimidazolyl (1-benzimidazolyl, 2-benzimidazolyl, 4-benzimidazolyl, 5-benzimidazolyl, 6-benzimidazolyl, 7-benzimidazolyl, 8-benzimidazolyl), benzoxazolyl (1-benzo-oxazolyl, 2-benzoxazolyl), benzothiazolyl (1-benzothiazolyl, 2-benzo-thiazolyl, 4-benzothiazolyl, 5-benzothiazolyl, 6-benzothiazolyl, 7-benzothiazolyl), carbazolyl (1-carbazolyl, 2-carbazolyl, 3-carbazolyl, 4-carbazolyl), 5H-dibenz[b,f]azepine (5H-dibenz[b,f]azepin-1-yl, 5H-dibenz-[b,f]azepine-2-yl, 5H-dibenz[b,f]azepine-3-yl, 5H-dibenz-[b,f]azepine4-yl, 5H-dibenz[b,f]-azepine-5-yl), 10,11-dihydro-5H-dibenz[b,f]azepine (10,11 -dihydro-5H-dibenz[b,f]azepine-1-yl, 10,11-dihydro-5H-dibenz[b,f]azepine-2-yl, 10,11-dihydro-5H-dibenz[b,f]azepine-3-yl, 10,11-dihydro-5H-dibenz-[b,f]azepine-4-yl, 10,11-dihydro-5H-dibenz [b,f]azepine-5-yl), piperidinyl (2-piperidinyl, 3-piperidinyl, 4-piperidinyl), pyrrolidinyl (1-pyrrolidinyl, 2-pyrrolidinyl, 3-pyrrolidinyl), phenylpyridyl (2-phenyl-pyridyl, 3-phenyl-pyridyl, 4-phenylpridyl), phenylpyrimidinyl (2-phenylpyrimidinyl, 4-phenyl-pyrimidinyl, 5-phenylpyrimidinyl, 6-phenylpyrimidinyl), phenylpyrazinyl, phenylpyridazinyl (3-phenylpyridazinyl, 4-phenylpyridazinyl, 5-phenyl-pyridazinyl).
The term “optionally substituted aryl” represents an mono-, di- or trisubstituted aryl as defined above wherein the substituents are independently selected from the group consisting of halo, nitro, cyano, trihalomethyl, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, COOR 3 , CONR 8 R 9 , C 1 -C 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, aryloxy, arylC 1 -C 6 alkyloxy, arylC 1 -C 6 alkyloxyC 1 -C 6 alkyl, thio, C 1 -C 6 alkylthio, C 1 -C 6 alkylthioC 1 -C 6 alkyl, arylthio, arylC 1 -C 6 alkylthio, arylC 1 -C 6 alkylthioC 1 -C 6 alkyl, NR 8 R 9 , C 1 -C 6 -alkylamino, C 1 -C 6 (alkyl-aminoC 1 -C 6 alkyl, arylamino, arylC 1 -C 6 alkylamino, arylC 1 -C 6 alkyl-aminoC 1 -C 6 alkyl, di(arylC 1 -C 6 alkyl)aminoC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkyl-carbonylC 1 -C 6 alkyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkylcarbonylC 1 -C 6 alkyl, C 1 -C 6 alkyl-carboxy, C 1 -C 6 alkylcarboxyC 1 -C 6 alkyl, arylC 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkyl-carboxyC 1 -C 6 alkyl, carboxyC 1 -C 6 -alkyloxy, C 1 -C 6 alkylcarbonylamino, C 1 -C 6 alkyl-carbonylaminoC 1 -C 6 alkyl, -carbonyINR 7 C 1 -C 6 alkylCOR 11 , arylC 1 -C 6 alkylcarbonyl-amino, arylC 1 -C 6 -alkylcarbonylaminoC 1 -C 6 alkyl, —CONR 8 R 9 , or —C 1 -C 6 alkylCONR 8 R 9 ; wherein R 3 , R 8 , R 9 , and R 11 , are defined as above and the alkyl and aryl groups are optionally substituted as defined in the definition section;
The term “arylcarbonyl” (e.g. 2-thiophenylcarbonyl, 3-methoxy-anthrylcarbonyl, oxazolylcarbonyl) represents an “aryl” group as defined above attached through a carbonyl group.
The term “arylalkylcarbonyl” (e.g. (2,3-dimethoxyphenyl)propylcarbonyl, (2-chloronaphthyl)pentenylcarbonyl, imidazolylcyclopentylcarbonyl) represents an “arylalkyl” group as defined above wherein the “alkyl” group is in turn attached through a carbonyl.
The compounds of the present invention have asymmetric centers and may occur as racemates, racemic mixtures, and as individual enantiomers or diastereoisomers, with all isomeric forms being included in the present invention as well as mixtures thereof.
Pharmaceutically acceptable salts of the Compounds of Formula 1, where a basic or acidic group is present in the structure, are also included within the scope of this invention. When an acidic substituent is present, such as —COOH, 5-tetrazolyl or —P(O)(OH) 2 , there can be formed the ammonium, morpholinium, sodium, potassium, barium, calcium salt, and the like, for use as the dosage form. When a basic group is present, such as amino or a basic heteroaryl radical, such as pyridyl, an acidic salt, such as hydrochloride, hydrobromide, phosphate, sulfate, trifluoroacetate, trichloroacetate, acetate, oxalate, maleate, pyruvate, malonate, succinate, citrate, tartarate, fumarate, mandelate, benzoate, cinnamate, methanesulfonate, ethane sulfonate, picrate and the like, and include acids related to the pharmaceutically acceptable salts listed in Journal of Pharmaceutical Science, 66, 2 (1977) and incorporated herein by reference, can be used as the dosage form.
Also, in the case of the —COOH or —P(O)(OH) 2 being present, pharmaceutically acceptable esters can be employed, e.g., methyl, tert-butyl, pivaloyloxymethyl, and the like, and those esters known in the art for modifying solubility or hydrolysis characteristics for use as sustained release or prodrug formulations.
In addition, some of the compounds of the present invention may form solvates with water or common organic solvents. Such solvates are encompassed within the scope of the invention.
The term “therapeutically effective amount” shall mean that amount of drug or pharmaceutical agent that will elicit the biological or medical response of a tissue, system, animal, or human that is being sought by a researcher, veterinarian, medical doctor or other. In a preferred embodiment, the present invention is concerned with compounds of Formula I
wherein
n is 0, 1 or 2;
m is 1 or 2;
X is S or O;
R 1 is hydrogen or COOR 3 , or R 1 is selected from the group consisting of the following 5-membered heterocycles:
R 2 is hydrogen, C 1 -C 6 alkyl, hydroxy or NR 8 R 9 ;
R 3 is hydrogen, C 1 -C 6 alkyl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyloxyC 1 -C 6 alkyl or C 1 -C 6 alkylcarbonyloxyarylC 1 -C 6 alkyl;
R 4 , R 5 and R 6 are independently hydrogen, trihalomethyl, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, oxo, carboxy, carboxyC 1 -C 6 alkyl, C 1 -C 6 alkyloxy-carbonyl, aryloxycarbonyl, arylC 1 -C 6 alkyloxycarbonyl, C 1 -C 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, aryloxy, arylC 1 -C 6 alkyloxy, arylC 1 -C 6 alkyloxyC 1 -C 6 alkyl, thio, C 1 -C 6 alkyl-thio, C 1 -C 6 alkylthioC 1 -C 6 alkyl, arylthio, arylC 1 -C 6 alkylthio, arylC 1 -C 6 alkylthioC 1 -C 6 alkyl, NR 8 R 9 , C 1 -C 6 alkylaminoC 1 -C 6 alkyl, arylC 1 -C 6 alkylaminoC 1 -C 6 alkyl, di(arylC 1 -C 6 alkyl)aminoC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkylcarbonylC 1 -C 6 alkyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkylcarbonylC 1 -C 6 alkyl, C 1 -C 6 alkyl-carboxy, C 1 -C 6 alkylcarboxyC 1 -C 6 -alkyl, arylcarboxy, arylcarboxyC 1 -C 6 alkyl, C 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkylcarboxyC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonylamino, C 1 -C 6 alkylcarbonylaminoC 1 -C 6 alkyl, -carbonylNR 8 C 1 -C 6 alkylCOR 12 , arylC 1 -C 6 alkylcarbonylamino, arylC 1 -C 6 alkylcarbonylaminoC 1 -C 6 alkyl, CONR 8 R 9 , or C 1 -C 6 alkylCONR 8 R 9 wherein the alkyl and aryl groups are optionally substituted and R 12 is NR 8 R 9 , or C 1 -C 6 alkynyl 8 R 9 ;
R 7 is hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkoxycarbonyl, arylcarbonyl, aryloxocarbonyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkoxycarbonyl, C 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkylcarboxy, R 10 R 11 NcarbonylC 1 -C 6 alkyl wherein R 10 and R 11 are independently selected from hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, arylcarbonyl, arylC 1 -C 6 alkylcarbonyl, C 1 -C 6 alkylcarboxy or arylC 1 -C 6 alkylcarboxy; wherein the alkyl and aryl groups are optionally substituted; R 8 and R 9 are independently selected from hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, C 1 -C 6 alkoxycarbonyl, arylcarbonyl, aryloxocarbonyl, arylC 1 -C 6 alkylcarbonyl, arylC 1 -C 6 alkoxycarbonyl, C 1 -C 6 alkylcarboxy, arylC 1 -C 6 alkylcarboxy, R 10 R 11 NcarbonylC l -C 6 alkyl wherein the alkyl and aryl groups are optionally substituted; or
R 8 and R 9 are together with the nitrogen to which they are attached forming a saturated, partially saturated or aromatic cyclic, bicyclic or tricyclic ring system containing from 3 to 14 carbon atoms and from 0 to 3 additional heteroatoms selected from nitrogen, oxygen or sulphur, the ring system can optionally be substituted with at least one C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, hydroxy, oxo, C 1 - 6 alkyloxy, arylC 1 -C 6 alkyloxy, C 1 -C 6 alkyloxyC 1 -C 6 alkyl, NR 10 R 11 or C 1 -C 6 alkylaminoC 1 -C 6 alkyl, wherein R 10 and R 11 are independently selected from hydrogen, C 1 -C 6 alkyl, aryl, arylC 1 -C 6 alkyl, C 1 -C 6 alkylcarbonyl, arylcarbonyl, arylC 1 -C 6 alkylcarbonyl, C 1 -C 6 alkylcarboxy or arylC 1 -C 6 alkylcarboxy; wherein the alkyl and aryl groups are optionally substituted; or
R 8 and R 9 are independently a saturated or partial saturated cyclic 5, 6 or 7 membered amine, imide or lactam;
or a salt thereof with a pharmaceutically acceptable acid or base, or any optical isomer or mixture of optical isomers, including a racemic mixture, or any tautomeric form.
In another preferred embodiment, the present invention is concerned with compounds wherein X is sulphur.
In another preferred embodiment, the present invention is concerned with compounds wherein R 1 is COOR 3 and R 2 is hydrogen; wherein R 3 is defined as above.
In another preferred embodiment, the present invention is concerned with compounds wherein n and m are 1.
In another preferred embodiment, the present invention is concerned with compounds wherein R 5 is C 1 -C 6 alkylNR 8 R 9 .
In another preferred embodiment, the present invention is concerned with compounds wherein R 4 and R 6 are hydrogen.
In another preferred embodiment, the present invention is concerned with compounds wherein R 1 is 5-tetrazolyl, R 2 is hydrogen, and R 5 is C 1 -C 6 alkylNR 8 R 9 .
In another preferred embodiment, the present invention is concerned with compounds wherein R 6 is C 1 -C 6 alkylNR 8 R 9 .
In another preferred embodiment, the present invention is concerned with compounds wherein R 4 and R 5 are hydrogen.
In another preferred embodiment, the present invention is concerned with compounds wherein R 1 is 5-tetrazolyl, R 2 is hydrogen, and R 6 is C 1 -C 6 alkylNR 8 R 9 .
In another preferred embodiment, the present invention is concerned with compounds wherein R 5 and R6 are C 1 -C 6 alkylNR 8 R 9 .
In another preferred embodiment, the present invention is concerned with compounds wherein R 1 is COOR 3 and R 2 is hydrogen; wherein R 3 is defined as above.
In another preferred embodiment, the present invention is concerned with compounds wherein R 1 is 5-tetrazolyl.
In another preferred embodiment, the present invention is concerned with compounds wherein R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with two oxo groups.
In another preferred embodiment, the present invention is concerned with compounds wherein the ring system is isoindolyl.
In another preferred embodiments, the present invention is concerned with compounds wherein R 7 is C 1 -C 6 alkoyxcarbonyl.
In another preferred embodiment, the present invention is concerned with compounds wherein R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with two oxo groups.
In another preferred embodiment, the present invention is concerned with compounds wherein the ring system is isoindolyl.
In another preferred embodiment, the present invention is concerned with compounds wherein R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 7 carbon atoms and one sulfur atom, the ring system being optionally substituted with three oxo groups.
In another preferred embodiment, the present invention is concerned with compounds wherein the ring system is 2,3-dihydro-benzo[d]isothiazoly.
In another preferred embodiment, the present invention is concerned with compounds wherein R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 7 carbon atoms and one sulfur atom, the ring system being optionally substituted with two oxo groups.
In another preferred embodiment, the present invention is concerned with compounds wherein the ring system is 2,3-dihydro-benzo[d]isothiazoly.
In another preferred embodiment, the present invention is concerned with compounds wherein R 7 is C 1 -C 6 alkoxycarbonyl.
In another preferred embodiment, the present invention is concerned with compounds wherein R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with one oxo group.
In another preferred embodiment, the present invention is concerned with compounds wherein the ring system is optionally substituted isoindolyl.
In another preferred embodiment, the present invention is concerned with compounds wherein the ring system is optionally substituted 1-oxo-1,3-dihydro-isoindolyl.
In another preferred embodiment, the present invention is concerned with compounds wherein R 7 is C 1 -C 6 alkoxycarbonyl.
In another preferred embodiment, the present invention is concerned with compounds wherein R 5 and R 6 are C 1 -C 6 alkylNR 8 R 9 .
In another preferred embodiment, the present invention is concerned with compounds of Formula I wherein R 5 is 1,3-dihydro-isoindol, substituted with 1 or 2 oxo groups at the atom positions adjacent to the nitrogen atom and optionally substituted with hydroxy, C 1-6 -alkyloxy, arylC 1-6 -alkyloxy or C 1-6 -alkylcarboxy, and wherein R 7 is hydrogen, alkyl, alkyloxycarbonyl, arylalkyl or aryl wherein aryl is optionally substituted with methoxy.
In another preferred embodiment, the present invention is concerned with compounds of Formula I wherein R 5 is 1,1,3-trioxo-1,2-dihydro-1H-benzo[d]isothiazol-2-yl and wherein R 7 is hydrogen or arylalkyl.
In another preferred embodiment, the present invention is concerned with compounds of Formula I wherein R 5 or R 6 is arylaminoalkyl, wherein aryl is 1,1-dioxo-1,2-dihydro-1H-benzo[d]isothiazol-3-yl.
In another preferred embodiment, the present invention is concerned with compounds of Formula I wherein R 5 or R 6 is arylcarbonylaminoalkyl, wherein aryl is phenyl, indol-3-yl, indol-2-yl, 1,2,3-triazol4-yl, quinolin-4-yl or naphth-1-yl wherein aryl is optionally substituted, and wherein R 7 is hydrogen or arylalkyl optionally substituted with methoxy.
In another preferred embodiment, the present invention is concerned with compounds of Formula I wherein R 5 is arylalkylaminoalkyl wherein aryl is phenyl, dibenzofuranyl, naphth-2-yl or indo-3-yl, and wherein alkyl and aryl are optionally substituted, and wherein R 7 is hydrogen or arylalkyl optionally substituted with methoxy.
In another preferred embodiment, the present invention is concerned with compounds of Formula I wherein R 6 is alkylNR 8 R 9 , wherein R 8 is alkylcarbonyl and R 9 is arylalkyl, wherein aryl is optionally substituted.
In a preferred embodiment of the invention X in formula 1 is sulphur. In another preferred embodiment of the invention R 1 is COOR 3 and R 2 is hydrogen; wherein R 3 is hydrogen, C 1 -C 6 alkyl or arylC 1 -C 6 alkyl.
In a further preferred embodiment of the invention n and m are 1.
In a further preferred embodiment of the invention R 4 and R 6 are both hydrogen and R 5 is C 1 -C 6 alkylNR 8 R 9 and R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with two oxo groups.
Most preferred are R 8 and R 9 together with the nitrogen to which they are attached forming an isoindolyl-1,3-dione optionally substituted.
In another preferred embodiment of the invention R 4 and R 5 are both hydrogen and R 6 is C 1 -C 6 alkylNR 8 R 9 and R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with three oxo groups.
Most preferred are R 8 and R 9 together with the nitrogen to which they are attached forming an 1,1-dioxo-1,2-dihydro-1H-benzo[d]isothiazolyl-3-one optionally substituted.
In a further preferred embodiment of the invention R 4 and R 5 are both hydrogen and R 6 is C 1 -C 6 alkylNR 8 R 9 and R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with two oxo groups.
Most preferred are R 8 and R 9 together with the nitrogen to which they are attached forming an isoindolyl-1,3-dione optionally substituted.
In a further preferred embodiment of the invention R 4 and R 6 are both hydrogen and R 5 is C 1 -C 6 alkylNR 8 R 9 and R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with one oxo group.
Most preferred are R 8 and R 9 together with the nitrogen to which they are attached forming an optionally substituted 1-oxo-1,3-dihydro-isoindolyl ring.
In another preferred embodiment of the invention R 4 and R 5 are both hydrogen and R 6 is C 1 -C 6 alkylNR 8 R 9 and R 8 and R 9 are together with the nitrogen to which they are attached forming a partially saturated bicyclic ring system containing 8 carbon atoms, the ring system being optionally substituted with one oxo group.
Most preferred are R 8 and R 9 together with the nitrogen to which they are attached forming an optionally substituted 1-oxo-1,3-dihydro-isoindolyl ring.
In a preferred embodiment of the invention R 7 is C 1 -C 6 alkoxycarbonyl.
The following compounds are preferred:
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 6-ethyl ester;
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
(L)-5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thien [2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(1,1-Dioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
or a pharmaceutically acceptable salt thereof.
The following compounds are also preferred:
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 6-ethyl ester;
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
(S)-5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno [2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-methyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Benzyloxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(S)-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(R)-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(6-Methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3-carboxylic acid;
7-Carbamoyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(2-oxo-tetrahydro-thiophen-3-ylcarbamoyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-phenylcarbamoyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-7-phenylcarbamoyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
or a pharmaceutically acceptable salt thereof.
The following compounds are also preferred:
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 6-ethyl ester;
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(S)-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(4-Hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-methyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Benzyloxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl1)-2-(oxalyl-amino-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(((5-Benzyloxy-1H-indole-2-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(((6-Bromo-2-p-tolyl-quinoline-4-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
6-(4-Methoxy-benzyl)-7-(((5-methyl-2-phenyl-2H-[1,2,3]triazole4-carbonyl)amino)methyl)-2(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(((1H-Indole-3-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-((4-Ethoxy-2-hydroxy-benzoylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino) -4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-((4-Benzoylamino-benzoylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(((Biphenyl4-carbonyl)-amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(((1H-Indole-2-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-((3-Biphenyl4-yl-acryloylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c)pyridine-3-carboxylic acid;
6-(4-Methoxy-benzyl)-7-(((5-methoxy-1H-indole-2-carbonyl)amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-((4-Benzyl-benzoylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
6-(4-Methoxy-benzyl)-7-(((naphthalene-1-carbonyl)amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
6-(4-Methoxy-benzyl)-5-((2-naphthalen-2-yl-ethylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-((2-Benzo[1,3]dioxol-5-yl-acetylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-((2-Dibenzofuran-2-yl-ethyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
6-(4-Methoxy-benzyl)-5-((2-(5-methoxy-2-methyl-1H-indol-3-yl)-acetylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-((2-(1H-Indol-3-yl)-2-oxo-acetylamino)methyl)-2-(Oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(R)-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(S)-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(S)-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(S)-((4-phenoxy-benzylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(S)-((4-Acetylamino-benzylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(S)-((Acetyl-(4-phenoxy-benzyl)amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(S)-((Acetyl-benzyl-amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(S)-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(4-Benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(6-Methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3-carboxylic acid;
7-(R)-Carbamoyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(S)-(2-oxo-tetrahydro-thiophen-3-ylcarbamoyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-5-(S)-phenylcarbamoyl4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
2-(Oxalyl-amino)-7-(R)-phenylcarbamoyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
5-(R),7-(R)-Bis-benzyloxymethyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
6-Benzyl-2-(oxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1,6-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid;
or a salt thereof with a pharmaceutically acceptable acid or base, or any optical isomer or mixture of optical isomers, including a racemic mixture, or any tautomeric form, or prodrug thereof.
PHARMACOLOGICAL METHODS
The compounds are evaluated for biological activity with a truncated form of PTPI B (corresponding to the first 321 amino acids), which was expressed in E. coli and purified to apparent homogeneity using published procedures well-known to those skilled in the art. The enzyme reactions are carried out using standard conditions essentially as described by Burke et al. ( Biochemistry 35; 15989-15996 (1996)). The assay conditions are as follows. Appropriate concentrations of the compounds of the invention are added to the reaction mixtures containing different concentrations of the substrate, p-nitrophenyl phosphate (range: 0.16 to 10 mM—final assay concentration). The buffer used was 50 mM HEPES pH 7.0, 100 mM sodium chloride, 0.1% (w/v) bovine serum albumin, 5 mM glutathione, and 1 mM EDTA. The reaction was started by addition of the enzyme and carried out in microtiter plates at 25° C. for 60 minutes. The reactions are stopped by addition of NaOH. The enzyme activity was determined by measurement of the absorbance at 405 nm with appropriate corrections for absorbance at 405 nm of the compounds and p-nitrophenyl phosphate. The data are analyzed using nonlinear regression fit to classical Michaelis Menten enzyme kinetic models. Inhibition is expressed as K i values in nM. The results of representative experiments are shown in Table 1.
TABLE 1
Inhibition of classical PTP1B by compounds
of the invention
Example
PTP1B
no.
K i values (nM)
8
250
10
270
11
240
12
570
36
830
42
220
46
300
Analysis for Blood Glucose Lowering Effects
The compounds of the invention are tested for blood glucose lowering effects in diabetic, obese female ob/ob mice. The mice are of similar age and body weights and they are randomized into groups of ten mice. They have free access to food and water during the experiment. The compounds are administered by either by gavage, subcutaneous, intravenous or intraperitoneal injections. The control group receives the same volume of vehicle as the mice that receive the compounds. Non-limiting examples of dose-range: 0.1, 0.3, 1.0, 3.0, 10, 30, 100 mg per kg body weight. The blood glucose levels are measured two times before administration of the compounds of the invention and vehicle (to the control group). After administration of the compound, the blood glucose levels are measured at the following time points: 1, 2, 4, 6, and 8 hours. A positive response is defined either as (i) a more than 25 percent reduction in blood glucose levels in the group receiving the compound of the invention compared to the group receiving the vehicle at any time point or (ii) statistically significant (i.e. p<0.05) reduction in the area under the blood glucose curve during the whole period (i.e. 8 hrs) in the group treated with the compounds of the invention compared to the group receiving the vehicle.
Compounds that show positive response can be used as development candidates and used for treatment of human diseases such as diabetes and obesity.
THE SYNTHESIS OF THE COMPOUNDS
In accordance with one aspect of the invention, the compounds of the invention are prepared as illustrated in the following reaction scheme:
a) NCCH 2 COOR 3 , sulphur, morpholine or triethylamine, ethanol; b) R 3 OCOCOimidazole, tetrahydrofuran; c) 25% trifluoroacetic acid/dichloromethane; wherein n, m, X, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 and R 7 are defined above;
When R 4 is hydrogen the reaction step a) in Method A gives a mixture of regioisomers which can be separated by use of column chromatography known to thus skilled in the art.
By allowing an amine (I) and a substituted oxalylamide (II) to react under basic conditions (e.g. K 2 CO 3 , in N,N-dimethylformamide or methylethylketone) or under Mitsunobu conditions (Oyo Mitsunobu, Synthesis , (1981) 1-28) to yield (III) wherein W is OH, OSO 2 Me or halo, and n, m, X, R 1 , R 2 , R 3 , R 4 , R 6 , R 7 and R 8 are defined above.
By allowing an amine (I) and a substituted oxalylamide (II) to react under basic conditions (e.g. K 2 CO 3 , in N,N-dimethylformamide or methylethylketone) or under Mitsunobu conditions (Oyo Mitsunobu, Synthesis , (1981) 1-28) to yield (III) wherein W is OH, OSO 2 Me or halo, and n, m, X, R 1 , R 2 , R 3 , R 4 , R 5 , R 7 and R 8 are defined above.
Pharmacological Preparations
In another aspect, the present invention includes within its scope pharmaceutical compositions comprising, as an active ingredient, at least one of the compounds of the general formula I or a pharmaceutically acceptable salt thereof together with a pharmaceutically acceptable carrier or diluent.
The present compounds may also be administered in combination with one or more further pharmacologically active substances e.g., selected from antiobesity agents, antidiabetics, antihypertensive agents, agents for the treatment and/or prevention of complications resulting from or associated with diabetes and agents for the treatment and/or prevention of complications and disorders resulting from or associated with obesity.
Thus, in a further aspect of the invention the present compounds may be administered in combination with one or more antiobesity agents or appetite regulating agents.
Such agents may be selected from the group consisting of CART (cocaine amphetamine regulated transcript) agonists, NPY (neuropeptide Y) antagonists, MC4 (melanocortin 4) agonists, orexin antagonists, TNF (tumor necrosis factor) agonists, CRF (corticotropin releasing factor) agonists, CRF BP (corticotropin releasing factor binding protein) antagonists, urocortin agonists, β3 agonists, MSH (melanocyte-stimulating hormone) agonists, MCH (melanocyte-concentrating hormone) antagonists, CCK (cholecystokinin) agonists, serotonin re-uptake inhibitors, serotonin and noradrenaline re-uptake inhibitors, mixed serotonin and noradrenergic compounds, 5HT (serotonin) agonists, bombesin agonists, galanin antagonists, growth hormone, growth hormone releasing compounds, TRH (thyreotropin releasing hormone) agonists, UCP 2 or 3 (uncoupling protein 2 or 3) modulators, leptin agonists, DA agonists (bromocriptin, doprexin), lipase/amylase inhibitors, PPAR (peroxisome proliferator activated receptor) modulators, RXR (retinoid X receptor) modulators or TR β agonists.
In one embodiment of the invention the antiobesity agent is leptin.
In another embodiment the antiobesity agent is dexamphetamine or amphetamine.
In another embodiment the antiobesity agent is fenfluramine or dexfenfluramine.
In still another embodiment the antiobesity agent is sibutramine.
In a further embodiment the antiobesity agent is orlistat.
In another embodiment the antiobesity agent is mazindol or phentermine.
Suitable antidiabetics comprise insulin, GLP-1 (glucagon like peptide-1) derivatives such as those disclosed in WO 98/08871 to Novo Nordisk A/S, which is incorporated herein by reference as well as orally active hypoglycaemic agents.
The orally active hypoglycaemic agents preferably comprise sulphonylureas, biguanides, meglitinides, oxadiazolidinediones, thiazolidinediones, glucosidase inhibitors, glucagon antagonists such as those disclosed in WO 99/01423 to Novo Nordisk A/S and Agouron Pharmaceuticals, Inc., GLP-1 agonists, potassium channel openers such as those disclosed in WO 97/26265 and WO 99/03861 to Novo Nordisk A/S which are incorporated herein by reference, insulin sesitizers, DPP-IV (dipeptidyl peptidase-IV) inhibitors, inhibitors of hepatic enzymes involved in stimulation of gluconeogenesis and/or glycogenolysis, glucose uptake modulators, compounds modifying the lipid metabolism such as antihyperlipidemic agents and antilipidemic agents as HMG CoA inhibitors (statins), compounds lowering food intake, PPAR and RXR agonists and agents acting on the ATP-dependent potassium channel of the β-cells.
