description stringlengths 2.98k 3.35M | abstract stringlengths 94 10.6k | cpc int64 0 8 |
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FIELD AND BACKGROUND OF THE INVENTION
The present invention relates in general to the field of coal gasification and, in particular, an apparatus for use with certain pressure vessels such as radiant syngas coolers (RSCs) to provide sealing between the hot syngas and the pressure vessel and to provide for instantaneous pressure relief against high differential pressures during transients.
A radiant syngas cooler (RSC) is a component of an integrated gasification combined cycle (IGCC) power plant. A stream of hot syngas and molten ash from the gasification process enters the top of the RSC, a vertical vessel. The RSC recovers heat from the syngas to generate steam, and removes most of the entrained solids. During normal operation, a seal must be maintained to prevent or minimize hot syngas from contacting certain parts of the vessel. During certain conditions, transient operating pressure excursions can occur which must be accommodated or relieved in order to protect conduit members which convey the synthesis gas within the vessel from being destroyed.
Various sealing devices with pressure release mechanisms have been developed. See, for example, U.S. Patent Application Publication No. US 2007/0119577, the text of which is hereby incorporated by reference as though fully set forth herein. None, however, disclose a sealing apparatus of a segmented ring construction positioned around an outer wall section of a conduit member with resiliently biased pressure device(s) or, pressure relief apparatus with resilient biased pressure for protection of the conduit member from high differential pressures.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a sealing apparatus for use in a pressure vessel for protection of the vessel shell and the back or outside of a conduit member from exposure to high syngas temperature and corrosive gases. The invention accommodates thermal and pressure differentials during operation. Another object of the present invention is to provide a pressure relief means for reducing pressure differential between opposite sides of a conduit member contained within the pressure vessel.
An exemplary sealing apparatus of the present invention comprises a flange member, ring segment retaining rods, ring segments, fastening members, and resilient members.
The flange member is preferably located concentric with and around the outer surface portion of the conduit member. The upper end of the flange member contains a slot for enclosing the segmented seal ring. The lower end is attached to the seal plate. Each seal ring segment is movably pressure loaded by at least one ring retaining rod. The plate segments are joined to each other preferably in a fluid tight manner, and are arranged around and overlap at least part of the conduit member along an axial direction as an elongated body or structure.
The retaining rods for the seal ring segments are held in position by fastening members that are attached in a fluid tight manner to the flange member. The resilient members are disposed between each fastening member and the respective ring segment to resiliently pressure or load the plate segments into a fluid tight relationship with the outer surface of the conduit member.
The pressure relief opening and a corresponding resiliently biased door are preferably provided on the flange member. The resiliently biased door is preferably located over and adapted to cover the pressure relief opening.
The other end of the plate segments is preferably attached in a fluid tight manner to a seal plate spaced at a distance from the conduit member.
The fluid tight connections formed between the various components of the sealing apparatus of the present invention and the pressure vessel provide a fluid tight seal between the opposite sides of the conduit member.
It is another object of the present invention to provide a pressure relieving apparatus with the resiliently biased door mounted on the flange member via at least one pair of spaced apart mounting assemblies. Each pair of door assemblies has one door each mounted on opposite sides of the flange member. The resilient members are arranged such that one door would open outwards and the opposite door would open inwards for opposite high differential pressure. Each mounting assembly preferably includes a rod member, a resilient member and a fastening member. One end of the rod member is attached to and extends outwardly from the surface of the plate segment. The resiliently biased door is movably mounted on each rod member, and the fastening member is mounted on the free end of the rod member to retain the resiliently biased door and the resilient member on the rod member. The mounting assemblies of each respective pair are preferably positioned opposite each other on opposite sides of the pressure relief opening.
The resiliently biased door is preferably adapted to close the pressure relief opening when the pressure differential is below a predetermined threshold value and to open and reduce the pressure differential when the pressure differential is equal to or exceeds the predetermined threshold value.
One problem solved by the present invention is the protection of the pressure vessel from the hot gas that contains corrosive compounds and protection of the heat absorbing pressure part cage (or conduit) from high differential pressures across the cage or between the hot gas volume and the annulus (or cavity) between the cage and the pressure vessel. The combination of the segmented seal ring with resiliently biased pressure and pressure relief doors with resiliently biased pressure responsive relief means is the complete assembly concept that prevents contact of the effluent gas with the inside wall of the pressure vessel, and allows for instantaneous pressure balance between the hot gas volume and the annulus.
In addition, the annulus is continuously purged with an inert gas to positively remove harmful gases from contacting the pressure vessel and to prevent the gases from entering the annulus volume. Too much purge flow is not desirable. The positive seal provided by the sealing apparatus of the present invention allows for placement of purge flow orifices to control the amount of inert purge gas.
The advantages offered by the segmented ring sealing apparatus with spring plate pressure relief of the present invention include but are not limited to:
There is a positive seal between the hot gas volume and the annulus between the cage and the pressure vessel, which keeps harmful gasification products away from the pressure vessel for corrosion protection and reduced exposure of high temperature gases on the pressure vessel;
The seal is maintained continuously through the differential growth movement between the cage and the pressure vessel during heat up and cool down cycles of the cooler; in addition, the seal is maintained for any lateral movement of the cage assembly that can be caused by ambient wind pressure loading on the outside of the pressure vessel;
The pressure differential between the hot gas volume and the annulus is minimized by the instantaneous pressure relief devices, which maintains the structural integrity of the cage; and
The amount of annulus purge flow is controlled and access is provided for inspection and replacement of the devices.
The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and specific objects attained by its uses, reference is made to the accompanying drawings and descriptive matter in which preferred embodiments of the invention are illustrated.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a sectional view of a sealing apparatus of the present invention installed inside a synthesis gas cooler;
FIG. 2 is a sectional side view of a sealing apparatus of the present invention;
FIG. 3 is a top plan view of a sealing apparatus of the present invention;
FIGS. 4A , 4 B and 4 C are a sectional views of FIG. 3 viewed in the direction of arrows 4 - 4 of FIG. 3 , and illustrate various spring configurations;
and
FIG. 5 is a partial sectional side view of a plate segment of the present invention with a pressure release assembly.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, in which like reference numerals are used to refer to the same or similar elements, FIG. 1 shows a sealing apparatus 9 and pressure relief apparatus 8 of the present invention operatively installed in a pressure vessel 10 such as a synthesis gas cooler (SGC) 10 . The pressure relief apparatus 8 is adapted to reduce the pressure difference between opposite sides of a conduit member or cage 28 when a predetermined pressure differential is reached, and the sealing apparatus 9 is adapted to provide a fluid tight seal between a flue 11 defined by the conduit member 28 and an inner cavity 42 located between the conduit member 28 and an outer shell 30 of the SGC. The flue 11 , as is shown in FIG. 1 , is defined by the conduit member or cage 28 , and typically comprises heat exchange elements such as fluid cooled tubes and/or radiant heat transfer surfaces. Synthesis gas or effluent 12 such as that produced by a gasification process is introduced into the flue 11 provided within the synthesis gas cooler 10 . A purge gas may be selectively introduced into the cavity 42 defined by the conduit member 28 and the outer shell 30 to remove any effluent 12 that might enter the cavity 42 to prevent or reduce corrosion and exposure to high gas temperatures of the wall of the outer shell 30 or the surfaces disposed within the cavity 42 .
As shown in FIG. 1 , although other arrangements are possible, the sealing apparatus 9 contacts on one end to a lower outer surface portion of the conduit member 28 and is mounted to a seal plate 13 on the other end. FIGS. 4A , 4 B and 4 C show by way of non-limiting example a conduit member 28 with a lower header 32 attached to its inner surface and the sealing apparatus 9 attached its outer surface. Other possible arrangements for the sealing apparatus 9 are shown in FIGS. 2 and 4A , 4 B and 4 C.
Referring to FIG. 1 , while other arrangements are possible, the pressure relief apparatus 8 is mounted on a flange member 15 of the sealing apparatus 9 .
The predetermined threshold pressure value at which the pressure relief apparatus 8 activates is preferably selected such that the pressure differential across the sealing apparatus 9 does not impair or compromise the structural integrity of the conduit member or cage 28 and/or the seal plate 13 . Alternatively, the predetermined threshold pressure value may be selected such that the pressure differential does not cause the walls of the conduit member or cage 28 and/or the seal plate 13 to fail and release the effluent 12 into the cavity 42 .
The conduit member 28 preferably has a cross sectional shape corresponding to that of the outer shell 30 . However, the conduit member 28 may have any suitable shape or configuration, and any suitable dimension for its intended application.
Referring now to FIGS. 2 and 4A , 4 B and 4 C, there are shown sectional side views of the sealing apparatus 9 of the present invention which comprises a flange member 15 , spaced apart plate retaining rods 17 , seal ring segments 18 , fastening members 16 , resilient members 14 , one or more pressure relief openings 21 , and door plate assemblies with resiliently biased doors 19 .
The seal ring segments 18 are preferably located on and extend around a lower outer surface portion of the conduit member 28 in a plane perpendicular to the central conduit axis 22 (see FIG. 1 ). The ring retaining rods 17 are preferably attached to and extend outwardly from the peripheral surface 38 of the seal ring segments 18 . The flange member 15 preferably has a slot 23 formed on one end thereof for receiving the seal ring segments 18 and at least one fastening bore 25 opening into the groove 23 for receiving one of the retaining rods 17 . Each seal ring segment 18 is movably mounted on at least one plate retaining rod 17 .
The seal ring segments 18 are preferably joined to each other in a fluid tight manner, and are arranged around and overlap at least part of the conduit member 28 along a lengthwise direction as an elongated body or structure. The flange member 15 may be provided with one or more port holes 26 to provide a flow path for the purge gas. Pressure applied to seal ring segments 18 may be applied by either compressing or extending the resilient member 14 from its neutral position when the pressure differential is lower than the predetermined threshold value. The neighboring seal ring segments 18 are preferably joined to each other via a tongue and groove interlocking structure, as illustrated in FIG. 3 .
The fastening members 16 are mounted on the flange member 15 and are adapted to retain the seal ring plate segment 18 with the slot 23 on the retaining rod 17 . Preferably, the fastening member 16 is threadably mounted on the retaining rod 17 and is axially displaceable along the retaining rod 17 for adjusting biasing force exerted by the resilient member 14 against the seal ring segments 18 . It will be appreciated that instead of using the fastening member 16 to adjust the tension or force of the resilient member 14 , a tension adjusting member 24 , disposed between the fastening member 16 and the flange member 15 may be used.
The resilient members 14 are disposed between each fastening member 16 and the respective seal ring segment 18 to resiliently pressure or load the seal ring segments 18 into a fluid tight relationship with the outer surface of the conduit member 28 . Examples of resilient members include coil springs made of metal, plastic or other suitable material for the pressure and temperature conditions expected.
Referring to FIG. 5 , the pressure relief opening 21 and the corresponding resiliently biased door 19 are preferably provided on the flange member 15 . The resiliently biased door 19 is preferably located over and adapted to cover the pressure relief opening 21 .
The other end of the flange member 15 is preferably attached in a fluid tight manner to a seal plate 13 spaced at a distance from the conduit member 28 . Preferably, the seal plate 13 is arranged perpendicular to the central conduit axis 22 .
The fluid tight connections formed between the various components of the sealing apparatus 9 of the present invention and conduit 28 10 provide a fluid tight seal between the opposite sides of the conduit member 28 , at least when the pressure difference across the conduit member 28 is within or below a predetermined threshold value(s).
The resiliently biased door plate assembly allows immediate pressure release during pressure excursions by means of the spring assemblies allowing the door 19 to open as required. Labyrinth seals may be employed to create additional sealing capabilities when the door 19 is in the closed position. Additional plate sleeves or stud sleeves may be used to act as a load leveling device in the event a twist in the door action becomes an issue (see FIG. 5 ). The resiliently biased door 19 of the door plate assembly is preferably adapted to close the pressure relief opening 21 when the pressure differential is below a predetermined threshold value and to open and reduce the pressure differential when the pressure differential is equal to or exceeds the predetermined threshold value.
In an embodiment, the conduit member 28 has a substantially circular cross section and the seal ring segments 18 are provided with an arcuate configuration with a rectangular configuration in cross-section to conform to the outer surface of the conduit member 28 . Although the number of seal ring segments 18 can vary, depending on, for example, the cross sectional size of the conduit member 28 or the operating parameters of the sealing apparatus 9 , the preferred number of seal ring segments 18 ranges from 2 to 10. It will be appreciated that more or fewer seal ring segments 18 can also be used. The seal ring segments 18 may all be substantially the same width or may comprise a variety of different widths. A sealing apparatus 9 of the present invention with 8 such seal ring segments 18 is shown in FIG. 3 .
Referring now to FIG. 5 , the resiliently biased doors 19 are preferably mounted on the flange member 15 via at least one pair of spaced apart mounting assemblies 27 . Each mounting assembly 27 preferably includes a rod member 29 , a resilient member 31 (e.g., a coil spring) and a fastening member 33 . One end of the rod member 29 is attached to and extends outwardly from the surface of the flange member 15 . The resiliently biased door 19 is movably mounted on the rod member 29 via opening 35 , and the fastening member 33 is mounted on the free end of the rod member 29 to retain the resiliently biased door 19 and the resilient member 31 on the rod member 29 . The mounting assemblies 27 of each respective pair are preferably positioned opposite each other on opposite sides of the pressure relief opening 21 . The resiliently biased door 19 preferably overlaps the edge extending around the pressure relief opening 21 and/or is in intimate surface contact with the outer surface of the flange member 15 .
As shown in FIG. 5 , a stud/guide sleeve 34 may be inserted between the resilient member 31 and the rod member 29 to permit even movement of the resiliently biased door 19 . A sleeve member 36 may also be provided on the side/surface of the door 19 facing the flange member 15 . The sleeve member 36 preferably abuts against a portion 39 of the pressure relief opening 21 to allow even movement of the resiliently biased door 19 . The stud/guide sleeve 34 or the sleeve member 36 may be used alone or together, as required.
While specific embodiments of the invention have been shown and described in detail to illustrate the application of the principles of the invention, it will be understood that the invention may be embodied otherwise without departing from such principles. | A sealing apparatus adapted for use in a pressure vessel such as a synthesis gas cooler. The sealing apparatus is of a segmented plate construction formed around an outer wall section of a conduit means of the pressure vessel that defines at least part of a passage for receiving effluent from a gasification process. Pressure responsive mechanisms are provided on the plate segments to maintain the pressure difference across the sealing apparatus within the acceptable operating limits as well as to permit instantaneous pressure release to prevent damage to the pressure part assembly or cage. The seal is also maintained continuously through the differential growth movement between the conduit means and the pressure vessel during heat up and cool down cycles. | 8 |
BACKGROUND OF THE INVENTION
The invention relates to portable computer systems, and particularly to a docking station for use with a notepad computer that provides ease of connection and pivotable positioning for viewing the display of the notepad computer.
DESCRIPTION OF THE RELATED ART
Portable computer systems are becoming more powerful, smaller and lighter with each few months.
Notebook computers have been available for some time. They are generally approximately 81/2"×11" in width and length and 11/2"-2" thick. An example of a conventional notebook computer is disclosed in U.S. Pat. No. 4,903,222.
A more recent arrival in the class of portable computers is the slate or notepad computer. In this type of computer, a stylus may be used to write directly on the LCD screen used in the unit. An underlay captures the movement of the stylus and software in the computer converts the movement to commands, either by monitoring location when the computer is being used in a touch screen-like mode, or by converting the movements into specific characters, which then forms the command or data.
The notepad computer generally includes a printed circuit board (PCB), hard drive, battery, power supply (DC to DC), memory, modem/DAA and an optional floppy drive that can be used with PCMCIA slots in the notepad computer. The notepad computer could also include an optional keyboard.
One device which has been present for sometime for use with laptop and notebook computers is a docking station to provide expansion capabilities and easier connection/disconnection of external devices such as CRTs and larger external keyboards. Examples of docking stations or expansion bases are disclosed in U.S. Pat. Nos. 4,903,222 and 5,199,888 that are assigned to the same assignee of the present invention and are incorporated herein by reference for all purposes. The docking station or expansion base includes connectors for receiving a CRT cable, a parallel printer cable, a keyboard cable, a serial port cable and certain expansion capabilities. The laptop or notebook computer includes a single expansion base connector to mate with a connector in the docking station to directly connect the notebook computer to the docking station. This is more convenient than requiring the user to remove and install a plurality of cables each time the computer is removed and returned. However, the conventional docking stations have been fixed items, receiving the laptop or notebook computer in a sliding horizontal fashion.
In notebook computers, such as disclosed in U.S. Pat. No. 4,903,222, the keyboard connected with the notebook computer is the data entry device and the desired typing position is approximately horizontal. Further, the display internal with the notebook computer is hinged from the notebook computer, so the internal display can be readily used, if desired, with the notebook computer in the horizontal position in the docking station.
However, this conventional docking station arrangement for the notebook computer is unacceptable for use with notepad computers. Since, the display of the notepad computer is not separately hinged, horizontal positioning of the notepad computer creates problems because the display can only be viewed from above and not at an angle. Thus a conventional notebook docking station configuration is not acceptable for use with a notepad computer. Yet the desire for easy connection with external devices and resulting peripheral ports remains, so a configuration which allows the easy connection and disconnection and yet allows for positioning of the notepad display at an angle for visibility while seated is needed. It is further desirable that the docking station allow the notepad computer to pivot to a more convenient writing position if an external monitor is used.
SUMMARY OF THE INVENTION
A docking station for use with a notepad computer includes a main electronic housing having a front pivot portion and a rear portion. A receiving tray is pivotably connected to the front pivot portion for receiving the notepad computer. A circuit board located in the main housing includes a plurality of connectors for receiving power cables and cables from various peripheral devices, with the connectors accessible from the rear and side portion of the main housing. A cable extends from the main housing to a connector in the receiving tray. The connector mates with an expansion connector in the notepad computer.
The main housing is pivotably mounted with the receiving tray to receive the notepad computer to provide a number of positions for the notepad computer between an upright position and a low angle position. The upright positions are useful when using the internal display of the notepad computer, particularly if an external keyboard or pointing device are used. The low angle position is useful when an external monitor is used and the overlay of the notepad computer is used for input.
BRIEF DESCRIPTION OF THE DRAWINGS
The objects, advantages and features of the invention will become more apparent by reference to the drawings which are appended hereto wherein like numerals indicate like parts and wherein an illustrated embodiment of the invention is shown of which:
FIG. 1 is a perspective view of the preferred embodiment of the docking station showing the notepad computer having a PCMCIA slot and PCMCIA card in phantom view;
FIG. 2 is an enlarged section view of the ejection lever and cam of the receiving tray as shown in FIG. 1;
FIG. 3 is a section view taken along lines 3--3 of FIG. 2 with the cam shown in the retracted position;
FIG. 4 is a view similar to FIG. 3 with the cam shown in the extended ejection position;
FIG. 5 is a side view of the preferred embodiment of the docking station showing the front pivot portion of the main housing spaced apart from the supporting surface and the rear portion engaging the supporting surface;
FIG. 6 is a view similar to FIG. 5 with the receiving tray and main housing pivoted towards the collapsed position;
FIG. 7 is a view similar to FIG. 5 but with the receiving tray pivoted at a lower angle relative to the supporting surface;
FIG. 8 is an enlarged section view of the preferred control means on the left side of the docking station taken along lines 8--8 of FIG. 5;
FIG. 9 a perspective exploded view of an alternative embodiment of the docking station with a notepad computer shown removed from its receiving tray;
FIG. 10 is a side view of the notepad computer received in the docking station of FIG. 9 showing the front pivot portion of the main housing spaced apart from the supporting surface and the rear portion engaging the supporting surface;
FIG. 11 is a view similar to FIG. 10 with the same base member and main housing but with a keyboard, a larger receiving tray and notepad computer;
FIG. 12 is a side view of the notepad computer and the docking station with the front pivot portion and the rear portion of the main housing engaging the supporting surface along with an external monitor;
FIG. 13 is an exploded enlarged perspective view of the main housing and the base member of the docking station of FIG. 9;
FIG. 14 is an enlarged exploded view of the main housing of FIG. 9;
FIG. 15 is a plan view of an alternative embodiment of the control means in the engaged position; and
FIG. 16 is a view similar to FIG. 15 with the control means in the disengaged position.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIGS. 1-16, a docking station, generally indicated at D for the preferred embodiment or D' for the alternative embodiment, for use with a notepad computer 18 is provided. The main electronic housing 10 and base member 12 of the docking station D can be used with different size receiving trays to receive corresponding sizes of notepad computers, as will be discussed in detail below.
Turning now to FIGS. 1 and 5-7, a notepad computer 18 is received for use with the docking station D. The main electronic housing 10 has a rear portion 10A and a front pivot portion 10B. A number of cables 14 extend from the rear portion 10A of the main housing 10. For example, these cables include a power cable 14A, and can include other cables used with the system depending on selected options, such as a keyboard cable 14B, a mouse cable, a printer cable, a network cable and a video monitor cable 14C. The main housing 10 is pivotably connected to the base member 12, as will be described below in detail. A tray 16 of the docking station D is releasably connected to the base member 12. The tray 16 has three resilient wrap around corner holding members 16A, 16B and 16C to provide interference with the notepad computer 18. The upper left side of the tray 16 includes a resilient holding member 16D that allows a PCMCIA card C access to a PCMCIA slot 18A in the notepad computer 18 though prevents side movement of the notepad computer. The notepad computer 18 includes an expansion base connector (not shown) that is releasably electrically coupled and aligned with the expansion base or docking station connector 20 of the docking system when the notepad computer is received in the tray. The connector 20 is electrically coupled to the electronics E in the main housing, as is shown in FIG. 14.
As best shown in FIG. 1, the receiving tray 16 includes ejection levers 20A, 20B on both sides. The levers 20A and 20B are fixedly connected to cams 22A and 22B by a shaft 24A (shaft 24B not shown). Preferably, the lever, shaft and cam are fabricated as a monolithic unit.