In one embodiment of the invention the present compounds are administered in combination with insulin.
In a further embodiment the present compounds are administered in combination with a sulphonylurea e.g. tolbutamide, glibenclamide, glipizide or glicazide.
In another embodiment the present compounds are administered in combination with a biguanide e.g. metformin.
In yet another embodiment the present compounds are administered in combination with a meglitinide e.g. repaglinide.
In still another embodiment the present compounds are administered in combination with a thiazolidinedione e.g. troglitazone, ciglitazone, pioglitazone, rosiglitazone or compounds disclosed in WO 97/41097 such as 5-[[4-[3-Methyl-4-oxo-3,4-dihydro-2-quinazolinyl]methoxy]phenyl-methyl]thiazolidine-2,4-dione or a pharmaceutically acceptable salt thereof, preferably the potassium salt.
Furthermore, the present compounds may be administered in combination with the insulin sensitizers disclosed in WO 99/19313 such as (-) 3-[4-[2-Phenoxazin-10-yl)ethoxy]phenyl]-2-ethoxypropanoic acid or a pharmaceutically acceptable salts thereof, preferably the arginine salt.
In a further embodiment the present compounds are administered in combination with an α-glucosidase inhibitor e.g. miglitol or acarbose.
In another embodiment the present compounds are administered in combination with an agent acting on the ATP-dependent potassium channel of the β-cells e.g. tolbutamide, glibenclamide, glipizide, glicazide or repaglinide.
Furthermore, the present compounds may be administered in combination with nateglinide.
In still another embodiment the present compounds are administered in combination with an antihyperlipidemic agent or antilipidemic agent e.g. cholestyramine, colestipol, clofibrate, gemfibrozil, lovastatin, pravastatin, simvastatin, probucol or dextrothyroxine.
In a further embodiment the present compounds are administered in combination with more than one of the above-mentioned compounds e.g. in combination with a sulphonylurea and metformin, a sulphonylurea and acarbose, repaglinide and metformin, insulin and a sulphonylurea, insulin and metformin, insulin, insulin and lovastatin, etc.
Furthermore, the present compounds may be administered in combination with one or more antihypertensive agents. Examples of antihypertensive agents are β-blockers such as alprenolol, atenolol, timolol, pindolol, propranolol and metoprolol, ACE (angiotensin converting enzyme) inhibitors such as benazepril, captopril, enalapril, fosinopril, lisinopril, quinapril and ramipril, calcium channel blockers such as nifedipine, felodipine, nicardipine, isradipine, nimodipine, diltiazem and verapamil, and α-blockers such as doxazosin, urapidil, prazosin and terazosin. Further reference can be made to Remington: The Science and Practice of Pharmacy, 19 th Edition, Gennaro, Ed., Mack Publishing Co., Easton, Pa., 1995.
It should be understood that any suitable combination of the compounds according to the invention with one or more of the above-mentioned compounds and optionally one or more further pharmacologically active substances are considered to be within the scope of the present invention.
For the above indications the dosage will vary depending on the compound of the invention employed, on the mode of administration and on the therapy desired. However, in general, satisfactory results are obtained with a dosage of from about 0.5 mg to about 1000 mg, preferably from about 1 mg to about 500 mg of compounds of the invention, conveniently given from 1 to 5 times daily, optionally in sustained release form. Usually, dosage forms suitable for oral administration comprise from about 0.5 mg to about 1000 mg, preferably from about 1 mg to about 500 mg of the compounds of the invention admixed with a pharmaceutical carrier or diluent.
The compounds of the invention may be administered in a pharmaceutically acceptable acid addition salt form or where possible as a metal or a C 1-6 -alkylammonium salt. Such salt forms exhibit approximately the same order of activity as the free acid forms.
This invention also relates to pharmaceutical compositions comprising a compound of the invention or a pharmaceutically acceptable salt thereof and, usually, such compositions also contain a pharmaceutical carrier or diluent. The compositions containing the compounds of this invention may be prepared by conventional techniques and appear in conventional forms, for example capsules, tablets, solutions or suspensions.
The pharmaceutical carrier employed may be a conventional solid or liquid carrier. Examples of solid carriers are lactose, terra alba, sucrose, talc, gelatine, agar, pectin, acacia, magnesium stearate and stearic acid. Examples of liquid carriers are syrup, peanut oil, olive oil and water.
Similarly, the carrier or diluent may include any time delay material known to the art, such as glyceryl monostearate or glyceryl distearate, alone or mixed with a wax.
If a solid carrier for oral administration is used, the preparation can be tabletted, placed in a hard gelatine capsule in powder or pellet form or it can be in the form of a troche or lozenge. The amount of solid carrier will vary widely but will usually be from about 25 mg to about 1 g. If a liquid carrier is used, the preparation may be in the form of a syrup, emulsion, soft gelatin capsule or sterile injectable liquid such as an aqueous or non-aqueous liquid suspension or solution.
Generally, the compounds of this invention are dispensed in unit dosage form comprising 10-200 mg of active ingredient in or together with a pharmaceutically acceptable carrier per unit dosage.
The dosage of the compounds according to this invention is 1-500 mg/day, e.g. about 100 mg per dose, when administered to patients, e.g. humans, as a drug.
A typical tablet that may be prepared by conventional tabletting techniques contains
Core:
Active compound (as free compound
100
mg
or salt thereof)
Colloidal silicon dioxide (Areosil ®)
1.5
mg
Cellulose, microcryst. (Avicel ®)
70
mg
Modified cellulose gum (Ac-Di-Sol ®)
7.5
mg
Magnesium stearate
Coating:
HPMC
approx. 9
mg
Mywacett ® 9-40 T
approx. 0.9
mg
* Acylated monoglyceride used as plasticiser for film coating.
The route of administration may be any route, which effectively transports the active compound to the appropriate or desired site of action, such as oral or parenteral e.g. rectal, transdermal, subcutaneous, intranasal, intramuscular, topical, intravenous, intraurethral, ophthalmic solution or an ointment, the oral route being preferred.
EXAMPLES
The process for preparing compounds of Formula 1 and preparations containing them is further illustrated in the following examples, which, however, are not to be construed as limiting.
Hereinafter, TLC is thin layer chromatography, CDCl 3 is deuterio chloroform, CD 3 OD is tetradeuterio methanol and DMSO-d 6 is hexadeuterio dimethylsulfoxide. The structures of the compounds are confirmed by either elemental analysis or NMR, where peaks assigned to characteristic protons in the title compounds are presented where appropriate. 1 H NMR shifts (δ H ) are given in parts per million (ppm) down field from tetramethylsilane as internal reference standard. M.p.: is melting point and is given in ° C. and is not corrected. Column chromatography was carried out using the technique described by W. C. Still et al., J. Org. Chem. 43:2923 (1978) on Merck silica gel 60 (Art. 9385). HPLC analyses are performed using 5 μm C18 4×250 mm column eluted with various mixtures of water and acetonitrile, flow=1 ml/min, as described in the experimental section.
Compounds used as starting material are either known compounds or compounds, which can readily be prepared by methods known per se.
Example 1
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 6-ethyl ester
To a solution of 4-(2-spiro[1,3]dioxolane)-piperidine (51.5 g, 0.36 moles) in a mixture of dichloromethane (500 ml) and saturated sodium bicarbonate (500 ml) was added di-tert-butyldicarbonate (69.8 g, 0.32 moles) and the reaction was vigorously stirred for 3 hours and the layers separated. The organic layer was washed with 1N hydrochloric acid (2×150 ml), brine (100 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo affording 75.5 g (97%) of 4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid tert-butyl ester as a crystallizing oil.
1 H-NMR (400 MHz, CDCl 3 ): δ3.96 (s, 4H), 3.49 (bm, 4H), 1.65 (bm, 4H), 1.45 (s, 9H)
To the above 4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid tert-butyl ester (4.0 g, 16.4 mmol) dissolved in dry diethyl ether (32 ml) was added 2,2′ bipyridyl (1 mg) and the solution was cooled to −75° C. Tetramethyl-ethylenediamine (3.2 ml, 21.4 mmol) was added followed by dropwise addition of sec-butyl lithium (16.4 ml, 21.4 mmol, 1.3M in cyclohexane). The mixture was stirred at −75° C. for 10 min, then slowly warmed to −20° C. and stirred at that temperature for 0.5 hour, then cooled to −30° C. At this temperature, formaldehyde was generated by heating paraformaldehyde at 150° C. and passed through the mixture with dry nitrogen until the color faded to off-white, at which time water (40 ml) was added. The layers were separated, and the aqueous layer was extracted with diethyl ether (2×50 ml). The combined organic extracts were washed with 1 N hydrochloric acid (2×75 ml), saturated sodium bicarbonate solution (50 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue (2.9 g) was purified by silica gel chromatography (hexane/ethyl acetate, 10% ethyl acetate to 30% ethyl acetate, gradient). Pure fractions were collected and the solvent evaporated in vacuo affording 1.3 g (29%) of 2-hydroxymethyl-4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid tert-butyl ester as a thick oil.
1 H-NMR (400 MHz, CDCl 3 ): δ4.42 (bm, 1H), 4.08-3.96 (m, 5H), 3.96-3.88 (m, 1H), 3.78-3.70 (m, 1H), 3.30-3.16 (bm, 1H), 2.30-1.98 (bs, 1H), 1.96-1.78 (m, 2H), 1.74-1.64 (m, 2H), 1.49 (s, 9H).
To 2-hydroxymethyl-4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid tert-butyl ester (0.4 g, 1.5 mmol) dissolved in dry tetrahydrofuran (20 ml) was added phthalimide (0.28 g, 1.9 mmol), triphenylphosphine (0.5 g, 1.9 mmol) and the mixture was cooled to 0° C. in an ice bath. Diethyl azodicarboxylate (0.29 ml, 1.82 mmol) was added dropwise and the mixture was stirred at 0° C. for 0.5 hour, then at ambient temperature for 18 hours. The solvent was removed in vacuo and the residue was purified by silica gel chromatography (hexane/ethyl acetate, 18% ethyl acetate to 25% ethyl acetate, gradient). Pure fractions were collected and the solvent evaporated in vacuo affording 0.29 g (48%) of 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid tert-butyl ester.
1 H-NMR (400 MHz, CDCl 3 ): δ7.94-7.80 (bs, 2H), 7.80-7.64 (bd, 2H), 4.96-4.70 (2bs, 1H) 4.66-4.52 (m, 1H), 4.30-4.14 (bm, 1H), 4.12-4.04 (m, 2H), 4.04-3.94 (m, 2H), 3.56-3.32 (m, 2H), 2.04-1.92 (m, 1H), 1.90-1.60 (m, 4H), 1.22-1.00 (bs, 9H).
MS: m/z: 403 [M+H] + , 303 [M−Boc]
To the above 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane) -piperidine1-carboxylic acid tert-butyl ester (1.1 g, 2.7 mmol) dissolved in dichloromethane (6 ml) was added 1.0 N hydrogen chloride in diethyl ether (50 ml) and the solution kept at ambient temperature for 62 hours. The precipitate was filtered off and washed with diethyl ether and dried with nitrogen which afforded 0.83 g (90%) of 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane)-piperidine hydrochloride as a solid.
1 H-NMR (400 MHz, DMSO-d 6 ): δ9.2-8.8 (2bs, 2H), 7.8-8.1 (m, 2H), 4,1-3.6 (m, 5H), 2.9 (bs, 1H), 2.2-1.6 (m, 5H).
MS: m/z: 303.5 [M+H] +
To a suspension of the above 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane)-piperidine hydrochloride (0.7 g, 2.1 mmol) and ethyl chloroformate (0.24 ml, 2.5 mmol) in dry tetrahydrofuran (14 ml) cooled in an ice bath under nitrogen was added diisopropyl-ethylamine (0.95 ml, 5.4 mmol) and the reaction mixture was stirred at ambient temperature for 3 hours. The volatiles were removed in vacuo and the residue was partitioned between dichloromethane (25 ml) and 1 N hydrochloric acid (25 ml). The layers were separated, and the aqueous layer extracted with dichloromethane (20 ml). The combined organic extracts were washed with a saturated sodium bicarbonate solution (50 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was triturated with n-butylchloride, filtered and dried with nitrogen which afforded 0.47 g (61%) of 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid ethyl ester as an oil.
1 H-NMR (400 MHz, CDCl 3 ): δ7.9 (s, 2H), 7.7(s, 2H), 4.9-4.7 (bs, 1H), 4.7-4.5 (m, 1H), 4.3-3.9 (m, 5H), 3.9-3.6 (bs, 1H), 3.6-3.3 (m, 2H), 2.0-1.9 (m, 1H), 1.9-1.5 (m, 4H), 1.1-0.7 (bs, 3H).
MS: m/z: 373 [M−H] 31 .
A solution of the above 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid ethyl ester (0.44 g, 1.2 mmol) in a mixture of 1 N hydrochloric acid (18 ml) and tetrahydrofuran (18 ml) was heated a 75° C. under nitrogen with stirring for 18 hours. The tetrahydrofuran was removed in vacuo and the residue was extracted with dichloromethane (2×75 ml). The combined organic extracts were washed with a saturated sodium bicarbonate solution (50 ml), dried (MgSO 4 ), filtered and the solvent removed in vacuo affording 0.42 g (>100%) of 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-oxo-piperidine-1-carboxylic acid ethyl ester as a solid.
1 H-NMR (400 MHz, CDCl 3 ): δ7.9 (s, 2H), 7.8 (s, 2H), 5.3-5.0 (bm, 1H), 4.6-4.2 (bm, 1H), 4.0 (m, 2H), 3.8-3.6 (bm, 3H), 2.8 (m, 1H), 2.7-2.4 (bm, 3H), 1.0 (bs, 3H).
MS: m/z: 330.6 [M+H] + .
A mixture of the above 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-oxo-piperidine-1-carboxylic acid ethyl ester (0.39 g, 1.2 mmol), tert-butyl cyanoacetate (0.22 g, 1.55 mmol), sulfur (42 mg, 1.3 mmol) in ethanol (1.5 ml) was degassed. To this mixture, under nitrogen, morpholine (205 μl) was added and the mixture was heated a 50° C. for 13 hours. The solvent was removed in vacuo. The residue (0.74 g) was purified by silica gel chromatography using a mixture of hexane/ethyl acetate (7:3) as eluent. Pure fractions were collected and the solvent evaporated in vacuo. The residue (0.29 g) was titurated with acetonitrile, filtered, and dried with nitrogen affording 84 mg (15%) of 2-amino-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 3-tert-butyl ester 6-ethyl ester.
1 H-MNR (400 MHz, CDCl 3 ): δ7.9-7.7 (2m, 4H), 6.0 (bs, 2H), 5.1-4.8 (bm, 1H), 4.8-4.5 (m, 1H), 4.5-4.2 (m, 1H), 4.1-3.4 (3m, 4H), 3.0 (m, 2H), 1.8-1.4 (m, 10H), 1.1-0.9 (m, 3H).
MS: m/z: 486 [M+H] + .
To the above 2-amino-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 3-tert-butyl ester 6-ethyl ester (48 mg, 0.1 mmol) dissolved in dry tetrahydrofuran (1 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (0.4 ml) and the solution stirred for 18 hours at ambient temperature. The solvent was removed in vacuo and the residue was dissolved in dichloromethane (25 ml) and a saturated sodium bicarbonate solution (25 ml) was added. The layers were separated and the aqueous layer was extracted with dichloromethane (25 ml). The combined organic extracts were dried (Na 2 SO 4 ), filtered and the solvent evaporated in vacuo. The residue (63 mg) was dissolved in ethyl acetate and passed through 1 g of silica gel and the solvent evaporated in vacuo affording 55 mg (90%) of 2-(tert-butoxyoxalyl-amino)-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 3-tert-butyl ester 6-ethyl ester as a solid.
The above 2-(tert-butoxyoxalyl-amino)-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid 3-tert-butyl ester 6-ethyl ester (55 mg, 0.09 mmol) was dissolved in 50% trifluoroacetic acid in dichloromethane (2 ml) and stirred at ambient temperature for 18 hours. The volatiles were removed in vacuo and the residue was purified by preparative HPLC (column: Kromasil C18, 250×4.6 mm., flow: 2 ml/min., gradient: acetonitrile/water, 20% acetonitrile to 60% acetonitrile over 20 min.) affording after evaporation of the solvent in vacuo 13.8 mg (31%) of the title compound as a solid trifluoroacetate.
1 H-NMR (400 MHz, DMSO-d 6 ): δ14-13 (bs, 1H), 12.4 (s, 1H), 7.9 (s, 4H), 4.9 (m, 2H), 4.4 (m, 1H), 4.0-2.8 (m, 13H), 0.8 (m, 3H).
MS: m/z: 502 [M+H] + .
Example 2
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
2-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-(2-spiro[1,3]dioxolane)-piperidine-1-carboxylic acid tert-butyl ester (353 mg, 0.88 mmol) was cooled in an ice bath and then dissolved in a solution of 20% trifluoroacetic acid/dichloromethane (7 ml). The reaction was stirred for 5 minutes in the ice bath then another 3 hours at ambient temperature, after which it was concentrated in vacuo affording a solid residue. To the solid was added 2N hydrochloric acid (9 ml) and the mixture was heated at 50° C. (oil bath) with stirring for 24 hours. The cooled reaction mixture was quenched with saturated sodium bicarbonate solution until the pH was basic. The aqueous layer was extracted with chloroform (3×20 ml) and the combined organic extracts dried (K 2 CO 3 ), filtered, and the solvent evaporated in vacuo to give 205 mg (91%) of 2-(4-oxo-piperidin-2-ylmethyl)-isoindole-1,3-dione as a solid.
1 H-NMR (400 MHz, CDCl 3 ): δ7.90-7.83 (m, 2H), 7.78-7.71 (m, 2H), 3.81-3.73 (m, 2H), 3.43-3.35 (m, 1H), 3.30-3.22 (m, 1H), 2.83 (dt, 1H, J=13 Hz and J=3 Hz), 2.46 (d, 1H, J=15 Hz), 2.42-2.32 (m, 2H), 2.21 (dd, 1H, J=14 Hz and J=13 Hz).
APCl-MS: m/z: 259 [M+H] +
The above 2-(4-oxo-piperidin-2-ylmethyl)-isoindole-1,3-dione (0.20 g, 0.76 mmol) was dissolved in dichloromethane (5 ml). Saturated sodium bicarbonate solution (5 ml) was added followed by di-tert-butyl dicarbonate (0.20 g, 0.91 mmol). The reaction was stirred vigorously for 16 hours after which the organic phase was separated. The aqueous layer was extracted with dichloromethane (2×10 ml) and the combined organic extracts were dried (Na 2 SO 4 ), filtered, and the solvent evaporated in vacuo. The residue was purified by silica gel chromatography using a gradient of ethyl acetate/dichloromethane (0 to 10% gradient) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 0.23 g (85%) of 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-oxo-piperidine-1-carboxylic acid tert-butyl ester.
1 H-NMR (400 MHz, CDCl 3 ): δ7.86 (bs, 2H), 7.72 (bs, 2H), 5.15-4.98 (m, 1H), 4.23-4.14 (m, 1H), 3.90 (t, 1H, J=12 Hz), 3.61-3.52 (m, 2H), 2.78-2.70 (m, 1H), 2.57-2.39 (m, 3H), 1.15 (s, 9H).
APCI-MS: m/z: 359 [M+H] +
The above 2-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-oxo-piperidine-1-carboxylic acid tert-butyl ester (0.43 g, 1.2 mmol) was dissolved in absolute ethanol (9 ml). To the solution was added sulfur (42 mg, 1.32 mmol) and tert-butyl cyanoacetate (0.22 g, 1.56 mmol). The mixture was placed under nitrogen and stirred in a 50° C. oil bath. Morpholin (0.21 ml, 2.4 mmol) was added and the reaction was stirred for 16 hours. The precipitate formed was filtered off and washed with acetonitrile (2×3 ml) and dried which afforded 0.18 g of 2-amino-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (A) (30%). The filtrate was concentrated in vacuo and the residue purified by silica gel chromatography using a gradient of ethyl acetate/hexane (1:4 to 1:3 gradient) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 0.3 g of a mixture of 2-amino-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester. HPLC purification of a small portion of the mixture gave 28 mg of pure 2-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (B).
(A)
1 H-NMR (400 MHz, CDCl 3 ): δ7.87-7.82 (m, 2H) 7.73-7.66 (m, 2H), 6.00 (bs, 2H), 5.02-4.87 (m, 1H), 4.72-4.21 (m, 2H), 4.03-3.93 (m, 1H), 3.51 (t, 1H, J=14 Hz), 2.97-2.91 (m, 2H), 1.56 (s, 9H), 1.12-1.09 (s, 9H).
LC-MS: R t =3.96 min, m/z: 514.4 [M+H] +
(B)
1 H-NMR (400 MHz, CDCl 3 ): δ7.88-7.82 (m, 2H), 7.74-7.66 (m, 2H), 5.39-5.19 (m, 1H), 4.30-4.02 (m, 2H), 3.78-3.70 (m, 1H), 3.33-3.18 (m, 1H), 2.86 (dd, 1H, J=18 Hz and J=4 Hz), 2.75-2.61 (m, 1H), 1.54 (s, 9H), 1.13-1.05 (s, 9H).
LC-MS: R t =4.01 min, m/z: 514.4 [M+H] +
To a solution of the above 2-amino-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (50 mg, 0.097 mmol) in dichloromethane (3 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (60 mg, 0.29 mmol). The reaction was placed under nitrogen and stirred for 3 hours at ambient temperature. The solution was concentrated in vacuo and the residue purified by silica gel chromatography using a 5% mixture of ethyl acetate/dichloromethane as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 54 mg (87%) of 2-(tert-butoxyoxalyl-amino)-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester.
1 H-NMR (400 MHz, CDCl 3 ): δ12.52 (s, 1H), 7.85 (bs, 2H), 7.74-7.67 (m, 2H), 5.08-4.92 (m, 1H), 4.93-4.40 (m, 2H), 3.97-3.87 (m, 1H), 3.53 (t, 1H, J=14 Hz), 3.11-2.99 (m, 2H), 1.62 (s, 18H), 1.14-1.12 (2s, 9H).
APCI-MS: m/z: 641 [M−H] −
The above 2-(tert-butoxyoxalyl-amino)-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (54 mg, 0.084 mmol) was dissolved in a solution of 50% trifluoroacetic acid/dichloromethane (2 ml). The reaction was stirred at ambient temperature for 7 hours, concentrated in vacuo and the residue evaporated in vacuo from dichloromethane (3×10 ml). The resulting precipitate was washed with dichloromethane, filtered off and dried in vacuo, which afforded 41 mg (90%) of the title compound as a solid trifluoroacetate.
1 H-NMR (400 MHz, DMSO-d 6 ): δ12.31 (s, 1H), 9.36 (bs, 2H), 7.93-7.90 (m, 2H), 7.88-7.85 (m, 2H), 4.43 (d, 1H, J=16 Hz), 4.26 (d, 1H, J=16 Hz), 4.03-3.91 (m, 2H), 3.83-3.76 (m, 1H), 3.31 (dd, 1H, J=18 Hz and J=4 Hz), 2.82 (dd, 1H, J=18 Hz and J=10 Hz).
APCI-MS: m/z: 430 [M+H] +
HPLC (254.4 nm): R t =6.72 min, 98%
Example 3
5-(S)-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of L-aspartic acid (120 g, 0.90 mol) in methanol (600 ml) cooled to −20° C. was added thionylchoride (93 ml, 1.29 mol) dropwise over 0.5 hour. The cooling bath was removed and the mixture was stirred for 1 hour, before diethyl ether (1.8 L, containing 50 ml 1 N hydrochloric acid in diethyl ether) was added upon cooling. The resulting precipitate was filtered off and washed with diethyl ether. The product was recrystallized twice: First recrystallization: The product was dissolved in warm methanol (600 ml) and reprecipitated with 1.8 ml diethyl ether (containing 50 ml 1 N hydrochloric acid in diethyl ether). Second recrystallization: The product was dissolved in warm methanol (250 ml) and reprecipitated with 1.0 m diethyl ether (containing 50 ml 1 N hydrochloric acid in diethyl ether).
This afforded 75 g (45%) of L-aspartic acid β-methyl ester hydrochloride as a solid.
To a solution of the above β-methyl ester (50 g, 0.27 mol) in water (120 ml) cooled to 0° C. was added triethylamine (95 ml, 0.68 mol) and methyl acrylate (74 ml, 0.82 mol). The reaction mixture was stirred for 3 hours before the cooling bath was removed. After stirring for an additional 1 hour the mixture was washed with petrol ether (2×400 ml), before tert-butanol (40 ml) and di-tert-butyl dicarbonate (74 g, 0.34 mol) was added and the reaction mixture was stirred for 16 hours. The mixture was washed with petrol ether (2×400 ml), cooled to 0° C. and the pH adjusted to 3 with concentrated hydrochloric acid. After extraction with ethyl acetate (3×200 ml) the organic phase was washed with brine (200 ml), dried (MgSO 4 ), filtered and the volatiles evaporated in vacuo. The residue was subjected to column chromatography on silicagel using a mixture of ethyl acetate/hexane/methanol/acetic acid (25:25:2.5:1) as eluent. Pure fractions were collected and the solvent evaporated in vacuo which afforded 60 g (66%) of 2-(tert-butoxycarbonyl-(2-methoxycarbonyl-ethyl)-amino)-succinic acid 4-methyl ester as a solid.
To a solution of the above di-ethyl ester (96.9 g, 0.29 mol) in dry degassed tetrahydrofuran (1.0 l) was added sodium methoxide (161 ml, 30% solution in methanol) and the reaction mixture was refluxed under nitrogen for 16 hours with mechanical stirring. The reaction mixture was cooled to room temperature; the volatiles remove in vacuo until a wet cage was observed. Water (500 ml) was added and the reaction mixture was refluxed for 16 hours. The remaining organic solvents were evaporated in vacuo before the pH was adjusted to 2.5 with concentrated hydrochloric acid. The aqueous phase was extracted with ethyl acetate (3×300 ml) and the combined organic phases were washed with brine (100 ml), dried (MgSO 4 ) and filtered. tert-Butyl amine (25.36 g, 0.350 mol) was added dropwise under stirring whereupon a off white precipitate was formed. The precipitate was filtered off and washed with ethyl acetate, dried in vacuo affording 74.4 g (81%) of 4-oxo-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester, tert-butyl amine salt as a solid.
Analytically pure compound can be obtained from recrystallisation of the crude product from ethanol-diisopropyl ether by heating the compound in ethanol (ca 100 ml per 10 g compound) and while still hot diisopropyl ether is added (ca 250 ml per 10 g compound). Yield in recrystallisation is approximately 50%.
A solution of the above 4-oxo-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester, tert-butyl amine salt (3.0 g, 9.48 mmol), tert-butyl cyanoacetate (2.01 g, 14.22 mmol), sulfur (0.46 g, 14.22 mmol) and diisopropyl-ethylamine (1.64 ml, 9.48 mmol) was heated to 50° C. under nitrogen for 12 hours. The solution was allowed to cool to room temperature before a small precipitate was filtered off. The filtrate was evaporated in vacuo and the residue was divided between ethyl acetate (50 ml) and saturated ammonium chloride (100 ml). The aqueous phase was extracted with ethyl acetate (3×50 m) and the combined organic phases were washed with brine (50 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was subjected to column chromatography using a mixture of petrol ether/ethyl acetate/methanol (8:4:1) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 2.22 g (58%) of 2-amino-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,5,6-tricarboxylic acid 3,6-di-tert-butyl ester as a solid.
To a solution of the above 3,5,6-tricarboxylic acid 3,6-di-tert-butyl ester (0.63 g, 1.58 mmol) in dimethoxyethane (10 ml) cooled to −20° C. was added N-methylmorpholine (174 ml, 1.58 mmol) followed by isobutylchoroformate (205 ml, 1.58 mmol) and the reaction mixture was stirred for two min. before a precipitate was filtered off. The precipitate was rapidly washed with dimethoxyethane (2×2.5 ml), recooled to −20° C. and a solution of sodium borohydride (90 mg, 2.37 mmol) in water (1 ml) was added in one lot to the filtrate. (Caution—gas evolution).
The reaction mixture was stirred until gas evolution ceases (app. 3 min.) and the mixture was poured into water (25 ml) and extracted with ethyl acetate (10 ml), washed with brine (5 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo affording 0.40 g (66% of 2-amino-5-(S)-hydroxymethyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
To a mixture of the above 2-amino-5-(S)-hydroxymethyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (2.00 g, 5.20 mmol), phthalimide (0.92 g, 6.24 mmol) and triphenylphosphine (1.64 g, 6.24 mmol) in dry tetrahydrofuran (30 ml) cooled to 0° C. under a nitrogen atmosphere was added diethyl azodicarboxylate (DEAD) (0.98 ml, 6.24 mmol). The reaction mixture was allowed to stir overnight, slowly warming to room temperature. Next day the reaction mixture was again cooled to 0° C. and phthalimide (0.46 g, 3.12 mmol), triphenylphosphine (0.82 g, 3.12 mmol) and diethyl azodicarboxylate (DEAD) (0.49 ml, 3.12 mmol) was added in sequence and the reaction mixture was allowed to stir overnight, slowly warming to room temperature. The volatiles were evaporated in vacuo and the resultant solid dissolved in dichloromethane (20 ml). The residue was subjected to flash column chromatography using a mixture of ethyl acetate/hexane (1:2) as eluent. Fractions were collected affording after evaporation in vacuo 1.0 g of the desired compound contaminated with phthalimide. Recrystallization from ethanol gave 0.23 g (9%) of pure 2-amino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
To the above di-tert-butyl ester (0.20 g, 0.39 mmol) dissolved in dichloromethane (4 ml) was added a mixture of imidazol-1-yl-oxo-acetic acid tert butyl ester (0.23 g, 1.17 mmol) in dichloromethane (1 ml) under nitrogen. The reaction mixture was allowed to stir at room temperature overnight. The reaction mixture was added dichloromethane (5 ml) and washed with 1% hydrochloric acid (10 ml), dried (Na 2 SO 4 ), filtered and the organic phase evaporated in vacuo affording 0.25 g (100%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester.
The above tri-tert-butyl ester (0.25 g, 0.39 mmol) was dissolved in 20% trifluoroacetic acid in dichloromethane (5 ml). The reaction was stirred at room temperature for 24 hours before diethyl ether (5 ml) was added. The precipitate was filtered off, washed with diethyl ether, dried in vacuo to give 150 mg of a solid. NMR revealed the presence of a trace amount of material arising from incomplete deprotection. 100 mg of the crude product was redissolved in 20% trifluoroacetic acid in dichloromethane (5 ml), and stirred at room temperature for 24 hours before diethyl ether (5 ml) was added. The product was filtered off and washed with diethyl ether and dried in vacuo to give 50 mg (40%) of the title compound as a solid trifluoroacetate.
M.p.: dec.>240° C. Calculated for C 19 H 15 N 3 O 7 S, 1/3×C 2 HF 3 O 2 , 0.5×H 2 O; C, 49.58%; H, 3.46%; N, 8.82%. Found: C, 49.84%; H, 3.83%; N, 8.99%.
Example 4
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of pure 2-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (28 mg, 0.057 mmol) in dichloromethane (2 ml) was added midazol-1-yl-oxo-acetic acid tert-butyl ester (35 mg, 0.17 mmol). The reaction was placed under nitrogen and stirred for 12 hours at ambient temperature. The volatiles were evaporated in vacuo and the residue was purified by silica gel chromatography using a mixture of ethyl acetate/hexane (1:3) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 25 mg (67%) of 2-(tert-butoxyoxalyl-amino)-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as an oil.
1 H-NMR (400 MHz, CDCl 3 ): δ12.59-12.53 (bs, 1H), 7.89-7.84 (m, 2H), 7.75-7.67 (m, 2H), 5.61-5.41 (m, 1H), 4.36-4.15 (m, 1H), 4.12-4.06 (m, 1H), 3.90-3.82 (m, 1H), 3.34-3.21 (m, 1H), 2.99-2.93 (m, 1H), 2.84-2.68 (m, 1H), 1.62-1.59 (s, 18H), 1.12-1.06 (s, 9H).
The above 2-(tert-butoxyoxalyl-amino)-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (25 mg, 0.039 mmol) was dissolved in a solution of 50% trifluoroacetic acid/dichloromethane (1.5 ml). The reaction was stirred at ambient temperature for 7 hours, concentrated in vacuo and the residue evaporated in vacuo from dichloromethane (3×10 ml). The resulting precipitate was washed with dichloromethane, filtered off and dried in vacuo to give 41 mg (85%) of the title compound as a solid trifluoroacetate.
1 H-NMR (400 MHz, DMSO-d 6 ): δ12.32 (s, 1H), 9.48 (bs, 2H), 7.95-7.91 (m, 2H), 7.89-7.84 (m, 2H), 4.89 (s, 1H), 4.15-4.07 (m, 2H), 3.43-3.28 (2m, 2H, partially obsured by water), 3.04 (bs, 2H).
LC-MS: R t =1.51 min, m/z: 428.4 [M−H] −
Example 5
5-(4-Hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-1,4-dioxa-8-aza-spiro[4.5]decane-8-carboxylic acid tert-butyl ester (1.55 g, 3.85 mmol) was cooled in an ice bath and then dissolved in a solution of 20% trifluoroacetic acid/dichloromethane (15 ml). The reaction was stirred and allowed to slowly warm to ambient temperature during 3 hours. The solution was concentrated in vacuo to give crude 2-(1,4-dioxa-8-aza-spiro[4.5]dec-7-ylmethyl)isoindole-1,3-dione which was used directly in the following step (assumed 100% yield).
1 H-NMR (400 MHz, CDCl 3 ): δ9.26 (bs, 1H), 8.19 (bs, 1H), 7.78-7.75 (m, 2H), 7.74-7.71 (m, 2H), 4.11-3.98 (m, 5H), 3.90-3.79 (m, 3H), 3.26-3.17 (m, 1H), 2.10-2.00 (m, 3H), 1.92-1.88 (m, 1H).
To a suspension of the above 2-(1,4-dioxa-8-aza-spiro[4.5]dec-7-ylmethyl)isoindole-1,3-dione (3.85 mmol) in absolute ethanol (25 ml) was added hydrazine (0.36 ml, 11.55 mmol). The reaction was stirred at 80° C. (oil bath) for 6 hours, then cooled to ambient temperature and stirred for an additional 12 hours. The thick precipitate was filtered off and washed with ethanol. The filtrate was concentrated in vacuo and reconstituted in dichloromethane (20 ml), forming a small amount of a second precipitate, which was filtered off. The filtrate was evaporated in vacuo and the resulting oil was dissolved in water (10 ml) and basified with 1 N sodium hydroxide until pH=10. The aqueous layer was extracted with 20% isopropyl alcohol/chloroform (12×40 ml). The combined organic extracts were dried (K 2 CO 3 ), filtered and the solvent evaporated in vacuo affording 0.42 g (63%) of (1,4-dioxa-8-aza-spiro[4.5]dec-7-yl)methylamine as an oil.
1 H-NMR (300 MHz, CDCl 3 ): δ3.94 (bs, 4H), 3.11-3.05 (m, 1H), 2.81 (dt, 1H, J=12 Hz and J=3 Hz), 2.76-2.65 (m, 2H), 2.58-2.50 (m, 1H), 1.70-1.57 (m, 3H), 1.31 (t, 1H, J=12 Hz).
APCI-MS: m/z: 173.2 [M+H] +
To a solution of 4-hydroxy-isobenzofuran-1,3-dione (0.51 g, 3.09 mmol) in anhydrous N,N-dimethylformamide (7 ml) under nitrogen was added sodium hydride (130 mg, 3.25 mmol). Immediate evolution of gas and bright yellow color was observed. The mixture was stirred for 5 minutes after which benzyl bromide (1.8 ml, 15.45 mmol) was added. The reaction was stirred for 72 hours. Saturated sodium bicarbonate (2 ml) was added and the mixture stirred for 2 minutes, diluted in ethyl acetate (35 ml) and washed with saturated sodium bicarbonate (5 ml), 1N hydrochloric acid (5 ml), and brine (2×5 ml). The organic layer was dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. To the crude material was added hexane and the formed precipitate was filtered off, washed further with hexane and dried in vacuo to give 0.54 g (69%) of 4-(benzyloxy)-isobenzofuran-1,3-dione as a solid.
1 H-NMR (300 MHz, CDCl 3 ): δ7.74 (t, 1H, J=8 Hz), 7.54 (d, 1H, J=8 Hz), 7.47-7.29 (m, 6H), 5.36 (s, 2H).
A solution of (1,4-dioxa-8-aza-spiro[4.5]dec-7-yl)methylamine (0.19 g, 1.1 mmol) and 4-(benzyloxy)-isobenzofuran-1,3-dione (0.27 g, 1.05 mmol) was prepared in a mixture of distilled dichloromethane (3 ml) and anhydrous N,N-dimethylformamide (2.5 ml) under nitrogen. 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.23 g, 1.21 mmol) was added followed by triethylamine (0.46 ml, 3.3 mmol) and the reaction stirred at ambient temperature for 18 hours. The solution was concentrated in vacuo and the residue diluted with ethyl acetate (25 ml) and washed with water (5 ml), saturated sodium bicarbonate (5 ml), and brine (5 ml). The organic layer was evaporated in vacuo and the residue purified by silica gel chromatography using a mixture of 5% methanol/dichloromethane/1% triethylamine as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 0.22 g (50%) of 4-benzyloxy-2-(1,4-dioxa-8-aza-spiro[4.5]dec-7-ylmethyl)-isoindole-1,3-dione as a semi-solid.
1 H-NMR (400 MHz, CDCl 3 ): δ7.57 (t, 1H, J=8 Hz), 7.48 (d, 2H, J=7 Hz), 7.42-7.29 (m, 4H), 7.18 (d, 1H, J=8 Hz), 5.31 (s, 2H), 3.94-3.90 (m, 4H), 3.65 (d, 2H, J=6 Hz) 3.16-3.09 (m, 1H), 3.07-3.02 (m, 1H), 2.76 (dt, 1H, J=13 Hz and J=3 Hz), 1.78 (d, 1H, J=12 Hz), 1.64-1.54 (m, 3H), 1.37 (t, 1H, J=12 Hz), 1.08 (t, 1H, J=7 Hz).
LC-MS: R t =2.59 min, m/z: 409 [M+H] +
To a solution of the above 4-benzyloxy-2-(1,4-dioxa-8-aza-spiro[4.5]dec-7-ylmethyl)-isoindole-1,3-dione (0.22 g, 0.54 mmol) in 1,4-dioxane (4 ml) was added 4N hydrochloric acid (4 ml) and the reaction stirred in a 65° C. (oil bath) for 6 hours. The mixture was basified with saturated sodium bicarbonate until pH=8 and extracted with dichloromethane (3×20 ml). The combined organic extracts were dried (MgSO 4 ), filtered, and the solvent evaporated in vacuo affording crude 4-benzyloxy-2-(4-oxo-piperidin-2-ylmethyl)-isoindole-1,3-dione as an oil. Which was used without further purification or characterization.
The above crude 4-benzyloxy-2-(4-oxo-piperidin-2-ylmethyl)-isoindole-1,3-dione (0.17 g, 0.47 mmol) was dissolved in dichloromethane (4 ml). Saturated sodium bicarbonate (4 ml) was added followed by di-tert-butyl dicarbonate (0.11 g, 0.52 mmol). The reaction was stirred vigorously for 16 hours, and then the layers were separated. The aqueous layer was extracted with dichloromethane (2×10 ml) and the combined organic phases were dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was purified by silica gel chromatography using a mixture of ethyl acetate/hexane (1:2) as eluent. Pure fractions were collected and the solvent was evaporated in vacuo affording 0.14 g (64%) of 2-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-oxo-piperidine-1-carboxylic acid tert-butyl ester.
1 H-NMR (400 MHz, CDCl 3 ): δ7.57 (bs, 1H), 7.47-7.31 (m, 6H), 7.18 (bs, 1H), 534 (s, 2H). 5.03 (bs, 1H), 4.45-4.14 (m, 1H), 3.89 (t, 1H, J=12 Hz), 3.55 (bs, 2H), 2.76-2.71 (m, 1), 2.57-2.38 (m, 3H), 1.17 (s, 9H).
A solution of 2-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4-oxo-piperidine-1-carboxylic acid tert-butyl ester (0.14 g, 0.30 mmol), sulfur (10.6 mg, 0.33 mmol), and tert-butyl cyanoacetate (55 mg, 0.39 mmol) in absolute ethanol (4 ml) was stirred at 50° C. (oil bath). Morpholine (53 μl, 0.6 mmol) was added and the reaction placed under nitrogen and stirred for 16 hours. The solution was cooled to ambient temperature, concentrated in vacuo and the residue purified by silica gel chromatography using a gradient of ethyl acetate/dichloromethane (0 to 5% gradient) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording a mixture of regioisomers 0.15 g (80%) of 2-amino-5-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-amino-7-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester which were not separable by chromatography.
To a solution of the above mixture of 2-amino-5-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-amino-7-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (0.15 g, 0.24 mmol) in distilled dichloromethane (4 ml) under nitrogen was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (0.14 g, 0.72 mmol) and the reaction mixture was stirred at ambient temperature for 1.5 hour. The volatiles were evaporated in vacuo and the crude residue was purified by silica gel chromatography using dichloromethane as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 50 mg of 2-(tert-butoxyoxalyl-amino)-5-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (A) and 50 mg of 2-(tert-butoxyoxalyl-amino)-7-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (B). Another 50 mg remained as a mixture of the two isomers (A) and (B).
(A)
1 H-NMR (300 MHz, CDCl 3 ): δ12.52 (s, 1H), 7.60-7.31 (m, 7H), 7.20-7.10 (m, 1H), 5.33 (s, 2H), 5.05-4.38 (m, 3H), 3.96-3.83 (m, 1H), 3.52-3.41 (m, 1H), 3.01 (bs, 2H), 1.60 (s, 9H), 1.59 (s, 9H), 1.17-1.14 (s, 9H).
LC-MS: R t =4.93 min, m/z: 748.1 [M+H] +
(B)
1 H-NMR (300 MHz, CDCl 3 ): δ12.58-12.52 (s, 1H), 7.60-7.30 (m, 7H), 7.20-7.10 (m, 1H), 5.60-5.39 (m, 1H), 5.34 (s, 2H), 4.36-4.02 (m, 2H), 3.86-3.75 (m, 1H), 3.33-3.18 (m, 1H), 2.97-2.90 (m, 1H), 2.83-2.68 (m, 1H), 1.60 (s, 9H), 1.58-1.57 (s, 9H), 1.15-1.09 (s, 9H)
LC-MS: R t =4.93 min, m/z: 748.1 [M+H] +
The above 2-(tert-butoxyoxalyl-amino)-5-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (50 mg, 0.067 mmol) was dissolved in a mixture of ethyl acetate/ethanol (3 ml, 1:1). Palladium on activated carbon (10%, 10 mg) was added and the solution degassed and stirred under hydrogen (1 atm.) for 72 hours. TLC analysis indicated that the reaction was incomplete. The mixture was filtered through celite and the filter cake washed with hot ethyl acetate. The filtrate was concentrated in vacuo and purified by silica gel chromatography using a gradient of ethyl acetate/dichloromethane (0 to 5% gradient) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 15 mg (30%) of 2-(tert-butoxyoxalyl-amino)-5-(4-hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester.
1 H-NMR (300 MHz, CDCl 3 ): δ12.50 (s, 1H), 7.61-7.51 (m, 1H), 7.39-7.34 (m, 1H), 7.17-7.09 (m, 1H), 5.04-4.64 (m, 2H), 4.49-4.34 (m, 1H), 3.90-3.78 (m, 1H), 3.51-3.42 (m, 1H), 3.02 (bs, 2H), 1.60 (s, 18H), 1.17-1.14 (2s, 9H).
The above 2-(tert-butoxyoxalyl-amino)-5-(4-hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (15 mg, 0.023 mmol) was dissolved in a solution of 50% trifluoroacetic acid/dichloromethane (2 ml). The reaction was stirred at ambient temperature for 12 hours, concentrated in vacuo and evaporated in vacuo from dichloromethane (3×10 ml). The resulting precipitate was washed with dichloromethane and dried in vacuo affording 6 mg (47%) of the title compound as a solid trifluoroacetate.
1 H-NMR (400 MHz, DMSO-d 6 ): δ12.32 (s, 1H), 11.17 (s, 1H), 9.25 (bs, 2H), 7.64 (t, 1H, J=8 Hz), 7.32 (d, 1H, J=8 Hz), 7.24 (d, 1H, J=8 Hz), 4.41-4.23 (m, 2H), 3.96-3.71 (m, 3H), 3.5-3.2 (obscured by water, 1H), 2.83-2.75 (m, 1H).
LC-MS: R t =1.53 min, m/z: 446.2 [M+H] +
Example 6
7-(4-Hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
2-(tert-Butoxyoxalyl-amino)-7-(4-benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (50 mg, 0.067 mmol) was dissolved in a mixture of ethyl acetate/ethanol (3 mL, 1:1). Palladium on activated carbon (10%, 10 mg) was added and the solution degassed and stirred under hydrogen (1 atm) for 72 hours. The mixture was filtered through celite and the filter cake washed with hot ethyl acetate. The filtrate was concentrated in vacuo and the residue purified by silica gel chromatography (10% ethyl acetate/dichloromethane) to obtain 42 mg (95%) of 2-(tert-butoxyoxalyl-amino)-7-(4-hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as an oil.
1 H-NMR (400 MHz, CDCl 3 ) δ12.59-12.53 (2s, 1H), 7.64-7.53 (m, 1H), 7.42-7.36 (m, 1H), 7.19-7.11 (m, 1H), 5.58-5.37 (m, 1H), 4.37-4.00 (m, 2H), 3.86-3.78 (m, 1H), 3.32-3.18 (m, 1H), 2.99-2.94 (m, 1H), 2.84-2.69 (m, 1H), 1.62-1.59 (3s, 18H), 1.17-1.11 (2s, 9);
LC-MS: R t =4.55 min, m/z: 658 [M+H] + ,
2-(tert-Butoxyoxalyl-amino)-7-(4-hydroxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (42 mg, 0.064 mmol) was dissolved in a solution of 50% trifluoroacetic acid/methylene chloride (3 mL). The reaction was stirred at ambient temperature for 7 hours, concentrated in vacuo and evaporated from dichloromethane (10 ml) three times. The resulting precipitate was washed with dichloromethane and dried in vacuo to give 29 mg (81%) of the title compound as a solid trifluoroacetate.
1 H-NMR (400 MHz, DMSO-d 6 ) δ12.32 (bs, 1H), 11.26 (s, 1H), 9.30 (bs, 2H), 7.64 (t, 1H, J=7 Hz), 7.33 (d, 1H, J=7 Hz), 7.25 (d, 1H, J=7 Hz), 4.84 (s, 1H), 4.06-3.96 (m, 2H), 3.56 (m, 2H), 3.05 (bs, 2H),
LC-MS: R t =1.26 min, m/z: 446 [M+H] + ,
Example 7
2-(Oxalyl-amino)-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
2-Methyl-benzoic acid methyl ester (1.50 g 10 mmol), N-bromo-succinimide (1.96 g, 11 mmol) and 2,2′-azobis(2-methyl-propionitrile) (AIBN) (25 mg, 0.15 mmol) were dissolved in chloroform (3 ml). The solution was heated at reflux for 16 hours cooled and the solvent evaporated in vacuo. The residue was purified by silica gel chromatography using a gradient of ethyl acetate/hexane (1-2%) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 2.05 g (89%) of 2-bromomethyl-benzoic acid methyl ester as a solid.
1 H-NMR (CDCl 3 ): δ7.97 (d, 1H, J=7.6 Hz), 7.45-7.52 (m, 2H), 7.38 (dt, 1H, J=1.2 Hz and J=7.6 Hz), 4.96 (s, 2H), 3.95 (s, 1H).
To a solution of 2-amino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (100 mg, 0.20 mmol) and pyridine (0.18 ml, 2.0 mmol) in acetonitrile (1 ml) at room temperature was added benzyl chloroformate (0.28 ml, 2.0 mmol) in 10 aliquots over 48 hours. The solution was then taken into ethyl acetate (30 ml), washed with 0.5 N hydrochloric acid (3×10 ml), saturated sodium bicarbonate (3×10 ml), brine (10 ml), dried (MgSO 4 ) and filtered. The solvent was evaporated in vacuo. The resulting oil crystallized upon standing for 2 days. The precipitate was filtered off and washed with diethyl ether (3×1 ml) affording after drying in vacuo 59 mg (47%) of 2-benzyloxy-carbonylamino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ10.60 (s, 1H), 7.60-7.92 (m, 4H), 7.38 (m, 5H), 5.26 (s, 2H), 4.30-5.10 (m, 3H), 3.40-4.00 (m, 2H), 1.57 (m, 9H), 1.15 (m, 9H).
To a solution of 1 N hydrochloric acid in ethyl acetate (1.0 ml) was added 2-benzyloxy-carbonylamino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (52 mg, 0.08 mmol). The solution was stirred at room temperature for 48 hours. A precipitate was filtered off which afforded 42 mg (90%) of 2-benzyloxy-carbonylamino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester hydrochloride as a solid.
1 H-NMR (DMSO-d 6 ): δ10.45 (s, 1H), 9.40 (s, 1H), 9.25 (s, 1H), 7.89 (m, 4H), 7.39 (m, 5H), 5.22 (s, 2H), 4.39 (d, 1H, J=15 Hz), 4.28 (m, 1H), 3.95 (m, 2H), 3.79 (m, 1H), 3.20 (m, 1H), 2.70 (m, 1H), 1.48 (s, 9H).
To a solution of the above 2-benzyloxy-carbonylamino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester hydrochloride (42 mg, 0.072 mmol) in ethanol (0.5 ml) was added hydrazine (68 μl, 0.22 mmol). The solution was stirred at 80° C. for 5 hours and at room temperature for 16 hours. The mixture was filtered and the filtrate evaporated in vacuo. The residue was extracted with dichloromethane (5×1 ml). The combined dichloromethane washes were evaporated in vacuo affording 20 mg (67%) of 5-(S)-aminomethyl-2-benzyloxy-carbonylamino-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ10.55 (bs, 1H), 7.37 (m, 5H), 5.23 (s, 2H), 3.92 (s, 2H), 2.60-3.10 (m, 3H), 1.53 (s, 9H).
To a solution of the above 5-(S)-aminomethyl-2-benzyloxy-carbonylamino-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (20 mg, 0.048 mmol) in acetonitrile (1 ml) at 0° C. was added diisopropylethylamine (18 l, 0.15 mmol) and 2-bromomethyl-benzoic acid methyl (12 mg, 0.048 mmol). The solution was stirred at 0° C. for 3 hours and at room temperature for 16 hours. Di-tert-butyl dicarbonate (21 mg, 0.096 mmol) was then added to the solution. The solution was then stirred at room temperature for 16 hours. The solution was taken into ethyl acetate (30 ml), washed with 0.5 N hydrochloric acid (3×10 ml), saturated sodium bicarbonate (3×10 ml) and brine (10 ml), dried (MgSO 4 ) and filtered. The solvent was evaporated in vacuo. The solid residue was purified by silica gel chromatography using a 5% mixture of ethyl acetate/hexane as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 10 mg (33%) of 2-(benzyloxy-carbonylamino)-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ10.59 (s, 1H), 7.81 (m, 1H), 7.52 (m, 1H), 7.39 (m, 7H), 5.25 (s, 1H), 4.22-5.00 (m, 4H), 4.40-4.80 (m, 2H), 2.80-3.10 (m, 2H), 1.55 (s, 9H), 1.25 (s, 9H).
To a solution of the above 2-benzyloxycarbonylamino-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (9 mg, 0.014 mmol) in methanol (2 ml) was added 10% Pd/C (4 mg). The mixture was stirred under hydrogen (1 atm.) for 3 hours and then filtered. The filtrate was evaporated in vacuo affording 6 mg (93%) of 2-amino-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ7.80 (m, 1H), 7.50 (m, 1H), 7.44 (m, 2H), 4.22-5.00 (m, 4H), 4.40-4.80 (m, 2H), 2.80-3.10 (m, 2H), 1.63 (s, 9H), 1.25 (s, 9H).
To a solution of the above 2-amino-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (6 mg, 0.013 mmol) in acetonitrile (0.5 ml) at room temperature was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (27 mg, 0.13 mmol). The solution was stirred for 3 hours at room temperature and then diluted with ethyl acetate (20 ml). washed with 0.5 N hydrochloric acid (2×5 ml), saturated sodium bicarbonate (2×5 ml), brine (5 ml), dried (MgSO 4 ) and filtered. The solvent was evaporated in vacuo. The residue was purified by silica gel chromatography using a gradient of ethyl acetate/hexane (10-25% gradient) as eluent. Pure fractions were collected and the solvent evaporated in vacuo affording 4 mg (50%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.49 (s, 1H), 7.80 (m, 1H), 7.50 (m, 1H), 7.44 (m, 2H), 4.22-5.00 (m, 4H), 4.20-4.90 (m, 2H), 2.90-3.20 (m, 2H), 1.63 (s, 9H), 1.60 (s, 9H), 1.25 (s, 9H).
To a solution of trifluoroacetic acid/dichloromethane (0.5 ml, 1:1) at room temperature was added the above 2-(tert-butoxyoxalyl-amino)-5-(S)-(1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (4 mg, 0.006 mmol). The solution was stirred for 3 hours. The solvent was removed in vacuo. The residue was washed with dichloromethane affording in quantitative yield the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.32 (s, 1H), 4.62 (s, 1H), 4.12 (m, 1H), 3.62-3.78 (m, 2H), 3.40-3.52 (m, 1H), 2.83 (m, 2H).
MS: m/z: 416 [M+H] + .
Example 8
5-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
Acetyl chloride (5.4 ml, 5.96 g, 76 mmol) was added dropwise to methanol (15 ml) at 0° C. in a sealed 50 ml round-bottom flask. This solution was allowed to warm to room temperature for 1 hour while stirring. To this solution 3-hydroxy-2-methyl-benzoic acid (519 mg, 3.4 mmol) was added and the solution was stirred at room temperature for 42 hours. The reaction was quenched with saturated aqueous sodium bicarbonate and solid sodium bicarbonate. The volatiles were removed in vacuo and the basic aqueous solution was then extracted with dichloromethane (4×40 ml). The combined organic extracts were dried (MgSO 4 ), filtered, and the solvent evaporated in vacuo affording 493 mg (87%) of 3-hydroxy-2-methyl-benzoic acid methyl ester as a solid.
1 H-NMR (300 MHz, CDCl 3 ): δ7.43 (d, 1H, J=9 Hz), 7.12 (t, 1H, J=8 Hz), 6.95 (d, 1H, J=8 Hz), 5.05 (bs, 1H), 3.90 (s, 3H), 2.47 (s, 3H).
To a solution of the above methyl ester (256 mg, 1.54 mmol) and N,N-diisopropylethylamine (530 μl, 3.0 mmol) in dichloromethane (8 ml) at 0° C. methyloxymethyl chloride (175 μl, 2.3 mmol) was added dropwise. The solution was allowed slowly to warm to room temperature and stired for 24 hours. The solution was diluted with dichloromethane (12 ml), washed with water (20 ml), brine (20 ml), dried (MgSO 4 ), filtered, and concentrated in vacuo. The resulting oil was purified by silica gel chromatography using a mixture of hexanes/ethyl acetate (4:1) as eluent, which afforded 269 mg (85%) of 3-methoxymethoxy-2-methyl-benzoic acid methyl ester as an oil.
1 H-NMR (300 MHz, CDCl 3 ): δ7.48 (d, 1H, J=8 Hz), 7.24-7.15 (m, 2H), 5.22 (s, 2H), 3.90 (s, 3H), 3.50 (s, 3H), 2.47 (s, 3H).