As best shown in FIGS. 3 and 4, when lever 20A is rotated back, as shown by the arrow in FIG. 1, the cam 22A is rotated from the retracted position (FIG. 3) to the extended position (FIG. 4) to eject the notepad computer 18 away from the base member 16.
As shown in FIG. 5, the docking station D positions the tray 16 to receive the notepad computer 18 in an upright position with the rear portion 10A of the docking station in engagement with the supporting surface S. In the upright position, the front pivot portion 10B is spaced apart from the supporting surface S. The surface S can be any surface such as a table, desk, user's lap or any similar supporting surface.
A preferred embodiment of the control means is one way clutch mechanisms 26A, 26B, as best shown in FIGS. 1 and 8, that are provided on each side of the docking station D. As best shown in the bottom view of FIG. 8, the one way clutch mechanism 26B on the left side of the tray 16 includes a bracket 28 that attaches the clutch mechanism 26B to the base member 12. Bracket 30 attaches the clutch mechanism 26B to the pivot portion 10B of the main housing 10. Any known fasteners, such as screws or rivets or similar fastening devices, can be used for attachment. The bracket 28 is fixed relative to shaft 32 and the bracket 30 is rotatably mounted about shaft 32 with bracket 30 preferably positioned between positioning rings 34 and 36. A coiled torque member 38 is received about the shaft 32 with one end 38A received in an opening in the bracket 30. The other end 38B of the coiled torque member 38 is positioned adjacent a release ring 40 that is positioned about the shaft 32. A release lever 42 having a pin 42A on one end and a slotted member 42B on the other end to engage and trap the release ring 40. Preferably, the lever 42 is removably positioned about one end of the shaft 32. Though the lever 42 is shown positioned on the shaft 32, since the lever is removable, it is not necessary that the lever be positioned on the shaft at all times. Two levers would be needed to simultaneously release both control means 26A, 26B.
The user of the docking station D can collapse or fold the main housing 10 with the base member 12 of the docking system from an upright to a collapsed position, as shown by the arrow in FIG. 6, or from a low angle position as shown in FIG. 12 to the upright position of FIG. 5 without using the release lever 42. However, to pivot the docking station the other direction (counter clockwise) so that the main housing is separated from the base member 12, the release lever 42 is positioned so that the key slot 42B is positioned about the radial projection 40A of the moving member 40 and the lever 26A is rotated as shown by the arrow in FIG. 7 to move the main housing 10 as shown by the arrow in FIG. 7. Moving of the lever 42 as shown in FIG. 7 forces the axial projection 40B of ring 40 to engage the end 38B of the coiled torque member 38 to allow free movement of the torque member 38 about the clutch shaft 32. Movement in the direction as shown in FIG. 7 without the lever 42 is prevented as the coiled torque member 38 wraps tighter about the shaft 32 to restrain pivoting. Therefore, this clutch mechanism prevents the docking station from inadvertently collapsing when in the upright position, such as due to forces imparted if the stylus 44 is used in this position, while allowing the docking station to be folded for storage or to the upright display position without the use of levers 42.
As shown in FIGS. 9-16, an alternative embodiment of the control means includes an actuator button 112, as will be discussed below, is provided to allow the base member 12' to pivot relative to the main housing 10'. As shown in FIGS. 9, 10 and 12, the notepad computer 18' with display L includes a stylus 44 used with the notepad computer 18'. As is known, the stylus 44 is used to write directly on the LCD display. An underlay captures the movement of the stylus and software of the computer converts the movement to commands, either by monitoring location when the computer is being used in a touch screen-like mode or by converting the movements into specific characters, which then form the command or data. Thus, there is no need for a keyboard with the notepad computer of FIGS. 1 and 9 since no information is typed into the notepad computer.
As can be seen in FIG. 12, the main housing 10' has both its rear portion 10A' and its front pivot portion 10B' in engagement with the surface S. In this low angle position, the notepad computer 18' and its LCD screen L are preferably 10° from the surface S. This low angle writing position of FIG. 12 provides a similar writing surface to that used with a conventional pen. In this low angle position, the docking station D' is generally used with an external monitor M connected by cable 14C to a video monitor connector to connector 70, as best shown in FIG. 13, in the rear of the main housing 10'.
Turning now to FIG. 11, a larger receiving tray 46 is releasably attached to the base 12' of the docking station D'. The tray 46 has a larger area than tray 16' but includes similar resilient holding members, as shown in FIGS. 1 and 9, to provide interference with the notepad computer 48. The expansion base connector 20' is removably positioned in the tray 46 to electrically couple the notepad computer 48 with the electronics E in the main housing 10'. While the notepad computer 48 includes an LCD screen, an optional conventional keyboard 50 supported by legs 52 (only one leg shown) provides input into the notepad computer 48. A cord 54 received in a connector in the front of the notepad computer 48 electrically couples the keyboard 50 to the notepad computer 48. The notepad computer 48 is in turn connected via the expansion base connector 20' to the electronics E in the main housing 10'. Though the notepad computer 48 is normally positioned as shown in FIG. 11 when used with a keyboard 50, the docking station could be positioned as shown in FIG. 12 for convenient pen input, storage, transportation or other purposes as previously discussed.
Turning to FIG. 13, the rear portion 10A' of the main housing 10' of the docking station D' is better disclosed. The rear portion 10A' includes a number of connectors 58, 60, 62, 64, 66, 68 and 70 to receive mating connectors from peripheral devices. Examples of conventional connectors in a portable computer are disclosed in U.S. Pat. No. 5,199,888 that is assigned to the same assignee of the present invention and is incorporated herein by reference for all purposes. Preferably, the docking station D or D' would include seven connectors to receive mating connectors including, arranged from left to right, SCSI II connection for attachment of various peripherals, keyboard connector, mouse connector, parallel port connector, serial port connector, tape/floppy interface connector, and a VGA video connector, respectively connectors 58, 60, 62, 64, 66, 68 and 70.
At the front pivot end 10B' of the main housing 10', opposing cylindrical pivot members 72 and 74 are shown preferably integral with the main housing 10'. Extending from one side of the main housing 10' is pin means or pin 76 having a slot 78. A bracket 80 having a fixed dowel 82 is provided so that the dowel 82 is received in the slot 78 of pin 76. The bracket 80 is received about cylindrical pivot member 72, as best shown in FIGS. 13, 14 and 15, to facilitate pivoting of the main housing 10' relative to the base member 12'. After the dowel 82 is received in the slot 78, the bracket 80 is connected to the base member 12'. Fasteners are received through the holes in the bracket 80 and into holes 84A and 84B of the base member 12'. Similar to bracket 80 but without dowel 82, the bracket 86 is received about cylindrical pivot member 74 and uses fasteners received into the holes for attachment to the base member 12'. The cylindrical member 72 rides on surfaces 88A, 88B and cylindrical member 74 rides on surfaces 90A and 90B. Shoulders 92A and 92B on the base member 12' and brackets retain the main housing 10'.
An opening 94, as best shown in FIG. 14, allows a ribbon cable (not shown), connected to a header 96 connected to electronics E, to extend from the main housing 10' through the slot 98 in the base member 12', as best shown in FIG. 13. The end of the ribbon cable includes the expansion base connector 20 or 20' that is removably positioned in the trays. As can be seen in FIG. 13, holes are provided in the top end of the base member 12' and holes are provided in the bottom of the base member 12' to receive screws or conventional quick connect fasteners to releasably attach the receiving trays to the base member 12'.
Turning to FIG. 14, the main housing 10' is shown exploded into its lower section and upper section. The lower section spans the full length of the main housing 10'. Preferably, the rear portion of the lower section includes feet 100, as best shown in FIGS. 5 and 6, fabricated from a non-slip material such as SANTOPRENE rubber. As can be best seen in FIGS. 15 and 16, the lower section of the main housing 10' includes a toothed frusto-conical counterbore or blocking member 102 therein and a thrust plate 104. Preferably, the upper section of the main housing includes a corresponding toothed frusto-conical counterbore and thrust plate to counterbore 102 and thrust plate 104. Movable pin 106 includes a frusto-conical groove member 108 having a plurality of teeth positioned thereon. The grooved member 108 could be fabricated integral with the pin 106 but is preferably separate from but fixed relative to the pin 106. Urging means such as spring 110 is provided between the grooved member 108 and thrust plate 104 for urging the grooved member into blocking engagement with the main housing 10'. Actuator button 112 is received onto the axial movable pin 106 to disengage the grooved member 108 from the counterbore 102 of the main housing 10'.
The main housing is connected intermediate the top end and the bottom end of the base member for relative pivotal movement of the main housing to the base member. However, the preferred control means, as shown in FIG. 8, or the control means, as shown in FIGS. 14-16, allow a plurality of positions of the main housing to the base member. However, the preferred control means allows positioning in any position while the alternative control means is limited by the engagement of the teeth on grooved member 108. When actuator button 112 is pushed in, as shown by the arrow in FIG. 16, member 108 disengages from the counterbore 102 in the main housing 10' to allow docking station to be positioned relative to the main housing. Preferably, the notepad computer in the docking station is positioned between 10° and 85° from the surface S during use as described above.
The foregoing disclosure and description of the invention are illustrative and explanatory thereof, and various changes in the size, shape and materials, as well as the details of the illustrative construction may be made without departing from the spirit of the invention. | A docking station for use with a notepad computer is disclosed. The main electronic housing of the docking station is pivotably mounted with a receiving tray to provide a number of positions for the notepad computer between an upright position and a low angle position. The more upright positions are useful when using the internal display of the notepad computer, particularly if an external keyboard and pointing device are used. The low angle position is useful when an external monitor is used and the overlay of the notepad computer is used for input. The receiving tray is removably mounted to the docking station and may be replaced with another receiving tray of a different size for use with a different notepad computer of a different size. | 8 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention generally relates to processing digitally modulated signals received in a communication system such as a WLAN (Wireless Local Area Network) system, and in particular to a receiver and an operation method that may be used for estimating the power of a received signal to compensate input power changes and to keep the receiver output constant.
[0003] 2. Description of the Related Art
[0004] A wireless local area network is a flexible data communication system implemented as an extension to, or as an alternative for, a wired LAN. Using radio frequency or infrared technology, WLAN systems transmit and receive data over the air, minimizing the need for wired connections. Thus, WLAN systems combine data connectivity with user mobility. Most WLAN systems use spread spectrum technology, a wide-band radio frequency technique developed for use in reliable and secure communication systems. The spread spectrum technology is designed to trade-off bandwidth efficiency for reliability, integrity and security. Two types of spread spectrum radio systems are frequently used: frequency hopping and direct sequence systems. The standard defining and governing wireless local area networks that operate in the 2.4 GHz spectrum, is the IEEE 802.11 standard. To allow higher data rate transmissions, the standard was extended to the 802.11b standard, that allows data rates of 5.5 and 11 Mbps in the 2.4 GHz spectrum. This extension is backwards compatible as far as it relates to the direct sequence spread spectrum technology, and both standards adopt various digital modulated techniques.
[0005] A digitally modulated signal in a wireless local area network has to be processed to compensate the influence of disturbances and to keep the output power constant. For compensating power changes in the input digitally modulated signal, usually an automatic gain control loop unit is provided in the receiver. A typical block diagram of such an automatic gain control loop unit is illustrated in FIG. 1. The unit of FIG. 1 comprises an amplifier 100 and a feedback loop having a power calculation unit 110 and a gain control unit 120 . The power calculation unit 110 calculates the current power of the output signal of said amplifier 100 , and the gain control unit 120 delivers a gain control signal to the amplifier 100 .
[0006] The amplitude or power of any digitally modulated signal may be represented by I (in-phase) and Q (quadrature-phase) values and the I and Q values can be displayed in a complex diagram. The I value represents the real part and the Q value represents the imaginary part of the signal. When the power calculation unit 110 calculates the output power it has to calculate a square root of the sum of the squared I value and the squared Q value for each received pair of I and Q values. The conventional techniques for calculating the output power comprise unnecessary and complicated calculation steps. In particular the calculation of the squared I and Q components and the calculation of the square root is disadvantageous. It has been found that circuits used for calculation of the power are needed to be of significant complexity and are therefore responsible for high development and manufacturing costs.
SUMMARY OF THE INVENTION
[0007] An improved receiver, integrated circuit chip and operation method are provided that may allow for performing a power estimation in a simple and less complex implementation. In one embodiment, there is provided a receiver for receiving a digitally modulated signal in a communication system. The receiver comprises a signal input unit adapted for determining at least one in-phase and at least one quadrature-phase value of the received signal. The receiver further comprises a signal generator connected to receive the in-phase and quadrature-phase values and to generate at least one modified in-phase value and at least one modified quadrature-phase value of a rotated phase constellation system. The receiver further comprises a signal processing unit that is adapted for processing the received signal dependent on the in-phase and quadrature-phase values and the modified in-phase and quadrature-phase values. The signal generator is a passive impedance network.
[0008] In a further embodiment, an integrated circuit chip may be provided for processing a digitally modulated signal received in a communication system. The integrated circuit chip comprises a signal input circuit that is adapted for determining at least one in-phase and at least one quadrature-phase value of a received digitally modulated signal. The integrated circuit chip further comprises a signal generator circuit adapted for generating at least one modified in-phase value and at least one modified quadrature-phase value of a rotated phase constellation system, and a signal processing circuit adapted for processing the received signal dependent on the in-phase and quadrature-phase values and the modified in-phase and quadrature-phase values. The signal generator circuit is an integrated passive impedance network.
[0009] In another embodiment, there is provided a method of operating a receiver in a communication system. The method comprises determining at least one in-phase and at least one quadrature-phase value of a received digitally modulated signal, generating at least one modified in-phase value and at least one modified quadrature-phase value of a rotated phase constellation system, and processing the received signal dependent on the in-phase and quadrature-phase values and the modified in-phase and quadrature-phase values. The generation of the modified values is performed by means of a passive impedance network.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The accompanying drawings are incorporated into and form a part of the specification for the purpose of explaining the principles of the invention. The drawings are not to be construed as limiting the invention to only the illustrated and described examples of how the invention can be made and used. Further features and advantages will become apparent from the following, and more particular description of the invention as illustrated in the accompanying drawings, wherein:
[0011] [0011]FIG. 1 is a typical block diagram of a conventional automatic gain control loop for controlling the gain of the amplifier;
[0012] [0012]FIG. 2 is a block diagram of a power estimation unit according to an embodiment and indicates the signal flow between the different units;
[0013] [0013]FIG. 3 is a flow chart illustrating the process of performing the power estimation according to an embodiment;
[0014] [0014]FIG. 4 illustrates a phase constellation system wherein the I and Q values represent a phase constellation point of the received signal, and the IX and QX values represent the phase constellation point rotated by 45°;
[0015] [0015]FIG. 5 is a block diagram of a power estimation unit according to another embodiment, implementing a resistor network;
[0016] [0016]FIG. 6 is a flow chart illustrating the process of performing the power estimation using the resistor network of FIG. 5;
[0017] [0017]FIG. 7 illustrates another phase constellation system;
[0018] [0018]FIG. 8 illustrates the realization of the power estimation unit with electronic devices in electronic circuits according to an embodiment;
[0019] [0019]FIG. 9 illustrates the resistor network of FIG. 5 with its input and output terminals;
[0020] [0020]FIG. 10 shows the constellation of the rotated phase constellation system, relating to the original phase constellation system;
[0021] [0021]FIG. 11 illustrates the function of the deviation of the maximum value from the true value depending on the signal phase angle;
[0022] [0022]FIG. 12 illustrates a BPSK modulated I signal represented in the time domain for a subset of phase shifts between 0° and 36°;
[0023] [0023]FIG. 13 illustrates a BPSK modulated Q signal represented in the time domain for a subset of phase shifts between 0° and 36°;
[0024] [0024]FIG. 14 illustrates the IX signal represented in the time domain for a subset of phase shifts between 0° and 36°;
[0025] [0025]FIG. 15 illustrates the QX signal represented in the time domain for a subset of phase shifts between 0° and 36°;
[0026] [0026]FIG. 16 illustrates an overlay of the absolute values of the Q signal, I signal, QX signal and IX signal, represented in the time domain for a subset of phase shifts between 0° and 36°;
[0027] [0027]FIG. 17 illustrates the envelope of the maximum of all absolute values of the Q signal, I signal, QX signal and IX signal represented in the phase domain;
[0028] [0028]FIG. 18 illustrates a BPSK modulated I signal represented in the time domain for phase shifts between 0° and 360°;
[0029] [0029]FIG. 19 illustrates a BPSK modulated Q signal represented in the time domain for phase shifts between 0° and 360°;
[0030] [0030]FIG. 20 illustrates the IX signal represented in the time domain for phase shifts between 0° and 360°;
[0031] [0031]FIG. 21 illustrates the QX signal represented in the time domain for phase shifts between 0° and 360°;
[0032] [0032]FIG. 22 illustrates an overlay of the absolute values of the Q signal, I signal, QX signal and IX signal, represented in the time domain for phase shifts between 0° and 360°;
[0033] [0033]FIG. 23 illustrates the envelope of the maximum of all absolute values of the Q signal, I signal, QX signal and IX signal represented in the phase domain for phase;
[0034] [0034]FIG. 24 illustrates a QPSK modulated I signal represented in the time domain for a subset of phase shifts between 0° and 36°;
[0035] [0035]FIG. 25 illustrates a QPSK modulated Q signal represented in the time domain for a subset of phase shifts between 0° and 36°;
[0036] [0036]FIG. 26 illustrates a QPSK modulated IX signal represented in the time domain for a subset of phase shifts between 0° and 36°; and
[0037] [0037]FIG. 27 illustrates a QPSK modulated QX signal represented in the time domain for a subset of phase shifts between 0° and 36°.
DETAILED DESCRIPTION OF THE INVENTION
[0038] The illustrative embodiments of the present invention will be described with reference to the figure drawings, wherein like elements and structures are indicated with like reference numbers.
[0039] Referring now to the drawings, in particular to FIG. 2, a block diagram is depicted of the power estimation unit according to an embodiment. An antenna receives a digitally modulated signal and the received signal is split into its I and Q components by an I value determination unit 200 and a Q value determination unit 210 , respectively. The I and Q values represent the real part and the imaginary part, respectively, of the power of the received digitally modulated signal.
[0040] A calculation unit 220 determines an IX value by calculating the difference of the I value and the Q value and dividing the result by a factor of two:
IX = I - Q 2
[0041] The calculation unit 220 further determines a QX value by calculating the sum of the I value and the Q value, and dividing the result by a factor of two:
QX = I + Q 2
[0042] The IX and QX values are then input to a weighting unit 230 . The weighting unit 230 multiplies the IX value and the QX value with a factor of the square root of two, i.e. {square root}{square root over (2)}. The weighted IX and QX values represent a point of a phase constellation system that is rotated by 45°.
[0043] The weighted IX and QX values and the originally received I and Q values are input to an absolute value determination unit 240 for calculating the absolute values of each of the I, Q, IX and QX values. The absolute value determination unit 240 is connected to a peak detector 250 which identifies the maximum of all absolute values that are input to the peak detector 250 . The now available peak value is input to a power calculation unit 260 for calculating a power estimate of the received signal. The power estimate may be used to control the gain of a subsequent amplifier to compensate for input power changes and to keep the output power constant.
[0044] With reference to FIG. 3, the illustrated flow chart describes a method of the power estimation according to an embodiment. In the first step 310 , I and Q values are measured simultaneously. The next step 320 comprises the calculation of the IX and QX values, i.e. the creation of a new complex signal within a 45° rotated constellation system.
[0045] The power estimation process comprises in the subsequent step the weighting 330 of the IX and QX values by multiplying the values with a factor of the square root of two ({square root}{square root over (2)}).
[0046] The I and Q values and the weighted IX and QX values are now available for being rectified in step 340 . The rectified I, Q, IX and QX values are then processed in a maximum determination step 350 to determine a maximum value of the rectified values, and provides the maximum value for the power calculation step 360 . This step 360 calculates a power estimate which may be used to control the gain of a subsequent amplifier.
[0047] At the end of the power estimation process, the entire process may step back to repeat the power estimation with new measured I and Q values.
[0048] [0048]FIG. 4 illustrates a phase constellation system wherein the I and Q values define the position of the received signal point. As apparent from FIG. 2, the weighted IX and QX values are determined by the calculation unit 220 and the weighting unit 230 . The weighted IX and QX values define the position of the received signal point, rotated by 45°.
[0049] As mentioned above, a power calculation may be performed in an automatic gain control loop. For this purpose, the receiver may use a passive impedance network.
[0050] Referring now to FIG. 5, a block diagram is depicted of the power estimation unit according to another embodiment. As above, an antenna receives a digitally modulated signal and the received signal is split in its I and Q components by an I value determination unit 200 and a Q value determination unit 210 , respectively. The I and Q values in the complex diagram will be explained in more detail later.
[0051] The I and Q values are input signals to a signal generator 500 . The signal generator 500 generates an IN and IP value, and a QN and QP value. The IN value is phase shifted by 180° relative to the phase of the IP value. The QN value is phase shifted by 180° relative to the phase of the QP value. The generated IN and IP values represent the negative or positive originally received I value and the generated QN and QP values represent the negative or positive originally received Q value, respectively. The signal generator is connected to a resistor network 510 and the generated IN, IP, QN and QP values are input to the resistor network.
[0052] The resistor network 510 comprises a plurality of resistors which are connected to scale down the input signals by a predetermined damping factor and to output the down scaled signals QN 71 , QP 71 , IN 71 and IP 71 . The resistors are further connected for providing the output signals IXN, IXP, QXN and QXP. The resistor network will be explained in more detail later. All output signals of the resistor network 510 are input to an absolute value determining unit 520 . The absolute value determining unit 520 determines the absolute values for each input value. The absolute value determining unit 520 is connected to a peak detector 530 which identifies the maximum of the absolute values delivered from the absolute value determining unit 520 . The identified maximum value is now input to the power calculation unit 260 . The power calculation unit 260 calculates a power estimate that may be used to control a gain of a subsequent amplifier.