In a 25 ml round-bottom flask, N-bromo succinimide (236 mg, 1.3 mmol) and azobis(cyclohexanecarbonitrile) (33 mg, 0.14 mmol) were added to a solution of 3-methoxymethoxy-2-methyl-benzoic acid methyl ester (265 mg, 1.26 mmol) in carbon tetrachloride (6.5 ml). The reaction was heated to reflux with stirring for 3.5 hours. The volatiles were removed in vacuo and the residue purified by silica gel chromatography using a mixture of hexanes/ethyl acetate (9:1) as eluent, which afforded 364 mg (100%) of 2-bromomethyl-3-methoxymethoxy-benzoic acid methyl ester as a solid.
1 H-NMR (300 MHz, CDCl 3 ): δ7.55 (dd, 1H, J=6,3 Hz), 7.29 (d, 2H, J=3 Hz), 5.27 (s, 2H), 5.05 (s, 2H), 3.91 (s, 3H), 3.50 (s, 3H).
In a 100 ml round-bottom flask, 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (298 mg, 0.74 mmol) and N,N-diisopropylethylamine (195 μl, 1.12 mmol) were dissolved in acetonitrile (40 ml). 2-Bromomethyl-3-methoxymethoxy-benzoic acid methyl ester (193 mg, 0.67 mmol) in acetonitrile (5 ml) was slowly added to the amine solution via gastight syringe over 24 hours, followed by stirring at room temperature for an additional 36 hours. The solution was concentrated in vacuo, the residue redissolved in ethyl acetate (25 ml), and washed with saturated aqueous sodium bicarbonate (25 ml) and brine (25 ml). The organic phase was dried (MgSO 4 ), filtered, and the solvent evaporated in vacuo. The residue was purified by silica gel chromatography using a mixture of hexanes/ethyl acetate (1:1) as eluent, which afforded 345 mg (81%) of 2-amino-6-(4-methoxy-benzyl)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (300 MHz, CDCl 3 ): δ7.67 (d, 1H, J=8 Hz), 7.57-7.38 (m, 5H), 7.14 (d, 2H, J=8 Hz), 6.96 (m, 2H), 6.77 (d, 2H, J=9 Hz), 6.20 (d, 2H, J=6 Hz), 5.96 (s, 2H), 4.69-2.58 (m, 17H), 1.55 (s, 9H).
In a 50 ml round-bottom flask a solution of 2-amino-6-(4-methoxy-benzyl)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (338 mg, 0.58 mmol) in dichloromethane (20 ml) was treated with imidazol-1-yl-oxo-acetic acid tert-butyl ester (575 mg, 2.9 mmol). After stirring for 18 hours at room temperature, the mixture was concentrated to dryness in vacuo. The residue was purified by silica gel chromatography using a mixture of hexanes/ethyl acetate (1:1) as eluent, which afforded 310 mg (75%) of 2-(tert-Butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (300 MHz, CDCl 3 ): δ12.57 (s, 1H), 7.53 (d, 1H, J=8 Hz), 7.43 (t, 1H, J=8 Hz), 7.26 (d, 1H, J=8 Hz), 7.13 (d, 2H, J=9 Hz), 6.78 (d, 2H, J=9 Hz), 5.28 (s, 2H), 4.47 (q, 2H, J=18 Hz), 4.02-3.44 (m, 11H), 2.97 (dd, 1H, J=18 Hz and J=5 Hz), 2.76 (dd, 1H, J=17 Hz and J=5 Hz), 1.63 (s, 9H), 1.59 (s, 9H).
10% Pd/C (145 mg, 50% by weight) was added to a mixture of 2-(tert-butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (283 mg, 0.40 mmol) in 10% formic acid and methanol (10 ml). After stirring at room temperature for 18 hours, more Pd/C (141 mg, 50% by weight) was added to the reaction mixture. After stirring at room temperature for an additional 20 hours, the catalyst was removed via fitration through celite. Fresh Pd/C (255 mg) and ammonium formate (1.0 g) were added to the residue (253 mg, 0.36 mmol) dissolved in 10% formic acid in methanol (10 ml). The solution was heated to 40° C. for 48 hours. Catalyst was removed via filtration through celite and liberal washing with methanol. Purification by chromatotron (ethyl acetate/triethylamine (99:1)) afforded 63 mg (27%) of 2-(tert-butoxyoxalyl-amino)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester A and 46 mg (19%) of 2-(tert-butoxyoxalyl-amino)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-methyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester B.
A
1 H-NMR (300 MHz, CDCl 3 ): δ12.54 (s, 1H), 7.50 (d, 1H, J=8 Hz), 7.41 (t, 1H, J=8 Hz), 7.25 (d, 1H, J=8 Hz), 5.27 (s, 2H), 4.52 (dd, 2H, J=30 Hz and J=19 Hz), 4.08-3.90 (m, 2H), 3.86-3.67 (m, 2H), 3.51 (s, 3H), 3.27 (m, 1H), 2.99 (dd, 1H, J=18 and J=4 Hz), 2.53 (dd, 1H, J=18 Hz and J=11 Hz), 1.61 (s, 9H), 1.53 (s, 9H).
LC-MS (APCI + ) m/z: 588 [M+H] + ; R t =1.32 min.
B
1 H-NMR (300 MHz, CDCl 3 ): δ12.56 (s, 1H), 7.50 (d, 1H, J=7 Hz), 7.41 (t, 1H, J=8 Hz), 7.25 (d, 1H, J=8 Hz), 5.27 (s, 2H), 4.50 (dd, J=28 Hz and J=18 Hz), 3.93-3.68 (m, 4H), 3.51 (s, 1H), 3.51 (s, 3H), 3.31 (m, 1H), 2.88 (dd, 1H, J=18 Hz and J=4 Hz), 2.68 (dd, 1H, J=19 Hz and J=9 Hz), 2.46 (s, 3H), 1.61 (s, 9H), 1.54 (s, 9H).
LC-MS (APCI + ) m/z: 602 [M+H] + ; R t =1.35 min.
2-(tert-Butoxyoxalyl-amino)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester A (63 mg, 0.11 mmol) was dissolved in 30% trifluoroacetic acid in dichloromethane (4 ml). The solution was left open to the atmosphere without stirring. After 24 hours the precipitate was filtered off and washed with diethyl ether, affording 57 mg (90%) of the title compound as a solid trifluoroacetate.
1 H-NMR (300 MHz, DMSO-d 6 ): δ12.30 (s, 1H), 10.17 (s, 1H), 9.23 (s, 2H, J=5 Hz and J=7 Hz), 7.34 (t, 1H, J=6 Hz), 7.19 (d, 1H, J=5 Hz), 7.03 (d, 1H, J=6 Hz), 5.76 (s, 2H), 4.53 (d, 1H, J=13 Hz), 4.43-4.22 (m, 3H), 4.07 (m, 1H), 3.91 (m, 1H), 3.70 (m, 1H), 3.10 (m, 1H), 2.82 (dd, 1H, J=14 Hz and J=8 Hz).
Example 9
5-(4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-methyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The above 2-(tert-butoxyoxalyl-amino)-5-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-methyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester B (46 mg, 0.08 mmol) was dissolved in 30% trifluoroacetic acid in dichloromethane (4 ml). The solution was left open to the atmosphere without stirring. After 24 hours the precipitate was filtered off and washed with diethyl ether, affording 41 mg (90%) of the title compound as a solid trifluoroacetate.
1 H-NMR (400 MHz, CDCl 3 ): δ12.39 (s, 1H), 10.19 (s, 1H), 10.10 (s, 1H), 7.32 (t, 1H, J=7.6 Hz), 7.17 (d, 1H, J=7.2 Hz), 7.02 (t, 1H, J=7.2 Hz), 4.55 (d, 2H, J=15 Hz), 4.0-4.5 (m, 4H), 2.95-3.70 (m, 5H), 2.85 (s, 3H).
LC-MS (APCI + ) m/z: 446 [M+H] + ; R t =1.02 min.
Example 10
5-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
Saccharin (8.8 g, 48 mmol) and phosphorous pentachloride (15 g, 72 mmol) were added neat to a round bottom flask equipped with a short path distillation column. The mixture was heated to 175° C. After approximately 0.5 hour, phosphorous oxychloride slowly distilled off. Upon completion of the reaction, the mixture was cooled and the resultant solid recrystallized from benzene affording 3.6 g (37%) of 3-chloro-benzo[d]isothiazole 1,1-dioxide as a solid.
1 H-NMR (CDCl 3 ): δ7.92 (d, 1H, J=6.9 Hz), 7.8 (m, 3H).
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (155 mg, 0.384 mmol) and triethylamine (59 μl, 0.423 mmol) in dichloromethane (2 ml) at 0° C., was added a solution of 3-chloro-benzo[d]isothiazole 1,1-dioxide (85.2 mg, 0.423 mmol) in dichloromethane (2 ml). The reaction mixture was stirred at 0° C. for 1 hour. The reaction was judged complete by tic (dichloromethane/ethyl acetate (1:1)). The reaction mixture was washed with water (3×20 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The crude residue was subjected to flash chromatography using a gradient from 100% dichloromethane to dichloromethane/ethyl acetate (80/20) as eluent, which afforded 200 mg (92%) of 2-amino-5-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a foam.
1 H-NMR (CD 3 OD): δ7.99 (m, 1H), 7.87 (m, 1H), 7.79 (m, 2H), 7.19 (d, 2H, J=8.4 Hz), 6.75 (d, 2H, J=8.7 Hz), 3.88-3.79 (m, 2H), 3.75-3.59 (m, 3H), 3.69 (s, 3H), 3.52-3.46 (m, 2H), 2.84 (dd, 1H, J=15.3 Hz and J=5.4 Hz), 2.68 (dd, J=18 Hz and J=4.5 Hz), 1.46 (s, 9H).
LC-MS: R t =2.83, m/z: 569 [M+H] +
To a solution of 2-amino-5-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (129 mg, 0.227 mmol) in tetrahydrofuran (3 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (1.1 ml, 1.1 mmol, 1 M in tetrahydrofuran). The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated in vacuo and the residue subjected to flash chromtography using a mixture of ethyl acetate/dichloromethane (10:90) as eluent, which afforded 142 mg (90%) of 2-(tert-butoxyoxalyl-amino)-5-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.92 (d, 1H, J=6.3 Hz), 7.73 (m, 2H), 7.56 (d, 1H, J=5.7 Hz), 7.20 (d, 2H, J=6.3 Hz), 7.05 (bs, 1H), 6.87 (d, 2H, J=6.6 Hz), 3.91 (m, 2H), 3.82-3.72 (m, 2H), 3.79 (s, 3H), 3.61-3.49 (m, 2H), 3.44 (m, 1H), 3.11 (dd, 1H, J=15 Hz and J=3.6 Hz), 2.72 (dd, 1H, J=12 Hz and J=4.2 Hz), 1.63 (s, 18H);
LC-MS: R t =3.48, m/z: 697 [M+H] +
2-(tert-Butoxyoxalyl-amino)-5-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (120 mg, 0.172 mmol) was dissolved in a mixture of ethanol (4 ml) and formic acid (0.5 ml). 10% Pd-C (20 mg) was added and the reaction mixture stirred at ambient temperature for 4 days (after the second day, 150 mg of additional 10% Pd-C was added). The reaction mixture was filtered through celite and the celite washed with dichloromethane. The organic fractions were combined and concentrated in vacuo. The resultant oil was subjected to preparative thin layer chromatography (dichloromethane/methanol (95:5)), which afforded 17 mg (17%) of 2-(tert-butoxyoxalyl-amino)-5-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ7.91 (m, 1H), 7.72 (m, 3H), 7.34 (bs, 1H), 4.16-4.08 (m, 1H), 4.07 (dd, 2H, J=36.3 Hz and J=8.7 Hz), 3.38-3.30 (m, 1H), 3.22-3.06 (m, 2H), 2.51 (dd, 1H, J=16.8 Hz and J=9.9 Hz), 1.61 (s, 18H).
2-(tert-Butoxyoxalyl-amino)-5-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (15 mg, 0.026 mmol) was dissolved in a solution of 50% trifluoroacetic acid/dichloromethane (3 ml). The reaction mixture was stirred at ambient temperature for 18 hours, concentrated in vacuo and re-evaporated from acetonitrile (2×). The residue was washed with dichloromethane and dried in vacuo to give 16 mg (90%) of the title compound as a solid trifluoroacetate.
1 H-NMR (CD 3 OD): δ7.98 (d, 1H, J=7.2 Hz), 7.92 (d, 1H, J=6.6 Hz), 7.83 (m, 2H), 4.51-4.39 (m, 2H), 4.11-4.08 (m, 1H), 3.97-3.91 (m, 2H), 3.53-3.47 (m, 1H), 3.16-3.10 (m, 1H).
Example 11
7-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
3-Chloro-benzo[d]isothiazole-1,1-dioxide (160 mg, 0.79 mmol) and diisopropylethylamine (150 μl, 0.86 mmol) were dissolved in dichloromethane (7 ml) at 0° C. 2-Amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (284 mg, 0.70 mmol) was added and the mixture was stirred for 15 minutes at 0° C., diluted with dichloromethane (10 ml) and washed with water (20 ml) and brine (20 ml). The organic phase was dried (MgSO 4 ), filtered, and the solvent evaporated in vacuo. The residue was purified by silica gel chromatography using a gradient of hexanes/ethyl acetate (1:1) to pure ethyl acetate as eluent, which afforded 309 mg (77%) of 2-amino-7-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an foam.
1 H-NMR (300 MHz, CDCl 3 ): δ7.89 (d, 1H, J=8 Hz), 7.77-7.63 (m, 2H), 7.37 (d, 1H, J=7 Hz), 7.25 (d, 2H, J=10 Hz), 6.82 (d, 2H, J=8 Hz), 6.62 (bs, 1H), 6.08 (s, 2H), 3.91 (m, 1H), 3.71 (s, 3H), 3.49-2.65 (m, 8H), 1.59 (s, 9H).
LC-MS (APCI + ) m/z: 569 [M+H] + , [M+Na] 591; R t =2.85 min.
2-Amino-7-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (102 mg, 0.18 mmol) in dichloromethane (10 ml) was treated with imidazol-1-yl-oxo-acetic acid tert-butyl ester (85 mg, 0.43 mmol). After stirring for 18 hours at room temperature, the reaction solution was concentrated to dryness in vacuo. The residue was purified by silica gel chromatography using a gradient of hexanes/ethyl acetate (1:1) to pure ethyl acetate as gradient, which afforded 98 mg (78%) of 2-(tert-butoxyoxalyl-amino)-7-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (300 MHz, CDCl 3 ): δ12.57 (s, 1H), 7.89 (d, 1H, J=8 Hz), 7.77-7.63 (m, 2H), 7.39 (d, 1H, J=7 Hz), 7.25 (d, 2H, J=9 Hz), 6.84 (d, 2H, J=9 Hz), 6.64 (bs, 1H), 3.99-2.76 (m, 12H), 1.64 (s, 9H), 1.63 (s, 9H).
10% Pd/C (100 mg) was added to a mixture of 2-(tert-butoxyoxalyl-amino)-7-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (98 mg, 0.14 mmol) in 10% formic acid in methanol (10 ml). After stirring at room temperature for 48 hours, the catalyst was removed via filtration through celite and liberal washing with methanol. The volatiles were removed in vacuo and the residue purified by chromatotron (ethyl acetate/triethylamine, 99:1), which afforded 32 mg (40%) of 2-(tert-butoxyoxalyl-amino)-7-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (300 MHz, CDCl 3 ): δ12.48 (s, 1H), 10.21-9.15 (m, 2H), 8.49-7.42 (m, 3H), 5.62-5.00 (bs, 1H), 4.53-2.87 (m, 8H), 1.61 (s, 18H).
HPLC (254.4 nm) R t =3.67 minutes.
2-(tert-Butoxyoxalyl-amino)-7-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (32 mg) was dissolved in a mixture of 30% trifluoroacetic acid in dichloromethane (4 ml). The solution was left open to the atmosphere without stirring. After 24 hours the precipitate was filtered off and washed with diethyl ether, affording 29 mg (90%) of the title compound as a solid trifluoroacetate.
1 H-NMR (300 MHz, DMSO-d 6 ): δ12.36 (s, 1H), 9.92 (bs, 1H), 9.73 (bs, 1H), 9.38 (bs, 1H), 8.20 (m, 1H), 8.05 (m, 1H), 7.89 (m, 2H), 4.95 (s, 1H), 4.12-3.00 (m partially obscured by water, 8H).
LC-MS (APCI + ) m/z: 466 [M+H] + ; R t =0.66 min.
Example 12
5-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
2-Methoxy-6-methylbenzoic acid ethyl ester (500 mg, 2.67 mmol), N-bromosuccinimide (483.8 mg, 2.72 mmol) and 2,2′-azobis(2-methyl-propionitrile) (30.2 mg, 0.123 mmol) in carbon tetrachloride (10 ml) were heated to reflux. After 18 hours, the reaction mixture was evaporated to dryness in vacuo. The residue was dissolved in dichloromethane (100 ml) and washed with water (2×50 ml). The organic layer was dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue (702 mg) was purified by column chromatography using a mixture of hexanes/dichloromethane (1:1) as eluent, which afforded 573 mg (85%) of 6-bromomethyl-2-methoxy-benzoic acid ethyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.37 (t, 1H, J=8.4 Hz), 7.01 (d, 1H, J=8.1 Hz), 6.90 (d, 1H, J=8.4 Hz), 4.54 (s, 2H), 4.45 (q, 2H, J=7.2 Hz), 3.82 (s, 3H), 1.42 (t, 3H, J=9 Hz).
6-Bromomethyl-2-methoxy-benzoic acid ethyl ester (71.1 mg, 0.260 mmol) dissolved in acetonitrile (5 ml) and diisopropylethylamine (453 μl, 2.60 mmol) was stirred at room temperature. To this mixture 2-amino-5-amino-methyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (200 mg, 0.52 mmol) dissolved in acetonitrile (5 ml) was added syringe pump (0.2 ml/min.). Once addition was complete, the reaction mixture was allowed to stir for 2 hours. The reaction mixture was concentrated in vacuo, and the residue diluted with ethylacetate (50 ml). The organic layer was washed with saturated sodium bicarbonate (2×25 ml) and brine (2×25 ml). The organic layer was dried (MgSO 4 ), filtered and concentrated in vacuo. The residue (308 mg) was subjected to column chromatography using a gradient of hexane/ethyl acetate (95:5) to (50:50) and then dichloromethane/ethyl acetate (95:5) as eluents, which afforded 106 mg (75%) of 2-amino-6-(4-methoxy-benzyl)-5-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.48 (t, 1H, J=7.5 Hz), 7.12 (d, 2H, J=8.4 Hz), 7.01 (d, 1H, J=7.5 Hz), 6.91 (d, 1H, J=8.4 Hz), 6.76 (d, 2H, J=7.8 Hz), 5.95 (bs, 2H), 4.37 (s, 2H), 4.05 (m, 1H), 3.97 (s, 3H), 3.88-3.78 (m, 2H), 3.81 (s, 3H), 3.71-3.39 (m, 4H), 2.90 (dd, 1H, J=18 Hz and J=5.4 Hz), 2.62 (dd, 1H, J=18 Hz and J=5.4 Hz), 1.53 (s, 9H).
To a solution of 2-amino-6-(4-methoxy-benzyl)-5-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (105 mg, 0.192 mmol) in tetrahydrofuran (3 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (0.534 ml, 0.534 mmol, 1 M in tetrahydrofuran). The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture concentrated in vacuo and the residue subjected to flash chromtography using a mixture of ethyl acetate/dichloromethane (10:90) as eluent, which afforded 85 mg (66%) of 2-(tert-butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
1 H-NMR (CDCl 3 ): δ7.47 (t, 1H, J=5.7 Hz), 7.10 (d, 2H, J=6 Hz), 6.99 (d, 1H, J=5.7 Hz), 6.90 (d, 1H, J=6.3 Hz), 6.76 (d, 2H, J=6.3 Hz), 4.37 (q, 2H, J=11.4 Hz), 3.99-3.92 (m, 1H), 3.97 (s, 3H), 3.79-3.76 (m, 2H), 3.77 (s, 3H), 3.66 (d, 1H, J=12.6 Hz), 3.58-3.50 (m, 3H), 2.95 (dd, 1H, J=13.5 Hz and J=3.6 Hz), 2.70 (dd, 1H, J=13.5 Hz and J=3.6 Hz) 1.61 (d, 9H), 1.57 (s, 9H).
2-(tert-Butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (66 mg, 0.12 mmol) was dissolved in ethanol (2 ml) and formic acid (0.3 ml). 10% Pd-C (15 mg) was added and the reaction mixture stirred at room temperature for 3 days. TLC (hexane/ethyl acetate (1/1)) indicated reaction complete. The reaction mixture was filtered through celite and the celite washed with dichloromethane. The organic fractions were combined and subjected to preparative thin layer chromatography (hexane/ethyl acetate (1/1) to yield 14.7 mg (22%) of 2-(tert-butoxyoxalyl-amino)-5-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.48 (t, 1H, J=7.5 Hz), 7.01 (d, 1H, J=7.2 Hz), 6.90 (d, 1H, J=8.4 Hz), 5.50 (d, 2H, J=6.6 Hz), 4.04-3.90 (m, 1H), 3.97 (s, 3H), 3.24 (m, 1H), 3.01-2.95 (m, 1H), 2.57-2.43 (m, 2H), 1.62 (s, 9H), 1.57 (s, 9H).
2-(tert-Butoxyoxalyl-amino)-5-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (14.7 mg, 0.026 mmol) was dissolved in a solution of 50% trifluoroacetic acid/dichloromethane (2 ml). The reaction mixture was stirred at ambient temperature for 18 hours, concentrated in vacuo and re-evaporated from acetonitrile (2×). The resulting precipitate was washed with dichloromethane and dried in vacuo to give 13 mg (89%) of the title compound as a solid trifluoroacetate.
1 H-NMR (CD 3 OD): δ7.56 (t, 1H, J=8.1 Hz), 7.13 (d, 1H, J=7.2 Hz), 7.01 (d, 1H, J=8.1 Hz), 4.87-4.44 (m, 4H), 4.15 (m, 1H), 3.90 (s, 3H), 3.88-3.79 (m, 1H), 3.43 (m, 1H), 2.98 (m, 2H);
LC-MS: R t =0.71, m/z: 446 [M+H] + .
Example 13
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-hydroxy-6-methyl-benzoic acid ethyl ester (5.00 g, 27.8 mmol) and t-butyl-di-methylsilyl chloride (6.27 g, 41.6 mmol) in dichloromethane (100 ml) was added diisopropyl ethylamine. The solution was stirred at 50° C. for 24 hours, washed with water, brine, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo, which afforded 7.6 g (93%) of 2-(tert-butyl-dimethyl-silanyloxy)-6-methyl-benzoic acid ethyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.13 (t, 1H, J=7.5 Hz), 6.78 (d, 1H, J=7.5 Hz), 6.67 (d, 1H, J=7.5 Hz), 4.35 (q, 2H, J=7.2 Hz), 2.29 (s, 3H), 1.38 (t, 3H, J=7.2 Hz), 0.97 (s, 9H), 0.23 (s, 6H).
2-(tert-Butyl-dimethyl-silanyloxy)-6-methyl-benzoic acid ethyl ester (7.6 g, 25.8 mmol), N-bromosuccinimide (4.82 g, 27.1 mmol) and azobis(cyclohexanecarbonitrile) (0.32 g, 1.3 mmol) were dissolved in tetrachlormethane (130 ml). The solution was stirred at room temperature for 60 hours. The solvent was evaporated in vacuo and the residue was chromatographed on silica gel column using a gradient of 1-2% ethyl acetate/hexane as eluent, which afforded 8.0 g (83%) of 6-bromomethyl-2-(tert-butyl-dimethyl-silanyloxy)-benzoic acid ethyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.21 (t, 1H, J=8.4 Hz), 7.00 (d, 1H, J=8.4 Hz), 6.81 (d, 1H, J=8.4 Hz), 4.51 (s, 2H), 4.40 (q, 2H, J=7.2 Hz), 1.42 (t, 3H, J=7.2 Hz), 0.98 (s, 9H), 0.23 (s, 6H).
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (3.00 g, 7.45 mmol) and diisopropyl ethylamine (1.93 ml, 11.2 mmol) in acetonitrile at room temperature was added a solution of 6-bromomethyl-2-(tert-butyl-dimethyl-silanyloxy)-benzoic acid ethyl ester (2.78 g, 7.45 mmol) in acetonitril over 48 hours. The solution was stirred for 12 hours after the addition was complete. The volatiles were evaporated in vacuo and the residue was taken into ethyl acetate (50 ml) and washed with water, 1 N hydrochloric acid, brine, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was chromatographed on silica gel column eluted with a mixture of 20% ethyl acetate/Hexane, which afforded 3.2 g (66%) of 2-amino-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl]-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.36 (t, 1H, J=8.0 Hz), 7.11 (d, 2H, J=8.8 Hz), 6.99 (d, 1H, J=8.0 Hz), 6.82 (d, 1H, J=8.0 Hz), 6.76 (d, 2H, J=8.8 Hz), 5.94 (s, 2H), 4.48 (d, 1H, J=16.8 Hz), 4.33 (d, 1H, J=16.8 Hz), 3.90-3.45 (m, 7H), 3.78 (s, 3H), 2.95 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 2.72 (dd, 1H, J=17 Hz and J=5.6 Hz), 1.52 (s, 9H), 1.05 (s, 9H), 0.26 (s, 6H).
To a stirred solution of 2-amino-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (2.37 g, 3.64 mmol) in tetrahydrofuran (50 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (2.14 mg, 10.9 mmol) in tetrahydrofuran (10 ml). The mixture was stirred at room temperature for 24 hours. The solvent was removed in vacuo. The residue was taken into ethyl acetate (100 ml). The solution was washed with 0.5 N hydrochloric acid solution (2×20 ml), saturated sodium bicarbonate (2×20 ml) and brine (20 ml), dried (MgSO 4 ), filtered and the solvent removed in vacuo. The residue was chromatographed using a gradient of 10-20% ethyl acetate/Hexane as eluent, which afforded 2.40 g (92%) of 2-(tert-butoxyoxalyl-amino)-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.59 (s, 1H), 7.37 (t, 1H, J=8.0 Hz), 7.10 (d, 2H, J=8.8 Hz), 7.00 (d, 1H, J=8.0 Hz), 6.83 (d, 1H, J=8.0 Hz), 6.77 (d, 2H, J=8.8 Hz), 4.50 (d, 1H, J=16.8 Hz), 4.34 (d, 1H, J=16.8 Hz), 3.90-3.45 (m, 7H), 3.77 (s, 3H), 2.95 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 2.72 (dd, 1H, J=18 and J=5.6 Hz), 1.61 (s, 9H), 1.58 (s, 9H), 1.06 (s, 9H), 0.26 (s, 6H).
To a solution of 2-(tert-butoxyoxalyl-amino)-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (2.40 g, 3.34 mmol) in 10% formic acid/methanol (50 ml) at room temperature under nitrogen was added 10% Pd/C (1.2 g). The mixture was stirred for 48 hours. The Pd/C was filtered off and the filtrate was evaporated in vacuo. The residue was dissolved in dichloromethane (10 ml). The resulting solution was poured into hexane. The precipitate was filtered off and dried in vacuo affording 1.3 g (61%) of 2-(tert-butoxyoxalyl-amino)-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
1 H-NMR (CDCl 3 ): δ12.45 (s, 1H), 8.05 (s, 1H), 7.39 (t, 1H, J=8.0 Hz), 7.00 (d, 1H, J=8.0 Hz), 6.83 (d, 1H, J=8.0 Hz), 4.50 (d, 1H, J=16.8 Hz), 4.45 (q, 2H, J=17 Hz), 4.05 (q, 2H, J=17 Hz), 3.82 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 3.72 (dd, 1H, J=17 Hz and J=5.6 Hz), 3.40 (s, 1H), 3.08 (d, 1H, J=17 Hz), 2.61 (dd, 1H, J=18 Hz and J=7.2 Hz), 1.61 (s, 9H), 1.54 (s, 9H), 1.05 (s, 9H), 0.26 (s, 6H).
To a solution of trifluoroacetic acid (33.3 ml) and H 2 O (2.7 ml) was added 2-(tert-butoxyoxalyl-amino)-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.70 g, 1.04 mmol). The solution was stirred at room temperature for 40 hours. The solvent was poured into ethyl ether (400 ml). The precipitate was filtered off and dried in vacuo, which afforded 450 mg (80%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.30 (s, 1H), 9.71 (s, 1H), 9.20 (s, 2H), 7.39 (t, 1H, J=8.0 Hz), 6.99 (d, 1H, J=8.0 Hz), 6.82 (d, 1H, J=8.0 Hz), 4.52 (d, 1H, J=16.8 Hz), 4.36 (d, 2H, J=17 Hz), 4.22 (d, 2H, J=17 Hz), 4.00 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 3.86 (s, 1H), 3.62 (d, 1H, J=17 Hz), 2.81 (dd, 1H, J=18 Hz and J=7.2 Hz);
LC-MS: R t =1.20 min; m/z=432 [M+H] +
Example 14
5-(7-Benzyloxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-(tert-butoxyoxalyl-amino)-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (2.40 g, 3.34 mmol) in 10% formic acid/methanol (50 ml) at room temperature under nitrogen was added 10% Pd/C (1.2 g). The mixture was stirred for 48 hours. The Pd/C was filtered off and the filtrate was evaporated in vacuo. The residue was dissolved in dichloromethane (10 ml) and the resulting solution was poured into hexane. The precipitate was filtered off (1.3 g) and the filtrate was evaporated in vacuo. The residual foam (1.1 g) was taken into dichloromethane (50 ml) and treated with di-tert-butyl-dicarbonate (1.1 g, 5.0 mmol) and saturated sodium bicarbonate (20 ml). The mixture was stirred for 2 hours and the organic layer was separated and dried (MgSO 4 ). The solvent was evaporated in vacuo and the residue was chromatographed using a gradient of 10-30% ethyl acetate/Hexane as eluent, which afforded 175 mg of 2-(tert-butoxyoxalyl-amino)-5-(7-hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-carboxylic acid di-tert-butyl ester.
1 H-NMR (CDCl 3 ): δ12.55 (s, 1H), 8.53 (s, 1H), 7.37 (t, 1H, J=7.6 Hz), 6.92 (d, 1H, J=7.6 Hz), 6.83 (d, 1H, J=7.6 Hz), 4.95 (s, 1H), 4.84 (d, 1H, J=16.4 Hz), 4.72 (d, 1H, J=16.0 Hz), 4.56 (d, 1H, J=16.0 Hz), 4.28 (d, 1H, J=17.6 Hz), 4.13 (m, 1H), 3.68 (s, 0.5H), 3.42 (s, 0.5H), 3.16-2.94 (m, 2H), 1.62 (s, 9H), 1.61 (s, 9H), 1.26 (s, 9H).
To a solution of 2-(tert-butoxyoxalyl-amino)-5-(7-hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-carboxylic acid di-tert-butyl ester (16 mg, 0.025 mmol) in N,N-dimethylformamide (0.5 ml) under nitrogen was added sodium hydride (1.0 mg, 0.026 mmol) at room temperature. The solution was stirred for 2 hours and followed by addition of benzyl bromide (5.9 ml, 0.050 mmol). The solution was stirred for 16 hours, diluted with ethyl acetate (20 ml) and washed with 0.5 N hydrochloric acid solution (2×10 ml), saturated sodium bicarbonate (2×10 ml), brine (10 ml), dried (MgSO 4 ), and filtered. The solvent was removed in vacuo. The residue was chromatographed using a gradient of 10-20% ethyl acetate/Hexane as eluent, which afforded 14 mg (76%) of 5-(7-benzyloxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(tert-butoxyoxalyl-amino)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-carboxylic acid di-tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.49 (s, 1H), 7.48 (d, 2H, J=7.2 Hz), 7.35 (m, 3H), 7.28 (d, 1H, J=7.2 Hz), 6.97 (d, 1H, J=7.6 Hz), 6.80 (d, 1H, J=7.6 Hz), 5.32 (s, 2H), 4.97 (m, 2H), 4.82-4.62 (m, 2H), 4.45-4.15 (m, 2H), 3.68 (s, 0.5H), 3.48 (s, 0.5H), 316-2.94 (m, 2H) 1.62 (s, 9H), 1.60 (s, 9H), 1.26 (s, 9H).
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (2.7 ml) was added 5-(7-benzyloxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(tert-butoxyoxalyl-amino)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-carboxylic acid di-tert-butyl ester (14 mg, 0.019 mmol).
The solution was stirred at room temperature for 40 hours. The reaction mixture was poured into ethyl ether (20 ml). The precipitate was filtered off and dried in vacuo affording 8.0 mg (68%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.25 (s, 1H), 9.28 (s, 1H), 9.02 (s, 1H), 7.53 (m, 3H), 7.39 (t, 2H, J=7.6 Hz), 7.13 (d, 1H, J=7.6 Hz), 7.11 (d, 1H, J=8.4 Hz), 5.27 (m, 2H), 4.54 (d, 1H, J=17.2 Hz), 4.38 (d, 2H, J=17.6 Hz), 4.22 (m, 2H), 4.00 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 3.86 (s, 1H), 3.64 (d, 1H, J=17.2 Hz), 2.81 (dd, 1H, J=18 Hz and J=7.2 Hz);
LC-MS: R t =2.96 min; m/z: 522 [M+H] +
Example 15
5-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (0.5 ml) was added 2-(tert-butoxyoxaly-amino)-5-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (11 mg, 0.014 mmol). The solution was stirred at room temperature for 16 hours. The reaction mixture was poured into ethyl ether (20 ml). The precipitate was filtered off and dried in vacuo, which afforded 7.0 mg (79%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.39 (s, 1H), 9.95 (s, 1H), 9.75 (s, 2H), 7.42 (t, 1H, J=8.0 Hz), 7.30 (s, 2H), 7.02 (d, 1H, J=7.2 Hz), 6.96 (s, 2H), 6.85 (d, 1H, J=7.2 Hz), 4.95-3.65 (m, 11H), 3.76 (s, 3H).
LC-MS: R t =1.93 min, m/z: 553 [M+H] +
Example 16
5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a stirred solution of 2-amino-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (15 mg, 0.028 mmol) in tetrahydrofuran (1.0 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (27 mg, 0.11 mmol) in tetrahydrofuran (1.0 ml). The mixture was stirred at room temperature for 24 hours. The solvent was removed in vacuo. The residue was taken into ethyl acetate (20 ml). The solution was washed with 0.5 N hydrochloric acid solution (2×10 ml), saturated sodium bicarbonate (2×10 ml) and brine (10 ml), dried (MgSO 4 ) and filtered. The solvent was removed in vacuo. The residue was chromatographed using a gradient of 10-25% ethyl acetate/hexane as eluent, which afforded 17 mg (93%) of 2-(tert-butoxyoxalyl-amino)-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.54 (s, 1H), 7.86 (m, 2H), 7.40 (m, 2H), 7.08 (d, 2H, J=8.4 Hz), 6.72 (d, 2H, J=8.4 Hz), 4.08 (dd, 1H, J=13.6 Hz and J=8.8 Hz), 3.94 (d, 1H, J=16.8 Hz), 3.82 (d, 1H, J=12.8 Hz), 3.78 (s, 3H), 3.92 (s, 3H), 3.70-3.56 (m, 3H), 3.53 (d, 1H, J=12.8), 2.93 (dd, 1H, J=16.8 Hz and J=4.8 Hz), 2.75 (dd, 1H, J=18.0 Hz and J=5.6 Hz), 1.61 (s, 9H), 1.58 (s, 9H).
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (0.5 ml) was added 2-(tert-butoxyoxalyl-amino)-5-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (15 mg, 0.023 mmol). The solution was stirred at room temperature for 40 hours. The reaction mixture was poured into ethyl ether (20 ml). The precipitate was filtered off and dried in vacuo, which afforded 13 mg (87%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.38 (s, 1H), 7.89 (d, 4H, J=11.2 Hz), 7.18 (s, 2H), 6.85 (s, 2H), 4.20-3.60 (m, 9H), 3.71 (s, 3H);
LC-MS: R t =2.05 min, m/z: 550 [M+H] +
Example 17
7-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (80 mg, 0.20 mmol) and diisopropyl ethylamine (35 μl, 0.40 mmol) in acetonitrile (10 ml) at room temperature was added a solution of 6-bromomethyl-2-(tert-butyl-dimethyl-silanyloxy)-benzoic acid ethyl ester (69 mg, 0.20 mmol). The solution was stirred for 12 hours at room temperature and the solvent was evaporated in vacuo. The residue was dissolved in ethyl acetate (50 ml) and washed with water, 1 N hydrochloric acid, brine, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was chromatographed on silica gel column eluted with 20% ethyl acetate/hexane to yield 42 mg (33%) of 2-amino-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ7.64 (d, 1H, J=8.8 Hz), 7.39 (t, 1H, J=8.0 Hz), 7.10-6.80 (m, 5H), 6.09 (s, 2H), 5.0-4.2 (m, 4H), 3.80 (s, 3H), 3.66-2.92 (m, 3H), 1.55 (s, 9H), 1.04 (s, 9H), 0.22 (s, 6H).
To a stirred solution of 2-amino-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (40 mg, 0.060 mmol) in tetrahydrofuran (1 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (59 mg, 0.30 mmol) in tetrahydrofuran (1 ml). The mixture was stirred at room temperature for 24 hours. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate (20 ml) and the solution was washed with 0.5 N hydrochloric acid (2×20 ml), saturated sodium bicarbonate (2×20 ml), brine (20 ml), dried (MgSO 4 ) and filtered. The solvent was removed in vacuo and the residue was chromatographed using a gradient of 10-20% ethyl acetate/Hexane as eluent, which afforded 40 mg (83%) of 2-(tert-butoxyoxalyl-amino)-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.52 (s, 1H), 7.37 (t, 1H, J=8.0 Hz), 6.97 (d, 2H, J=8.4 Hz). 6.94 (d, 1H, J=8.0 Hz), 6.83 (d, 1H, J=8.0 Hz), 6.54 (d, 1H, J=8.4 Hz), 4.26 (d, 1H, J=16.8 Hz), 3.93-3.84 (m, 2H), 3.77 (d, 1H, J=16.8 Hz), 3.69 (s, 3H), 3.66-3.48 (m, 3H), 3.42-3.32 (m, 1H), 2.95 (dd, 1H, J=14.4 Hz and J=4.8 Hz), 2.92-2.82 (m, 1H), 2.73 (dd, 1H, J=14.4 Hz and J=4.8 Hz), 1.60 (s, 9H), 1.59 (s, 9H), 1.02 (s, 9H), 0.22 (d, 6H, J=1.6 Hz).
To a solution of 2-(tert-butoxyoxalyl-amino)-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (4.0 mg, 5.1 mol) in 10% formic acid/methanol (1 ml) at room temperature under nitrogen was added 10% Pd/C (4 mg). The mixture was stirred for 1 hour. The Pd/C was filtered off and the filtrate was evaporated in vacuo to afford 2.8 mg (82%) of 2-(tert-butoxyoxalyl-amino)-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-5H-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.45 (s, 1H), 8.05 (s, 1H), 7.39 (t, 1H, J=8.0 Hz), 6.99 (d, 1H, J=8.0 Hz), 6.79 (d, 1H, J=8.0 Hz), 4.50 (d, 1H, J=17.2 Hz), 4.45 (d, 1H, J=17.2 Hz), 4.24 (d, 1H, 8.4 Hz), 4.03 (dd, 1H, J=16.0 Hz and J=7.2 Hz), 3.78-3.68 (m, 2H), 3.38-3.28 (m, 1H), 3.21 (d, 1H, J=18.8 Hz), 3.08-2.98 (m, 1H), 1.57 (s, 9H), 1.56 (s, 9H), 0.98 (s, 9H), 0.15 (d, 6H, J=1 Hz).
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (0.5 ml) was added 2-(tert-butoxyoxalyl-amino)-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-5H-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (2.8 mg, 0.0042 mmol). The solution was stirred at room temperature for 16 hours. The solvent was removed in vacuo and the residue was washed with dichloromethane affording 1.8 mg (79%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.30 (s, 1H), 9.76 (s, 1H), 9.40 (s, 1H), 8.95 (s, 1H), 7.40 (t, 1H, J=7.6 Hz), 7.00 (d, 1H, J=7.6 Hz), 6.83 (d, 1H, J=7.6 Hz), 4.92 (s, 1H), 4.54 (d, 1H, J=18.4 Hz), 4.40 (d, 2H, J=18.4 Hz), 4.08-4.00 (m, 1H), 3.91 (d, 1H, J=15.2 Hz), 3.60 (s, 2H), 3.06 (s, 2H);
LC-MS: R t : 1.41 min, m/z: 432 [M+H] +
Example 18
7-(7-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (0.5 ml) was added 2-(tert-butoxyoxalyl-amino)-7-(7-(tert-butyl-dimethyl-silanyloxy)-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (10 mg, 0.013 mmol). The solution was stirred at room temperature for 16 hours. The solvent was removed in vacuo and the residue was washed with dichloromethane, which afforded 6.8 mg (92%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.35 (s, 1H), 9.90 (s, 1H), 9.70 (s, 2H), 7.41 (t, 1H, J=8.0 Hz), 7.28 (s, 2H), 7.04 (d, 1H, J=7.2 Hz), 6.92 (s, 2H), 6.83 (d, 1H, J=7.2 Hz), 4.90-3.60 (m, 11H), 3.80 (s, 3H).
LC-MS: R t =1.92 min, m/z: 552 [M+H] +
Example 19
7-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a stirred solution of 2-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (10 mg, 0.019 mmol) in tetrahydrofuran (1.0 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (18 mg, 0.092 mmol) in tetrahydrofuran (1.0 ml). The mixture was stirred at room temperature for 24 hours. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate (20 ml) and washed with 0.5 N hydrochloric acid solution (2×10 ml), saturated sodium bicarbonate (2×10 ml), brine (10 ml), dried (MgSO 4 ), and filtered. The solvent was removed in vacuo and the residue was chromatographed using a gradient of 10-25% ethyl acetate/hexane as eluent, which afforded 11 mg (89%) of 2-(tert-butoxyoxalyl-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.54 (s, 1H), 7.76 (m, 4H), 6.82 (d, 2H, J=11.6 Hz), 6.33 (d, 2H, J=11.6 Hz), 4.02 (d, 1H, J=14.4 Hz), 3.98 (d, 1H, J=14.4 Hz), 3.62 (s, 3H), 3.62-3.54 (m, 2H), 3.48-3.34 (m, 2H), 3.02-2.70 (m, 3H), 1.60 (s, 9H), 1.59 (s, 9H).
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (0.5 ml) was added 2-(tert-butoxyoxalyl-amino-7-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (10 mg, 0.015 mmol). The solution was stirred at room temperature for 16 hours. The solvent was removed in vacuo and the residue was washed with dichloromethane, which afforded 6.8 mg (80%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ): δ12.38 (s, 1H), 7.86 (m, 4H), 6.82 (s, 2H), 6.30 (s, 2H), 4.00-2.86 (m, 9H), 3.58 (s, 3H);
LC-MS: R t =2.02 min; m/z: 550 [M+H] +
Example 20
7-(((5-Benzyloxy-1H-indole-2-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
2-Amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.50 g; 1.2 mmol) was dissolved in N,N-dimethylformamide (20 ml). 1-Hydroxy-7-azabenzotriazole (0.19 g; 1.3 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.26 g; 1.3 mmol) and diisopropyl-ethylamine (0.23 ml; 1.3 mmol) were added and the mixture was stirred for 15 min. 5-Benzyloxyindole (0.36 g; 1.3 mmol) was dissolved in N,N-dimethylformamide (20 ml) and added. Diisopropylethylamine (0.23 ml; 1.3 mmol) was added and the mixture was stirred overnight. The solvent was removed in vacuo, the residue dissolved in dichloromethane (30 ml) and the organic phase washed with an aqueous solution of sodium hydrogencarbonate (15 ml). The organic phase was dried (MgSO 4 ), filtered and the solvent removed in vacuo. The residue was chromatographed on silica using ethyl acetate/heptane (1:1) as eluent affording 569 mg of 2-amino-7-(((5-benzyloxy-1H-indole-2-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
The title compound was prepared in a similar way as described in Example 1 using the two last steps.
MS: m/z: 669.4 [M+H] +
Calculated for C 35 H 32 N 4 O 8 S, 2/3×C 2 HF 3 O 2 , 4/3×H 2 O; C, 56.77%; H, 4.63%; N, 7.29%. Found: C, 56.43%; H, 4.57%; N, 7.13%.
Example 21
7-(((6-Bromo-2-p-tolyl-quinoline-4-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 6-bromo-2-p-tolyl-quinoline-4-carboxylic acid and 2-amino-7-aminomethyl6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 745.2 [M+H] +
Calculated for C 36 H 31 BrN 4 O 7 S, 2×C 2 HF 3 O 2 ; C, 49.44%; H, 3.42%; N, 5.77%. Found: C, 49.19%; H, 3.59%; N, 6.00%.
Example 22
6-(4-Methoxy-benzyl)-7-(((5-methyl-2-phenyl-2H-[1,2,3]triazole-4-carbonyl)amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 5-methyl-2-phenyl-2H-[1,2,3]triazole-4-carboxylic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 605.2 [M+H] +
Calculated for C 29 H 28 N 6 O 7 S, 1.3×C 2 HF 3 O 2 , 1.7×H 2 O; C, 48.14%; H, 3.94%; N, 10.94%. Found: C, 48.35%; H, 4.19%; N, 10.68%.
Example 23
7-(((1H-indole-3-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 3-indole-carboxylic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 563.2 [M+H] +
Calculated for C 28 H 26 N 4 O 7 S, 5/3×C 2 HF 3 O 2 ; C, 49.63%; H, 3.82%; N, 7.35%. Found: C, 50.00%; H, 3.71%; N, 7.44%.
Example 24
7-((4-Ethoxy-2-hydroxy-benzoylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 4-ethoxy-2-hydroxy-benzoic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 584 [M+H] +
HPLC: (B6): 23.8 min.
Example 25
7-((4-Benzoylamino-benzoylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 4-benzoylaminobenzoic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 643.1 [M+H] +
Calculated for C 33 H 30 N 4 O 8 S, 3×C 2 HF 3 O 2 ; C, 47.57%; H, 3.38%; N, 5.69%. Found: C, 47.34%; H, 3.55%; N, 5.62%.
Example 26
7-(((Biphenyl-4-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 4-phenylbenzoic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 599.0 [M+H] +
Calculated for C 32 H 29 N 3 O 7 S, 2×C 2 HF 3 O 2 , 1×H 2 O; C, 51.13%; H, 3.93%; N, 4.97%. Found: C, 52.02%; H, 4.02%; N, 5.16%.
Example 27
7-(((1H-Indole-2-carbonyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using indole-2-carboxylic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 563.2 [M+H] +
HPLC (B6) R t =23.07 min.
Example 28
7-((3-Biphenyl-4-yl-acryloylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c)pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 3-biphenyl-4-yl-acrylic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 626.2 [M+H] +
HPLC (B6) R t =28.74 min.
Calculated for C 34 H 31 N 3 O 7 S, 2×C 2 HF 3 O 2 ; C, 53.46%; H, 3.90%; N, 4.92%. Found: C, 53.89%; H, 4.23%; N, 5.08%.
Example 29
6-(4-Methoxy-benzyl)-7-(((5-methoxy-1H-indole-2-carbonyl)amino)-methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 5-methoxyindole-2-carboxylic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 593.2 [M+H] +
HPLC (B6) R t =21.81 min.
Example 30
7-((4-Benzyl-benzoylamino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 4-benzylbenzoic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 614.2 [M+H] +
HPLC (B6) R t =27.23 min.
Calculated for C 33 H 31 N 3 O 7 S, 1.5×C 2 HF 3 O 2 , 1×H 2 O; C, 53.87%; H, 4.33%; N, 5.23%. Found: C, 53.92%; H, 4.24%; N, 5.18%.
Example 31
6-(4-Methoxy-benzyl)-7-(((naphthalene-1-carbonyl)amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as in Example 19 using 1-napthylcarboxylic acid and 2-amino-7-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as the starting material.
LC-MS: m/z: 574.0 [M+H] +
HPLC (B6) R t =22.51 min.
Calculated for C 30 H 27 N 3 O 7 S, 2×C 2 HF 3 O 2 ; C, 50.94%; H, 3.65%; N, 5.24%. Found: C, 51.39%; H, 3.79%; N, 5.16%.
Example 32
6-(4-Methoxy-benzyl)-5-((2-naphthalen-2-yl-ethylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
A solution of 2-naphthalen-2-yl-ethanol (1.02 g, 5.8 mmol), 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) (9 mg, 0.058 mmol) and sodium bromide (0.65 g, 6.4 mmol) in a mixture of toluene (18 mL), ethyl acetate (18 mL), and water (3 mL) was cooled to 0° C. and added dropwise over 1 hour a solution containing the following: sodium hypochlorite (17.2 mL, 0.37 M, 6.4 mmol) and sodium hydrogencarbonate (1.46 g, 17.4 mmol). The reaction mixture was stirred at 0° C. for 10 min., and the phases separated. The aqueous layer was extracted with ethyl acetate (150 mL). The combined organic phases were washed with a solution of potassium iodone (0.2 g) in 10% aqueous potassium hydrogensulfate (150 mL), water (150 mL), brine (150 mL), dried (MgSO 4 ), filtered, and concentrated in vacuo to provide 980 mg of a 3:1 mixture of naphthalen-2-yl-acetaldehyde and 2-naphthalen-2-yl-ethanol.
1 H-NMR (CDCl 3 ): δ9.81 (t, 1H, J=1.5 Hz), 7.92-7.80 (m, 3H), 7.68 (bs, 1H), 7.55-7.42 (m, 3H), 3.87 (d, 2H, J=1.5 Hz).
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (290 mg, 0.71 mmol) in 1,2-dichloroethane (3 ml) was added the above mixture of 2-naphthyl-acetaldehyde (100 mg, 0.59 mmol), sodium triacetoxyborohydride (190 mg, 0.88 mmol) and the mixture was stirred at room temperature under nitrogen for 2.5 hours. The crude reaction mixture was quenched with saturated sodium bicarbonate (50 ml) and the solution extracted with ethyl acetate (100 ml). The organic phase was dried (MgSO 4 ), filtered, and concentrated in vacuo providing a foam, which was taken directly to the next step. LC-MS showed that 2-amino-6-(4-methoxy-benzyl)-5-((2-naphthalen-2-yl-ethylamino)-methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was the major component. LC-MS: m/z: 558.1 [M+H] + , R f =2.23 min.
To a solution of 2-amino-6-(4-methoxy-benzyl)-5-((2-naphthalen-2-yl-ethylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester in tetrahydrofuran (3 ml) was added di-tert-butyl-dicarbonate (188 mg, 0.85 mmol) and N,N-dimethylformamide (18 mg, 0.14 mmol). The reaction was stirred at room temperature for 7 hours under nitrogen. The crude reaction mixture was diluted with dichloromethane (50 ml) and washed with water (50 ml) and brine (50 ml). The organic phase was dried (MgSO 4 ), filtered, and concentrated in vacuo affording a foam, which was used without further purification in the next step.
LC-MS showed that 2-amino-5-((tert-butoxycarbonyl-(2-naphthalen-2-yl-ethyl)-amino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was the major component.
R f =2.74, m/z: 658.1 [M+H] + , Calculated: 657.4.
To crude 2-amino-5-((tert-butoxycarbonyl-(2-naphthalen-2-yl-ethyl)-amino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was added dichloromethane (5 ml) and imidazol-1-yl-oxo-acetic acid tert-butyl ester (400 mg, 1.78 mmol) and the reaction mixture stirred at room temperature for 12 hours. The crude reaction mixture was added to dichloromethane (50 ml) and washed with water (50 ml) and brine (50 ml). The organic phase was dried (MgSO 4 ), filtered, and concentrated in vacuo. The residue was purified by flash chromatography using a mixture of dichloromethane/ethyl acetate (10:1) as eluent, which afforded 20.3 mg (39% over tree steps) of 2-(tert-butoxyoxalyl-amino)-5-((tert-butoxycarbonyl-(2-naphthalen-2-yl-ethyl)-amino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a foam.
1 H NMR (CDCl 3 ) δ7.99-7.92 (m, 3H), 7.88 (s, 1H), 7.68-7.57 (m, 3H), 7.45 (d, 2H, J=7.8 Hz), 6.99 (d, 2H, J=8.1 Hz), 3.90-3.75 (m, 7H), 3.56-3.42 (m, 5H), 3.19-3.13 (m, 2H), 2.88-2.82 (m, 2H), 1.79 (s, 9H), 1.71 (s, 18H);
LC-MS: m/z: 786.2 [M+H] + , R f =3.03 min.
To a solution of 2-(tert-butoxyoxalyl-amino)-5-((tert-butoxycarbonyl-(2-naphthalen-2-yl-ethyl)-amino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (20 mg, 0.03 mmol) in dry dichloromethane (200 μl) at 0° C. was added 50% trifluoroacetic acid in dichloromethane (2.5 ml). The reaction was stirred for 14 hours at room temperature and then concentrated in vacuo. The resultant solid was re-suspended in dichloromethane, filtered, and dried in vacuo to provide 13 mg (90%) of the title compound as a solid.
1 H NMR (DMSO-d 6 ) δ9.15 (s, 1H), 8.09-8.01 (m, 3H), 7.93 (s, 1H), 7.68-7.57 (m, 3H), 7.45 (d, 2H, J=7.8 Hz), 6.99 (d, 2H, J=8.1 Hz), 4.18-4.12 (m, 2H), 3.90-3.75 (m, 7H), 3.56-3.42 (m, 3H), 3.19-3.13 (m, 2H), 2.88-2.82 (m, 2H);
LC-MS: m/z: 574.7 [M+H] + , R f =1.36 min.
Example 33
5-((2-Benzo[1,3]dioxol-5-yl-acetylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a mixture of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (300 mg, 0.74 mmol), benzo[1,3]dioxol-5-yl-acetic acid (134 mg, 0.74 mmol), 1-hydroxybenzotriazole hydrate (111 mg, 0.82 mmol), and N,N-diisopropyl-ethylamine (258 μL, 1.48 mmol) in acetonitrile (5 ml) at room temperature was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (157 mg, 0.82 mmol). The reaction mixture was stirred for 16 hours and the solvent evaporated in vacuo. The residue was taken into ethylacetate (50 ml), washed with water, 1 N hydrochloric acid, saturated sodium bicarbonate, brine, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was subjected to flash chromatography using a gradient of 10-20% ethylacetate/hexanes as eluent, which afforded 268 mg (64%) of 2-amino-5-((2-benzo[1,3]dioxol-5-yl-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ6.95 (bs, 2H), 6.75-6.85 (m, 5H), 5.96 (bs, 2H), 5.95 (s, 2H), 3.81 (s, 3H), 3.75-3.30 (m, 5H), 3.53 (s, 2H), 3.18 (bs, 2H), 2.82 (d, 1H, J=17 Hz), 2.52 (d, 1H, J=17 Hz).
To a solution of 2-amino-5-((2-benzo[1,3]dioxol-5-yl-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (133 mg, 0.235 mmol) in tetrahydrofuran (1 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (100 mg, 0.51 mmol). The mixture was stirred at room temperature for 24 hours. The solvent was removed in vacuo. The residue was taken into ethyl acetate (50 ml) washed with saturated sodium bicarbonate, brine, dried (Na 2 SO 4 ) and filtered. The solvent was removed in vacuo and the residue was chromatographed using a gradient of 10-20% ethyl acetate/dichloromethane, which afforded 130 mg (80%) of 2-(tert-butoxyoxalyl-amino)-5-((2-benzo[1,3]dioxol-5-yl-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ12.50 (s, 1H), 7.95-7.75 (m, 7H), 5.96 (s, 2H), 3.81 (s, 3H), 3.80-3.40 (m, 5H), 3.15 (bs, 2H), 2.90 (d, 1H, J=17 Hz), 2.58 (d, 1H, J=17 Hz), 1.61 (s, 9H), 1.60 (s, 9H).