[0053] The power estimation process performed by the device of FIG. 5 will now be explained with reference to FIG. 6. In the flow chart, the I and Q values are measured simultaneously in step 300 . In step 600 , the IN, IP, QN and QP values are generated using the measured I and Q values. As mentioned above, the IN value is phase shifted by 180° relative to the phase of the IP value and the QN value is phase shifted by 180 ° relative to the phase of the OP value.
[0054] As shown in FIG. 6, the power estimation process then splits into step 610 of scaling the values down and step 620 of calculating the rotated values. Both steps of the power estimation process may be performed simultaneously, using the IN, IP, QN and QP values previously generated.
[0055] Step 610 scales down the input values by a factor of the inverse (reciprocal) of the square root of two, and delivers the down scaled values IN 71 , IP 71 , QN 71 and QP 71 to the rectifying unit 520 . Step 620 calculates the IXN, IXP, QXN and QXP values which are also delivered to the rectifying unit 520 .
[0056] The rectifying step 630 determines the absolute value for each previously determined value, and in step 640 , the maximum of all rectified values is identified. The identified maximum value is now used in the power calculation step 360 to calculate a power estimate which may then be used to control the gain of a subsequent amplifier.
[0057] Again, the power estimation process may return to step back to repeat the entire process using a resistor network with new measured I and Q values.
[0058] As mentioned before, the I and Q values can be displayed in a phase constellation system. FIG. 7 shows a phase constellation system wherein the I and Q values define a phase constellation point of a received signal. Downscaling the phase constellation point of the received signal by a factor of an inverse of the square root of two (1/{square root}{square root over (2)}) results in a downscaled signal point located on the depicted dashed circle line. This dashed circle line represents a level of a phase constellation system that is shrunken by the factor of an inverse of the square root of two.
[0059] The downscaled signal point represents the related pair of the output signals IN 71 , IP 71 , QN 71 and QP 71 of the resistor network 510 in FIG. 5. In addition, when operating the resistor network 510 , a signal point in the shrunken phase constellation system is generated that is rotated by 450 . The position of the rotated signal point in the phase constellation system is defined by the IX and QX values. The rotated signal point represents the related pair of the resistor network output signals IXN, IXP, QXN and QXP.
[0060] Turning now to FIG. 8, the electronic devices are shown that may be used to perform the power estimation process. The depicted resistors 840 are connected to form the modified value calculation unit 220 and the resistors of the present embodiment have all the same resistor values.
[0061] Four peak detector devices 800 to 830 are implemented in the circuit of FIG. 8 for identifying the maximum of the respective signal. Each peak detector is connected to receive a clear signal to be reset. Further, four electronic switches 850 to 880 are provided to switch the output signals to the output terminals, thereby acting as diodes.
[0062] The function of the resistor network will now be explained in more detail with reference to FIG. 9. The signal generator 500 is connected to the resistor network 510 and delivers the IN, IP, QN and QP values to respective input terminals of the resistor network 510 . Between the IN and IP input terminals, and between the QN and QP input terminals, there is provided a resistor divider, to generate the downscaled values. Further, the resistor network comprises a plurality of resistors which each have the same resistor value, to generate the rotated signal point values.
[0063] The output terminals IN 71 and IP 71 provide the I input signals, downscaled by a first resistor divider connected between the IN and IP input terminals. The output terminals QN 71 and QP 71 provide the Q input signals, downscaled by a second resistor divider that is connected between the QN and QP input terminals. The downscale factor for the IN 71 , IP 71 , QN 71 and QP 71 is the inverse of the square root of two. Thus, downscaling effects a shift of the received signal point in the phase constellation system down to the dashed circle line of FIG. 7.
[0064] Still discussing FIG. 9, the resistors are connected for delivering both the IN 71 , IP 71 , QN 71 and QP 71 values and the IXN, IXP, QXN and QXP values. As apparent from the above formulas, IXN and IXP represent a difference of the related resistor network input signals and QXN and QXP represent the sum of the resistor network input signals, respectively. Determining the sum and the difference by means of the resistor network 510 effects both an amplitude reduction by a factor of the inverse of square root of two, and a rotation by 450 in the phase constellation system. Thus, the resulting signal point is positioned on the dashed circle of FIG. 7, in addition to the signal point that is generated by downscaling the input signals by means of the resistor dividers.
[0065] To summarize, the resistor network 510 provides the IN 71 , IP 71 , QN 71 , QP 71 output signals as well as the IXN, IXP, QXN and QXP output signals. In the power estimation process, the output signals of the resistor network 510 are then rectified and the maximum of the rectified signals is input to the power calculation unit 260 for calculating a power estimate.
[0066] [0066]FIG. 10 shows schematically the constellation of the input and the output terminals connected via resistors. Referring now to FIG. 11, the deviation of the maximum value depending on the signal phase angle is illustrated. The function of the deviation has a periodic form and shows a local maximum at the signal phase angle of 22.5°. The deviation function has its maximum recurring in steps of 45°.
[0067] Examples of signal waveforms will now be discussed for explaining in detail the operation of the power estimation unit according to one of the embodiments. For this purpose, reference is made to FIGS. 12 to 27 .
[0068] FIGS. 12 to 15 illustrate the BPSK modulated I, Q, IX and QX signals in the time domain for a subset of phase shift angles between 0° and 36°. The phase shiftings influence the amplitude of the signal, and the direction of the variation of the amplitude of the signal is indicated by an arrow.
[0069] The diagram in FIG. 16 illustrates an overlay of the rectified I, Q, IX and QX signals for a subset of phase shift angles between 0° and 36°.
[0070] [0070]FIG. 17 shows the envelope of the peak value depending on the phase that has a maximum peak value at 0° phase, and a maximum deviation at 22.50. The curve of FIG. 17 can be thought as corresponding to the most left portion of the curve FIG. 11.
[0071] FIGS. 18 to 21 illustrates the I, Q, IX and QX signals in the time domain for a phase shift angle between 0° and 360°. The phase shiftings influence the amplitude of the signal and each plotted function represents a respective phase shift angle.
[0072] [0072]FIG. 22 illustrates an overlay of the rectified I, Q, IX and QX signals depicted for a phase shift angle between 0° and 360°.
[0073] [0073]FIG. 23 illustrates the envelope of the maximum of the rectified I, Q, IX and QX signals in dependency of the phase between 0° and 360°. The plotted maximum value shows a periodic form wherein the maximum is at 0° and is recurring in steps of 45°.
[0074] FIGS. 24 to 27 correspond to FIGS. 12 to 15 but illustrate QPSK modulated I, Q, IX and QX signals in the time domain for a subset of phase shift angles between 0° and 36°.
[0075] As apparent from the foregoing description, all of the embodiments as described may advantageously provide a high-precision, high-accuracy and high-density technique that may be used in particular in an automatic gain control loop, thus improving overall efficiency.
[0076] The arrangements may have the advantage to allow for a process such as the power estimation process wherein solving of complicated formulas is no longer necessary.
[0077] Further, the arrangements may have the advantage due to the fact that a resistor network is used for voltage scaling of signals. This allows for evaluating the power of a digitally modulated signal without using an active amplifier having a gain of the square root of two. Avoiding active elements in the circuits reduces power consumption.
[0078] Moreover, the manufacturing is simplified and therefore, the above described embodiments effect lower production costs.
[0079] While the invention has been described with respect to the physical embodiments constructed in accordance therewith, it will be apparent to those skilled in the art that various modifications, variations and improvements of the present invention may be made in the light of the above teachings and within the purview of the appended claims without departing from the spirit and intended scope of the invention. In addition, those areas in which it is believed that those of ordinary skill in the art are familiar, have not been described herein in order not to unnecessarily obscure the invention described herein. Accordingly, it is to be understood that the invention is not to be limited by the specific illustrative embodiments, but only by the scope of the appended claims. | A receiver is provided for receiving a digitally modulated signal in a communication system. The receiver comprises a signal input unit adapted for determining at least one in-phase and at least one quadrature-phase value of the received signal. The receiver further comprises a signal generator connected to receive the in-phase and quadrature-phase values and to generate at least one modified in-phase value and at least one modified quadrature-phase value of a rotated phase constellation system. The receiver further comprises a signal processing unit that is adapted for processing the received signal dependent on the in-phase and quadrature-phase values and the modified in-phase and quadrature-phase values. The signal generator is a passive impedance network. Further, a corresponding integrated circuit chip and operation method are provided. Using a passive impedance network may simplify the hardware implementation by avoiding the need to provide an active amplifier. | 7 |
FIELD OF THE INVENTION
The present invention generally relates to write-once read-many (WORM) storage and in particular to a WORM storage system utilizing rewriteable media.
BACKGROUND OF THE INVENTION
As critical data are increasingly stored in electronic form, it is imperative that the critical data be stored reliably in a tamper-proof manner. Furthermore, a growing subset of electronic data (e.g., electronic mail, instant messages, drug development logs, medical records, etc.) is subject to regulations governing long-term retention and availability of the data. Recent high-profiled accountability issues at large public companies have further caused regulatory bodies such as the Securities and Exchange Commission (SEC) to tighten their regulations. For instance, Securities Exchange Commission Rule 17a-4, which went into effect in May 2003, specifies storage requirements for email, attachments, memos, and instant messaging as well as routine phone conversations.
A requirement in many such regulations is that data must be stored reliably in non-erasable, non-rewritable storage such that the data, once written, cannot be altered or overwritten. Such storage is commonly referred to as WORM (Write-Once Read-Many) storage as opposed to WMRM (Write-Many Read-Many) storage, which can be written many times.
Conventional WORM storage media comprises WORM tape, ablative WORM optical disk, and magnetic WORM disk. For ablative WORM-based optical CD, the non-overwritable property is inherent in the physical media. Although conventional WORM technology has proven to be useful, it would be desirable to present additional improvements. Writing data to ablative WORM optical disk invokes a permanent change to media itself and cannot be reversed. However, for existing tape-based and magnetic hard-disk based WORM storage system, the media is rewriteable and the WORM property is guaranteed in microcode rather than by media itself.
Guaranteeing the WORM property in microcode rather than by the media introduces a potential trust problem. The data stored on the rewritable media can be modified by malicious applications through another I/O interface that does not support WORM-safe microcode. Conventional rewritable media has no means of protection to prevent data from being overwritten. Once the rewritable media is disconnected from the media drive (disk controller or tape drive) that implements the WORM feature, the data on the media can be overwritten by non-WORM tape drives or disk controllers.
The use of rewritable media as WORM storage is attractive because the random access performance of magnetic hard disks is orders of magnitude improved over that of optical WORM disks. In practice, the fast read performance of rewritable magnetic disks is desirable to meet the search requirement of the current data regulations. One conventional approach to providing WORM storage with rewritable media is to lock the whole storage enclosure (disks, WORM controllers) physically together to avoid tampering. This approach protects the rewritable media from being altered by intruding non-WORM controllers. However, a super key can easily tamper a physical lock. This approach further imposes difficulties and overhead on storage management.
WORM properties of a storage system can be guaranteed on a software level, a firmware level, or a media level. Implementing a WORM property at the media level (e.g., inside hard drives) requires significant changes to the existing commodity hardware. Data storage and access regulations are continually changing, requiring flexibility in configuring WORM storage. The overhead of altering any logic in hardware is usually larger than that of upgrading microcode or software. However, conventional rewritable storage such as a hard drive typically does not provide a programmable environment. Consequently, a WORM storage based on customized hard drives may be unable to meet changes in data regulations.
Implementing a WORM property in a programmable level such as that of a firmware level or software level provides the flexibility required to comply with continually changing data regulations. However, once the binding of the media and the WORM logic is implemented in the firmware level or the software level, the media content can be easily altered.
One conventional approach uses a physical lock on an enclosure in which the components of the WORM storage system reside. The physical lock ensures that the rewritable hard drives and the WORM logic implemented in a storage controller or a processor are physically bound together. Consequently, a malicious adversary has no opportunity to tamper the hard disks through a non-WORM storage controller. However, the anti-tampering barrier of a physical lock is low. For example, an intruder can use a super key to open the locked enclosure. Another conventional approach uses magnetic latches to lock the rewritable disks into an enclosure together with the WORM logic. Such physical binding, however, requires extensive changes to current systems and limits incremental growth.
Another conventional approach uses password verifications to bind the WORM logic with the rewritable storage. This approach requires no hardware modifications. Certain commodity hard drives already have built-in hard-drive password protection. However, authentication passwords can be easily tampered. The following is a scenario describing how an intruder tampers a password-based authentication. Assume the WORM logic is implemented in the firmware of a disk controller. Suppose a controller and disk pair comprises a controller C 0 and a disk D 0 . A malicious controller and disk pair comprises a malicious controller C 1 and a malicious disk D 1 .
The controller C 0 and disk D 0 operate in an open, accessible environment or cabinet such that disks can be freely plugged in and out. The intruder removes the disk D 0 from the cabinet. The intruder inserts the malicious disk D 1 to steal the password of the controller C 0 . Once disk D 1 has this password, the disk D 1 passes it the password to malicious controller C 1 . Now the intruder can use this password to authenticate malicious controller C 1 with disk D 0 and alter the data on disk D 0 .
To comply with continually changing regulations for data storage and use rewritable media as WORM data storage, data management systems require a configuration that maximizes performance, flexibility, and growth capability. A secure binding of WORM logic and storage media is desired to achieve true data immutability without sacrificing ease of storage management tasks such as failure recovery, etc. What is therefore needed is a system, a computer program product, and an associated method for providing a virtual binding for a WORM storage system on rewritable media. The need for such a solution has heretofore remained unsatisfied.
SUMMARY OF THE INVENTION
The present invention satisfies this need, and presents a system, a service, a computer program product, and an associated method (collectively referred to herein as “the system” or “the present system”) for providing a virtual binding for a WORM storage system on rewritable media. The virtual binding ensures that WORM logic protecting data immutability cannot be circumvented.
The present system comprises a WORM logic controller and a WORM storage module. The WORM storage module resides in a storage enclosure with a rewritable media. The WORM logic of the WORM logic controller can be implemented in any form such as, for example, application software, file system software, or firmware of a storage controller. As a WORM logic controller, the WORM logic is realized in a programmable storage controller to avoid hardware modifications to the rewritable media of the WORM storage module.
To close any security holes between the WORM storage module and the WORM logic controller, a controller authenticator of the WORM storage module securely authenticates legitimacy of the WORM logic controller before granting data access to the rewritable media. Similarly, a storage authenticator of the WORM logic controller authenticates the WORM storage module. The present system virtually binds the WORM logic controller and the WORM storage module together even though the WORM logic controller and the WORM storage module may be physically separated. Consequently, the present system enables storage media mobility and allows easy and secure information transfer in an open and malicious environment. The present system further enables flexible system capacity scaling and ease of storage management.
The WORM logic controller and the WORM storage module each comprise a public key and a private key. The WORM logic controller and the WORM storage module mutually register using their respective public key. The registered public key of the WORM logic controller is stored in a storage user table in the controller authenticator on the WORM storage module. The registered public key of the WORM storage module is stored in a controller user table in the storage authenticator on the WORM logic controller. The WORM storage module grants media access rights only to a legitimate WORM logic controller authenticated by the controller authenticator. This authentication requirement prevents overwriting of data in a malicious attack.
A WORM storage module that is blank and comprising an empty user table admits any WORM logic controller. A WORM storage module with user table that is not empty admits WORM logic controllers only until an associated registration phase closes.
The virtual binding of the present system is provided through secure authentication. During the authentication phase, no secret information is transmitted for authentication. Consequently, the authentication phase of the present system is more secure than conventional password authentication. Once the registration and initialization is securely performed, only the registered controllers can access the target hard drives. To avoid hardware modifications to existing hard disks, the authentication logic is implemented on a customized and permanently sealed storage enclosure. The rewritable media is permanently locked in the sealed storage enclosure.
The present system does not rely on physical locks to bind the WORM logic controller and the WORM storage module together. The present system provides WORM protection for each WORM storage module even if the WORM storage module is disconnected from the WORM logic controller. To achieve minimum total system cost, the present system minimizes the required modifications to media hardware. Compared to WORM storage on magnetic disks using mechanical lock protection, the present system offers improved disk mobility and system scalability.
The virtual binding seamlessly ties together the WORM logic controller and WORM storage module for the rewritable media of a storage enclosure. With virtual binding, the present system achieves a secure WORM property for a WORM storage system using rewritable media. Every user for a storage enclosure is securely authenticated before any data access is allowed. The barrier for tampering is much higher for the present system than that of conventional WORM storage systems relying on a physical lock or no binding at all. The present system further achieves high system throughput and retrieval performance.
The present system achieves ease of storage management. Virtual binding does not require any physical lock or physical enclosure for security. A storage enclosure and a WORM logic controller can join or leave a storage system through a relatively simple procedure. The present system further provides flexibility in capacity scaling. Virtual binding allows addition of new storage enclosures at system run time.
The present system provides low total system cost. WORM logic is programmed in a programmable environment of the WORM logic controller. The WORM logic controller comprises a commodity storage controller or application software. Authentication logic for the controller authenticator is built in a customized storage enclosure. No hardware modification is required for the rewritable media. The present system further provides ease of function extension. WORM logic and other functions required for data compliance can be easily upgraded in a programmable environment.
The present system may be embodied in a utility program such as a virtual binding utility program. The present system also provides means for the user to identify a set of data to be stored in WORM storage provided by the present system and then invoke the virtual binding utility program to process and store the data in WORM storage.
BRIEF DESCRIPTION OF THE DRAWINGS
The various features of the present invention and the manner of attaining them will be described in greater detail with reference to the following description, claims, and drawings, wherein reference numerals are reused, where appropriate, to indicate a correspondence between the referenced items, and wherein:
FIG. 1 is a schematic illustration of an exemplary operating environment in which a virtual binding system of the present invention can be used;
FIG. 2 is a process flow chart illustrating a method of operation of the virtual binding system of FIG. 1 ;
FIG. 3 comprises FIGS. 3A , 3 B, and 3 C, and represents a process flow chart illustrating a method of operation of the virtual binding system of FIG. 1 in a registration and authentication phase;
FIG. 4 is a process flow chart illustrating a method of operation of the virtual binding system of FIG. 1 in an operation phase;
FIG. 5 is comprised of FIGS. 5A and 5B and represents a process flow chart illustrating a method of operation of the virtual binding system of FIG. 1 in a maintenance and management phase; and
FIG. 6 is a process flow chart illustrating a method of operation of the virtual binding system of FIG. 1 in a migration phase.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 portrays an exemplary overall environment (a WORM storage system 100 ) in which a system, a service, a computer program product, and an associated method (the “virtual binding system 10 ” or the “system 10 ”) for providing a virtual binding for a WORM storage system on rewritable media according to the present invention may be used. System 10 comprises a software programming code or a computer program product that is typically embedded within, or installed on a computer 15 .
System 10 comprises a worm logic controller 20 and a WORM storage module 25 . The WORM logic controller 20 comprises a storage authenticator 30 for authenticating a security-enhanced storage enclosure 35 . The WORM storage module 25 comprises a controller authenticator 40 for authenticating the WORM logic controller 20 . The WORM logic controller 20 and the WORM storage module 25 communicate via a network 45 through communication links 50 , 55 , respectively. While the system 10 is described for illustration purpose only in relation to network 45 , it should be clear that the WORM logic controller 20 and the WORM storage module 25 can communicate locally as well as remotely and may be co-located or located remote from each other.
The security-enhanced storage enclosure 35 (interchangeably referenced herein as storage enclosure 35 ) comprises the WORM storage module 25 and a rewritable media 60 . The WORM storage module 25 controls access to data in the rewritable media 60 , allowing only an authenticated WORM logic controller 20 to have access privileges to the rewritable media 60 . Consequently, the process of authentication between the WORM storage module 25 and the WORM logic controller 20 forms a virtual binding 65 that achieves a secure WORM property for the security-enhanced storage enclosure 35 .
In one embodiment, additional WORM logic controllers may have access to the rewritable media. For example, WORM logic controller A, 70 , may form a virtual binding 75 through network 45 . Worm logic controller A, 70 , and WORM logic controller 20 are collectively referenced as WORM logic controllers 80 and represent any number of worm logic controllers. The maximum number of controllers that can be registered depends on the size of the storage memory. In practice, the storage memory size is typically large and does not pose a limitation on the number of controllers.
The rewritable media 60 comprises, for example, standard rewritable ATA or SCSI magnetic hard drives. In one embodiment, the WORM logic controller 20 comprises a built-in WORM logic controller 20 . While the WORM logic controller 20 is described for illustration purposes only in terms of a built-in WORM logic controller 20 , it should be clear that the WORM logic of the WORM logic controller 20 can be built in any layer. System 10 is applicable to any WORM logic implementation and storage media binding.
The WORM storage module 25 comprises a rewritable non-volatile media (a storage memory 85 ). In one embodiment, the storage memory 85 comprises a few hundred bytes. The storage memory 85 stores a storage public key and a storage private key (collectively referenced as the storage public/private key pair). The WORM storage module 25 further comprises the processing power required to perform public-key and private-key based encoding or decoding. While the worm storage module 25 is described for illustration purposes only as being implemented in the security-enhanced storage enclosure 35 , it should be clear that the WORM storage module 25 can be implemented in the rewritable media 60 .
The WORM logic controller 20 comprises a rewritable non-volatile media (a controller memory 90 ). In one embodiment, the controller memory 90 comprises a few hundred bytes. The controller memory 90 stores an identifier for the WORM logic controller (further referenced herein as the controller ID). The controller ID is optional, and is not necessary to maintain the controller ID. The public key could alternatively serve as the controller ID. The controller memory 90 further stores a controller public key and a controller private key (collectively referenced herein as the controller public/private key pair). The controller memory 90 stores an optional controller certificate. For ease of replication, the controller ID, the controller public/private key pair, or the optional controller certificate can be stored in persistent storage other than the controller memory 90 . For example, the controller ID, the controller public/private key pair, or the optional controller certificate can be stored in a hard disk accessible only to authorized users.
When the WORM storage module 25 is implemented in the security-enhanced storage enclosure 35 , the mobile granularity is a security-enhanced storage enclosure 35 . The security-enhanced storage enclosure 35 is loaded with rewriteable media 60 comprising, for example, disks. The security-enhanced storage enclosure 35 is permanently sealed before being shipped. Consequently, the rewritable media 60 and the WORM storage module 25 are inseparable from the security-enhanced storage enclosure 35 and form a single entity in the WORM storage system 100 .