A solution of 2-(tert-butoxyoxalyl-amino)-5-((2-benzo[1,3]dioxol-5-yl-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (130 mg, 0.188 mmol) in tetrahydrofuran (2 ml) was passed through a Raney Ni bed (120 mg, 50% Raney Ni-water washed with methanol (6 ml) and tetrahydrofuran (6 ml) and dried before use). The Raney Ni bed was washed with tetrahydrofuran (10 ml). The filtrate and washes were combined and the solvent evaporated in vacuo. The residue was dissolved in 10% formic acid/methanol (6 ml) and stirred with 10% Pd/C (120 mg) for 13 hours. Saturated sodium bicarbonate solution (60 ml) was added to the solution. The mixture was extracted with dichloromethane. The extracts were combined, dried (Na 2 SO 4 ) and filtered. The solvent was removed in vacuo and the residue was washed with 50% hexane/diethyl ether to afford 62 mg (57%) of 2-(tert-butoxyoxalyl-amino)-5-((2-benzo[1,3]dioxol-5-yl-acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ12.59 (s, 1H), 6.80-6.70 (m, 3H), 5.96 (s, 2H), 4.05 (q, 2H, J=15 Hz), 3.85-3.60 (m, 2H), 3.25-3.00 (m, 4H), 2.58 (m, 1H), 1.61 (s, 9H), 1.59 (s, 9H);
LC-MS: R t =1.75 min, m/z: 574 [M+H] + .
A solution of 2-(tert-butoxyoxalyl-amino)-5-((2-benzo[1,3]dioxol-5-yl-acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (62 mg, 0.11 mmol) in 50% trifluoroacetic acid-dichloromethane (2 ml) was left in an open flask over the weekend and then the solvent was removed in vacuo. The residue was washed with dichloromethane and the solid filtered off affording 39 mg (62%) of the title compounds as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ) δ12.39 (s, 1H), 9.18 (bs, 1H), 9.10 (bs, 1H), 8.35 (s, 1H), 6.83 d, 1H, J=1.2 Hz), 6.82 (d, 1H, J=8.4 Hz), 6.70 (dd, 1H, J=8.4 Hz and J=1.2 Hz), 5.96 (s, 2H), 4.38 (d, 1H, J=14 Hz), 4.28 (m, 1H), 3.60-3.40 (m, 4H), 3.16 (d, 2H, J=14 Hz), 2.80 dd, 1H, J=14 Hz and J=11 Hz);
LC-MS: R t =1.11 min, m/z: 462 [M+H] + .
Example 34
5-((2-Dibenzofuran-2-yl-ethyl)amino)methyl)-6-(4-methoxy-benzyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-dibenzofuran-2-yl-ethanol (200 mg, 0.94 mmol) and 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) (2 mg, 0.009 mmol) in dichloromethane (2 mL) was added an aqueous solution of sodium bromide (97 mg in 1.3 mL of water for a 0.7M solution, 0.94mmol) and cooled to 0° C. To this mixture was added dropwise over 30 min., a solution containing the following: sodium hypochlorite (1.4 mL, 0.74 M, 1.03 mmol) and sodium hydrogencarbonate (120 mg, 1.4 mmol) and water (1.4 mL). The reaction mixture was stirred at 0° C. for 0.5 hour and allowed to warm to room temperature. The organic phase and aqueous layer were separated and the aqueous layer extracted with dichloromethane (20 mL). The combined organic phases were washed with a solution of potassium iodone (0.2 g) in 10% aq. Potassium hydrogensulfate (20 mL), water (20 mL), brine (20 mL), dried (MgSO 4 ) filtered, and concentrated in vacuo to provide 198 mg of a 5:1 mixture of dibenzofuran-2-yl-acetaldehyde and 2-dibenzofuran-2-yl-ethanol as an oil.
1 H-NMR (CDCl 3 ): δ9.80 (t, 1H, J=1.5 Hz), 8.02 (d, 2H, J=8.2 Hz), 7.71 (bs, 1H), 7.75-7.42 (m, 4H), 3.82 (d, 2H, J=1.5 Hz).
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (340 mg, 0.85 mmol) in 1,2-dichloroethane (3 ml) was added the above mixture of dibenzofuran-2-yl-acetaldehyde (150 mg, 0.70 mmol), and sodium triacetoxyborohydride (225 mg, 1.07 mmol) and the mixture was stirred at room temperature under nitrogen for 2.5 hours. The crude reaction mixture was quenched with saturated sodium bicarbonate (50 ml) and the solution extracted with ethylacetate (100 ml). The organic phase dried (MgSO 4 ), filtered, and the solvent evaporated in vacuo. The crude residue was taken directly to the next step. LC-MS showed that 2-amino-5-((2-dibenzofuran-2-yl-ethylamino)methyl]-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was the major component in the crude mixture: m/z: 598.1 [M+H] + , R f =2.40 min).
Crude 2-amino-5-((2-dibenzofuran-2-yl-ethylamino)methyl]-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was diluted in tetrahydrofuran (3 ml) and di-tert-butyl dicarbonate (262 mg, 1.20 mmol) and 4-(N,N-dimethylamino)pyridine (25 mg, 0.20 mmol) were added. The reaction was stirred at room temperature for 7 hours under nitrogen. The crude reaction mixture was added to dichloromethane (50 ml) and washed with water (50 ml) and brine (50 ml). The organic phase was dried (MgSO 4 ), filtered, and concentrated in vacuo. The residue was used directly in the next step. LC-MS showed that 2-amino-5-((tert-butoxycarbonyl-(2-dibenzofuran-2-yl-ethyl)amino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was the major component in the crude: R f =2.76, m/z: 698.2 [M+H] + .
To compound 2-amino-5-((tert-butoxycarbonyl-(2-dibenzofuran-2-yl-ethyl)amino)-methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was added dichloromethane (5ml) and imidazol-1-yl-oxo-acetic acid tert-butyl ester (420 mg, 2.12 mmol). The reaction mixture was stirred at room temperature for 12 hours. The crude reaction mixture was added to dichloromethane (50 ml) and washed with water (50 ml) and brine (50 ml). The organic phase was dried (MgSO 4 ), filtered, and concentrated in vacuo. The residue was subjected to flash chromatography using a mixture of dichloromethane/ethyl acetate (10:1) as eluent, which afforded 35.2 mg (51% over 3 steps) of 2-(tert-butoxyoxalyl-amino)-5-((tert-butoxycarbonyl-(2-dibenzofuran-2-yl-ethyl)amino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a foam.
1 H-NMR (CDCl 3 ) δ7.95-7.90 (m, 3H), 7.84 (s, 1H), 7.68-7.57 (m, 3H), 7.45 (d, 2H, J==7.8 Hz), 6.95 (m, 3H), 3.90-3.75 (m, 7H), 3.56-3.42 (m, 5H), 3.19-3.13 (m, 2H), 2.88-2.82 (m, 2H), 1.79 (s, 9H), 1.71 (s, 18H);
LC-MS: R f =3.03 min, m/z: 826.2 [M+H] + .
To a solution of 2-(tert-butoxyoxalyl-amino)-5-((tert-butoxycarbonyl-(2-dibenzofuran-2-yl-ethyl)amino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (28 mg, 0.034 mmol) in dry dichloromethane (200 μL) at 0° C. was added 50% trifluoroacetic acid in dichloromethane (2.5 ml). The reaction was stirred for 14 hours at room temperature and then concentrated in vacuo. The resultant solid was re-suspended in dichloromethane, filtered, and dried in vacuo, which afforded 22 mg (90%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ) δ9.15 (s, 1H), 8.11-8.21 (m, 3H), 7.93 (s, 1H), 7.68-7.57 (m, 3H), 7.45 (d, 2H, J=7.8 Hz), 6.99 (d, 2H, J=8.1 Hz), 4.18-4.12 (m, 2H), 3.90-3.75 (m, 7H), 3.56-3.42 (m, 3H), 3.19-3.13 (m, 2H), 2.88-2.82 (m, 2H);
LC-MS: R f =3.03, m/z: 614.7 [M+H] + .
Example 35
6-(4-Methoxy-benzyl)-5-((2-(5-methoxy-2-methyl-1H-indol-3-yl)-acetylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (202 mg, 0.50 mmol), in N,N-dimethylformamide (4 ml) was added 5-methoxy-2-methyl-3-indole acetic acid (170 mg, 0.74 mmol), 1-(3-dimethylamino-propyl)-3-ethylcarbodiimide, hydrochloride (150 mg, 0.75 mmol), and 1-hydroxybenzotriazole (105 mg, 0.74 mmol). The mixture was stirred at room temperature for 12 hours. The crude reaction mixture was diluted with dichloromethane (100 ml) and washed with water (100 ml), brine (100 ml), dried (MgSO 4 ), filtered, and concentrated in vacuo, which afforded 2-amino-6-(4-methoxy-benzyl)-5-((2-(5-methoxy-2-methyl-1H-indol-3-yl)acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ7.16 (d, 2H, J=10.8 Hz), 6.99 (d, 1H, J=2.5 Hz), 6.94 (m, 1H), 6.85 (dd, 1H, J=8.4 Hz and J=1.2 Hz), 6.78 (dd, 1H, J=8.3 Hz and J=1.2 Hz), 6.65 (m, 3H), 6.57 (m, 4H), 3.57 (t, 4H, J=3.0 Hz), 3.53 (m, 6H), 3.59-3.29 (m, 5), 3.12-2.92 (m, 4H), 2.39 (s, 3H), 1.6 (s, 9H);
LC-MS R t =2.19, m/z: 605 [M+H] + .
To a solution of 2-amino6-(4-methoxy-benzyl)-5-((2-(5-methoxy-2-methyl-1H-indol-3-yl)acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (96 mg, 0.5 mmol) in dichloromethane (5 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (583 mg, 3.0 mmol) and the reaction stirred at room temperature for 24 hours. The mixture was then concentrated in vacuo. The residue was purified by flash column chromatography (25% ethylacetate/dichloromethane) to give 53 mg (15%) of 2-(tert-butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-((2-(5-methoxy-2-methyl-1H-indol-3-yl)acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ7.16 (d, 2H, J=10.8 Hz), 6.99 (d, 1H, J=2.5 Hz), 6.94 (m, 1H), 6.85 (dd, 1H, J=8.4 Hz and J=1.2 Hz), 6.78 (dd, 1H, J=8.3 Hz and J=1.2 Hz), 6.65 (m, 3H), 6.56 (m, 3H), 3.57 (m, 3H), 3.53 (m, 6H), 3.59-3.29 (m, 5H), 3.12-2.92 (m, 4H), 2.39 (s, 3H), 1.6 (s, 18H);
LC-MS R t =2.36 min, m/z: 733 [M+H] + .
2-(tert-Butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-((2-(5-methoxy-2-methyl-1H-indol-3-yl)acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was dissolved in 50% trifluoroacetic acid/dichloromethane (3 ml) and stirred at room temperature for 48 hours. The solvent was removed in vacuo and the residual trifluoroacetic acid was removed under reduced pressure to give 17 mg (49%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ) δ10.62 (s, 1H), 7.31 (s, 1H), 7.08 (d, 1H, J=10.2 Hz), 6.93 (s, 2H), 6.58 (dd, 1H, J 1 =5.25 Hz and J 2 =2.8 Hz), 3.84-3.44 (m, 19H, partially obscured by solvent), 2.95 (s, 1H), 2.28 (s, 3H), 1.31 (s, 1H), 1.19 (s, 2H);
LC-MS R t =1.89 min, m/z: 621 [M+H] + .
Example 36
5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-2-(Oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (209 mg, 0.51 mmol) in dry N,N-dimethylformamide (4 ml) was added 3-indole-glyoxylic acid (141 mg, 0.74 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, hydrochloride (152 mg, 0.76 mmol), and 1-hydroxy-benzotriazole (100 mg, 0.74 mmol). The mixture was stirred at room temperature for 16 hours, diluted with dichloromethane (100 ml) and washed with water (100 ml), brine (100 ml), dried (MgSO 4 ), filtered, and concentrated in vacuo. The residue was subjected to flash chromatography using a mixture of ethyl acetate/hexanes (2:5) as eluent, which afforded 143 mg (40%) of 2-amino-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
LC-MS R t =2.31 min, m/z: 574.9 [M+H] + .
To a solution of 2-amino-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (143 mg, 0.25 mmol) in dichloromethane (5 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (144 mg, 0.75 mmol) and the flask was purged with nitrogen. After 24 hours an additional portion of imidazol-1-yl-oxo-acetic acid tert-butyl ester (169 mg, 0.86 mmol) was added and the reaction mixture allowed stirred for an additional 24 hours. The mixture was then concentrated in vacuo. The residue was purified by flash chromatography using a mixture of ethyl acetate/hexanes (2:5) as eluent, which afforded 101 mg (58%) of 2-(tert-butyoxyoxalyl-amino)-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a oil.
1 H-NMR (CDCl 3 ) δ9.23 (s, 1H), 9.07 (d, 1H, J=3.6 Hz), 8.50 (d, 1H, J=7.6 Hz), 8.15 (d, 1H, J=4.0 Hz), 7.47 (d, 2H, J=7.2 Hz), 7.38-7.27 (m, 6H), 6.89 (d, 2H, J=8.8 Hz), 3.87-3.59 (m, 6H), 3.04 (dd, 2H, J=23.6 Hz), 2.74 (dd, 2H, J 22.4 Hz), 1.62 (s, 18H);
LC-MS R t =2.49 min, m/z: 703 [M+H] + .
2-(tert-Butyoxyoxalyl-amino)-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (101 mg, 0.143 mmol) was dissolved in dry tetrahydrofuran (6 ml) and passed through a pipette, plugged with cotton containing Raney 2800 Nickel (0.38 g). The pipette was flushed with dry tetrahydrofuran (6 ml) and the filtrate was concentrated in vacuo. Pd on carbon (10%, 102 mg, source: Avocado) and formic acid (10% in methanol, 5 ml) were added to the flask containing 2-(tert-Butyoxyoxalyl-amino)-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino) methyl)-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester. After stirring for 18 hours, the solution was filtered through a pad of celite and concentrated in vacuo. The residue was diluted in ethyl acetate, washed with saturated sodium bicarbonate (2×25 ml), brine (2×25 ml), dried (MgSO 4 ), filtered and concentrated in vacuo. The residue was subjected to flash chromatography using a mixture of 10% methanol/dichloromethane as eluent, which afforded 2-(tert-butyoxyoxalyl-amino)-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
1 H-NMR (CDCl 3 ) δ9.23 (s, 1H), 9.07 (d, 1H, J=3.6 Hz), 8.50 (d, 1H, J=7.6 Hz), 8.15 (d, 1H, J=4.0 Hz), 7.27 (s, 2H), 7.09 (d, 1H, J=8.8 Hz), 6.81 (d, 1H, J=8.8 Hz), 3.79 (s, 1H), 2.29 (s, 1H), 1.62-1.57 (m, 18H), 0.08 (s, 5H);
LC-MS: R t =2.17 min, m/z: 583 [M+H] + .
The above 2-(tert-butyoxyoxalyl-amino)-5-((2-(1H-indol-3-yl)-2-oxo-acetylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was dissolved in 50% trifluoroacetic acid/dichloromethane (3 ml) and stirred at room temperature for 18 hours. The solvent was removed in vacuo and residual trifluoroacetic acid was removed under reduced pressure affording 17.1 mg of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ) δ12.28 (s, 2H), 9.26 (s, 1H), 9.13 (s, 1H), 8.83 (d, 1H, J=2.8 Hz), 8.26 (d, 1H, J=8.8 Hz), 7.55 (d, 1H, J=4.8 Hz), 7.27 (d, 2H, J=7.6 Hz), 4.42 (d, 1H, J=15.2 Hz), 4.29 (d, 1H, J=16.4 Hz), 3.76-3.22 (m, 4H, partially obscured by solvent), 2.91-2.834 (m, 1H), 1.23 (s, 1H);
LC-MS: R t =0.99 min, m/z 471.4 [M+H] + .
General Chiral Synthesis
4-Oxo-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester
Dichloromethane (1 L) and mol sieves 3 Å (113 g) and amine (S)-(−)α-methylbenzylamin (71,7 ml) were mixed in a 2 l three-necked bottle cooled to −5° C. (using a ethanol/water/ice bath). A 50% solution of ethylglyoxylate in toluene (117,6 ml) was added drop wise over 20 min., keeping the temperature between −5° C. and 0° C. The mixture was stirred for 0.5 hour before it was cooled to −30° C. Trifluoroacetic acid (45,2 ml) was added over 3-4 minutes. Boron trifluoride diethyl ether (69,8 ml) was added drop wise over 5 min at −55° C. The ice bath was removed and the mixture was allowed to warm up to −45° C. whereupon 2-(trimethylsilyloxy)-1,3-butadiene (100 ml) was added drop wise over 10 minutes. During the addition the mixture was cooled and the temperature kept below −20° C. The above additions are all exothermic hence the cooling bath should have sufficient capacity to remove the heat generated during the rapid addition. The reaction mixture was stirred for 2 hours at −15° C. and 1 hour at 0° C. and then poured on ice/water and stirred for 15 minutes. Solid sodium hydrogen carbonate was added until pH 7-8. The mixture was stirred overnight at room temperature. The layers wee separated and the aqueous phase extracted with dichloromethane. The combined organic phases were filtered through a plug of silica eluting with dichloromethane. The relevant fractions were concentrated in vacuo. The residue was dissolved in hot heptane and cooled. This leaves a yellowish gummy material on the side of the flask and crystals starts forming. The heptane solution was heated again to dissolve crystals, leaving the gummy material on the side of the flask and the mixture was filtered hot. The heptane solution was cooled to room temperature and the precipitate was filtered off and dried in vacuo, which afforded 38 g of 4-oxo-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester as a solid.
The filtrate was put in a refrigerator and a second crop was formed which was less pure and needed recrystallization from heptane to yield another 7,5 g of 4-oxo-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester.
4,4-Diethoxy-1-((S)-1-phenyl-ethyl)-piperidine-(S)-2-carboxylic acid ethyl ester
The mother liquor from the above crystallization was concentrated in vacuo. 5.0 g of the resulting material (18.16 mmol) was dissolved in ethanol (100 ml) and triethylorthoformate (26.9 g, 181.6 mmol) and para-toluensulphonic acid (6.9 g, 36.32 mmol) was added. The reaction was stirred at room temperature for 16 hours before the mixture was poured on aqueous sodium hydrogen carbonate (200 ml) and extracted with ethyl acetate (4×75 ml). The combined extracts were concentrated in vacuo and purified by column chromatography (SiO 2 , Flash 40, petrol ether-ethyl acetate 10:1). Collection of the first band (R f =0.68) gave 1.14 g (18%) of 4,4-diethoxy-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester and collection of the second band (R f =0.4) gave 3.60 g (57%) of the title compound.
4,4-Diethoxy-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester
4-Oxo-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester (11.0 g, 0.040 mmol) was dissolved in a 1:1 mixture of triethyl orthoformate and ethanol (140 ml) and para-toluene-4-sulphonic acid (15.2 g, 80 mmol) was added and the reaction mixture was stirred for 16 hours. The reaction mixture was neutralized with sodium bicarbonate (to pH 7-8), and extracted with dichloromethane (3×100 ml), dried (MgSO 4 ), filtered and concentrated in vacuo. The residue was purified by column chromatography (SiO 2 , petrol ether/ethyl acetate 10:1), which afforded 12.0 g (86%) of the title compound as an oil.
4,4-Diethoxy-1-((S)1-phenyl-ethyl)-(R)-2-hydroxymethyl-piperidine
To a solution of 4,4-diethoxy-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester (36.0 g, 0.103 mol) in dry diethyl ether (150 ml) was added a suspension of lithium aluminum hydride (5.88 g, 0.155 mol) in dry diethyl ether (300 ml) under an atmosphere of nitrogen at such a rate that the solution gently reflux. The reaction mixture was stirred over night before it was cooled to 0° C. and ethyl acetate (30 ml) was added drop wise to destroy excess lithium aluminum hydride. After stirring for another 0.5 hour, water (12 ml) was added drop wise. After stirring for 10-15 min the precipitate was filtered off through celite and the filter cage was washed with plenty of diethyl ether. The filtrate was washed with brine (100 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo, which afforded 30 g (95%) of the title compound as an oil.
4,4-Diethoxy-1-((S)-1-phenyl-ethyl)-(R)-2-phthalimidomethyl-piperidine
A solution of 4,4-Diethoxy-1-((S)1-phenyl-ethyl)-(R)-2-hydroxymethyl-piperidine (65.35 g, 0.213 mmol), triphenylphosphine (61.3 g, 0.234 mol) and phthalimide (34.4 g, 0.234 mol) in tetrahydrofuran (700 ml) cooled to 0° C. was added diethyl azodicarboxylate over the course of 1.5 hour. The reaction mixture was stirred at 0° C. for another 2 hours before the solvent was removed in vacuo. The residue was dissolved in hot heptane-toluene (3:2) (650 ml) before it was cooled on an ice bath. The precipitate consisting of triphenyl phosphine oxide was filtered off and washed with heptane. The filtrate was concentrated in vacuo and the residue subjected to column chromatography using a mixture of toluene-ethyl acetate-heptane (3:1:3) as eluent. The solvent was evaporated in vacuo whereupon a viscous oil was obtained. Upon addition of light petrol ether the product crystallized to give 67.4 g (73%) of the title compound as a solid.
Example 37
5-(R)-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-clpyridine-3-carboxylic acid
A mixture of 4,4-diethoxy-1-((S)-1-phenyl-ethyl)-(R)-2-phthalimidomethyl-piperidine (5.25 g, 12.0 mmol) and hydrazine hydrate (2.92 ml, 60 mmol) was stirred overnight in ethanol (100 ml) at room temperature. The solvent was removed in vacuo and the solid residue was extracted with refluxing diethyl ether. The diethyl ether fractions were combined and evaporated in vacuo, which afforded 3.94 g (94%) of 4,4-diethoxy-1-((S)-1-phenyl-ethyl)-(R)-2-aminomethyl-piperidine as an oil.
4,4-Diethoxy-1-((S)-1-phenyl-ethyl)-(R)-2-aminomethyl-piperidine (2.25 g, 7.37 mmol), and triethyl amine (1.49 g, 14.7 mmol) in acetonitrile (50 ml) was heated to 60° C. before 2-chlormethyl-6-methoxy-benzoic acid methyl ester (1.58 g, 7.37 mmol) in acetonitrile (25 ml) was added over the course of 1.5 hour. After addition the reaction mixture was stirred overnight at 60° C. The solvent was removed in vacuo and the residue was dissolved in dichloromethane (50 ml) and washed with saturated sodium bicarbonate. After drying (MgSO 4 ), filtration and evaporation of the solvent in vacuo the residue was subjected to flash column chromatography (SiO 2 , ethyl acetate-light petrol ether (1:1)) to give 2.3 g (69%) of 2-(R)-(7-methoxy-2,3-dihydro-isoindol-1-one-2-ylmethyl)-4,4-diethoxy-1-(1-(S)-phenyl-ethyl)-piperidine.
2-(R)-(7-Methoxy-2,3-dihydro-isoindol-1-one-2-ylmethyl)-4,4-diethoxy-1(1-(S)-phenyl-ethyl)-piperidine (2.0 g, 4.4 mmol) was dissolved in a ice cold mixture of trifluoroacetic acid and water (10 ml, 9:1) and stirred or 0.5 hour on an ice bath. The reaction mixture was poured on aqueous sodium carbonate (100 ml) and extracted with dichloromethane (2×50 ml). The organic phase was dried (MgSO 4 ), filtered and evaporated in vacuo, affording 1.67 g (100%) of 2-(R)-(7-methoxy-2,3-dihydro-isoindol-1-one-2-ylmethyl)-4-oxo-1(1-(S)-phenyl-ethyl)-piperidine.
2-(R)-(7-Methoxy-2,3-dihydro-isoindol-1-one-2-ylmethyl)-4-oxo-1(1-(S)-phenyl-ethyl)-piperidine (1.67 g, 4.41 mmol), sulphur (0.155 g, 4.85 mmol), tert-butylcyanoacetate (0.684 g, 4.85 mmol), N-methylmorpholine (0.892 g, 8.82 mmol) and molecular sieves (4 Å, 2 g) was heated to 50° C. in ethanol under an atmosphere of nitrogen for 16 hours. The reaction mixture was filtered through a plug (1 cm) of SiO 2 , the silica was washed with dichloromethane-ethyl acetate and the solvent was removed in vacuo. The resulting residue was subjected to column chromatography (Flash 40, SiO 2 , toluene-ethyl acetate (3:1)), which yielded 1.17 9 (50%) of 2-amino-5-(R)-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester and 2-amino-7-(S)-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a 3:1 mixture.
The above mixture of 5- and 7-regioisomers (1.17 g, 2.19 mmol) and imidazol-2-yl-oxo-acetic acid tert-butyl ester (1.29 g, 7.57 mmol) and triethylamine (0.66 g, 6.57 mmol) was stirred under an atmosphere of nitrogen in dichloromethane (25 ml) for 16 hours. The solvent was removed in vacuo and the residue was subjected to column chromatography (SiO 2 , Flash 40, ethyl acetate-petrol ether (1:1)). Collection of relevant fractions gave 0.61 g (42%) of 2-(tert-butoxyoxalyl-amin)-5-(R)-(7-methoxy-1-oxo-1 ,3-dihydro-isoindo-2-ylmethyl)-6-(1-(S)-phenyl-ethyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
2-(tert-Butoxyoxalyl-amin)-5-(R)-(7-methoxy-1-oxo-1,3-dihydro-isoindo-2-ylmethyl)-6-(1-(S)-phenyl-ethyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.60 g, 0.91 mmol) was stirred for 16 hours in a mixture of methanol and formic acid (10:1) (20 ml) in the presence of 10% palladium on carbon (50% water). The reaction mixture was filtered through a plug of Celite and washed with methanol. The volatiles were removed in vacuo and the residue was dissolved in dichloromethane (50 ml), washed with semi saturated aqueous sodium carbonate (50 ml), dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was purified by column chromatography (SiO 2 , Flash 40, ethyl acetate-methanol (100:15)), which afforded 0.36 g (71%) of 2-(tert-butoxyoxalyl-amin)-5-(R)-(7-methoxy-1-oxo-1,3-dihydro-isoindo-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
2-(tert-Butoxyoxalyl-amin)-5-(R)-(7-methoxy-1-oxo-1,3-dihydro-isoindo-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (349 mg, 0.63 mmol) was stirred for 16 hours in a mixture of trifluoroacetic acid and dichloromethane (1:1) (10 ml) whereupon diethyl ether (20 ml) was added. The precipitate was filtered off and washed with diethyl ether, which afforded 215 mg (61%) of the title compound as a solid trifluoroacetate.
LC-MS: R t =1.17 min, m/z: 446 [M+H] +
Calculated for C 20 H 19 N 3 O 7 S, C 2 HF 3 O 2 , 0.5×H 2 O C, 46.48%; H, 3.72%; N, 7.39%; Found: C, 46.45%; H, 3.97%; N, 7.43%;
Example 38
5-(S)-(7-Methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno]2,3-clpyridine-3-carboxylic acid
A solution of 4,4-diethoxy-1-((S)-1-phenyl-ethyl)-piperidine-(S)-2-carboxylic acid ethyl ester (35.98 g, 0.103 mol) in diethyl ether (150 ml) was added drop wise to a suspension of lithium aluminum hydride (5.88 g, 0.155 mol) in diethyl ether (300 ml) over the course of 1 hour. The reaction mixture was stirred at room temperature overnight before it was cooled on an ice bath and the reaction was quenched by dropwise addition of ethyl acetate (30 ml), followed by drop wise addition of water (12 ml) whereupon a gray precipitate was formed. The mixture was filtered through a plug of Celite and the filter cage was washed with plenty of diethyl ether. The filtrate was dried (MgSO 4 ) before it was filtered and the solvent removed in vacuo, which afforded 24.5 g (79%) of 4,4-diethoxy-1-(1-(S)-phenyl-ethyl)-(S)-2-hydroxymethyl-piperidine as an oil.