Data access to the rewritable media 60 is locked from any attempting WORM logic controller 20 unless the authentication process of the controller authenticator 40 is successful. The controller authenticator 40 maintains a storage user table in the storage memory 85 comprising a controller public key and an optional controller ID for each of the WORM logic controllers 80 that have data access to the rewritable media 60 .
The WORM storage module 25 maintains the storage private/public key pair as an identity for the WORM storage module to be authenticated by the WORM logic controller 25 . In one embodiment, the WORM storage module 25 further maintains a flag to indicate a registration status. WORM logic controllers 80 can be admitted to the WORM storage module 25 only if registration is open.
In one embodiment, the WORM storage module 25 and related secret information are replicated in the security-enhanced storage enclosure 35 to avoid single point of failure. In another embodiment, the security-enhanced storage enclosure 35 is made tamper-resistant to avoid physical intrusion to the storage user table and the rewritable media 60 . A tamper-resistant security-enhanced storage enclosure 35 erases any confidential information and self-destructs if any physical intrusion occurs to the security-enhanced storage enclosure.
System 10 can bind together in the virtual binding 65 the rewritable media 60 and any form of the WORM logic controller 20 (i.e., software or firmware). For fault tolerance, the WORM storage system can comprise dual WORM logic controllers 80 or additional WORM logic controllers 80 . The WORM logic controller 20 is the only channel through which applications can read data on or write data to the rewritable media 60 .
In one embodiment, the controller public key and the controller ID are stored in the controller certificate. The controller certificate is signed by a trusted party to prove the benevolentness of the WORM logic controller 20 . The WORM logic controller 20 passes the controller certificate to any entity requiring authentication of the WORM logic controller 20 .
In another embodiment, the WORM logic controller 20 is tamper-resistant to further avoid exposure of the controller public/private key pair. However, since the controller public/private key pair is kept within the WORM logic controller 20 and is not exposed to any other software or user, it is difficult to steal the controller public/private key pair from software channels. Tamper-resistance of the WORM logic controller 20 is necessary only if the probability of physical intrusion is high. In most applications of the WORM storage system 100 , tamper-resistance for the WORM logic controller 20 is not required to achieve a secure virtual binding 65 .
System 10 utilizes an encrypted content signature comprising a hash of data content (a content hash, for example a SHA-1 hash) to avoid traffic snooping and alternation between the WORM logic controller 20 and the rewritable media 60 . The hash of the data content generates an encrypted content signature that certifies the validity of the bytes received by the rewritable media 60 . Periodically, the content hash of these bytes is sent to the WORM storage module 25 . The content hash is a unique encrypted content signature of the bytes that the content hash verifies. Furthermore, the content hash is encrypted using the controller private key of the WORM logic controller 20 .
The WORM storage module 25 decrypts the encrypted content signature and verifies the bytes and command codes received from the WORM logic controller 20 . Similarly, to defeat traffic alternation from the rewritable media 60 to the WORM logic controller 20 , the WORM logic controller 20 verifies the received bytes from the rewriteable media 60 . The WORM storage module 25 computes an encrypted operations signature for the results for any operations before sending the results back to the WORM logic controller 20 . The encrypted operations signature is computed based on the storage private key of the WORM storage module 25 . The WORM logic controller 20 trusts only those results with matching signatures.
FIG. 2 illustrates a method 250 of operation of system 10 . Method 250 comprises an initialization phase (step 205 ), a registration and authentication phase (method 300 , further described in FIG. 3 ), an operation phase (method 400 , further described in FIG. 4 ), a maintenance and management phase (method 500 , further described in FIG. 5 ), and a migration phase (method 600 , further described in FIG. 6 ).
The initialization phase (step 205 ) comprises initializing the WORM logic controller 20 or the security-enhanced storage enclosure 35 . The security-enhanced storage enclosure 35 is shipped from the manufacturer with a storage user table that is blank and the registration flag set to “open”. The WORM logic controller 20 is shipped from the manufacturer with the controller public/private key pair un-initialized. The customer initializes the controller public/private key pair when the WORM logic controller 20 is received. The manufacturer sets the controller ID to the serial number of the WORM logic controller 20 .
FIG. 3 ( FIGS. 3A , 3 B, 3 C) illustrates a method 300 of the registration and authentication phase of system 10 in which a newly arrived security-enhanced storage enclosure 35 is detected by the WORM logic controller 20 . The security-enhanced storage enclosure 35 is connected to the WORM storage system 100 (step 305 ). The WORM logic controller 20 detects the arrival of the security-enhanced storage enclosure 35 (step 310 ).
System 10 performs a mutual authentication phase for the WORM storage module 25 and the WORM logic controller 20 . The WORM storage module 25 retrieves the controller public key of the WORM logic controller 20 (step 315 ). The controller authenticator 40 authenticates the WORM logic controller 20 (step 320 ).
To authenticate the WORM logic controller 20 , the controller authenticator 40 encrypts a challenge string with the controller public key of the WORM logic controller 20 and sends the controller public key to the WORM logic controller 20 . A genuine, verifiable WORM logic controller 20 is able to decode the encrypted challenge and return the decoded challenge to the controller authenticator 40 as proof. If the controller authenticator 40 cannot authenticate the WORM logic controller 20 (decision step 325 ), the authentication phase aborts (step 330 ). Otherwise, the authentication phase continues.
The controller authenticator 40 determines whether the retrieved controller public key is in the storage user table of the WORM storage module 25 (decision step 335 ). If yes, the WORM storage module 25 unlocks the rewritable media 60 for access by the WORM logic controller 20 (step 340 ). If the retrieved controller public key is not in the storage user table of the WORM storage module 25 (decision step 345 ), the WORM logic controller 20 has not registered with the WORM storage module 25 .
The WORM storage module 25 determines whether registration criteria have been met (decision step 345 ). The registration criteria require that the security-enhanced storage enclosure 35 is blank and the registration flag is “open”. If the registration criteria are not met, the authentication phase aborts (step 330 ). Otherwise, the controller authenticator 40 adds the controller public key of the WORM logic controller 20 to the storage user table (step 350 ).
The security-enhanced storage enclosure 35 may be brand new or partially used. If the security-enhanced storage enclosure 35 is brand new with an empty storage user table, the registration flag of the WORM storage module 25 is in “open” mode. When the registration flag is in “open” mode, the WORM storage module 25 allows addition of any WORM logic controller 20 to the storage user table. Once data is written to the rewritable media 60 , the WORM storage module 25 switches the registration flag to “closed” mode and disallows admission of any new WORM logic controllers 80 . Any authorized WORM logic controller 20 can set the registration flag.
To provision for fault tolerance and provide a multi-path WORM storage system 100 , additional WORM logic controllers 80 can register with the security-enhanced storage enclosure 35 while registration is open. Once the registration is closed, no additional WORM logic controllers 80 can be admitted. This requirement disables registration by malicious controllers intent on tampering with the data in the security-enhanced storage enclosure 35 . Consequently, to accommodate potential failure by the WORM logic controller 20 , the security-enhanced storage enclosure 35 is over-provisioned with WORM logic controllers 80 before the registration for the security-enhanced storage enclosure 35 is closed. In another embodiment, over-provisioning can be avoided by a certificate-based authentication, as it will be explained below.
To enable flexible capacity scale-up, system 10 allows the security-enhanced storage enclosure 25 to register at any time with the WORM logic controller 20 . When the WORM logic controller 20 registers a brand new security-enhanced storage enclosure 35 , the WORM logic controller 20 formats and overwrites all the existing data on the rewritable media 60 of the newly registered security-enhanced storage enclosure 35 . This formatting procedure avoids polluting data already in the WORM storage system 100 with the data on the newly introduced security-enhanced storage enclosure 35 . If the WORM storage module 25 has been previously registered, the WORM logic controller 20 does not format the data on rewritable media 60 .
In one embodiment, the WORM logic controller 20 proves a legitimate identity or trustworthiness to enable on-demand registration for the WORM logic controller 20 in which registration is always open for the security-enhanced storage enclosure 35 . The registration phase for the storage enclosure is always on, in this embodiment. Hence, no over-provisioning is necessary. To prove the legitimate identity of the WORM logic controller 20 , the controller public key and the controller ID are stored in a certificate signed by a trusted manufacturer. The trusted manufacturer encrypts the certificate with the private key of the manufacturer. This certificate cannot be altered since only the manufacturer knows the private key of the manufacturer. The public key of the manufacturer is known to all.
The security-enhanced storage enclosure 35 can verify legitimacy of the WORM logic controller 20 comprising a certificate. The WORM storage module 25 decodes the certificate with the public key of the manufacturer. The controller authenticator 40 authenticates the WORM logic controller 20 . A malicious WORM logic controller 20 attempting to replicate the certificate fails authentication because the malicious WORM logic controller 20 does not have the private key that matches the encrypted public key.
Method (or process) 300 continues at step 355 wherein the WORM logic controller module storage authenticator 30 retrieves the storage public key from the WORM storage module 25 . The storage authenticator 30 authenticates the WORM storage module 25 (step 360 ).
At decision step 365 , method 300 inquires if such authentication was successful. If it was not, then method 300 terminates at step 370 . Otherwise, method 300 proceeds to decision step 375 and inquires if the retrieved public key in found in the controller user table. If it is, the controller is unlocked at step 380 . Otherwise, method 300 proceeds to step 385 , to format the storage and to add the storage public key to the controller user table of the storage.
FIG. 4 illustrates a method 400 of system 10 in accessing the rewritable media 60 of the security-enhanced storage enclosure 35 . The controller authenticator 40 and the storage authenticator 30 perform mutual authentication (step 405 ), as described by method 300 of FIG. 3 . If authentication fails (decision step 410 ), the WORM storage module 25 denies access to the WORM logic controller 20 (step 415 ).
If authentication succeeds (decision step 410 ), the WORM storage module 25 receives a command such as, for example, a write request (step 420 ). The controller authenticator 40 periodically authenticates the data stream from the WORM logic controller 20 (step 425 ). If the authentication of the data stream is invalid (decision step 430 ), the WORM storage module 25 fails the command execution (step 435 ), and the storage is locked from further access from the command sender. If the authentication of the data stream is valid (decision step 430 ), the WORM storage module 25 executes the command on the rewritable media 60 (step 440 ).
FIG. 5 ( FIGS. 5A , 5 B) illustrates a method 500 of system 10 in performing the maintenance and management phase. A user begins the maintenance and management phase (step 505 ). If the user is adding a new security-enhanced storage enclosure 35 (decision step 510 ), system 10 performs the registration phase of method 300 in FIG. 3 (step 515 ). If the user is adding a new WORM logic controller 20 (decision step 520 ), system 10 performs the registration phase of method 300 in FIG. 3 (step 525 ).
If the user is removing a broken storage enclosure 35 (decision step 530 ), the WORM logic controller 20 removes the storage public key of the broken security-enhanced storage controller 35 from the controller user table (step 535 ). A new security-enhanced storage enclosure 35 can be installed in the WORM storage system 100 to replace the broken security-enhanced storage enclosure 35 . The new security-enhanced storage enclosure 35 follows the new security-enhanced storage enclosure 35 addition procedure as described in step 510 through 515 .
If the user is removing a working storage enclosure 35 (decision step 540 ), the security-enhanced storage enclosure 35 detects the disconnection of the WORM logic controllers 80 and marks the disconnect event (step 545 ), and disallows any further access by the WORM logic controllers 80 . When the security-enhanced storage enclosure 35 is reinstalled in the WORM storage system 100 , system 10 performs the authentication phase as described in method 300 of FIG. 3 .
If the user is removing a broken WORM logic controller 20 (decision step 550 ), the WORM storage module 25 removes the controller public key of the broken WORM logic controller 20 from the storage user table (step 555 ). When a WORM logic controller 20 fails, a registered sibling WORM logic controller provides data access to the rewritable media 60 .
If the user is removing a working WORM logic controller 20 (decision step 560 ), the WORM storage module 25 detects the removal (step 565 ) either through notification by system 10 or after a period of idle time by the removed WORM logic controller 20 . The WORM storage module 25 unlocks the data access of the rewritable media 60 from the disconnected WORM logic controller 20 (step 570 ). When the WORM logic controller 20 is reinstalled in the WORM storage system 100 , the system 10 performs the authentication phase as described in method 300 of FIG. 3 . System 10 ends the maintenance and management phase (step 575 ).
FIG. 6 illustrates a method 600 of system 10 in performing a migration phase. System 10 disconnects the virtual binding (step 605 ). If the user is migrating the security-enhanced storage enclosure 35 (decision step 610 ), the WORM logic controller 20 removes the controller public key from the storage user table (step 615 ). System 10 registers the storage enclosure 35 in a “new” location as describe by method 300 , FIG. 3 . The “new” location may be logically new rather than physically new. Step 615 and 620 apply to the embodiment in which a WORM logic controller 20 has a signed certificate from a trusted manufacturer and registration is always open.
In the embodiment in which registration closes after an initial byte of useful data is written to the security-enhanced storage enclosure 35 , a partially written, working security-enhanced storage enclosure 35 can only quit association with one WORM logic controller 20 . In this embodiment, the partially written, working security-enhanced storage enclosure 35 cannot admit a new WORM logic controller 20 .
If the user is migrating the WORM logic controller 20 (decision step 625 ), the WORM logic controller 20 notifies the security-enhanced storage enclosure 35 . The security-enhanced storage enclosure 35 removes the controller public key from the storage user table (step 630 ). The WORM logic controller 20 can register with any other security-enhanced storage enclosure 35 in a “new” location (step 635 ). The “new” location may be logically new rather than physically new. System 10 ends the migration phase (step 640 ).
It is to be understood that the specific embodiments of the invention that have been described are merely illustrative of certain applications of the principle of the present invention. Numerous modifications may be made to the system and method for providing a virtual binding for a WORM storage system on rewritable media described herein without departing from the spirit and scope of the present invention. | A virtual binding system ensures that the WORM logic for protecting data immutability cannot be circumvented, effectively guaranteeing WORM property of a WORM storage system composed of rewritable magnetic hard disks. To close the security hole between the rewritable media and the WORM logic, virtual binding securely authenticates the legitimacy of a WORM logic controller before granting data access on a WORM storage media. Furthermore, the system verifies the legitimacy of the WORM logic controller during data access. This approach virtually binds together the WORM logic controller and the WORM storage media even though the WORM logic controller and the WORM storage media may be physically separate. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a control method of an AC/DC power converter for input current harmonic suppression. More particularly, the present invention relates to the control method for applying to the AC/DC power converter without detecting an AC voltage so as to adjust an input AC current to approximate nearly as a sinusoidal wave and to obtain an unity power factor, and to supply an output of an adjustable DC voltage.
2. Description of the Related Art
Power converters have been widely used in many areas recently. These power converters include AC/DC, DC/DC and DC/AC converters. Conventionally, the AC/DC power converter is configured by a diode rectifier. There are advantages of simplified configuration and reduced cost in using the diode rectifier. However, a DC side of the diode rectifier cannot be controlled, and a great amount of input harmonic components and poor input power factors occur in its AC side.
In order to improve the problems of harmonic pollution effectively, many harmonic control standards, such as IEEE519-1992, IEC1000-3-2, and IEC1000-3-4 etc., have been established. In this way, the modern power electronic equipment need to meet the requirements for low input harmonic distortion and high input power factor. Recently, a variety of power factor correctors are developed to solve the harmonic problems caused by the AC/DC power converter.
Referring to FIG. 1 , a schematic circuitry of a conventional power factor corrector is illustrated. Generally, the power factor corrector includes a diode rectifier 10 , an inductor 11 , a power electronic switch 12 , a diode 13 , a DC capacitor 14 and a controller 15 . Control methods for the power factor corrector are well known and described in U.S. Pat. No. 6,650,554 and U.S. Pat. No. 6,388,429, for example. The output DC voltage of the power factor corrector can be controlled by controlling the power electronic switch 12 . The output DC voltage of the power factor corrector is higher than a peak value of an input AC voltage. An input current approximated nearly as a sinusoidal wave and an unity input power factor can be obtained at an input AC side of the power factor corrector. The conventional control method for controlling the power factor corrector employs a detected output DC voltage for regulating the output DC voltage so as to determine a reference amplitude of the input AC current. Subsequently, a detected AC voltage is employed to determine a reference waveform of the input AC current. The reference waveform multiplies the reference amplitude, thereby obtaining a reference signal of the input AC current. Subsequently, the reference signal and a detected input AC current are operated in a closed-loop control to produce a modulation signal. Finally, the modulation signal is sent to a pulse-width-modulation circuit and a driving circuit to produce a driving signal for the power electronic switch 12 . In this way, the conventional control method for the power factor corrector disadvantageously requires to detect three signals, including the output DC voltage, the input AC voltage and the input AC current.
Generally, an AC/DC power converter must employ a power converter having a bridge configuration. Referring now to FIGS. 2 a and 2 b , schematic circuitry of conventional single-phase AC/DC power converters applied to a single-phase AC power system in accordance with the prior art are illustrated.
Still referring to FIG. 2 a , the conventional single-phase AC/DC power converter having a half-bridge configuration is disclosed. The half-bridge configuration of the single-phase AC/DC power converter includes a power electronic switch set 20 , a pair of capacitors 21 , 22 , an inductor 32 and a controller 24 . The power electronic switch set 20 has two power electronic switches. The capacitors 21 , 22 have the same capacitance. The controller 24 can control the power electronic switch set 20 , thereby controlling the AC/DC power converter to receive an input AC current supplied from an AC power source through the inductor 23 . Advantageously, the input AC current is approximated nearly as a sinusoidal wave and in phase with the input voltage of the AC power source. Consequently, the harmonics in the AC/DC power converter can be suppressed, the power factor is nearly unity, and the output DC voltage can be controlled.
Referring again to FIG. 2 b , the conventional single-phase AC/DC power converter having a full-bridge configuration is disclosed. The full-bridge configuration of the single-phase AC/DC power converter includes a power electronic switch set 30 , a capacitor 31 , an inductor 32 and a controller 33 . The power electronic switch set 30 has four power electronic switches. The controller 33 can control to switch the power electronic switch set 30 , thereby controlling the AC/DC power converter to receive an input AC current supplied from an AC power source through the inductor 23 . Advantageously, the input AC current is approximated nearly as a sinusoidal wave and in phase with the input voltage of the AC power source. Consequently, the harmonics in the AC/DC power converter can be suppressed, the power factor is nearly unity, and the output DC voltage can be controlled.
Referring to FIG. 3 , a schematic circuitry of a conventional three-phase AC/DC power converter applied to a three-phase AC power system in accordance with the prior art is illustrated. The three-phase AC/DC power converter includes a power electronic switch set 40 , a capacitor 41 , a three-phase inductor set 42 and a controller 43 . The power electronic switch set 40 has six power electronic switches. The controller 43 can control to switch the power electronic switch set 40 , thereby controlling the AC/DC power converter to produce a balanced three-phase sine-wave currents on the three-phase inductor set 42 . Advantageously, phases of the three-phase sine-wave currents are identical with those of the input voltages of a three-phase power source. Consequently, the harmonics in the three-phase AC/DC power converter can be suppressed, and the power factor can be improved to nearly unity.
The conventional control method for both the single-phase AC/DC power converter and the three-phase AC/DC power converter employs a detected output DC voltage for regulating the output DC voltage so as to determine a reference amplitude of the input AC current. Subsequently, a detected AC voltage of the AC power source is employed to determine a reference waveform of the input AC current. The reference waveform multiplies the reference amplitude, thereby obtaining a reference signal of the input AC current. Subsequently, the reference signal and the detected input AC current are operated in closed-loop control to produce a modulation signal. Finally, the modulation signal is sent to a pulse-width-modulation/driving circuit to produce a set of driving signals for the power electronic switch sets 20 , 30 , 40 . In this way, the conventional control method for the single-phase AC/DC power converter and the three-phase AC/DC power converter disadvantageously require to detect three signals, including the output DC voltage, the input AC voltage and the input AC current.
Even though the conventional control methods of the AC/DC power converters can suppress the harmonic components of the input AC current and improve the power factor, the controller must detect the output DC voltage and the input AC voltage to determine the reference signal. Subsequently, the input AC current is detected and operated in closed-loop control to obtain a sine-wave input AC current. Advantageously, the sine-wave input AC current is in phase with the input voltage of the AC power source. However, the conventional control methods for the AC/DC power converter disadvantageously require detecting three signals, including the output DC voltage, the input AC voltage and the input AC current. Accordingly, the control circuit can be complicated and cannot be normally operated due to fluctuations in frequency of the AC power system.
The present invention intends to provide a simplified control method of an AC/DC power converter for suppressing the input current harmonics. The control circuit only detects two signals from the output DC voltage and the input AC current. Additionally, the control method can be normally operated under fluctuations in frequency of the AC power system for controlling an input AC current to approximate nearly as a sinusoidal wave and a unity power factor, and to supply an adjustable output DC voltage.
SUMMARY OF THE INVENTION
The primary objective of this invention is to provide a simplified control method of an AC/DC power converter for suppressing the input current harmonics. The AC/DC power converter can convert energy of an AC power source into a regulated output DC voltage to supply to a DC load. The control method permits the AC/DC power converter without detecting a voltage of an AC power source for simplifying the entire structure. Accordingly, the AC/DC power converter can be normally operated under the variable frequency of the AC power source for controlling an input AC current to approximate nearly as a sinusoidal wave with the performance of high input power factor and low input harmonic current. Consequently, the purposes of harmonic suppression and power factor improvement can be achieved.
The AC/DC power converter in accordance with the present invention employs a control method for permitting the AC/DC power converter only to detect an input AC current and an output DC voltage. The control method can control the AC side of the AC/DC power converter to generate a voltage which is proportional to the input AC current. Thereby, the AC/DC power converter acts as a virtual resistor having a linear resistance characteristic. The detected output DC voltage is used for regulating the output DC voltage so as to determine a value of the virtual resistor for operation of the AC/DC power converter. Accordingly, the input AC current of the AC/DC power converter can be controlled to approximate nearly as a sinusoidal wave with the performance of high power factor and low harmonic distortion. Since the AC/DC power converter acts as a virtual resistor, frequency of the input AC current can be synchronously changed in response to the change in frequency of the AC power source. Consequently, the AC/DC power converter can be normally operated under the variable frequency of an AC power source for controlling the input AC current to approximate nearly as a sinusoidal wave with the performance of high power factor and low harmonic distortion.
Further scope of the applicability of the present invention will become apparent from the detailed description given hereinafter. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various will become apparent to those skilled in the art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will become more fully understood from the detailed description given hereinbelow and the accompanying drawings which are given by way of illustration only, and thus are not limitative of the present invention, and wherein:
FIG. 1 is a schematic circuitry of a conventional power factor corrector in accordance with the prior art;
FIG. 2 a is a schematic circuitry of a conventional single-phase AC/DC power converter applied to a single-phase AC power system in accordance with the prior art;
FIG. 2 b is a schematic circuitry of another conventional single-phase AC/DC power converter applied to a single-phase AC power system in accordance with the prior art;
FIG. 3 is a schematic circuitry of a conventional three-phase AC/DC power converter applied to a three-phase AC power system in accordance with the prior art;
FIG. 4 is a control block diagram illustrating a control circuitry of a harmonic-suppressing AC/DC power converter applied to a power factor corrector in accordance with a first embodiment of the present invention;
FIG. 5 is a control block diagram illustrating a control circuitry of a harmonic-suppressing single-phase AC/DC power converter employing a half-bridge or full-bridge structure in accordance with a second embodiment of the present invention; and
FIG. 6 is a control block diagram illustrating a control circuitry of a harmonic-suppressing single-phase AC/DC power converter in accordance with a third embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 4 , a control block diagram of a harmonic-suppressing AC/DC power converter applied to a power factor corrector in accordance with a first embodiment of the present invention is illustrated. The power factor corrector in accordance with the preferred embodiment has similar configuration and similar function as that of the conventional power factor corrector, as shown in FIG. 1 , and detailed descriptions may be omitted. In the first embodiment, the control block diagram of the AC/DC power converter includes a voltage-regulation circuit, a current-detecting circuit, a multiplier circuit and a pulse-width-modulation/driving circuit.
Still referring to FIG. 4 , the voltage-regulation circuit includes a voltage detector 50 , a first subtracter 51 , a controller 52 and a second subtracter 53 ; the current-detecting circuit includes a current detector 54 ; the multiplier circuit includes a multiplier 55 ; and the pulse-width-modulation/driving circuit includes a third subtracter 56 , a pulse-width-modulation circuit 57 and a driving circuit 58 .
Referring back to FIGS. 1 and 4 , the voltage detector 50 detects an output DC voltage of the power factor corrector, and then sends to the first subtracter 51 which subtracts the detected output DC voltage from a first predetermined value. Subsequently, the result is sent to the controller 52 to obtain an output, and the output of controller 52 is sent to the second subtracter 53 which subtracts the output of the controller 52 from a second predetermined value. Accordingly, the second subtracter 53 can generate a control signal V R which provides a value acting as a virtual resistor for the power factor corrector. Preferably, the first predetermined value of the first subtracter 51 is set at an expected value of the output DC voltage, and it can be changed as the desired output DC voltage is changed. Since the power factor corrector is acted as the virtual resistor, the power factor corrector can absorb lesser real power as the value of the resistor is greater; namely, the resistance of the virtual resistor is inversed-proportional to the conversion real power of the power factor corrector. Accordingly, the output of the controller 52 must be subtracted from the second predetermined value by the second subtracter 53 . Under these conditions the second predetermined value of the second subtracter 53 equals a maximum value of the virtual resistor as well as a minimum value of the conversion real power of the power factor corrector. Consequently, this ensures a positive value for the input real power of the power factor corrector.
Still referring to FIGS. 1 and 4 , the current detector 54 is used to detect an input AC current passing through the inductor 11 of the power factor corrector, as best shown in FIG. 1 . Subsequently, the input AC current and the control signal V R of the second subtracter 53 are sent to the multiplier 55 , and then the result is sent to the pulse-width-modulation/driving circuit. With reference to FIG. 1 , when the power electronic switch 12 of the power factor corrector is turned on, a voltage V 1 across the power electronic switch 12 is nearly zero; conversely, when the power electronic switch 12 of the power factor corrector is turned off, a voltage V 1 across the power electronic switch 12 is the same with the output DC voltage of the power factor corrector. Accordingly, an average value of the voltage V 1 is reduced as a duty ratio of the power electronic switch 12 is increased, wherein the duty ratio is the ratio of a conduction time to a switching period of the power electronic switch 12 ; namely, the voltage V 1 is inversed-proportional to the duty ratio of the power electronic switch 12 . Prior to sending to the pulse-width-modulation/driving circuit, the output of the multiplier 55 , must be sent to the third subtracter 56 which can subtract the output of the multiplier 55 from a third predetermined value. Subsequently, the result of the third subtracter 56 is sent to the pulse-width-modulation circuit 57 to operate as a modulation signal. Typically, the pulse-width-modulation circuit 57 can select a high-frequency triangular or saw-tooth wave acting as a carrier wave. In the pulse-width-modulation circuit 57 , the modulation signal is compared with the carrier wave so as to generate a high-frequency pulse-width-modulation signal. Finally, an output of the pulse-width-modulation circuit 57 is sent to the driving circuit 58 so as to generate a driving signal for the power electronic switch 12 of the power factor corrector. Preferably, the third predetermined value of the third subtracter 56 is set for a peak value of the high-frequency carrier wave of the pulse-width-modulation circuit 57 . When the driving circuit 58 sends the driving signal to drive the power electronic switch 12 of the power factor corrector, the voltage V 1 across the power electronic switch 12 is obtained and proportional to the input AC current. Consequently, the power factor corrector can be acted as the virtual resistor, and used to absorb real power from the AC power source and to convert it into a DC power with an adjustable output DC voltage. Furthermore, a current waveform identical with the voltage waveform of the AC power source is generated at the AC side of the power factor corrector so as to adjust the input AC current to be approached to the unity power factor. Since the AC power source supplies an AC voltage with sinusoidal waveform, the input AC current is approximated nearly as a sinusoidal wave which has low harmonic distortion.
Turning now to FIG. 5 , a control block diagram of a harmonic-suppressing single-phase AC/DC power converter employing a half-bridge or full-bridge configuration in accordance with a second embodiment of the present invention is illustrated. The half-bridge or full-bridge configuration of the single-phase AC/DC power converter in accordance with the preferred embodiment has similar configuration and similar function as that of the conventional single-phase AC/DC power converter, as shown in FIGS. 2 a and 2 b , and detailed descriptions may be omitted. In the second embodiment, the control block diagram of the single-phase AC/DC power converter includes a voltage-regulation circuit, a current-detecting circuit, a multiplier circuit and a pulse-width-modulation/driving circuit.
Still referring to FIG. 5 , the voltage-regulation circuit includes a voltage detector 60 , a first subtracter 61 , a controller 62 and a second subtracter 63 ; the current-detecting circuit includes a current detector 64 ; the multiplier circuit includes a multiplier 65 ; and the pulse-width-modulation/driving circuit includes a pulse-width-modulation circuit 66 and a driving circuit 67 .
Referring back to FIGS. 2 a , 2 b and 5 , the voltage detector 60 detects an output DC voltage of the single-phase AC/DC power converter, and then sends to the first subtracter 61 which subtracts the detected output DC voltage from a first predetermined value. Subsequently, the result is sent to the controller 62 to obtain an output, and the output of controller 62 is sent to the second subtracter 63 which subtracts the output of the controller 62 from a second predetermined value. Accordingly, the second subtracter 63 can generate a control signal V R which provides a value acting as a virtual resistor for the single-phase AC/DC power converter. Preferably, the first predetermined value of the first subtracter 61 is set at an expected value of the output DC voltage, and it can be changed as the desired output DC voltage is changed. Since the single-phase AC/DC power converter acts as the virtual resistor, the single-phase AC/DC power converter can absorb lesser real power as the value of virtual resistor is greater; namely, the resistance of the virtual resistor is inversed-proportional to the conversion real power of the single-phase AC/DC power converter. Accordingly, the output of the controller 62 must be subtracted from the second predetermined value by the second subtracter 63 . Under these conditions the second predetermined value of the second subtracter 63 equals a maximum value of the virtual resistor as well as a minimum value of the conversion real power of the single-phase AC/DC power converter. Consequently, this ensures a positive value for the input real power of the single-phase AC/DC power converter.
Still referring to FIGS. 2 a , 2 b and 5 , the current detector 64 is used to detect an input AC current passing through the inductor 23 or 32 of the single-phase AC/DC power converter, as best shown in FIGS. 2 a and 2 b . The input AC current of the single-phase AC/DC power converter is detected. Subsequently, the input AC current and the control signal V R of the second subtracter 63 are sent to the multiplier 65 , and then the result is sent to the pulse-width-modulation circuit 66 to obtain a modulation signal. Typically, the pulse-width-modulation circuit 66 can select a high-frequency triangular or saw-tooth wave acting as a carrier wave. In the pulse-width-modulation circuit 66 , the modulation signal is compared with the carrier wave so as to generate a high-frequency pulse-width-modulation signal. Finally, an output of the pulse-width-modulation circuit 66 is sent to the driving circuit 67 so as to generate the driving signals for the power electronic switch set 20 or 30 of the single-phase AC/DC power converter, as shown in FIGS. 2 a and 2 b . When the driving circuit 67 sends the driving signals to drive the power electronic switch set 20 or 30 of the single-phase AC/DC power converter, the voltage across the output of power electronic switch set 20 or 30 is proportional to the input AC current. Consequently, the single-phase AC/DC power converter acts as the virtual resistor, and used to absorb real power from the AC power source and to convert it into a DC power with an adjustable output DC voltage. Furthermore, a current waveform identical with the voltage waveform of the AC power source is generated at the AC side of the single-phase AC/DC power converter so as to adjust the input AC current to be approached to the unity power factor. Since the AC power source supplies an AC voltage with sinusoidal waveform, the input AC current is approximated nearly as a sinusoidal wave which has low harmonic distortion.
Turning now to FIG. 6 , a control block diagram of a harmonic-suppressing three-phase AC/DC power converter in accordance with a third embodiment of the present invention is illustrated. The three-phase AC/DC power converter in accordance with the preferred embodiment has similar configuration and similar as that of the conventional three-phase AC/DC power converter, as shown in FIG. 3 , and detailed descriptions may be omitted. In the third embodiment, the control circuitry of the three-phase AC/DC power converter includes a voltage-regulation circuit, a current-detecting circuit, a multiplier circuit and a pulse-width-modulation/driving circuit.
Still referring to FIG. 6 , the voltage-regulation circuit includes a voltage detector 70 , a first subtracter 71 , a controller 72 and a second subtracter 73 ; the current-detecting circuit includes a first current detector 74 a and a second current detector 74 b ; the multiplier circuit includes a first multiplier 75 a and a second multiplier 75 b ; and the pulse-width-modulation/driving circuit includes an inverting adder 76 , a three-phase pulse-width-modulation circuit 77 and a driving circuit 78 .
Referring back to FIGS. 3 and 6 , the voltage detector 70 detects an output DC voltage of the three-phase AC/DC power converter, and then sends to the first subtracter 71 which subtracts the detected output DC voltage from a first predetermined value. Subsequently, the result is sent to the controller 72 to obtain an output, and the output of controller 72 is sent to the second subtracter 73 which subtracts the output of the controller 72 from a second predetermined value. Accordingly, the second subtracter 73 can generate a control signal V R which provides a value acting as a virtual resistor for the three-phase AC/DC power converter. Preferably, the first predetermined value of the first subtracter 71 is set at an expected value of the output DC voltage, and it can be changed as the desired output DC voltage is changed. Since the three-phase AC/DC power converter acts as the virtual resistor, the three-phase AC/DC power converter can absorb lesser real power as the value of the virtual resistor is greater; namely, the resistance of the virtual resistor is inversed-proportional to conversion real power of the AC/DC power converter. Accordingly, the second subtracter 73 must subtract the output of the controller 72 from the second predetermined value. Under these conditions the second predetermined value of the second subtracter 73 equals a maximum value of the virtual resistor as well as a minimum value of the conversion power of the three-phase AC/DC power converter. Consequently, this ensures a positive value for the input real power of the three-phase AC/DC power converter.
Still referring to FIGS. 3 and 6 , the three-phase AC/DC power converter in accordance with the present invention is applied to a three-phase AC power system which supplies a three-phase current, including a first-phase input AC current, a second-phase input AC current and a third-phase input AC current. In the third embodiment, the first current detector 74 a and the second current detector 74 b are used to detect two of the three-phase input AC currents passing through the three-phase inductor set 42 of the three-phase AC/DC power converter, as shown in FIG. 3 , are detected. Subsequently, the input AC currents and the control signal V R of the second subtracter 73 are sent to the first multiplier 75 a and the second multiplier 75 b to obtain a first modulation signal and a second modulation signal respectively. The first and second modulation signals are then sent to the pulse-width-modulation/drive. Concretely, the summation of three phase AC currents is zero in the three-phase three-wire AC power system. In order to obtain a third modulation signal for a third phase of the three-phase AC/DC power converter, the first and second modulation signals are sent to the inverting adder 76 . Subsequently, the first modulation signal, the second modulation signal and the third modulation signal are sent to the three-phase pulse-width-modulation circuit 77 to obtain pulse-width-modulation signals. Typically, the three-phase pulse-width-modulation circuit 77 can select a high-frequency triangular or saw-tooth wave acting as a carrier wave. In the three-phase pulse-width-modulation circuit 77 , the modulation signals are compared with the carrier wave so as to generate high-frequency pulse-width-modulation signals. Finally, outputs of the three-phase pulse-width-modulation circuit 77 are sent to the driving circuit 78 so as to generate the driving signals for the power electronic switch set 40 of the three-phase AC/DC power converter, as shown in FIG. 3 . When the driving circuit 78 sends the driving signals to drive the power electronic switch set 40 of the three-phase AC/DC power converter, the voltages across the power electronic switch set 60 are proportional to the input AC currents. Consequently, the single-phase AC/DC power converter acts as the virtual resistor, and used to absorb real power from the AC power source and to convert it into a DC power with an adjustable output DC voltage. Furthermore, a current waveform identical with the voltage waveform of the AC power source is generated at the AC side of the three-phase AC/DC power converter so as to adjust the input AC currents to be approached to the unity power factor. Since the AC power source supply three-phase voltages with sinusoidal waveform, the input AC currents are approximated nearly as sinusoidal wave which has low harmonic distortion.
As has been discussed above, the harmonic-suppressing AC/DC power converter in accordance with the present invention can produce a voltage proportional to the input AC current. This permits the AC/DC power converter acting as a virtual resistor which can be used to absorb real power from the AC power source and to convert it into an adjustable output DC voltage of the output DC voltage to supply to a DC load. Consequently, the purposes of harmonic suppression and power factor improvement can be achieved. Conversely, the conventional control circuit must detect the output DC voltage and the input AC voltage to generate a reference signal. Subsequently, the input AC current is detected and operated in closed-loop control to obtain a sine-wave input AC current, and the input AC current is in phase with the AC voltage of the AC power source. However, the conventional control method for the AC/DC power converter must disadvantageously require detecting the output DC voltage, the input AC voltage and the input AC current. Accordingly, the control circuit can be sophisticated and cannot be normally operated due to the frequency variation of the AC power system.
The control method in accordance with the present invention permits the AC/DC power converter to detect only the input AC current and the output DC voltage for simplifying the entire structure. Additionally, the control method for the AC/DC power converter can omit to detect a voltage of an AC power source, and acts as the virtual resistor which can be normally operated under the power source with frequency variation.
Although the invention has been described in detail with reference to its presently preferred embodiment, it will be understood by one of ordinary skill in the art that various modifications can be made without departing from the spirit and the scope of the invention, as set forth in the appended claims. | A harmonic-suppressing AC/DC power converter employs a control method for permitting the AC/DC power converter only to detect an input AC current and an output DC voltage. The control method can control the AC side of the AC/DC power converter to generate a voltage which is proportional to the input AC current. Thereby, the AC/DC power converter acts as a virtual resistor having a linear resistance characteristic. Accordingly, the input AC current of the AC/DC power converter can be controlled to approximate nearly as a sinusoidal wave with the performance of high input power factor and low input harmonic current. | 7 |
FIELD OF THE INVENTION
[0001] This invention is directed towards cellulosic fibers of fabric or other fibrous substrates coated with amines.
BACKGROUND OF THE INVENTION
[0002] Fabrics composed of only natural (e.g. cotton, wool, silk) or synthetic (e.g. polyester, nylon, acrylic) fibers are often lacking in desirable attributes. It is common in the textile industry to add a small weight component of various chemicals to the fabric to impart desired properties; these treatments are commonly referred to as “finishes”. Such chemical enhancers include dyes, optical brighteners, softeners, water repellents, water/oil repellents, insect repellents, anti-microbial and/or anti-fungal treatments, anti-static finishes, and hydrophilic finishes.
[0003] Durability is simultaneously a desired property and a significant challenge for any finish. Even molecules with only slight volatility will eventually evaporate; sunlight and air will slowly degrade others. Cleaning procedures such as laundering, dry-cleaning, and shampooing are the most significant challenges to fabric finish durability. Many finishes are removed from fabrics after only a few cleanings.
[0004] Various approaches have been taken to provide durable finishes. One method is to deposit chemicals (typically polymers) that are not readily solubilized and washed away after being precipitated onto the fabric. Alternatively, the active ingredient of a finish may be embedded in a laminant film that is applied to fabric; this procedure often allows for the slow release of the active ingredient into the surrounding fabric. However, the detergents and mechanical agitation of conventional cleaning procedures often eventually remove the polymer or laminant film when it is merely deposited onto the fiber surface.
[0005] U.S. Pat. No. 6,187,856, issued to Incorvia et al, teaches the use of crosslinked resins, formed from polyamidoamines and polychlorohydrin crosslinkers, to form durable films on fabrics. The resins of this patent are claimed to give durable anti-static properties to the fabric. Durability is defined in this patent as evidence of anti-static properties after dipping treated fabric into water heated at 80° C. for two twenty-minute intervals.
[0006] Anti-microbial finishes are highly desirable for many textile applications. They may be employed on fabrics used in settings requiring antiseptic conditions, such as in hospitals. They may also be useful for fabrics worn or used in commercial food preparation, hospitality settings, and other areas where there is the significant potential of exposing people to infectious bacteria.
[0007] There are only a handful of classes of anti-microbial compounds. Durability is a significant problem for them, as most are small molecules that evaporate readily or can be washed away. Moreover, many anti-microbial compounds exhibit toxicity to humans. It would be desirable to invent a durable anti-microbial fabric finish that is innocuous to humans.
[0008] The ability to eliminate or significantly diminish malodorous axillary (body) odor and foot odor is a desirable attribute for apparel fabrics. The chemical components of axillary odor are the waste by-products of certain bacteria that live off of the secretions from human sweat glands. These species of bacteria are called lipophilic diptheroids. Some three dozen molecules with potentially offensive odors have been identified in body odor (see, Preti, G. et al, J. Chem. Ecology, 1991, 17, 1469; Preti, G. et al, J. Chem. Ecology, 1992, 18, 1039; Preti, G. et al, J. Chem. Ecology, 1996, 22, 237 ; Proc. Nat. Acad. Sci. USA, 1996, 93, 6626). All of them are organic acids and the main contributor to the odor has been identified as trans-3-methyl-2-hexenoic acid. The chemical components of foot odor have similar origin; they are waste products of the bacteria brevidium epidermis. These molecules are also organic acids, and the most significant component is isovaleric acid (see, Kanda, F. et al, Brit. J. of Dermatology, 1990, 122, 771). It would be desirable to have a durable finish that would eliminate or significantly diminish malodorous body odor on fabrics. One approach is to include a bacteriocidal finish. However, these may not kill bacteria living on the skin and so odor may still be produced. Another method is to use a finish that absorbs the malodorous organic acids responsible for axillary and foot odor so that the volatile concentrations of the offensive organic acids are below the threshold of detectability. It would be greatly desirable to be able to recharge the absorptive capacity of such a finish by standard cleaning procedures.
[0009] U.S. Pat. No. 4,244,059, issued to Pflaumer, teaches the use of an odor-absorbent compound selected from alkali metal bicarbonates, alkali metal carbonates, water-soluble polyamines derived from ethylenimine, and mixtures thereof. The compound is deposited over the surface of air-permeable fabric composed of cellulosic fibers, to adsorb acidic and basic odorous molecules which are the major components of crotch odors. The patent makes no claims as to durability, nor does it make provisions to provide for durability of the polymer to the fabric during common cleaning processes such as laundering.
[0010] International patent publication WO 97/34040, issued to Koizumi et al., teaches the use of polyamines as coatings for acrylic fibers to produce deodorizing fibers. In this patent, wet gel acrylic fibers containing acid groups are brought into contact with “an amino compound” with the stoichiometry adjusted so that there is an excess of amine groups. Electrostatic interactions between the amines and acid groups presumably are the source of durability. The fibers have been wet spun and not previously dried. After contacting the amine compound, the coated fiber is heated at between 100 and 180° C. under wet heat conditions. Fiber products constructed from these fibers are able to deodorize acidic odors.
SUMMARY OF THE INVENTION
[0011] The present invention is directed to durable finishes for cellulose-containing fibers and fibrous substrates. The active components of the finishes are hydroxyl-containing amines, and preferably trialkanol amines. When combined with a suitable crosslinker, the amines become attached to and crosslinked on the substrate fiber, and form a soft resinous coating that is durable to cleaning procedures. These polymeric finishes impart durable anti-microbial activity, renewable control of certain odors, and the capacity to bind certain materials to the fabric surface.
[0012] This invention is further directed to the cellulosic fibers; yarns; woven, knitted or nonwoven fabrics and textiles; and finished goods (all of which are encompassed herein under the term “fibrous substrates”) treated with the hydroxyl-containing amine coating of the invention.