A suspension of 4,4-diethoxy-1-(1-(S)-phenyl-ethyl)-(S)-2-hydroxymethyl-piperidine (20 g, 65 mmol), triphenylphosphine (18.76 g, 72 mmol) and phthalimide (10.52 g, 72 mmol) in tetrahydrofurane (200 ml) cooled to 0° C. was added diethyl azodicarboxylate (11.34 ml, 72 mmol) over the course of 1 hour. The reaction mixture was stirred at 0° C. for another 2 hours before the volatiles were removed in vacuo. The residue was dissolve in hot heptane-toluene (3:2) (100 ml) before it was cooled on an ice bath. The precipitate was filtered off and washed with heptane. The filtrate was concentrated in vacuo and the residue subjected to column chromatography using a mixture of toluene/ethyl acetate/heptane (3:1:3) as eluent. The solvent was evaporated in vacuo and the residue was crystallized by addition of light petrol ether (250 ml). The precipitate was filtered off, which afforded 24 g (85%) of 4,4-diethoxy-1-(1-(S)-phenyl-ethyl)-2-(S)-phthalimidomethyl-piperidine as a solid.
4,4-Diethoxy-1-(1-(S)-phenyl-ethyl)-2-(S)-phthalimidomethyl-piperidine (4.0 g, 9.2 mmol) was dissolved in a mixture of trifluoroacetic acid and water (9:1) (100 ml) at 0° C. and stirred for 2 hours at this temperature. The mixture was basified with half saturated aqueous sodium carbonate, extracted with ethyl acetate and dried (MgSO 4 ) for 2 hours. The solvent was removed in vacuo and the residue was dried in a vacuum own at 40° C. for to days. This afforded 3.23 g (98%) of 4-oxo-1-(1-(S)-phenyl-ethyl)-2-(S)-phthalimidomethyl-piperidine pure without further purification (98%).
A mixture of 4-oxo-1-(1-(S)-phenyl-ethyl)-2-(S)-phthalimidomethyl-piperidine (17.28 g, 47.73 mmol), tert-butylcyanoacetat (7.41 g, 52.17 mmol), sulphur (1.71 g, 52.17 mmol) and morpholine (8.31 g, 95.46 mmol) in ethanol (150 ml) was heated under an atmosphere of nitrogen at 50° C. The volatiles were removed in vacuo and the residue was subjected to column chromatography on silica gel (heptane-ethyl acetate 5:1). The fractions consisting of a mixture of 5- and 7-isomer were collected and the solvent evaporated in vacuo. The residue was purified on a reverse phase (C 18 ) column using a Flash 40 system. The residue was applied in a minimum volume of acetonitrile and eluted with 40% acetonitrile in water containing 0.1% trifluoroacetic acid. When the 5-isomer was collected the eluent was changed to 50% acetonitrile in water with 0.1% trifluoroacetic acid and the 7-isomer was collected. Yield of 2-amino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was 7.96 g and yield of 2-amino-7-(R)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester was 3.72 g (47% total).
2-Amino-5-(S)-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (7.96 g, 15.4 mmol) and hydrazine hydrate (3.85 g, 77.0 mmol) in ethanol (250 ml) was stirred for 16 hours at room temperature. The solvent was removed in vacuo and the solid residue was extracted with diethyl ether (3×200 ml). The fractions were combined and the solvent removed in vacuo to give 5.9 g (100%) of 2-amino-5-(S)-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
2-Amino-5-(S)-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.55 g, 1.42 mmol) and triethylamine (396 I, 2.84 mmol) was heated in acetonitrile (15 ml) under an atmosphere of nitrogen to 60° C. whereupon a solution of 2-chloromethyl-6-methoxy-benzoic acid methyl ester (0.32 g, 1.49 mmol) in acetonitrile (5 ml) was added dropwise over the course of 3 hours, keeping the reaction mixture at 60° C. The reaction was allowed to cool to room temperature and was left for 16 hours before the solvent was evaporated in vacuo. The product was purified by column chromatography (SiO 2 , Flash 40, ethyl acetate-petrol ether) to give 400 mg (53%) of 2-amino-5-(S)-(7-methoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-((S)-1-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
The title compound was obtained as a trifluoroacetate in a similar way as described in example 32 using the last three steps.
Example 39
5-(S)-4-Hydroxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
3-Hydroxy-2-methylbenzoic acid (0.5 g, 3.2 mmol) was dissolved in HPLC grade methanol (5 ml) and cooled to 0° C. under nitrogen. Acetyl chloride (5 ml) was added dropwise. Once the addition was complete, the ice bath was removed and the reaction mixture allowed warming to room temperature over a period of 18 hours. The reaction was complete by tlc (R f =0.5, 1:1 ethyl acetate/hexanes) and quenched with saturated sodium bicarbonate. The reaction mixture was concentrated, diluted with dichloromethane and water and the layers separated. The aqueous layer was extracted with dichloromethane (3×). The organic layers were combined, dried (MgSO 4 ), filtered and concentrated in vacuo, which afforded 0.5 g (91%) of 3-hydroxy-2-methylbenzoic acid methyl ester as a solid.
1 H-NMR (CDCl 3 ) δ7.39 (dd, 1H, J=8.1 Hz and J=1.5 Hz), 7.09 (t, 1H, J=8.1 Hz), 6.92 (dd, 1H, J=8.1 Hz and J=1.2 Hz), 5.11 (bs, 1H), 3.87 (s, 3H), 2.43 (s, 3H).
3-Hydroxy-2-methylbenzoic acid methyl ester (0.5 g, 3.01 mmol) in dichloromethane (15 ml) and N,N-diisopropylethylamine (1.57 ml, 9.03 mmol) was cooled to 0° C. under nitrogen. Chloromethyl methyl ether (0.46 ml, 6.02 mmol) was added dropwise and the reaction allowed warming to room temperature over a period of 18 hours. The reaction was judged to be 50% complete by tlc (1:2 ethyl acetate/hexanes, 12) and therefore, N,N-diisopropylethylamine (1.57 ml, 9.03 mmol) was added, the reaction mixture cooled to 0° C. and chloromethyl methyl ether (0.46 ml, 6.02 mmol) added once more. The reaction mixture was warmed to room temperature and stirred for 5 hours. The reaction was quenched with water and the layers separated. The aqueous layer was extracted once with dichloromethane and the organic layers combined, dried (MgSO 4 ), filtered, and concentrated in vacuo. The crude residue was purified by column chromatography (20% ethyl acetate/hexanes) affording 0.44 g (69%) of 3-methoxymethoxy-2-methyl-benzoic acid methyl ester as an oil.
1 H-NMR (CDCl 3 ) δ7.46 (dd, 1H, J=7.6 Hz and J=1.2 Hz), 7.21 (dd, 1H, J=8 Hz and J=1.2 Hz), 7.18 (d, 1H, J=8 Hz), 5.21 (s, 2H), 3.88 (s, 3H), 3.48 (s, 3H), 2.46 (s, 3H).
To a mixture of 3-methoxymethoxy-2-methyl-benzoic acid methyl ester (0.44 g, 2.09 mmol) in carbon tetrachloride (10 ml) was added N-bromosuccinimide (0.39 g, 2.19 mmol) and 1,1′-azo bis(cyclohexane-carbonitrile) (0.051 g, 0.21 mmol). The mixture was heated at reflux for 3 hours, at which time the reaction was judged complete by tlc (1:4 ethyl acetate/hexanes). The reaction mixture was cooled to room temperature and concentrated in vacuo to a solid. The solid was recrystallized from hexane leaving 0.44 g (82%) of 2-bromomethyl-3-methoxymethoxy-benzoic acid methyl ester as a solid.
1 H-NMR (CDCl 3 ) δ7.58 (dd, 1H, J=6.8 Hz and J=2.4 Hz), 7.33-7.29 (m, 2H), 5.30 (s, 2H), 5.07 (s, 2H), 3.94 (s, 3H), 3.52 (s, 3H).
To a stirred mixture of 2-amino-5-(S)-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.24 g, 0.67 mmol) in acetonitrile (30 ml) was added N,N-diisopropylethylamine (0.16 ml, 0.93 mmol) under nitrogen. 2-Bromo-methyl-3-methoxymethoxy-benzoic acid methyl ester (0.16 g, 0.55 mmol) dissolved in acetonitrile, was added via syringe pump at a rate of 0.3 ml/hour. Once the addition was complete, the reaction mixture was stirred at room temperature for 24 hours. Tlc analysis (1:1 ethyl acetate/hexanes) indicated the reaction to be complete. The volatiles were removed in vacuo and the resultant oil dissolved in ethyl acetate/water. The layers were separated and the aqueous layer extracted with ethyl acetate (3×). The organic layers were combined, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo, which afforded 0.34 g (100%) of 2-amino-5-(S)-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester, which was used without further purification in the next step.
1 H-NMR (CDCl 3 ) δ7.51 (d, 1H, J=6.8 Hz), 7.42 (t, 2H, J=7.6 Hz), 7.23-7.17 (m, 5H), 5.93 (s, 2H), 5.25 (s, 2H), 4.23 (s, 2H), 4.12 (q, 1H, J=7.2 Hz), 3.94 (m, 1H), 1H, J=6.4 Hz), 3.66 (d, 1H, J=16.4 Hz), 3.50 (s, 3H), 3.48-3.46 (m, 1H), 3.20 (dd, 1H, J=14 Hz and J=6 Hz), 2.94-2.87 (m, 1H), 2.60 (m, 1H), 1.49 (s, 9H), 1.36 (d, 3H, J=6.4 Hz);
LC-MS: m/z: 564.1 [M+H] + .
To a solution of 2-amino-5-(S)-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.34 g, 0.60 mmol) in dichloromethane (10 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (0.35 g, 1.8 mmol). The reaction mixture was stirred at room temperature for 18 hours and the solvent concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with water (2×20 ml) and brine (2×25 ml). The organic layer was dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was subjected to flash chromatography using a mixture of ethyl acetate/hexanes (1:1) as eluent. The obtained residue was then subjected to chromatotron purification (1% methanol/dichloromethane) and later to another flash chromatography (20% ethyl acetate/hexanes to 25% ethyl acetate/hexanes) to obtain 210 mg (50%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ12.50 (s, 1H), 7.51 (dd, 1H, J=6.8 Hz and J=1.2 Hz), 7.42 (t, 2H, J=8 Hz), 7.25-7.17 (m, 5H), 5.23 (s, 2H), 4.24 (q, 2H, J=16.8 Hz), 4.08 (d, 1H, J=16.8 Hz), 4.01 (dd, 1H, J=14Hz and J=8.8Hz), 3.89 (d, 1H, J=17.6Hz), 3.82 (q, 1H, J=6.8 Hz), 3.56 (q, 1H, J=6.4 Hz), 3.51 (s, 3H), 2.28 (dd, 1H, J=14 Hz and J=6.4) 2.98-2.92 (m, 1H), 2.69 (d, 1H, J=17.2), 1.56 (s, 9H), 1.54 (s, 9H), 1.38 (d, 3H, J=6.8 Hz);
LC-MS: m/z: 692.5 [M+H] + .
To a solution of 2-(tert-butoxyoxalyl-amino)-5-(S)-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.16 g, 0.23 mmol) in formic acid (10% in methanol, 5 ml total) was added 10% palladium on carbon (85 mg, source: Avacado) and the reaction mixture allowed to stir at room temperature. After 6 hours, tlc (1:1 ethyl acetate/hexanes) analysis indicated reaction complete. The reaction mixture was filtered through a pad of celite and concentrated in vacuo. The crude product was purified via flash chromatography (gradient: 3% isopropyl alcohol/dichloromethane to 5% isopropyl alcohol/dichloromethane (in 1% increments of isopropyl alcohol)) to provide 0.11 g (82%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ12.50 (bs, 1H), 7.48 (dd, 1H, J=7.6 Hz and J=0.8 Hz), 7.38 (t, 1H, J=8 Hz), 7.22 (dd, 1H, J=8 Hz and J=0.8Hz), 5.24 (s, 2H), 4.50 (q, 2H, J=17.3 Hz), 4.02-3.90 (m, 2H), 3.74 (ddd, 2H, J=34 Hz, J=13.6 Hz and J=5.6 Hz), 3.49 (s, 3H), 3.24 (m, 1H), 2.97 (ddd, 1H, J=20 Hz, J=4.4 Hz and J=2.8 Hz), 2.50 (m, 1H), 1.59 (s, 9H), 1.51 (s, 9H);
LC-MS: m/z: 587.8 [M+H] + .
2-(tert-Butoxyoxalyl-amino)-5-(S)-(4-methoxymethoxy-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.11 g, 0.18 mmol) was dissolved in neat trifluoroacetic acid (4 ml) and stirred at room temperature for 48 hours. The reaction mixture was concentrated in vacuo and the resultant solid washed with dichloromethane several times affording 100 mg (83%) of the title compound as a solid trifluoroaceatet.
1 H-NMR (DMSO-d 6 ) δ12.29 (bs, 1H), 10.13 (s, 1H), 9.29 (bs, 1H), 9.10 (bs, 1H), 7.32 (t, 1H, J=7.6 Hz), 7.17 (d, 1H, J=7.2 Hz), 7.01 (d, 1H, J=8 Hz), 4.52 (d, 1H, J=17.2 Hz), 4.40-4.22 (m, 3H), 4.05 (dd, 1H, J=14.4 Hz and J=9.6 Hz), 3.90 (bs, 1H), 3.69 (dm, 1H), 3.22 (dm, 1H), 2.80 (dm, 1H);
LC-MS: m/z: 432.2 [M+H] + .
Example 40
2-(S)-(Oxalyl-amino)-5-((4-phenoxy-benzylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
A solution of 2-amino-5-(S)-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (500 mg, 1.29 mmol) and 4-phenoxybenzaldehyde (256 mg, 1.29 mmol) was heated to 50° C. in ethanol (50 ml) for 1 hour in the presence of molecular sieves (4 A, 5 ml). The reaction mixture was cooled on an ice bath before sodium borohydride (98 mg, 2.59 mmol) was added in three portions over 45 min. The cooling bath was removed and the reaction mixture was allowed to reach room temperature. The mixture was filtered through a plug of Celite and the filter cage was washed with dichloromethane (3×25 ml). The solvent was removed in vacuo and the residue was redissolved in ethyl acetate (50 ml), washed with sodium bicarbonate (50 ml) and dried (MgSO 4 ). The solvent was removed in vacuo before the residue was redissolved in acetonitrile (20 ml). Triethylamine (130 mg, 1.29 mmol), di-tert-butyl dicarbonate (282 mg, 1.29 mmol) and 4-(N,N-dimethyl-amino)pyridine (5 mg, cat.) was added and the reaction mixture was stirred for 16 hours at room temperature. The volatiles were removed in vacuo and ethyl acetate (50 ml) was added and the solution was washed with saturated sodium bicarbonate (50 ml) and dried (MgSO 4 ). The crude product was purified by column chromatography (SiO 2 , petroleum ether-ethyl acetate (9:1)) to give 325 mg (38% overall) of 2-amino-5-(S)-((4-phenoxy-benzylamino)methyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
The title compound was obtained as a trifluoroacetate in a similar way as described in example 32 using the last three steps.
Oxalation: Standard procedure (16 hours, 82%)
Hydrogenolysis: standard procedure (Pd/C, 10% Pd, methanol-formic acid, 16 hours, ((10:1)) (82% yield)
TFA cleavage: Standard procedure. Yield 150 mg (87%).
LC-MS m/z: 482 [M+H] + , R t =1.87 min
Calculated for C 24 H 23 N 3 O 6 S, 2×(C 2 HF 3 O 2 ) C, 47.40%; H, 3.55%; N, 5.92%; Found: C, 47.47%; H, 3.87%; N, 5.88%;
Example 41
5-(S)-((4-Acetylamino-benzylamino)-methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared as a trifluoroacetate in a similar way as described in Example 35 using 2-amino-5-(S)-aminomethyl-6-(l-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester and N-(4-formyl-phenyl)acetamide as the starting material.
Calculated for C 20 H 22 N 4 O 6 S, 1.5×C 2 HF 3 O 2 , 1.5×H 2 O C, 43.78%; H, 3.99%; N, 8.88%; Found: C, 44.20%; H, 4.43%; N, 8.75%;
Example 42
7-(S)-((Acetyl-(4-phenoxy-benzyl)amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
A solution of 2-amino-7-(S)-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (500 mg, 1.29 mmol) and 4-phenoxybenzaldehyde (256 mg, 1.29 mmol) was heated to 50° C. in ethanol (50 ml) for 1 hour in the presence of molecular sieves (4 A, 5 ml). The reaction mixture was cooled on an ice bath before sodium borohydride (98 mg, 2.59 mmol) was added in three portions over 45 min. The cooling bath was removed and the reaction mixture was allowed to reach room temperature. The mixture was filtered through a plug of Celite and the filter cage was washed with dichloromethane (3×25 ml). The solvent was removed in vacuo and the residue was redissolved in ethyl acetate (50 ml), washed with sodium bicarbonate (50 ml) and dried (MgSO 4 ). The solvent was removed in vacuo before the product was dissolved in dichloromethane (10 ml). The solution was cooled on an ice bath before di-isopropyl-ethyl amine (101 mg, 1.29 mmol) was added followed by drop wise addition of acetyl chloride (101 mg, 1.29 mmol) in dichloromethane (1 ml). The reaction mixture was stirred 1 hour at 0° C. and the solution was washed with sodium bicarbonate (10 ml) and dried (MgSO 4 ). The crude product was purified by flash column chromatography (SiO 2 , ethyl acetate-petrol ether 1:3) to give 320 mg (41%) of 7-(S)-((acetyl-(4-phenoxy-benzyl)amino)methyl)-2-amino-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was obtained as a trifluoroacetate in a similar way as described in example 32 using the last three steps.
Oxalation: Standard procedure (Yield 69%)
Hydrogenolysis and trifluoroacetic acid cleavage in one step, Standard procedure (Overall yield 6%)
LC-MS m/z=524 [M+H] + , R t =2.58 min
Calculated for C 26 H 25 N 3 O 7 S, C 2 HF 3 O 2 , 0.5×H 2 O C, 52.01%; H, 4.21%; N, 6.50%; Found: C, 51.82%; H, 4.34%; N, 6.36%.
Example 43
7-(S)-((Acetyl-benzyl-amino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
A solution of 2-amino-7-(S)-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (400 mg, 1.03 mmol) and benzaldehyde (105 mg, 1.03 mmol) was heated to 50° C in ethanol (20 ml) for 1 hour in the presence of molecular sieves (4 A, 7 ml). The reaction mixture was cooled on an ice bath before sodium borohydride (78 mg, 2.06 mmol) was added in three portions over 45 min. The cooling bath was removed and the reaction mixture was allowed to reach room temperature. The mixture was filtered through a plug of Celite and the filter cage was washed with dichloromethane (3×25 ml). The solvent was removed in vacuo and the residue was redissolved in ethyl acetate (50 ml), washed with sodium bicarbonate (50 ml) and dried (MgSO 4 ). The solvent was removed in vacuo before the product was dissolved in dichloromethane (20 ml). The solution was cooled on an ice bath before di-isopropyl-ethyl amine (267 mg, 2.06 mmol) was added followed by drop wise addition of acetyl chloride (81 mg, 1.03 mmol) in dichloromethane (1 ml). The reaction mixture was stirred 1 hour at 0° C. before sodium bicarbonate (20 ml) was added. The mixture was extracted with dichloromethane (2×10 ml) and the combined organic fractions were dried (MgSO 4 ). The crude product was purified by flash column chromatography (petrol ether/ethyl acetate (3:1)), which afforded 250 mg (46%) of 7-(S)-((acetyl-benzyl-amino)methyl)-2-amino-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
The title compound was obtained as a trifluoroacetate in a similar way as described in example 32 using the last three steps.
Oxalation: Standard procedure (54%)
Hydrogenolysis: Standard procedure (methanol-formic acid (10:1)) Yield 38 mg (26%)
Trifluoroacetic acid cleavage: Standard procedure 33 mg (80%)
LC-MS m/z: 432 [M+H] + , R t =1.52 min
Calculated for C 20 H 21 N 3 O 6 S×1.5×C 2 HF 3 O 2 , 2×H 2 O C, 43.26%; H, 4.18%; N, 6.58%; Found: C, 43:19%; H, 3.86%; N, 6.46%.
Example 44
5-(S)-((1,1-Dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of (S)-2-amino-5-aminomethyl-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (1.0 g, 2.58 mmol) in dichloromethane (10 ml) at 0° C. was added N,N-diisopropylethylamine (0.54 ml, 5.16 mmol). A solution of 3-chloro-benzo[d]isothiazole 1,1-dioxide (0.52 g, 2.58 mmol) in dichloromethane (10 ml) was then added dropwise and stirred for 30 min. The solution was warmed to room temperature and washed with water and dried (MgSO 4 ). The solvent was then removed in vacuo. The residue was taken into dichloromethane (15 ml) and imidazol-1-yl-oxo-acetic acid tert-butyl ester (1.0 g, 5.16 mmol) was added. The solution was stirred for 2 hours. The solvent was removed in vacuo. The residue was taken into ethyl acetate (100 ml). The solution was washed with 0.5 N hydrochloric acid solution, saturated sodium bicarbonate and brine, dried (MgSO 4 ) and filtered. The solvent was removed in vacuo. The residue was chromatographed using a mixture of 0-5% ethyl acetate/dichloromethane as eluent, which afforded 0.6 g (34%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-((1,1-dioxo-1H-benzo[d] isothiazol-3-ylamino)methyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil
1 H-NMR (CDCl 3 ) δ12.50 (s, 1H), 7.94-7.92 (m, 1H), 7.79-7.71 (m, 2H), 7.59-7.50 (m, 1H), 7.38-7.27 (m, 4H), 6.86 (d, 1H, J=4 Hz), 4.14 (d, 1H, J=12 Hz), 3.95 (d, 1H, J=17 Hz), 3.88 (q, 1H, J=6 Hz), 3.70-3.62 (m, 1H), 3.47 (t, 1H, J=13 Hz), 3.34-3.24 (m, 1H), 3.06 (dd, 1H, J=17, 6 Hz), 2.53 (d, 1H, J=17 Hz), 1.62 (s, 9H), 1.61 (s, 9H), 1.44 (d, 3H, J=7 Hz).
A solution of 2-(tert-butoxyoxalyl-amino)-5-(S)-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-6-(1-(S)-phenyl-ethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (252 mg, 0.37 mmol) in tetrahydrofuran (12 ml) was passed through Raney Ni (0.95 g, 50% Raney Ni-Water washed with methanol (6 ml) and tetrahydrofuran (10 ml) and dried before use). The solvent was removed in vacuo. The residue was dissolved in acetic acid (7 ml) and hydrogenated with 10% Pd/C (250 mg) at 50 psi for 15 hours. The mixture was filtered and the filtrate was added to saturated sodium bicarbonate solution. The solution was then extracted with ethylacetate (3×100 ml). The extracts were combined and dried (MgSO 4 ). The solvent was removed in vacuo. The residue was washed with diethyl ether affording 156 mg (73%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)-methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ) δ12.59 (s, 1H), 7.94-7.90 (m, 1H), 7.70-7.66 (m, 3H), 7.51 (s, 1H), 4.11 (d, 1H, J=12 Hz), 4.08 (q, 2H, J=17 Hz), 3.40 (dd, 1H, J=12, 6 Hz), 3.26-3.18 (m, 1H), 3.18 (d, 1H, J=17 Hz), 2.55 (dd, 1H, J=12, 6 Hz), 1.62 (s, 18H).
LC-MS: R t =3.58 min, m/z: 577 [M+H] + .
A solution of 2-(tert-butoxyoxalyl-amino)-5-(S)-((1,1-dioxo-1H-benzo[d]isothiazol-3-ylamino)methyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (149 mg, 0.26 mmol) in 50% trifluoroacetic acid/dichloromethane (1 ml) was left in an open flask for 60 hours. The volatiles were removed in vacuo and the residue was washed with dichloromethane to yield 80 mg (54%) of the title compound as a solid trifluoroacetate.
1 H-NMR (DMSO-d 6 ) δ12.29 (s, 1H), 9.80 (s, 1H), 9.51 (bs, 2H), 8.19 (d, 1H, J=5 Hz), 8.02-8.00 (m, 1H), 7.89-7.84 (m, 2H), 4.46 (d, 1H, J=16 Hz), 4.30 (d, 1H, J=16 Hz), 3.96-3.80 (m, 3H), 3.30 (d, 1H, J=17 Hz), 2.93 (dd, 1H, J=18, 10 Hz);
LC-MS: R t =0.68 min, m/z: 465 [M+H] + .
Example 45
5-(4-Benzyloxy-1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
The title compound was prepared in a similar way as described in Example 5 as a trifluoroacetate. 1 H-NMR (400 MHz, DMSO-d 6 ) δ12.31 (s, 1H), 9.25 (bs, 2H), 7.80 (t, 1H, J=8 Hz), 7.59-7.32 (m, 7H), 5.37 (s, 2H), 4.42-4.21 (m, 2H), 3.95-3.70 (m, 3H), 3.4-3.2 (obscure by water, 1H), 2.83-2.75 (m, 1H)
LC-MS: R t =2.16 min, m/z: 536.1 [M+H] +
Example 46
5-(6-Methoxy-4-methoxycarbonyl-1-oxo-1 ,3-dihydro-isoindol-2-ylmethyl)-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-amino-5-aminomethyl-6-(4-methoxy-benzyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (57.4 mg, 0.142 mmol) and diisopropyl ethylamine (49 μl, 0.28 mmol) in acetonitrile (20 ml) at room temperature was added 2-bromomethyl-5-methoxy-isophthalic acid dimethyl ester (3.00 g, 7.45 mmol). The solution was stirred for 16 hours and the solvent evaporated in vacuo. The residue was taken into ethyl acetate (50 ml) and washed with water (2×20 ml), 1 N hydrochloric acid (20 ml), brine, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was chromatographed on silica gel column using a mixture of ethyl acetate/hexane (1:1) as eluent, which afforded 62 mg (71%) of 2-amino-6-(4-methoxy-benzyl)-5-(6-methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR δ(CDCl 3 ): δ7.75 (d, 1H, J=2.4 Hz), 7.55 (d, 1H, J=2.4 Hz), 7.11 (bs, 2H), 6.74 (d, 2H, J=8.0 Hz), 5.97 (s, 2H), 4.71 (d, 1H, J=18.4 Hz), 4.62 (d, 1H, J=18.4 Hz), 4.09 (m, 1H), 3.93 (s, 3H), 3.92 (s, 3H), 3.80 (m, 1H), 3.76 (s, 3H), 3.66-3.40 (m, 5H), 2.80 (d, 1H, J=17.2 Hz), 2.64 (d, 1H, J=17.2 Hz), 1.52 (s, 9H).
To a stirred solution of 2-amino-6-(4-methoxy-benzyl)-5-(6-methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (60 mg, 0.10 mmol) in tetrahydrofuran (1.0 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (60 mg, 0.30 mmol) in tetrahydrofuran (1.0 ml). The mixture was stirred at room temperature for 24 hours. The solvent was removed in vacuo. The residue was taken into ethyl acetate (20 ml) and washed with 0.5 N hydrochloric acid (2×10 ml), saturated sodium bicarbonate (2×10 ml) and brine (10 ml), dried (MgSO 4 ) and filtered. The solvent was removed in vacuo and residue was chromatographed using a gradient ethyl acetate/hexane (10-25%) as eluent, which afforded 40 mg (58%) of 2-(tert-butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-(6-methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid.
1 H-NMR δ(CDCl 3 ): δ12.54 (s, 1H), 7.75 (d, 1H, J=2.4 Hz), 7.55 (d, 1H, J=2.4 Hz), 7.10 (d, 2H, J=8.0 Hz), 6.74 (d, 2H, J=8.0 Hz), 4.74 (d, 1H, J=18.4 Hz), 4.62 (d, 1H, J=18.4 Hz), 4.05-3.90 (m, 2H), 3.94 (s, 3H), 3.92 (s, 3H), 3.82-3.48 (m, 5H), 3.77 (s, 3H), 2.95 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 2.67 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 1.61 (s, 9H), 1.58 (s, 9H).