[0013] The fibrous substrates treated with the finish described herein take on properties that are not found in the native fabric, including the ability to eliminate or greatly diminish the most offensive component of malodorous body odor, while surprisingly reducing the yellowing of the substrates experienced with prior art amine treatments. Additionally, the treated cellulosic substrates remain hydrophilic and soft.
DETAILED DESCRIPTION OF THE INVENTION
[0014] As used herein and in the appended claims, “a” and “an” mean one or more, unless otherwise indicated.
[0015] The terms “durable” and “durability” as used herein describe a finished fibrous substrate in which the desired properties imparted to the substrate by the finish are observed after multiple launderings or dry cleanings.
[0016] The “cellulose-containing” or “cellulosic” fibrous substrates to be treated according to the present invention include any cellulosic fiber and any blend of fibers that contains a cellulosic, whether as a majority or a minority component. Cellulosic-based substrates include paper, cotton, rayon and other regenerated cellulosics and cellulose-containing materials, linen, jute, ramie, industrial hemp, and the like. In a presently preferred embodiment, the cellulose-containing fiber or fibrous substrate is cotton.
[0017] The hydroxyl-containing amines for use in the invention may be primary, secondary or tertiary amines, or mixtures thereof, and may come from natural sources or from synthetic preparation. Tertiary amines are preferred because of their greatly reduced tendency to yellow compared to primary and secondary amines, which in turn exhibit reduced yellowing than that experienced with prior art amine treatments. Presently preferred embodiments of the invention include alkanol amines and preferably are selected from the tertiary amines of Formula (A):
wherein, each of R 1 , R 2 and R 3 is independently selected from lower alkyl groups, unsubstituted or substituted with one or more hydroxyl groups; and each of X 1 , X 2 and X 3 is independently —OH or —H. Only one hydroxyl group per molecule is necessary for crosslinking of the molecule to the surface of the fibrous substrate. Having two or, preferably, all of X 1 , X 2 and X 3 being hydroxyl groups, while not required, is desirable as it increases the likelihood of binding to the surface of the substrate and also allows crosslinking to other amines to improve the durability of the finish. By “lower alkyl groups” is meant alkyl groups, straight-chained or branched, having from one to eight carbon atoms.
[0018] Exemplary hydroxyl-containing amines useful in the present invention include, but are not limited to, triethanol amine; tris(hydroxymethyl)amino methane; 1-aza-3,3′-dioxabicyclo[3.3.0]octane-5-methanol; 1,3-bis[tris(hydroxymethyl)-methylamino]propane; and bis(2-hydroxyethyl)imino-tris(hydroxymethyl)methane.
[0019] The terms “crosslinkers” and “suitable crosslinkers” as used herein describes molecules that contain two or more hydroxyl-reactive functional groups that form bonds with the hydroxyl groups on the hydroxyl-containing amine and on the cellulosic fibrous substrates. The crosslinkers bind the hydroxyl-containing amines together, as well as to bind the hydroxyl-containing amines directly to the fiber surface. It is particularly desirable that the crosslinking reaction does not affect the basicity of the amines in the resulting coating. A catalyst may optionally be included to facilitate crosslinking. Hydroxyl-reactive functional groups include epoxides, halohydrins, oxiranes, carbonyl diimidazole, N,N′-disuccinimidyl carbonate or N-hydroxysuccinimidyl chloroformate, alkyl halogens, isocyanates, and N-methylol ureas. Preferred cross-linkers are diepoxides (Sigma-Aldrich corp.), N-methylol ureas, and blocked polyisocyanates such as Repearl MF (Mitsubishi Chemical Co.). Particularly preferred cross-linkers are the N-methylol ureas, such as dimethyloldihydroxyethyleneurea (DMDHEU) (PatCoRez P-53, BFGoodrich).
[0020] The finish that is applied to the fibrous substrate is a solution comprising at least a hydroxyl-containing amine, a crosslinker, and a volatile solvent. It is desirable that the amine and the crosslinker be soluble in the solvent. A particularly preferred solvent is water. The pad solution preferably contains hydroxyl-containing amine at between about 0.01% and about 75% by weight, more preferably about 0.05% and about 50% by weight, and most preferably about 0.1% and about 20% by weight. The pad solution preferably contains a crosslinker at between about 0.001% and about 40% by weight, more preferably about 0.01% and about 30% by weight, and most preferably about 0.05% and about 15% by weight. The finish solution may also include other components as described below.
[0021] The reaction of the hydroxyl-containing amine with certain crosslinker functional groups, such as halohydrins, results in the formation of mineral acids that lower the pH of the finish and may slow the rate and decrease the extent of crosslinking. To control this deleterious effect, a buffering agent may be added to the finish solution. Buffering agents are weak acids or bases that tend to hold solutions containing them within ±1 pH point of the buffering agents' pK a . One skilled in the art will appreciate that an optimal buffer solution consists of equimolar portions of the buffering agent and its corresponding conjugate acid or base, the latter often being formed by addition of a strong acid or base. Lists of buffering agents can be found in Lange's Handbook of Chemistry, 14 th edition, ed. J. A. Dean, McGraw-Hill, Inc., section 8, p.p. 103-112. If used, a buffering agent should be chosen so that the pK a of the buffer lies within the optimal pH range of the reaction. This pH range is dependent on the identities of the reactive group of the hydroxyl-containing amine and of the crosslinker. The buffer must also be chosen so as to be unreactive with the crosslinker or the hydroxyl-containing amine. The amount of buffering agent should be slightly more than equimolar to the theoretical total amount of acid generated by complete reaction of the crosslinker. The finish solution may also include other additives. For example, the finish solution may also contain a wetting agent, such as WetAid NRW (BF Goodrich Corp.), to aid the equal spread of the finish over the fibers. Additional additives can be added to the solution as needed and as known by those generally skilled in the art.
[0022] The finish can be applied to the cellulosic fibrous substrate by exposing the substrate to the finish solution by methods known in the art, such as soaking, spraying, dipping, fluid-flow, and padding. The exposed fibrous substrate is then heated to remove the volatile solvent and to speed up the reaction of the hydroxyl groups on the substrate and in the hydroxyl-containing amine with the crosslinker. Alternatively, the cellulosic fibers or yarns may be exposed to the finish solution by soaking, spraying or dipping. After the finish is cured in place, the fibers or yarns may be woven or knit into fabrics.
[0023] The finish solution may be applied to the fibrous substrate at any temperature above the freezing point and below the boiling point of the solvent. In the present embodiment, the application temperature is preferably between 5 and 90° C., more preferably between 10 and 50° C., and most preferably at room temperature. The treated fabric should be cured at a temperature high enough to induce the crosslinking reaction in a very short time, preferably less than five minutes, more preferably a minute or less. In the present embodiment, the curing temperature is preferably between 100 and 200° C., more preferably between 130 and 180° C.
[0024] The present invention is further directed to the cellulosic fibrous substrates treated with the finish described above. Substrates thus treated will possess properties not found in untreated substrates, while maintaining desirable properties such as a soft hand and hydrophilicity. These new properties include the ability to absorb malodorous organic acids via acid-base reactivity of the acids with the amine groups of the finish. The finishes of the invention are durable.
[0025] An embodiment of the present invention is the preparation of treated cellulosic fibrous substrates that absorb and deodorize organic acids, which gives such substrates the ability to eliminate or greatly diminish offensive body odor. The odor-absorbing capacity of the fabric can be recharged when necessary by conventional laundering procedures. The molecular sources of offensive body odor are primarily the waste products of a species of bacteria named lipophilic diphtheroids. This species of bacteria lives on the skin surface of humans and primarily digests the secretions of the apocrine glands. The malodorous waste products of lipophilic diphtheroids are organic acids, with the most significant component being 3-methyl-2-hexenoic acid. Volatile organic acids are commonly considered to have highly offensive odors even in extremely low concentrations.
[0026] The odor-absorptive capacity of the treated fibrous substrate stems from the basicity of the amine groups of the finish. Acids react with the free amine groups of the hydroxyl-containing amine to form non-volatile ionic complexes. The extent to which this ionic complexation occurs depends on the relative strength of the acid and base. In the case of the present invention, the reaction is biased towards formation of the ionic complex to such a degree that only between one acid molecule in ten thousand to one acid molecule in a million would be found in the non-ionized, potentially volatile form. Thus, as long as unreacted amine groups are available in the treated fabric, the concentration of volatilized organic acid around the treated fabric will be lowered to the point of being undetectable or scarcely detectable.
[0027] An advantage to the present invention over conventional odor-absorbing material such as activated carbon is the ability to recharge the odor-absorptive capacity of the fibrous substrate. As amines are weak bases, exposing the substrate to an aqueous solution with a pH at or above the pK b of the base will deprotonate most of the amine complexes and result in separation of the amine-acid complexes. The conjugate base forms of the malodorous organic acids will be washed away in the laundry liquor, leaving behind free amine groups on the fiber surface. A pH of 10 is above the pK b of most amines, and laundry detergent solutions such as Tide® typically have this pH or higher. Therefore, a conventional laundering procedure is normally sufficient to recharge the odor-absorptive capacity of the fabric.
[0028] The following examples are intended for illustrative purposes only. Those of skill in the art will recognize other embodiments, all of which are considered part of the present invention.
EXAMPLES
Example 1
[0029] Samples (16×12 inch square) of untreated cotton twill fabric were immersed in either a test solution (6.0 wt % triethanol amine, 10.0 wt % Patcorez P-53, and 0.25 wt % Wet Aid NRW in water, final pH=4.0; Sample A) or in a control solution (water only, final pH=4.0; Sample B), and padded at 30 psi. The samples were cured in a Mathis oven set at 330° F. (166° C.) overall temperature with a 310° F. (154° C.) trigger temperature for one minute. The whiteness of the resulting samples, compared to the untreated fabric, was measured using a UV-Vis integrating sphere following AATCC Test Method 110-2000. The samples were then home laundered (“HL”) using 24 g. of AATCC standard detergent in warm water on normal washer and dryer settings, after which the whiteness index was again measured. The results are shown in Table 1 below.
TABLE 1 Whiteness Index Sample 0 HL 1 HL 5 HL 10 HL 15 HL 20 HL A 71.14 67.36 75.98 76.98 77.78 76.93 B 74.43 73.98 82.13 82.65 84.08 84.40
[0030] Hydrophilicity/hydrophobicity tests were run on the samples by measuring the amount of time it takes for a drop of water to completely soak into the fabric. In all cases with both the treated and control samples, the time was less than 2 seconds.
[0031] Finally, a smell test was run by placing solutions of various concentrations (in ppm) of butyric acid on the fabric samples and recording the lowest concentration of butyric acid that is noticeable on the sample by a panel of judges. These results are presented in Table 2, below.
TABLE 2 Smell Test Results Average minimum conc. (ppm) Sample 0 HL 1 HL 5 HL 10 HL 15 HL 20 HL A — 750 750 775 850 600 B — 38 50 63 50 38 | The present invention is directed to durable finishes for cellulose-containing fibers and fibrous substrates. The active components of the finishes are hydroxyl-containing amines, and preferably trialkanol amines. When combined with a suitable crosslinker, the amines become attached to and crosslinked on the substrate fiber, and form a soft resinous coating that is durable to cleaning procedures. This polymeric coating imparts durable anti-microbial activity and renewable control of certain odors. | 3 |
BACKGROUND OF THE INVENTION
[0001] The present invention related to fuel injector devices for internal combustion engines using an alternative fuel with respect to petrol or diesel oil, such as for instance methane, LPG, hydrogen or other fuels, either in gaseous or liquid state.
[0002] In internal combustion engines using alternative fuels such as those referred to above, the fuel is introduced into the intake manifold or engine cylinders by means of injector devices. Said injector devices are currently obtained from petrol injector devices. This is because engines using alternative fuels are not so widespread yet as to justify huge investments that would be required to back up designing activities dedicated to a new type of injector device. As a consequence, injector devices used until today in methane or LPG engines are the result of a compromise and therefore do not meet in an optimal way the specific requirements related to the injection of said alternative fuels. Namely, a main requirement is to adjust the injector device to working pressures related to the use of such fuels, which are far higher than the pressure at which petrol and diesel oil injectors work. For instance, a common petrol injector device injects petrol at a pressure of about 3-4 bars, whereas working pressures of LPG and methane are certainly above 10 bars. On the other hand, an injector device for a fuel such as LPG or methane does not have to meet other requirements that are specific for petrol injection, such as the one related to the particular shape of the injected spray (spray pattern) and to its granulometry. In the case of LPG or methane injection, adulterations of petrol injector devices aiming at obtaining shape and granulometry are useless, being it sufficient to meter the correct amount of fuel during injection.
SUMMARY OF THE INVENTION
[0003] The present invention therefore aims at carrying out a fuel injector device whose characteristics are such as to make it optimal specifically for the injection of alternative fuels such as LPG or methane, which is at the same time simple and cheap.
[0004] Given this aim, the object of the invention is an injector device comprising:
a valve body, having an inlet designed to be connected to a source of pressurized fuel and an outlet designed to be connected to an engine intake, a shutter cooperating with a corresponding valve seat inside the valve body, so as to check the communication between said inlet and said outlet, elastic means holding the shutter in its closing position, a solenoid for causing a shift of the shutter towards its opening position, metering means with gauged hole for metering the amount of fuel getting out of the injector device when the shutter is open, said injector device being characterized in that said metering means with gauged hole are separated from said shutter and its valve seat.
[0011] In the injector device according to the invention there is a separation of fuel metering function, performed through said metering means with gauged hole, from sealing function, performed by the shutter in its closing condition. The main advantage of this feature is that it enables to exploit a further important contrivance, which is also an object of the invention, i.e. said metering means with gauged hole are placed upstream, referring to the fuel flow inside the device, from the aforesaid shutter and its valve seat. Thanks to this contrivance, in the device according to the invention the solenoid control of the shutter is arranged downstream from the aforesaid metering means, i.e. on the low pressure side, thus ensuring an efficient sealing action of the shutter in spite of relatively high fuel supply pressures with respect to petrol injection.
[0012] Thanks to the aforesaid characteristics, the injector device according to the invention can also be used with quite high injection pressures, for instance of about 30 bars, which advantageously enables short injection times, short response times in engine transistors, an efficient adjustment and an optimization of strategies for controlling and reducing polluting emissions.
[0013] The injector device according to the invention is also characterized by an intrinsic safety function, since in case of faulty working it is kept in closing position by supply pressure and can therefore ensure sealing also up to pressures of 200 bars.
[0014] The simpler structure of the device according to the invention with respect to a “petrol”-derived injector device also enables to reduce its size, particularly in axis direction.
[0015] As was mentioned above, solenoid arrangement on the low pressure side, where pressure is of about 1 bar, ensures sealing towards outside of the solenoid in a simple and reliable way.
[0016] According to a further preferred characteristic of the invention, the solenoid is equipped with a mobile ferromagnetic element for controlling the shutter, which element includes an anchor facing an end of the solenoid, which is attracted by said end when the solenoid is actuated. In an example of embodiment, said anchor is equipped with a pin arranged through the solenoid and pushing the shutter towards its opening position when the solenoid is actuated. In another embodiment, the anchor is connected directly to the shutter body and “pulls” it towards its opening position when the solenoid is actuated.
[0017] The metering means with gauged hole are typically made up of a disk or a bushing, with a gauged hole for metering fuel, which is fastened inside the valve body. Said mounting can be carried out in any known manner, but for sake of simplicity it can be carried out for instance by using a spring that holds the disk or bushing inside a seat obtained in the valve body.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Further characteristics and advantages of the invention will be evident from the following description with reference to the accompanying drawings, provided as mere non-limiting examples, in which:
[0019] FIG. 1 is a sectioned view of an injector device according to a first embodiment of the invention,
[0020] FIG. 2 is a perspective view of a detail of FIG. 1 ,
[0021] FIG. 3 shows a variant of the embodiment of FIG. 1 , and
[0022] FIG. 4 shows a second embodiment of the device according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0023] With reference to FIG. 1 , number 1 globally refers to a fuel injector device for an internal combustion engine, carried out according to the present invention in order to meet the specific requirements concerning the specific injection of a fuel such as for instance LPG or methane in an optimal manner. The device 1 includes a valve body 1 , which in the example shown in the figure comprises a cylindrical element 3 mounted with the interposition of a sealing gasket 5 inside a cup-shaped element 4 and placed axially between said cup-shaped element and the bottom wall 6 of a housing support 7 . The device comprises an inlet connection 8 getting out through an opening of the wall 6 , and an outlet connection 9 defined by the aforesaid cup-shaped element 4 , having a channel 9 a.
[0024] Still referring to the example shown in the figure, the inlet 8 and the outlet 9 of the device communicate one with the other through a passage including the axial channel 10 inside the connection 8 , an axial hole 11 obtained inside the element 3 , and the outlet duct defined by the connection 9 .
[0025] The communication between inlet 8 and outlet 9 is controlled by a shutter 12 shaped as a disk with peripheral notches 12 a for fluid passage ( FIG. 2 ). The shutter 12 cooperates with the valve seat comprising a ring-shaped abutting surface defined in the wall of the hole 11 of the element 3 . It is pushed against said seat by a coil spring 13 placed between the shutter 12 and a disk 14 fastened inside a corresponding seat obtained in the inner hole 11 of the element 3 . The disk 14 has a central gauged hole 15 acting as fuel meter during injection. In the example shown in the figure, said disk is held against its seat by a further ring-shaped disk 15 , which is again pressed by an inner rounded end of the tubular element making up the connection 8 . Said element is blocked in position by a threaded bushing 16 screwed into a corresponding threaded hole of the element 3 .
[0026] Number 17 refers to a solenoid for controlling the shutter 12 . Said solenoid is housed inside a ring-shaped seat obtained in the lower end (with reference to the drawing) of the element 3 and cooperates with a ferromagnetic mobile element made up of an anchor 18 , basically disk-shaped with a slightly smaller outer diameter than the inner diameter of the cup-shaped element 4 and facing the lower end of the solenoid 17 . The anchor 18 is pushed by a spring 19 towards a lower rest position, and it is attracted against the element 3 , against the action of the spring 19 , when the solenoid 17 is actuated. The anchor 18 is associated to a bar 20 arranged through the inner hole 11 of the element 3 and pushing with its upper end the shutter 12 towards an opening position against the action of the spring 13 , when the solenoid 17 is actuated.
[0027] As is evident from the previous description, in the injection device shown in FIG. 1 the fuel metering function is performed by the disk 14 with the gauged hole 15 , which is a separate element with respect to the shutter 12 , the latter performing conversely the sealing function when the valve is closed. Moreover, the solenoid 17 and the anchor 18 are placed downstream from the gauged hole 15 , with reference to fuel flow direction, i.e. on the low pressure side (for instance around 1 bar), which enables to obtain the advantages mentioned above referring to the reduction of the strength required for controlling the shutter 12 . The sealing function of the shutter can thus be ensured despite far higher working pressures than in the case of petrol injection. The aforesaid peculiar characteristics of the invention also affect a reduction of the overall size of the device, especially in axial direction. Moreover, the device has an intrinsic safety feature, since in case of faulty working sealing is ensured up to very high pressures of about 200 bars. Obviously, the possibility of working with high injection pressures, for instance in the range of 10 to 30 bars, enables to reduce injection times and therefore to reduce also response times of engine transistors with a more efficient adjustment and an optimization of strategies for controlling and reducing polluting emissions.
[0028] Still referring to FIG. 1 , it should be pointed out that when the shutter 12 is in its opening position, fuel flows through the channel 10 of the connection 8 , through the gauged hole 15 and then through the inner hole 11 of the element 3 until it reaches the outlet channel 9 a flowing through holes or passages arranged on the anchor 18 (not shown in the figure).
[0029] FIG. 3 refers to a construction variant of the injector device shown in FIG. 1 . In said figure, the same parts as those shown in FIG. 1 are referred to with the same number. Leaving aside the different structure of the valve body, as is evident from the drawings, the main difference consists in that the device of FIG. 3 is equipped with a sphere shutter cooperating with a conical valve seat 12 b . As for the rest, the embodiment of FIG. 3 resembles on a functional level the one of FIG. 1 , except for the different shape of the various elements constituting it.
[0030] Eventually, FIG. 4 shows a further embodiment in which the axis of the solenoid 17 , instead of coinciding with the common axis of inlet and outlet connections 8 , 9 , as in the case of FIGS. 1, 3 , is orthogonal to the latter. Again, in FIG. 4 the components corresponding to those shown in FIGS. 1 and 3 are referred to with the same number. As can be seen, the connections 8 , 9 are defined by elements mounted on opposite faces of the element 3 , whereas the solenoid 17 with its ends 17 a is placed inside a body 33 housed in a cylindrical seat defined by the element 3 and blocked in position by means of a further element 31 mounted onto the element 3 . A closing element 30 for the inner cavity 11 is fastened, for instance screwed, onto the end of the element 3 opposite the one with the element 31 . Said cavity is in direct communication with the channel 10 of the inlet connection 8 and faces a bushing 14 with the gauged metering hole 15 , which bushing is held in position by a spring 34 placed between the bushing 14 and the closing element 30 . The gauged hole 15 ends above into a broadened cavity of the bushing 14 , which acts as seat for the shutter 12 , basically spherical and connected directly to the anchor 18 . The latter is controlled by the solenoid 17 , which is mounted, as was already mentioned, inside the element 3 in such a position that the solenoid axis is orthogonal to the axis of the channel 10 of the inlet connection 8 , and—as shall be seen—to the axis of the channel of the outlet connection 9 . When the solenoid is actuated, it attracts the anchor 18 “pulling” the shutter 12 upwards, so as to open the communication between the cavity 11 and a hole 32 communicating with the channel 9 a of the outlet 9 , which is coaxial to the channel 10 , on the opposite side of the element 3 .
[0031] As is evident, the embodiment of FIG. 4 preserves all the advantages referred to above despite the different shape and arrangement of the elements constituting the device.