To a solution of 2-(tert-butoxyoxalyl-amino)-6-(4-methoxy-benzyl)-5-(6-methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (38 mg, 0.055 mmol) in 10% formic acid/methanol (1.0 ml) at room temperature under nitrogen was added 10% Pd/C (38 mg). The mixture was stirred for 16 hours and the Pd/C was filtered off and the filtrate evaporated in vacuo. The residue was taken into dichloromethane (1.0 ml) poured into hexane. The precipitate was filtered off, affording 28 mg (82%) of 2-(tert-butoxyoxalyl-amino)-5-(6-methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as a solid. 1 H-NMR δ(CDCl 3 ): δ12.45 (s, 1H), 10.90 (s, 1H), 10.69 (s, H), 7.73 (s, 1H), 7.42 (s, 1H), 4.85 (bs, 2H), 4.65 (bs, 1H), 4.42 (bs, 2H), 3.99 (bs, 2H), 3.96 (s, 3H), 3.89 (s, 3H), 3.35 (bs, 1Hz), 3.21 (bs, 1H), 1.62 (s, 9H), 1.56 (s, 9H).
To a solution of trifluoroacetic acid (0.5 ml) and dichloromethane (0.5 ml) was added 2-(tert-butoxyoxalyl-amino)-5-(6-methoxy-4-methoxycarbonyl-1-oxo-1,3-dihydro-isoindol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (14 mg, 0.023 mmol). The solution was stirred at room temperature for 40 hours. The reaction mixture was poured into diethyl ether (20 ml). The precipitate was filtered off, which afforded 10 mg (75%) of the title compound as a solid trifluoroacetate.
1 H-NMR δ(DMSO-d 6 ): δ12.28 (s, 1H), 9.32 (s, 1H), 9.10 (s, 1H), 7.65 (d, 1H, J=2.4 Hz), 7.50 (d, 1H, J=2.4 Hz), 4.82 (d, 1H, J=17.2 Hz), 4.65 (d, 1H, J=17.6 Hz), 4.40 (d, 1H, J=17.6 Hz), 4.30 (m, 1H), 4.10 (dd, 1H, J=17.2 Hz and J=5.2 Hz), 3.95 (s, 1H), 3.89 (s, 6H), 3.85 (d, 1H, J=17.2 Hz), 2.81 (dd, 1H, J=18 Hz and J=7.2 Hz).
LC-MS: R t =1.30 min; m/z: 504 [M+H] +
Example 47
2-(Oxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3-carboxylic acid and 2-(Oxalyl-amino)-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-aminomethyl-4-(2-spiro[1,3]dioxolane)-piperidine (193 mg, 1.12 mmol) and diisopropyl ethylamine (0.46 ml, 2.55 mmol) in acetonitrile (10 ml) cooled to 0° C. was added 2-chlorosulfonyl-benzoic acid methyl ester (278 mg. 1.18 mmol). The solution was stirred at 25° C. for 24 hours. Solvent was removed in vacuo and the residue was chromatographed using a mixture of ethyl acetate/hexane (1:3) as eluent, which afforded 199 mg (51%) of 2-(4-(2-spiro[1,3]dioxolane)piperidin-2-ylmethyl)-1,1-dioxo-1,2-dihydro-1H-benzo[d]isothiazol-3-one as a solid.
1 H-NMR (CDCl 3 ): δ7.99-7.96 (m, 1H), 7.66-7.53 (m, 3H), 5.01 (s, 1H), 4.73 (dm, 1H, J=14.4 Hz), 4.06-3.93 (m, 6H), 3.25 (dd, 1H, J=12.6 Hz), 3.06 (td, 1H, J=13.5 Hz and J=3.6 Hz), 1.93 (dd, 1H, J=14.1 Hz and J=5.7 Hz), 1.87 (dd, 1H, J=14.1 Hz and J=3.0 Hz), 1.76 (dd, 1H, J=13.5 Hz and J=5.1 Hz).
LC-MS: R t =1.78; m/z: 339 [M+H] + .
2-(4-(2-Spiro[1,3]dioxolane)piperidin-2-ylmethyl)-1,1-dioxo-1,2-dihydro-1H-benzo[d]isothiazol-3-one (199 mg, 0.588 mmol) was dissolved in 2 M hydrochloric acid (12 ml) and the solution was heated to 50° C. for 24 hours. The volatiles were removed in vacuo and the residue (341 mg) was treated without further purification with saturated sodium carbonate (12 ml), dichloromethane (8 ml) and di-t-butyl dicarbonate (1.64 g, 7.5 mmol). The mixture was stirred at 35° C. for 3 days and extracted with dichloromethane (30 ml). The organic solution was washed with saturated sodium bicarbonate, brine, dried (MgSO 4 ), filtered and the solvent evaporated in vacuo. The residue was chromatographed on silica gel column using a mixture of ethyl acetate/hexane (1:3) as eluent, which afforded 115 mg (50%) of 4-oxo-2-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-piperidine-1-carboxylic acid tert-butyl ester as an oil.
1 H-NMR (CDCl 3 ): δ8.06 (dd, 1H, J=6.0, 1.8 Hz), 7.95-7.80 (m, 3H), 5.02 (bs, 1H), 4.35 (bs, 1H), 3.91 (dd, 1H, J=15.0 Hz and J=8.4 Hz), 3.78 (dd, 1H, J=14.7 Hz and J=5.7 Hz), 3.53 (t, 1H, J=10.8 Hz), 2.74 (dd, 1H, J=15.0 Hz and J=7.5 Hz), 2.60-2.38 (m, 3H), 1.32 (s, 9H).
To a solution of 4-oxo-2-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-piperidine-1-carboxylic acid tert-butyl ester (115 mg, 0.292 mmol) in absolute ethanol (5 ml) was added t-butyl cyanoacetate (57 l, 0.41 mmol), sulfur (13 mg, 0.41 mmol) and morpholine (55 μl, 0.63 mmol). The solution was stirred at 50° C. for 14 hours. The solvent was evaporated in vacuo and the residue was chromatographed on silica gel column using a mixture of ethyl acetate/hexane (1:4) as eluent, which afforded 100 mg (62%) of 2-amino-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-amino-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a mixture.
1 H-NMR (CDCl 3 ): δ8.10-8.00 (m, 1H), 7.98-7.77 (m, 2.8H), 7.66-7.58 (m, 0.2H), 6.11 (s, 0.4H), 6.06 (s, 0.6H), 5.59 (m, 0.2H), 5.39 (t, 0.3H, J=5.7 Hz) 5.23 (bs, 0.3H), 5.04 (bs, 0.4H), 4.77 (d, 0.4H, J=14.4 Hz), 4.60 (d, 0.4H, J=14.4 Hz), 4.45-4.18 (m, 1H), 4.02-3.82 (m, 1.5H), 3.64 (dd, 0.5H, J=14.7 Hz and J=5.2 Hz), 3.30-2.60 (m, 2H), 1.54 (s, 7H), 1.53 (s, 2H), 1.26 (s, 7H), 1.21 (s, 2H).
To a stirred solution of the above 2-amino-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-amino-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester mixture (100 mg, 0.18 mmol) in acetonitrile (7 ml) was added imidazol-1-yl-oxo-acetic acid tert-butyl ester (290 mg, 1.46 mmol) in acetonitrile (1 ml). The mixture was stirred at room temperature for 16 hours. The solvent was removed in vacuo and the residue was taken into ethyl acetate. The solution was washed with 0.5 N hydrochloric acid solution, saturated sodium bicarbonate, brine, dried MgSO 4 ) and filtered. The solvent was removed in vacuo and the residue was chromatographed on silicagel using a mixture of ethyl acetate/hexane (1:4) as eluent, which provided 98 mg (80%) of a mixture of 2-(tert-butoxyoxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-(tert-butoxyoxalyl-amino)-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester as a solid.
1 H-NMR (CDCl 3 ): δ12.60 (s, 0.3H), 12.54 (s, 0.7H), 8.12-8.06 (m, 1H), 7.98-7.80 (m, 2.8H), 7.66-7.58 (m, 0.2H), 5.83 (bs, 0.1H), 5.61 (t, 0.2H), 5.40-4.54 (m, 0.9H), 4.53-4.40 (m, 0.8H), 4.02-3.70 (m, 1.42H), 3.66 (dd, 0.58H, J=14.7 Hz and J=5.2 Hz), 3.30-2.99 (m, 3H), 1.68 (s, 6H), 1.62 (s, 6H), 1.60 (s, 6H), 1.31 (s, 4.5H), 1.25 (s, 4.5H)
LC-MS: R t =4.45; m/z: 678 [M+H] + .
To a solution of trifluoroacetic acid (4 ml) and dichloromethane (2 ml) was added the mixture of 2-(tert-butoxyoxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester and 2-(tert-butoxyoxalyl-amino)-7-(1,1,3-trioxo-1,3-dihydro-1H-benzo[d]isothiazol-2-ylmethyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (78 mg, 0.12 mmol). The solution was stirred at room temperature for 24 hours. The solvent was then evaporated in vacuo, which afforded 50 mg (72%) of the title compounds as a mixture of trifluoroacetates.
1 H-NMR (DMSO-d 6 ): δ12.32 (s, 1H), 9.75-9.20 (m, 2H), 8.40 (t, 1H, J=6.0 Hz), 8.22-8.02 (m, 3H), 5.03 (bs, 0.5H), 4.52 (d, 1H), 4.38-4.10 (m, 2H), 3.88 (bs, 0.5H), 3,70-3.64 (m, 0.5H), 3.44-3.34 (m, 0.5H), 3.20-2.90 (m, 2H).
LC-MS: R t =1.28 min, m/z: 466 [M+H] +
Example 48
7-(R)-Carbamoyl-2-(oxalyl-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-(S)-4-oxo-piperidine-1,2-dicarboxylic acid 1-tert butyl ester (18.4 g, 75.6 mmol) and triethylamine (12.65 mL, 90.79 mmol) in tetrahydrofuran (50 mL) cooled to −20° C. was added isobutylchloro-formate (11.81 mL, 90.79 mmol) and the mixture was stirred for 10 min at −20° C. before a 25% solution of ammonia in water (100 mL) was added. The temperature was kept at −20° C. for 30 min before the cooling bath was removed and the reaction mixture was allowed to reach room temperature and stirring was continued for another hour. The reaction mixture was extracted with ethyl acetate (6×50 mL) and the combined organic phases were dried (MgSO 4 ). The solvent was removed in vacuo and the residue was purified by column chromatography (SiO 2 , Flash 40, ethyl acetate) to give 8.51 g (46%) of 2-(S)-carbamoyl-4-oxo-piperidine-1-carboxylic acid 1-tert-butyl ester.
A solution of 2-(S)-carbamoyl-4-oxo-piperidine-1-carboxylic acid 1-tert butyl ester (3.51 g, 14.48 mmol), tert-butyl cyanoacetate (2.04 g, 14.48 mmol), sulphur (0.464 g, 14.48 mmol) and diisopropyl ethylamine (2.5 mL, 14.48 mmol) in methanol (20 mL) was heated 16 hours at 40° C. under N 2 . The volatiles were removed in vacuo and the residue was purified using column chromatography (SiO 2 , Flash 40, petroleum ether/ethyl acetate 3:1) to give 1.33 g (23%) of a mixture 2-amino-5-(S)-carbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-di-carboxylic acid di-tert-butyl ester and 2-amino-7-(R)-carbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-di-carboxylic acid di-tert-butyl ester isomers.
0.5 g (1.25 mmol) of the above mixture was dissolved dichloromethane (10 mL) and imidazole-1-yl-oxo-acetic acid tert-butyl ester (0.74 g, 3.77 mmol) and triethylamine (525 μL, 3.77 mmol) was added. The reaction mixture was stirred for 16 hours at room temperature before the volatiles were removed in vacuo. The residue was purified by column chromatography (SiO 2 , Flash 40, petroleum ether/ethyl acetate (4:1)) too give 75 mg (11%) of 2-(tert-butoxyoxalyl-amino)-7-(R)-carbamoyl-4,7-dithydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester.
This was dissolved in a mixture of trifluoacetic acid/dichloromethane (1:1) (10 mL) and stirred for 16 hours at room temperature before the solvent was removed in vacuo. The residue was recrystallized from methanol to give 24 mg (39%) of the title compound.
LC-MS; R t =1.56 min, m/z: 314 [M+H] +
Calculated for C 11 H 11 N 3 O 6 S, 0.25×C 2 HF 3 O 2 , 0.75×H 2 O C, 38.88%; H, 3.62%; N, 11.83%; Found: C, 38.92%; H, 3.92%; N, 11.81%.
Example 49
2-(Oxalyl-amino)-5-(S)-(2-oxo-tetrahydro-thiophen-3-ylcarbamoyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
A solution of 2-amino-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,5-(S),6-tri-carboxylic acid 3,6-di-tert-butyl ester (0.30 g, 0.75 mmol) and triethylamine (0.21 mL, 1.51 mmol) in tetrahydrofuran (10 mL) was cooled to −20° C. before isobutyl chloroformate (103 μL, 0.75 mmol) was added. The reaction mixture was stirred 15 min at −20° C. before homocystein hydrochloride (116 mg, 0.75 mmol) was added. The cooling bath was removed and the reaction mixture was left for 16 hours at room temperature. The solvent was removed in vacuo and the residue was subjected to column chromatography (SiO 2 , Flash 40, heptane/ethyl acetate 2:1) to give 212 mg (56%) of 2-amino-5-(S)-(2-oxo-tetrahydro-thiophen-3-ylcarbamoyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester
A solution of 2-amino-5-(S)-(2-oxo-tetrahydro-thiophen-3-ylcarbamoyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester (200 mg, 0.40 mmol), imidazole-1-yl-oxo-acetic acid tert-butyl ester (235 mg, 1.20 mmol) and triethylamine (168 μL, 1.20 mmol) in dichloromethane (10 mL) was stirred for 16 hours at room temperature before the solvent was removed in vacuo. The residue was purified by column chromatography (SiO 2 , Flash 40, heptane/ethyl acetate 2:1) to give 250 mg (100%) of 2-(tert-butoxyoxalyl-amino)-5-(S)-(2-oxo-tetrahydro-thiophen-3-ylcarbamoyl)-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester.
This was dissolved in a mixture of trifluoroacetic acid/dichloromethane (1:1) (3 mL) and stirred for 16 hours at room temperature before diethyl ether (6 mL) was added. The precipitate was filtered off and washed with diethyl ether to give 172 mg (81%) of the title compound as a solid trifluoroacetate.
LC-MS; R t =0.41 min, m/z: 414 [M+H] +
Calculated for C 15 H 15 N 3 O 7 S 2 , 1.5×C 2 HF 3 O 2 , H 2 O; C, 35.88%; H, 3.10%; N, 6.97%; Found: C, 35.91%; H, 3.54%; N, 6.97%.
Example 50
2-(Oxalyl-amino)-5-(S)-phenylcarbamoyl-4,5,6,7-tetrahydro-thieno[2,3-clpyridine-3-carboxylic acid
A solution of 2-amino-4,5,6,7-tetrahydro-thieno[2,3-c]-pyridine-3,5-(S),6-tricarboxylic acid 3,5-di-tert-butyl ester (300 mg, 0.75 mmol) and triethylamine (210 μL, 1.51 mmol) in tetrahydrofuran (10 mL) was cooled to −20° C. before isobutylchloroformate (103 mg, 0.75 mmol) was introduced. The reaction mixture was stirred for 20 min before aniline (70 mg, 0.75 mmol) was added. The cooling bath was removed and the reaction was left for 16 hours at room temperature before the solvent was removed in vacuo. The residue was partitioned between ethyl acetate (50 mL) and water (50 mL). The organic phase was dried (MgSO 4 ) and the solvent was removed in vacuo. The residue was dissolved in dichloromethane (10 mL) and imidazole-1-yl-oxo-acetic acid tert-butyl ester (443 mg, 2.26 mmol) and triethylamine (315 μL, 2.26 mmol) was added. The reaction mixture was stirred 16 hours at room temperature before the solvent was removed in vacuo. The residue was purified by column chromatography (SiO 2 , Flash 40, heptane/ethyl acetate (3:1) to give 250 mg 2-(tert-butoxyoxalyl-amino)-5-(S)-phenylcarbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester.
2-(tert-Butoxyoxalyl-amino)-5-(S)-phenylcarbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-dicarboxylic acid di-tert-butyl ester was dissolved in a mixture of trifluoroacetic acid/dichloromethane (1:1) (3 mL) and stirred for 16 hours at room temperature before di-ethyl ether (6 mL) was added. The precipitate was filtered off and washed with diethyl ether to give 155 mg (41%) of the title compound as a solid trifluoroacetate.
LC-MS; R t =0.86 min, m/z: 390 [M+H] +
Calculated for C 17 H 15 N 3 O 6 S, 1.5×C 2 HF 3 O 2 , H 2 O; C, 41.53%; H, 3.22%; N, 7.26%; Found: C, 41.77%; H, 3.29%; N, 7.28%.
Example 51
2-(Oxalyl-amino)-7-(R)-phenylcarbamoyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
To a solution of 2-(S)-4-oxo-piperidine-1,2-dicarboxylic acid 1-tert butyl ester (2.06 g, 8.47 mmol) and triethylamine (1.42 mL, 10.16 mmol) in tetrahydrofuran (20 mL) cooled to −20° C. was added isobutylchloroformate (1.39 g, 10.16 mmol) and the mixture was stirred for 10 min at −20° C. before aniline (946 mg, 10.16 mmol) was added. The cooling bath was removed and the reaction mixture was stirred for 16 hours at room temperature before the solvent was removed in vacuo. The residue was divided between water (50 mL) and ethyl acetate (50 mL). The organic phase was washed with saturated sodium chloride (25 mL) and dried (MgSO 4 ). After filtration and concentration in vacuo the residue was purified using column chromatography (SiO 2 , Flash 40, petroleum ether/ethyl acetate 5:1) to give 1.3 g (48%) of 4-oxo-2-(S)-phenyl-carbamoyl-piperidine-1-carboxylic acid tert-butyl ester.
A solution of 4-oxo-2-(S)-phenylcarbamoyl-piperidine-1-carboxylic acid tert-butyl ester (1.3 g, 4.08 mmol), tert-butylcyanoacetate (0.58 g, 4.08 mmol), sulphur (0.133 g, 4.08 mmol) and diisopropyl ethylamine (0.7 mL, 4.08 mmol) in methanol (10 mL) was heated under nitrogen to 40° C. for 16 hours before the solvent was removed in vacuo. The residue was subjected to column chromatography (SiO 2 , Flash 40, petroleum ether/ethyl acetate 6:1) to give 0.70 g (36%) of a mixture of 2-amino-5-(S)-phenylcarbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-di-carboxylic acid di-tert-butyl ester and 2-amino-7-(R)-phenylcarbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-di-carboxylic acid di-tert-butyl ester isomers.
The above mixture was dissolved in dichloromethane (20 mL) and imidazole-1-yl-oxo-acetic acid tert-butyl ester (872 mg, 4.44 mmol) and triethylamine (618 μL, 4.44 mmol) was added. The reaction mixture was stirred 16 hours before the solvent was removed in vacuo and the residue was subjected to column chromatography (SiO 2 , Flash 40, petroleum ether/ethyl acetate 5:1) to give 0.50 g (56%) as a mixture of 2-(tert-butoxyoxalyl-amino)-5-(S)-phenylcarbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-di-carboxylic acid di-tert-butyl ester and 2-(tert-butoxyoxalyl-amino)-7-(R)-phenylcarbamoyl-4,7-dihydro-5H-thieno[2,3-c]pyridine-3,6-di-carboxylic acid di-tert-butyl ester.
300 mg of the mixture was dissolved in a mixture of trifluoacetic acid/dichloromethane (1:1) (6.0 mL) and the solution was stirred for 16 hours at room temperature before the solvent was removed in vacuo. The residue was purified on preparative HPLC to give 70 mg (34%) of the title compound as a solid trifluoroacetate.
LC-MS; R t =0.95 min, m/z: 390 [M+H] +
Calculated for C 17 H 15 N 3 O 6 S, C 2 HF 3 O 2 , H 2 O; C, 43.77%; H, 3.48%; N, 8.06%; Found: C, 43.92%; H, 3.44%; N, 7.97%.
Example 52
5-(R),7-(R)-Bis-benzyloxmethyl-2-(oxalin-amino)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
Benzyloxyacetaldehyde (0.90 9; 6.0 mmol) and dimethyl (2-oxomethyl)-phosphonate (1.0 g; 6.0 mmol) were dissolved in a mixture of tetrahydrofuran (25 ml) and water (20 ml). 1N Aqueous potassium hydroxide (6 ml) was added and the mixture was stirred for 30 min. Di-chloromethane (50 ml) was added and the organic phase was separated, dried (MgSO 4 ) and evaporated in vacuo leaving 5-benzyloxypent-3-en-2-one.
1 H-NMR: (CDCl 3 ): δ2.25 (s, 3H); 4.19 (dd, 2H); 4.55 (s, 2H); 6.34 (dt; 1H); 6.70 (dt, 1H); 7.26 (m, 5H).
5-benzyloxypent-3-en-2-one was dissolved in methanol (5 ml) and ammonium acetate (13 mmol, 1.03 g) was mixted together with benzyloxyacetaldehyde (1.8 g; 12 mmol) and acetic acid (0.69 ml) and the mixture was stirred for 2 days. The solvent was removed in vacuo and the residue was chromatographed on silica using gradient elution from 100% di-chloromethane to 100% ethyl acetate. A fraction (411 mg) contained (according to LC-MS; m/z 340.4) 2,5-di(benzyloxymethyl)-4-piperidone in an impure state was isolated. The crude mixture was dissolved in ethanol (3 ml) and tert-butylcyanoacetate (400 mg), sulfur (100 mg) and triethylamine was added and the mixture was stirred at room temperature overnight. The mixture was filtered and the solvent removed in vacuo. The residue was chromatographed on silica in a mixture of dichloromethane/(7% of 25% aqueous ammonia in ethanol) (40:1), which afforded 0.14 g of 2-amino-5-(R),7-(R)-bis-benzyloxymethyl4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
LC-MS: R t : 6.03 min; m/z: 495.2 [M+H] +
2-Amino-5-(R),7-(R)-Bis-benzyloxymethyl -4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (0.14 9; 0.28 mmol) was dissolved in dichloromethane (5 ml) and treated with imidazol-1-yl-oxo-acetic acid tert-butyl ester (0.1 g; 0.5 mmol) and triethylamine (70 μl; 0.5 mmol), and stirred overnight, washed with water, dried (MgSO 4 ) and the solvent removed in vacuo. The residue was chromatographed on silica using ethyl acetate/dichloromethane (1:3) as eluent. The residue was treated with trifluoroacetic acid (0.5 ml) in dichloromethane (0.5 ml) and stirred for 4 hours. Evaporation of the solvent in vacuo afforded 37 mg of the title compound.
LC-MS: R t : 4.74 min; m/z: 511.4 [M+H] + .
Example 53
6-Benzyl-2-(oxalyl-amino)-5-(1,1,3-trioxo-1,3-dihydro-1,6-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid
1-Benzyl4-oxo-piperidine-2-carboxylic acid ethyl ester (2.9 g; 11.1 mmol) (prepared in a similar way as described in “GENERAL CHIRAL SYNTHESIS” for 4-oxo-1-((S)-1-phenyl-ethyl)-piperidine-(R)-2-carboxylic acid ethyl ester using benzylamine instead of 1-(S)-phenethylamine) was dissolved in abs. ethanol (50 ml) and sulfur (0.35 g, 11.1 mmol), triethylamine (1.6 ml, 11.1 mmol), and tert-butylcyanoacetate (1.7 g, 11.1 mmol) were added and the mixture was stirred 2 days at room temperature. The solvent was removed in vacuo and the residue was chromatographed on silica using a mixture of ethyl actetate/heptane (1:4) as eleuent leaving a mixture (700 mg; 1:1 based on NMR) of 2-amino-6-benzyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,7-dicarboxylic acid 3-tert-butyl ester-7-ethyl ester and 2-amino-6-benzyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3,7-dicarboxylic acid 3-tert-butyl ester 5-ethyl ester which was used in the next step without separation. To this mixture was added tetrahydrofuran (5 ml) and lithium borohydride (1.1 ml of a 2M solution in tetrahydrofuran) and the mixture was stirred 18 hours. More lithium borohydride (5.0 ml of a 2M solution in tetrahydrofuran) was added and the mixture stirred for an additiona 4 days. Ethyl acetate (10 ml) was added dropwise and after 1 hour the mixture was poured onto water (100 ml) and extracted with dichloromethane (2×100 ml) and chromatographed on silica (using ethylacetate/heptane 1:1 as eluent), which afforded a mixture of 2-amino-6-benzyl-7-hydroxymethyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester and 2-amino-6-benzyl-5-hydroxymethyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (in total 187 mg). To this mixture was added dry tetrahydrofuran (10 ml), 2,3-dihydro-1,2-benzisothiazol-3-one-1,1-dioxide (100 mg; 0.55 mmol), triphenylphosphine (144 mg 0.55 mmol) and the mixture was cooled with ice. Diethyl azodicarboxylate (86 μl) was added and the mixture was stirred overnight at room temperature. The solvent was evaporated in vacuo and the residue was chromatographed on silica using a mixture of ethyl acetate/heptane (1:1) as eluent leaving 94 mg of 2-amino-6-benzyl-5-(1,1,3-trioxo-1,3-dihydro-1,6-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester.
1 H-NMR: (CDCl 3 ): δ1.52 (s, 9H); 2.75 (dd, 1H); 2.90 (dd, 1H); 3.55 (d, 1H); 3.72 (m, 4H); 3.94 (d, 1H); 4.12 (d, 1H); 5.97 (s, 2H); 7.14-7.37 (m, 5H); 7.80-8.0 (m, 4H).
LC-MS: R t 5.47 min, m/z: 540.4 [M+H] +
2-Amino-6-benzyl-5-(1,1,3-trioxo-1,3-dihydro-1,6-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (94 mg; 0.17 mmol) was dissolved in dichloromethane (5 ml) and treated with imidazol-1-yl-oxo-acetic acid tert-butyl ester (0.07 g; 0.3 mmol) and triethylamine (49 μl; 0.3 mmol), and stirred overnight, washed with water, 1N aqueous citric acid, dried (MgSO 4 ) and the solvent removed in vacuo leaving 104 mg of 2-(tert-butoxyoxalyl-amino)-6-benzyl-5-(1,1,3-trioxo-1,3-dihydro-1,6-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester as an oil.
LC-MS: R t : 5.50 min, m/z: 668.6 [M+H] +
2-(tert-Butoxyoxalyl-amino)-6-benzyl-5-(1,1,3-trioxo-1,3-dihydro-1,6-benzo[d]isothiazol-2-ylmethyl)-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine-3-carboxylic acid tert-butyl ester (100 mg; 0.15 mmol) was treated with trifluoroacetic acid (1 m) in dichloro-methane (4 ml) and stirred for 2 days. Evaporation of the solvent in vacuo afforded 90 mg of the title compound as a solid trifluoroacetate.
Calc. for C 25 H 21 N 3 O 8 S 2 , 1.5×C 2 HF 3 O 2 , 0.5×H 2 O C, 45.72%; H, 3.22%; N, 5.71%. Found: C, 45.48%; H, 3.46%; N, 5.72%
LC-MS: R t : 4.16 min; m/z: 556.2 [M+H] +
|
Disclosed are novel compounds, novel compositions, methods of their use, and methods of their manufacture, where such compounds of Formula 1 are pharmacologically useful inhibitors of Protein Tyrosine Phosphatases (PTPase's) including PTP1B, T cell PTP,
wherein n, m, X, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , and R 7 are defined more fully in the description. The compounds are useful in the treatment of type I diabetes, type II diabetes, impaired glucose tolerance, insulin resistance, obesity, and other diseases.
| 0
|
Subsets and Splits
No community queries yet
The top public SQL queries from the community will appear here once available.