[0032] Obviously, though the basic idea of the invention remains the same, construction details and embodiments can widely vary with respect to what has been described and shown by mere way of example, however without leaving the framework of the present invention. | The invention describes an injector device specifically designed for the injection of an alternative fuel such as LPG, methane, hydrogen or others, in an internal combustion engine. In the injector device, the shutter ensuring sealing in closing condition is separated with respect to the metering means with gauged hole, which perform the function of metering fuel during injection, and it is arranged downstream from said metering means. The shutter is controlled by a solenoid, which is again arranged on the downstream side with respect to said metering means. | 5 |
TECHNICAL FIELD
[0001] The invention relates to biotechnology, especially to a method for highly expressing a recombinant protein of engineering bacteria and the use thereof.
BACKGROUND ART
[0002] In earlier studies, the inventor conducted creative experiments and invented/obtained a series of new recombinant peptides with colicin as attack point, which operationally connects a polypeptide (natural or artificial design) with identification and binding ability to target cells. For example, the new antibiotic PMC-AM1 disclosed in patent No. ZL200910092128.4, named “Novel Antibiotic Comprising an Antibody Mimetic, Its Preparation and Uses Thereof,” shows a broad-spectrum antibiotic property and has stronger antibacterial activity on Neisseria meningitidis, Multidrug - resistance Pseudomonas aeruginosa, Vancomycin - resistant Enterococcus faecalis or Methicillin - resistant Staphylococcus aureus compared to the known antibiotics. The inventor's another invention entitled “A Novel Antibiotic, Its Nucleotide Sequence, Methods of Construction and Uses Thereof,” with CN patent No. ZL200910157564.5, disclosed a series of new anti-staphylococcus antibiotics, such as PMC-SA1, PMC-SA2, PMC-SA3, PMC-SA4, PMC-SE as well as PMC-PA. In vivo and in vitro experiments, these antibiotics showed better targeting ability and stronger antibacterial activity than current antibiotics, antifungal antibiotic and chemotherapeutics drugs. Additionally compared with current antibiotics, these new antibiotics showed incomparable biological security and anti-drug-resistance characteristic.
[0003] The foresaid novel antibiotics as a whole are a kind of water-soluble proteins with 600 amino acid residues, but in which there is a hydrophobic domain with 40 amino acid residues near carboxyl terminal. Compared to preparation of other water-soluble proteins with one fold structure, there is more difficult in assembling and expressing of the novel antibiotics, which inevitably affects protein yield. It is necessary to improve current expression process to achieve high yield and priority of the novel antibiotics. It will make sense for bringing the novel antibiotics into actual clinical application and practice.
DISCLOSURE OF THE INVENTION
[0004] According to the peptide structure and characteristics of the new antibiotics disclosed in the current patent application, the present disclosure provides for a method for highly expressing recombinant protein of engineering bacteria.
[0005] In one aspect, the present disclosure provides for A method for highly expressing recombinant protein of engineering bacteria, wherein the end with hydrophilicity of the recombinant protein is colicin polypeptide and the other end with hydrophobic nature is polypeptide of target moiety which is capable of binding target, the method comprising:
[0006] (1) transfecting recombinant plasmid of expressing the recombinant protein into E. coli engineering bacteria with pET system to obtain positive monoclonal colonies,
[0007] (2) producing seed bacteria solution of the positive monoclonal colonies, and inducing protein expression and enlargement culturing of the seed bacteria solution; the supernatant of the enlargement cultured solution contains expressed recombinant protein,
[0008] (3) extracting and purifying the recombinant protein from the supernatant, wherein the E. coli engineering bacteria with pET system is E. coli B834 (DE3).
[0009] In some exemplary embodiments, the enlargement culturing medium used for said inducing enriching growth of the seed bacteria solution has water as solvent and comprises following components: NaCl 6.0-6.7 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 0.6-2.0 g/L, Na 2 HPO 4 .7H 2 O 6.8-18.3 g/L, KH 2 PO 4 3.0-4.3 g/L, NH 4 Cl 1.0-1.4 g/L, MgSO 4 0.2-0.4 g/L, CaCl 2 0.01 g/L, methionine 0-40 mg/L.
[0010] In a preferable exemplary embodiment, said enlargement culturing medium has water as solvent and comprises following components: NaCl 6.0 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 2.0 g/L, Na 2 HPO 4 .7H 2 O 6.8 g/L, KH 2 PO 4 3.0 g/L, NH 4 Cl 1.0 g/L, MgSO 4 0.2 g/L, CaCl 2 0.01 g/L, methionine 0-40 mg/L.
[0011] In some exemplary embodiments, said enlargement culturing of the seed bacteria solution comprises following steps: the seed bacteria liquid was added into a container and started growth for 2 to 3 hours at 30° C., when the OD value reached 0.4-0.6, the seed bacteria solution was conducted heat shock at 42° C. for 30 minutes, and then cooled down to 37° C. and kept growth for 1.5 to 2 hours before being collected.
[0012] In some exemplary embodiments, wherein in conducting heat shocks the IPTG with the final density 0.5 mmol/L was added into said enlargement-culturing medium.
[0013] In some exemplary embodiments, said extracting and purifying the recombinant protein from the supernatant was by CM ion exchange column, and the loading quantity of the supernatant depends on the ratio value which is 2.5 mg/ml between the weight of the recombinant protein in the supernatant and the volume of gel particles used in the CM ion exchange column
[0014] In some exemplary embodiments, the eluent solution used for said extracting and purifying in CM ion exchange column is boric acid buffer solution with 0.2 mol/L NaCl.
[0015] In most exemplary embodiments, said recombinant plasmid of expressing the recombinant protein is selected from the group consisted of pBHC-SA1, pBHC-SA2, pBHC-SA3 pBHC-SA4, pBHC-SE, pBHC-PA and pBHC-PorA1.
[0016] In a further aspect, the present disclosure provides for the applications of any foresaid methods in preparing the recombinant peptides PMC-SA1, PMC-SA2, PMC-SA3, PMC-SA4, PMC-SE, PMC-PA or PMC-AM.
[0017] In another aspect, the present disclosure provides for a medium used for E. coli engineering bacteria with pET system, the medium has water as solvent and comprises following components: NaCl 6.0-6.7 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 0.6-2.0 g/L, Na 2 HPO 4 .7H 2 O 6.8-18.3 g/L, KH 2 PO 4 3.0-4.3 g/L, NH 4 Cl 1.0-1.4 g/L, MgSO 4 0.2-0.4 g/L, CaCl 2 0.01 g/L, methionine 0-40 mg/L.
[0018] In some exemplary embodiments, said E. coli engineering bacteria with pET system is E. coli B834 (DE3), and the medium has water as solvent and comprises following components: NaCl 6.0 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 2.0 g/L, Na 2 HPO 4 .7H 2 O 6.8 g/L, KH 2 PO 4 3.0 g/L, NH 4 Cl 1.0 g/L, MgSO 4 0.2 g/L, CaCl 2 0.01 g/L, methionine 0-40 mg/L.
[0019] The pET expression system provided by Novagen Company is a common system for cloning and expressing recombinant proteins in Escherichia coli . In this invention, a series of BL-21 (DE3) cells are transected with recombinant mutated plasmid disclosed in former patents and produced a higher protein expression yield than the TG1 cells does in this invention. By experimental data, we found that B834 (DE3), which is parent strain of BL-21 (DE3), has a more ideal expression productivity than BL-21 (DE3). The experimental data showed that the B834 (DE3) has dozens time of protein expression productivity than TG1 system does.
[0020] Medium is used for providing required carbon source, nitrogen source and inorganic salts for bacterium growth and multiplication. In present a medium with capability of improving the expression productivity of target protein is provided in present invention, which has an optimum formula for engineering bacteria fermentation. In this invention, the medium, named FB-M9 compound medium has an increased carbon source and nitrogen source and MgSO4, CaCl2 as well as some special amino acids that are required in growth of engineering bacteria with pET system. The medium moderately improved engineering bacteria reproduction speed and protein expression rate. And material cost of the improved medium is relatively low, which provides larger research space and higher development value for enlargement production in the future.
[0021] According to guide of the product manual, the carrying rate of CM ion gel particles used in purification system in this invention could not reach the ideal standard described in the product manual, which limits the recovery rate of target protein. In the present invention, the recovery rate has been significantly improved by the means of reducing loading quantity of sample while moderately increasing the gel volume, etc. The result also reflected that it is necessary to find or develop a kind of ion exchange gel with more efficient for large-scale industrial production of the target protein. In addition, the recombinant protein has fewer impurities owing to eluent with optimized concentration used in the ion exchange steps of this invention.
[0022] In summary, this invention provides a variety of optional more optimized method of expressing E. coli engineering bacteria recombinant proteins by the means of choosing engineering strains, optimizing the composition of medium, improving the purification and recovery rate, etc. This also provides a possible research direction and technical route for finally finding optimal procedure of high-efficiently expressing fusion protein needed. Compared with the original expressing system disclosed in former patents, the expressing system developed by present invention has improved the expressing production of fusion protein dozens of times, and provided a beneficial basis of theory and practice for the subsequent large-scale industrial production.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] FIG. 1 shows the conductance value of eluent in the protein elution process with different volume gel column FIG. 2 a shows the elution process of protein with 150 ml CM gel column FIG. 2 b shows the elution process of protein with 600 ml CM gel column. The curve signified by two arrows in the figure represent the conductance value of the eluent. The area indicated by the arrows is a conductance peak caused by the loss of the sample PMC-SA in loading process. The area of the conductance peak caused by the loss of the sample PMC-SA reduced by 70% after increasing the volume of gel. Another curve: OD value of eluotropic protein.
[0024] FIG. 2 shows SDS-PAGE Gel electrophoresis of the PMC-S. From left to right in the order: a. Marker, 2. PMC-SA1 produced by TG1, 3. PMC-SA1 produced by BL-21, 4. PMC-SA1 produced by B834; b. Marker, 2. PMC-SA1 eluted by boric acid buffer solution with 0.1 M NaCl, 3. PMC-SA1 eluted by boric acid buffer solution with 0.2 M NaCl, 4. PMC-SA1 eluted by boric acid buffer solution with 0.3 M NaCl.
[0025] FIG. 3 . Shows the inhibition curve of the PMC-SA against MRSA (BAA42). Y-axis represents light absorption value; X-axis represents bacterial growth time. Control: control group; Amp: ampicillin sodium; OXA: oxacillin; Ia-wt: wild type colicin Ia; PMC-SA1: anti- staphylococcus aureus polypeptide; PMC-AM: anti- diplococcus meningitides polypeptide.
DETAILED DESCRIPTION OF THE INVENTION
[0026] Following examples are just used for explaining the invention rather than limiting the scope of the invention.
[0027] The experimental equipment and instruments used in present invention as follows:
[0028] 1. Bacterial Strain
[0029] E. coli TG1 engineering bacteria (AECOM, K. Jakes).
[0030] E. coli BL-21(DE3), B834(DE3), Nova Blue(DE3) and 618 engineering bacteria are all purchased from Novagen company.
[0031] Staphylococcus aureus ATCC BAA-42 is purchased from ATCC (American Type Culture Collection).
[0032] Plasmid: pBHC-SA1, pBHC-SA2, pBHC-SA3 pBHC-SA4, pBHC-SE, pBHC-PA, pBHC-PorA1. (These plasmids are recorded in patents ZL200910092128.4 and ZL200910157564.5, and preserved in the applicant's laboratory. The applicant promised to offer them to the public for necessary verification tests)
[0033] 2. Main Reagents and Medicine
[0034] Yeast powder (OXIOD LP0021), peptone (OXIOD LP0042) as well another chemical reagent are all analytical reagent;
[0035] Dialysis bag Snake Skin Dialysis Tubing (Pierce, intercept molecular weight 1×104, Lot# KD32324):
[0036] Streptomycin Sulfate for injection (NCPC)
[0037] AMP ampicillin sodium for injection (Harbin pharmaceutical)
[0038] Anion exchange column gel (Pharmacia Biotech CM Sepharose™ Fast Flow Lot No. 225016).
[0039] LB liquid medium: Sodium chloride 1 g, peptone 1 g, and yeast 0.5 g were added into a 250 ml flask with the addition of 100 ml water, dissolved and autoclaved at 120° C. for 8 min
[0040] LB solid medium:100 ml LB solid medium containing sodium chloride 0.5-1.5 g, peptone 0.5-2 g, yeast 0.3-1 g and agar 0.8-3 g. The LB solid medium is used for plate culture of single colony after strain recovery. Reagents were added into a 250 ml flask with the addition of 100 ml water, dissolved and autoclaved at 120° C. for 8 min
[0041] FB-M9 complex medium: NaCl 6.0-6.7 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 0.6-2.0 g/L, Na 2 HPO 4 0.7H2O 6.8-18.3 g/L, KH 2 PO 4 3.0-4.3 g/L, NH 4 Cl 1.0-1.4 g/L, MgSO 4 0.2-0.4 g/L, CaCl 2 0.01 g/L, methionine 0-40 mg/L.
[0042] Improved FB-M9 complex medium: NaCl 6.0 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 2.0 g/L, Na 2 HPO 4 .7H 2 O 6.8 g/L, KH 2 PO 4 3.0 g/L, NH 4 Cl 1.0 g/L, MgSO 4 0.2 g/L, CaCl 2 0.01 g/L, methionine 0-40 mg/L. The methionine is 40 mg/L in the process with E. coli B834 (DE3) as engineering bacteria.
[0043] 3. Key Instrument
[0044] Bio-Rad Protein chromatography purification system (BioLogic™ DuoFlow™ BioLogic™ Maximizer,™ BioLogic™ QuadTec™ UV-Vis Detector, BioLogic™ Econo™ Pump);
[0045] Ultrasonic Cell Disruptor (Soniprep 150), protein purification ion exchange column with 5 cm diameter (Pharmacia Biotech XK50), protein purification ion exchange column with 11 cm diameter (Shanghai Huamei);
[0046] Centrifuge (Beckman Coulter Avanti™ J-20XP, Beckman Coulter Avanti™ J-25);
[0047] Spectrophotometer (Bio-Rad SmartSpec™ Plus spectrophotometer);
[0048] Automatic fermenter (Bioengineering AG LP351-42L);
[0049] High pressure homogenizer (Italian NiroSoavi NS1001L2KSN 6564).
[0050] Statement: the biological materials adopted in this invention have been known before the application filing date and have been also preserved in this applicant's lab. The applicant promised to offer them to the public for necessary verification tests in the twenty years since application filing date.
Example 1
The Option Experiment of Engineering Bacterial Strains
[0051] Classic plasmid carried the colicin Ia and its immune protein gene (GenBank M13819) are from laboratory of Dr. Finkelstein. (Qiu, X. Q., et al. An engineered multi domain bactericidal peptide as a model for targeted antibiotics against specific bacteria. Nat Biotechnol (2003) 21:1480-1485). The classic plasmids were modified into following seven kinds of restructuring mutation plasmids in former researches: pBHC-SA1, pBHC-SA2, pBHC-SA3 pBHC-SA4, pBHC-SE, pBHC-PA, pBHC-PorA1.
[0052] Step 1. Transformation of Competent Cell
[0053] 40 μL Novagen pET system engineering bacteria BL-21(DE3), B834(DE3), Nova Blue(DE3), 618 were respectively transformed with 100 ng recombinant mutant plasmids pBHC-SA1, and then ice-incubated for 5 minutes, heat-shocked at 42° C. for 30 seconds, kept in ice for 2 minutes, added with 160 μl SOC medium and shake-cultivated at 220 rpm, 37° C. for 1 hour and then coated (LB medium with 1% agar and 50 ug/ml ampicillin, and cultured overnight at 37° C.). Single colonies are picked out and cultivated to obtain the seed strain, which is conserved at a low temperature.
[0054] Step 2: Strain Recovery
[0055] 1. Preparing Recovered Bacteria Solution
[0056] The conserved strain was thawed at 4° C.; 1.5 ml of the strain is transferred into 10 ml LB medium (containing 50 μg/ml of AMP) and cultivated at 220 rpm, 37° C. for 5-8 hours.
[0057] 2. Inoculation of Single Colony
[0058] The recovered bacteria solution was diluted 10 4 or 10 5 times; and 10 ul of the diluted bacteria solution was transferred on to LB solid medium plate (containing 50 μg/ml of AMP) and coated on the plate. The plate was placed in a humid box and cultivated in incubator at 37° C. for 10-12 hours till round single colonies have grown out on the surface of the medium.
[0059] Step 3. Enlargement Culturing the Single Colonies
[0060] (1) Single colonies with regular round shape and smooth edge were picked up from the plate and respectively added into 1.5 ml LB medium, and cultivated at 220 rpm, 37° C. for 5-8 hours.
[0061] (2) Each 1.5 ml LB bacteria solution was transferred into a 100 ml LB medium, and cultivated at 220 rpm, 37° C. for 5-8 hours.
[0062] (3) Primary stage of enlargement culturing: the 100 ml of bacteria solution from the last step was added into 700 ml of improved FB-M9 complex medium and cultivated at 220 rpm, 37° C. for 5-8 hours.
[0063] (4) Secondary stage of enlargement culturing: 700 ml of bacteria solution from the primary stage is added into 6×700 ml of the improved FB-M9 complex medium and cultivated at 220 rpm, 37° C. for 5-8 hours.
[0064] (5) Third stage of enlargement culturing: 6×700 ml of bacteria solution from the secondary stage was added into 20 L of the improved FB-M9 complex medium and cultivated in a fermenter with stiffing rate of 220 rpm and maximum oxygen flow volume, 37° C. for 3-5 hours.
[0065] (6) Fermentation of engineered bacteria and induced expression of protein: 20 L of bacteria solution from the third stage of enlargement culturing was added into 200 L of improved FB-M9 complex medium and cultivated in a fermenter for induced expression of protein with stiffing rate of 220 rpm and maximum oxygen flow volume, at 30° C. for 2-4 hours; 42° C. for 0.5 hours; and 37° C. for 1-2 hours, note that IPTG is added at 42° C. with a final concentration of 0.5 mM.
[0066] Step 4. Collecting Bacteria by Centrifugation
[0067] 6000 g fermentation liquor obtained from step 3 was centrifuged at 4° C. for 20 min. The precipitate was collected and added into 50 mM boric acid buffer (pH 9.0) for resuspend of the bacteria. Note: the boric acid buffer has 2 mM PMSF (phenylmethylsulfonyl fluoride serine protease inhibitor). All consequent steps after bacteria resuspend was conducted at 4° C.
[0068] Step 5. Cells Fragmentation
[0069] After suspension in pH 9.0 boric acid buffer completely, the bacteria cells was fragmented by a High Pressure Homogenizer at 500-600 bar for 7 times, with intervals of 3-5 minutes.
[0070] Step 6. Precipitation of the Bacteria DNA
[0071] The fragmented bacteria solution was centrifuged at 55000 g, 4° C. for 40 min. The supernatant was added with streptomycin sulfate (16 bottles of 1 million unit streptomycin sulfate were added into every 200 ml liquid supernatant), and stirred for 1 h with a magnetic stirrer.
[0072] Step 7. Dialysis
[0073] The bacteria solution from the step 6 was centrifuged at 55000 g, 4° C. for 20 min. The supernatant was placed into a dialysis bag and dialyzed for 8-12 hours in boric acid buffer, which was changed once every 4 hours.
[0074] Step 8. Purifying the Protein Medicine and Obtaining Antibacterial-Engineered Polypeptide
[0075] The dialyzed bacteria solution was centrifuged at 55000 g, 4° C. for 20 min. The supernatant was measured the protein concentration in unit volume and placed into a Bunsen beaker for conducting protein purification by ion exchange method. The supernatant with known protein concentration was uploaded onto a CM ion exchange column. The sample loading and its ratio with the CM iron gel particular are according to the Product Manuals of CM ion exchange column. After being washed completely the CM ion exchange column was eluted with 50 mM boric acid buffer containing 0.3 M NaCl to obtain the novel antibacterial-engineered polypeptide.
[0076] The results are shown as Table 1, the expressing efficiency of PMC-SA by E. coli B834 (DE3) is the highest.
[0000]
TABLE 1
Expressing efficiency of different bacterial strain
Engineering strain
TG1
BL-21
618
NavaBlue
B834
Average unit production (mg/L)
0.8
10
5.8
8.1
24.4
(Average unit production = Gross production of extracted PMC-SA1/volume of bacterial liquid)
[0077] The same operation was conducted on the other six restructuring mutation plasmids, the results appeared similar trend as the result listed in Table 1, namely, in contrast to other engineering bacteria, E. coli B834 (DE3) showed the highest expressing efficiency on all seven restructuring mutation plasmids.
[0078] The operation of heat shock as following adopted to inducing expression of protein in this embodiment was different from that in prior arts: After transferring the seed bacteria liquid into the tank, cultured the bacteria at an initial temperature 30° C. for 2 hours, when OD value had reached 0.4-0.6, conducted the heat shock at 42° C. for 30 minutes, then when the temperature low down to 37° C., cultured the bacteria again for 1.5 to 2 hours again. At this stage the OD value of bacteria liquid can reach to 1-3 or even more, and can be conducted collection. During this process, 0.5 mM IPTG was added to induce expression of pET engineering bacteria.
[0079] Before proposing present method, the usual process for preparing the recombinant peptides was as following:
[0080] 100 ng of the mutant plasmids was ice-incubated with 40 μl competent cell of BL-21 engineered bacteria for 5 minutes, heat-shocked at 42° C. for 30 seconds, ice-incubated for 2 minutes, added with 160 μl of SOC medium, shake-cultivated at 220 rpm, 37° C. for 1 hour and then coated plate (LB medium with 1% agar and 50 μg/ml ampicillin, and cultured overnight at 37° C.). Single colonies were picked out for enlargement culturing.
[0081] Enlargement culturing: 8-10 L FB medium, 250 rpm, at 37° C. for 3-4 hours; was added with IPTG, 250 rpm, at 28° C. grew for 4 hours again; conducted centrifugation to precipitate bacteria at 4° C., 6000 g, 20 minutes. The precipitated bacteria was added with 80-100 ml 50 mM boric acid buffer (pH 9.0, 2 mM EDTA) kept at 4° C. to suspend, then added with 50 μg PMSF and broken by ultra sonication (4° C., 400 w, 1 minutes, repeat 4 to 5 times with intermittent 2-3 minutes for keeping the temperature of the liquid). Then the broken bacteria was conducted high-speed centrifugation (4° C., 75000 g, 90 minutes), the supernatant was added with 5 million units streptomycin sulfate to precipitate DNA (4° C. stirred for 1 hour), and 10000 g, 4° C., for 10 minutes centrifugation. The supernatant was put into dialysis bag with the molecular weight 15000 on 4° C., and dialyzed by 10 L 50 mM boric acid buffer overnight, then conducted centrifugation at 4° C., 10000 g, for 10 minutes once again. The supernatant was loaded on CM ion exchange column, after being flushed completely, eluted by 0.3 M NaCl+50 mM boric acid buffer, the new antibiotics can be obtained.
Example 2
Improving Medium
[0082] The classic FB medium for colicin Ia preparation (Qiu, X. Q., et al., “An engineered multi domain bactericidal peptide as a model for targeted antibiotics against specific bacteria,” Nat Biotechnol (2003) 21:1480-1485; Jakes, K., et al., “Alteration of the pH-dependent Ion Selectivity of the Colicin E1 Channel by Site-directed Mutagenesis,” JBC (1990) 265:6984-6991) has components as follows: peptone 25.0 g/L, yeast powder 7.5 g/L, NaCl 6.0 g/L and glucose 1.0 g/L.
[0083] In this invention, we adopted FB medium without glucose, the components of which as follows: peptone 25.0 g/L, yeast powder 7.5 g/L and NaCl 6.0 g/L. And the FB medium without glucose was configured with M9 medium at a special volume proportion to obtain the FB-M9 compound medium.
[0084] The mother liquor of M9 medium is 5×M9 and has components as follows: Na 2 HPO 4 .7H 2 O 64.0 g/L, KH 2 PO 4 15.0 g/L, NH 4 Cl 5.0 g/L, NaCl 2.5 g/L, MgSO 4 1.5 g/L, CaCl 2 0.05 g/L, and 2% glucose.
[0085] A preliminary attempt of the compound medium:
[0086] FB-M9: volume ratio between FB:M9 was 7:10, the components as follows: NaCl 6.7 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, Na 2 HPO 4 .7H 2 O 18.3 g/L, KH 2 PO 4 4.3 g/L, NH 4 Cl 1.4 g/L, MgSO 4 0.4 g/L, CaCl 2 0.01 g/L and glucose 0.6 g/L.
[0087] This invention adopted this formula for bacteria fermentation. The process was as step 3 in Example 1. The result shows in Table 2, wet bacteria weight got from per liter culture solution is significantly higher than that done through FB medium. The collected protein production is significantly improved with average production up to 30 mg/L.
[0000]
TABLE 2
Contrast of target protein production from test medium
(PMC-SA1/BL-21 engineering bacteria)
Fermenting in BF medium
Fermenting in FB-M9 (7:10) medium
Bacterial
Protein
Bacterial
Protein
weight
contents
weight
contents
(g)
(mg)
(g)
(mg)
1
255.07
280.8
349.82
847.82
2
246.3
519.94
343.47
643.71
3
302.28
461.965
366
779.3
4
276.67
465.179
388.44
946.34
AVG
270.8
431.971
361.9325
804.2925
[0088] The final improved FB-M9 medium was obtained by further researches and repeated comparison in this invention. The production rate of the target protein can reach 34 mg/L as Table 3 shows, in the same fermentation conditions as Example 1.
[0089] The components of the improved FB-M9 medium as follows: NaCl 6.0 g/L, peptone 25.0 g/L, yeast powder 7.5 g/L, glucose 2.0 g/L, Na 2 HPO 4 .7H 2 O 6.8 g/L, KH 2 PO 4 3.0 g/L, NH 4 Cl 1.0 g/L, MgSO 4 0.2 g/L and CaCl 2 0.01 g/L. As the methionine was required in the growth of B834 engineering bacterium, in the process of B834 as engineering bacteria the methionine (40 mg/L) is added into the final improved FB-M9 medium.
[0000]
TABLE 3
Comparison of improved FB-M9 medium with other medium on
productivity
BL-21
B834
Engineering strains and
the medium
FB-M9
Improved
FB-M9
Improved
FB
(7:10)
FB-M9
FB
(7:10)
FB-M9
Average unit
10
24
25
22.3
30
34
production
(mg/L)
Example 3
Optimizing Conditions for Purifying Protein
[0090] The basic structure of recombinant polypeptide (PMC-SA1, PMC-SA2, PMC-SA3, PMC-SA4, PMC-SE, PMC-PA, PMC-AM) prepared in this invention is Colicin Ia. The isoelectric point of colicin Ia is about 9.15, therefore the classic purification adopted is Ion Exchange Chromatography (Qiu, X. Q., et al., “An Engineered Multidomain Bactericidal Peptide as a Model for Targeted Antibiotics Against Specific Bacteria,” Nat Biotechnol (2003) 21:1480-1485).
[0091] The principle is: In pH 9.0 boric acid buffer system, the majority of PMC-SA molecules exist as positive charge ions. When the CM gel particles with negative charge go through the chromatographic column, the recombinant protein molecules with positive charge was hung on the CM gel particles due to the electric charges attraction, while the other miscellaneous protein was rushed out of the gel column
[0092] In this example, the other steps were as that in Example 1, but after the miscellaneous protein was rushed out completely, using boric acid buffer of 0.1 to 0.3 M NaCl gradiently to elute the gel column
[0093] Owning to Na + ions having stronger positive property than the recombinant protein molecules, the recombinant protein was replaced from CM gel particles by Na + ion. There are two variables to be manipulated in the process of ion exchange and purification for a better protein yield: (1) NaCl with different concentration within 0.05-1 M can be chosen respectively to elute protein molecules with different positive charge mounted on CM gel particles. (2) The amount of CM gel particles adopted can be optimized: In the environment with certain ionic strength, the amount of protein carried by every CM gel particles is relatively constant. The volume of gel column is indispensable to be enlarged in order to increase the amount of protein carried by gel column
[0094] CM Sepharose™ Fast Flow is anion exchange column gel produced by GE company. According to the manual, every 100 ml gel can combine with 9 mM cation. The actual usable combination capacity varies with the nature of sample in the process of dynamic combination, and molecular weight is inversely proportional with combined capacity. Its standard sample that has equivalent molecular weight with the recombinant peptides manufactured in this invention is Bovine COHb-(Mr69 kD), which has theoretically dynamic combined capacity 30 mg/ml. Namely, with 100 ml CM Sepharose™ Fast Flow glue to retrieve recombinant protein molecules, the theoretically highest recovery rate is about 300 mg (0.004 mM). But according to its manual operation, the actual dynamic combination capacity of recombinant protein molecules to CM gel particles reached only 3 mg/ml, just reached 10% of theoretical combined capacity.
[0095] In the experiment, we found that in the latter half process of washing out the miscellaneous protein, conductance curve will raise a small peak (as shown in FIG. 1 a ). According to this phenomenon, we speculate that when there is a large amount of recombinant protein in the sample, due to the limited capacity of CM gel particles with target protein, only a little part of the recombinant protein molecules can be recovered. The recombinant protein without being mounted on the CM gel particles has to be flushed out gel column together with miscellaneous protein. As the recombinant protein is positively charged, a short rising peak appears in the conductance curve.
[0096] In an optimized example of this invention: in order to reduce the loss of recombinant proteins, we reduced loading amount of sample to ⅓ of the manual regulation, and increased the volume of gel from 150 ml to 600 ml, namely the protein amount in the supernatant fluid: gel particle volume=2.5 mg/ml. The loss of the recombinant protein decreased in the process of elution. The experimental data showed that the recovery rate of recombinant proteins was increased 3.5 times; the results shown in FIG. 1 b.
[0097] In addition, we set the gradient concentration of NaCl as 0.1 M-0.2 M-0.3 M in the boric acid buffer used in elution, and 0.2 M showed the highest eluting efficiency and protein purity, as shown in FIG. 2 b.
Example 4
Detecting Protein Purity and Activity
[0098] Step 1. SDS-PAGE Electrophoresis
[0099] The fusion protein samples obtained by optimized conditions of example 4 were conducted SDS-PAGE electrophoresis and silver nitrate dyeing. As shown in FIG. 2 , there is a clear protein-imprinting stripe at the point of about 70 kD relative molecular weight, namely PMC-SA1 manufactured in this invention in the electrophoresis map a the map b shows the protein has eliminated mixed zone through the improved gradient elution in Example 4 and the purity is improved. The rest six kinds of recombinant proteins manufactured through the optimized method of this invention have also showed similar improved purification.
[0100] Step 2. Detecting the Antibacterial Activity
[0101] With the recombinant protein PMC-SA1 and PMC-AM that produced by the improved manufacturing method in the Examples 1, 2, 3, we conduct the following antibacterial activity test.
[0102] The Methicillin-resistant staphylococcus aureus (MRSA, ATCC BAA-42) bacteria liquid 10 μl (10 5 CFU/ml) was inoculate into 10 ml BM medium and added with antimicrobial agents. According to the antimicrobial agents we set six parallel groups: ampicillin sodium 2 μg/ml, oxazocilline 4 μg/ml, wild type colicin Ia, PMC-SA and Ph-NM (4 μg/ml), and blank control group. Culturing at 37° C., 210 rpm, and testing optical density value per hour (595 nm), drawing the bacteriostasis curve, as shown in FIG. 3 .
[0103] The bacteriostatic curve shows that the recombinant proteins produced by improved methods of this invention have good antibacterial activity. | Provided are methods for highly expressing recombinant protein of engineering bacteria and the use thereof. The method comprises the following steps: (1) engineering bacteria of Escherichia coli with pET system are transfected with recombinant mutated plasmid to obtain positive monoclonal colonies; (2) the positive monoclonal colonies are enriched to obtain a seed bacteria solution, and the seed bacteria solution is induced to enrichment and growth in a large amount; and (3) the bacteria supernatant containing the recombinant protein as the expression target is separated, and then the recombinant protein in the bacteria supernatant is extracted and purified. The method is characterized in that the engineering bacteria of Escherichia coli with pET system are E. coli B834 (DE3). The components of the mass enrichment medium and the protein purification steps are also optimized such that a significant improvement in the yield and purity of the protein is achieved and the method is suitable for applying to the large-scale production of recombinant protein expressed by the engineering bacteria of Escherichia coli. | 2 |
BACKGROUND OF THE INVENTION
The present invention relates to a hydraulic system and more particularly relates to hydraulic systems including one or more variable displacement pumps having their displacements controlled automatically in response to the requirement of various hydraulic functions as indicated by power beyond flow emanating from control valves for the various functions.
Power beyond is a typical option available on most valves used in open center or constant flow hydraulic systems. With a plurality of control valves connected in series, this option gives the first control valve priority on the hydraulic flow available and when the flow is not used it is directed out the power beyond port to the next valve rather than back to the hydraulic reservoir as is done with conventional open center valves.
The most common open center power beyond valves use open center spools for function control. The spools are moved to restrict the flow through the open center passage causing a pressure increase to the load pressure. The flow is divided between the open center passage and the work ports with the open center flow being directed out the power beyond port and the returning load flow being directed back to sump. Dividing flow in this manner makes it difficult for an operator to control the speed of a function since fluctuations in function load must be compensated for by spool movement.
This problem of control is somewhat alleviated by a more specialized type of open center, power beyond valve which incorporates a pressure compensated flow control valve which operates to divide flow in response to the demand for fluid of a function controlled by the valve. Flow is related to spool movement with the flow being maintained constant for varying function loads and also being limited to a predetermined rate. Examples of pressure compensated, open center, power beyond valves are found in U.S. Pat. No. 3,455,210 issued to Allen on July 15, 1969; U.S. Pat. No. 3,465,519 issued to McAlvay et al on Sept. 9, 1969; and U.S. Pat. No. 3,718,159 issued to Tennis on Feb. 27, 1973.
For the sake of efficiency, systems employing open center valves use variable displacement pumps which are automatically controlled in some way to meet the instantaneous demand of the systems. One example of a system employing a variable displacement pump controlled in this manner is disclosed in the aforementioned McAlvay et al patent. Specifically, McAlvay et al disclose a system employing a single variable displacement pump, a multiplicity of functions and control valves therefore with the power beyond flow from the last control valve being coupled to a pressure responsive displacement controller for decreasing the output of the pump in response to increasing power beyond flow.
The McAlvay et al system suffers from the disadvantage that it does not make provision for having functions of equal priority connected in parallel to a common source of fluid pressure or for situations where a second pump is needed for supplying the maximum possible demand that the functions might have for fluid.
SUMMARY OF THE INVENTON
According to the present invention there is provided a novel hydraulic system incorporating control valves of the pressure compensated, power beyond type and a pair of variable displacement controllers associated therewith and controlled by certain power beyond pressures.
It is an object to provide a hydraulic system wherein a displacement controller for a variable displacement pump is subject to the lesser of power beyond pressure emanating from the power beyond ports of a pair of control valves for selectively controlling a pair of parallel-connected functions.
Another object of the invention is to provide a hydraulic system including first and second variable displacement pumps each having their displacements controlled in accordance with the lesser of the power beyond pressure emanating from respective control valves receiving fluid from the pumps, the hydraulic system further including a fluid transfer conduit for permitting flow from the power beyond port of the first pump to be added to the flow from the second pump when the pressure of the power beyond flow of the control valve(s) supplied by the first pump is greater than the pressure of the power beyond flow of the control valve(s) supplied by the second pump.
These and other objects of the invention will become apparent from a reading of the ensuing description together with the appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The sole FIGURE is a schematic representation of a hydraulic control system for an excavator.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawing, therein is shown an excavator hydraulic control system indicated in its entirety by the reference numeral 10. The hydraulic control system 10 incorporates various control valves of the pressure compensated, power beyond type and preferably these valves are of a construction similar to that of the valve disclosed in the aforementioned U.S. Pat. No. 3,718,159 except that some of the control valves include only one function control section stacked together with an inlet section as compared to the patented structure which discloses three function control sections stacked together with an inlet section.
Specifically, the control system 10 includes a hoe control valve 12, a house swing control valve 14 and right and left travel control valves 16 and 18, respectively, which are all shown here in block form for simplicity.
The hoe control valve 12 comprises an inlet section 20 stacked together with boom, arm and bucket control sections 22, 24 and 26, respectively. The inlet section 20 includes an inlet port 28 and a power beyond port 30 and embodies a pressure compensated flow control valve (not shown) which divides the flow entering the inlet between the power beyond port and a passage leading to the function control sections in accordance with the location of respective control valve spools located in the sections and the demand of a function being controlled. The boom, arm and bucket control sections have pairs of service passages 32, 34 and 36, respectively with each of the pairs being adapted for connection to opposite ends of double-acting hydraulic cylinders.
The house swing control valve 14 includes an inlet section 38 stacked together with a swing control section 40. The inlet section 38 is similar to the inlet section 20 of the valve 12 described above and includes an inlet port 42 and a power beyond port 44. The swing control section 40 includes a pair of service ports 45 adapted for connection to opposite ports of a reversible swing motor.
The right and left travel control valves 16 and 18 are identical and include respective inlet sections 46 and 48 and respective travel control sections 50 and 52. The inlet sections 46 and 48 include inlet ports 54 and 56, respectively, and power beyond ports 58 and 60, respectively. The travel control sections 50 and 52 include pairs of service ports 62 and 64, respectively, adapted for connection to opposite ports of reversible right and left traction drive motors.
Provided for supplying fluid to the control valves are first and second variable displacement hydraulic pumps 66 and 68, respectively, having pressure responsive displacement controllers 70 and 72 associated therewith and operative to increase the displacements of the pumps 66 and 68 in response to receipt of respective decreased pressure signals.
The pump 66 has an inlet connected to a sump 74 and an outlet connected to the inlet port 28 of the inlet section 20 of the hoe control valve 12 by a fluid supply conduit 76. A first power beyond fluid conduit 78 has a first end connected to the power beyond port 30 of the inlet section 20 and a branched second end connected to the inlet ports 54 and 56 of the travel control valves 16 and 18. Second and third power beyond fluid conduits 80 and 82, respectively, connect the power beyond ports 58 and 60 of the control valves 16 and 18 to first and second inlet ports 84 and 86, respectively of a shuttle valve 88. The shuttle valve 88 includes an outlet port 90 connected to the inlet ports 84 and 86 by a central passage 92. First and second check balls 94 and 96 are located in the passage 92 on opposite sides of the connection of the latter with the outlet port 90 and are respectively located for engagement with first and second valve seats 98 and 100, respectively, for preventing flow from the inlet ports 84 and 86 to the outlet port 90. A pin represented schematically at 102 is reciprocably mounted in the passage 92 between the check balls 94 and 96 and is of a length greater than the distance between the valve seats 98 and 100 so that only one of the check balls may be seated at one time (see FIG. 3 of U.S. Pat. No. 3,863,449 granted Feb. 4, 1975 for a shuttle valve of this type). Thus, it will be appreciated that the greater of the pressures in the power beyond conduits 80 and 82 will act on the shuttle valve 88 to seat one of the check balls 94 and 96 and unseat the other so that the lesser of the pressures in the conduits 80 and 82 is communicated to the outlet port 90.
The outlet port 90 of the shuttle valve 88 is connected, as by a pilot fluid conduit 104, to the displacement controller 70 of the pump 66.
The pump 68 has an inlet connected to the sump 74 and an outlet connected to the inlet port 42 of the swing control valve 14 by a fluid supply conduit 106. A fourth power beyond fluid conduit 108 connects the power beyond port 44 to a first inlet port 110 of a shuttle valve 112 having a construction identical to the aforedescribed shuttle valve 88. The valve 112 includes a second inlet port 114 connected to the pilot fluid conduit 104 and an outlet port 116 connected to the displacement controller 72 of the pump 68 by a pilot fluid conduit 118. A central passage 120 interconnects the ports 110, 114 and 116 and provided for controlling the flow of fluid from the inlet ports 110 and 114 to the outlet port 116 are first and second check balls 122 and 124, respectively, positioned for seating against first and second valve seats 126 and 128. A pin shown diagrammatically at 130 is reciprocably mounted in the passage 120 between the check balls 122 and 124 and is of a length sufficient to prevent simultaneous seating of the check balls. Thus, it will be appreciated then that the shuttle valve 112 will act to connect the lesser of the two fluid pressures respectively existing in the pilot fluid conduit 104 and the fourth power beyond fluid conduit 108 to the pilot fluid conduit 118 and, hence, to the displacement controller 72 of the pump 68.
A bypass circuit including a bypass conduit 132 is connected between the fourth power beyond fluid conduit 108 and the fluid supply conduit 76. Located in the bypass conduit 132 is a one-way valve 134 which permits flow only in the direction from the conduit 108 to the conduit 76. Accordingly, when the pressure in the conduit 108 is greater than that in the pilot fluid conduit 104, the shuttle valve 112 will act to prevent flow from the conduit 108 to the pilot fluid conduit 118 and the pressure in the conduit 108 will open the valve 134 to thereby connect the power beyond conduit 108 to the fluid supply conduit 76 thus resulting in the flow from the pump 68 supplementing that from the pump 66.
In order that the displacement of the pump 66 may more quickly be adjusted to accommodate changes in the demands of the hoe functions served by the valve 12, a pair of lead compensators 136 and 138 are connected in the circuitry leading to and from the hoe control valve 12. Specifically, the lead compensators 136 and 138 respectively comprise stepped cylindrical chambers 140 and 142. The chamber 140 has a small end connected to the fluid supply conduit 76 by a conduit 144 while the chamber 142 has a small end connected, as at 146, to the first power beyond fluid conduit 78. The chambers 140 and 142 have respective large ends connected to each other and to the pilot fluid conduit 104 by a branched conduit 148. Respectively reciprocably mounted in the small and large sections of the chamber 140 are small and large pistons 150 and 152, which are interconnected by a rod 154. A pair of centering springs 156 and 158 are located on opposite sides of the large piston 152 and bias it toward a centered position in the large section of the chamber 140. Similarly, the chamber 142 has small and large pistons 160 and 162, respectively, reciprocably mounted therein and interconnected by a rod 164. A pair of centering springs 166 and 168 are located on opposite sides of the large piston 162.
It will thus be appreciated that when there is a sudden high demand for flow for operation of the hoe function controlled by the hoe control valve 12, the power beyond flow in the power beyond fluid conduit 78 will diminish so as to reduce the pressure acting against the small piston 160 of lead compensator 138. The piston 160 will then be shifted leftwardly by unbalanced forces resulting in an increased volume in the end of large section of the chamber 142 which in turn results in a decrease in the pressure in the branched conduit 148 and, hence, a decrease of pressure in the pilot fluid line 104. The displacement controller 70 of the pump 66 will respond to this decrease in pressure and increase the displacement of the pump 66. The increased flow from the pump 66 will initially effect increased pressure against the small piston 150 of the lead compensator 136 so as to create a force imbalance causing the piston to shift leftwardly to cause the large piston 152 to force fluid from the large end of the chamber 140. By this time, the initial drop in fluid pressure in the power beyond fluid conduit 78 will probably have found its way through the circuit so as to appear in the pilot pressure fluid line 104 so any increase in the pressure in the line 104 occasioned by the leftward shift of the piston 152 will be overshadowed by the decrease in pressure and the displacement of the pump 66 will be increased in accordance with any net decrease in pressure in the line 104.
Also connected to the branched conduit 148 is an outlet port 170 of a solenoid operated power limiting valve 172 having an inlet port 174 connected to the fluid supply conduit 76 by a section of the bypass conduit 132 downstream of the one-way valve 134. The power limiting valve 172 is shown in a normally deenergized position wherein it blocks fluid communication between the conduit 132 and the pilot fluid conduit 104. Actuation of the power limiting valve 172 is preferrably made in response to the output speed of the excavator engine falling to a preselected minimum. Any well known speed sensing circuit may be utilized for sensing the output speed of the engine and energizing the solenoid of the valve 172 at the preselected minimum speed. When the valve 172 is energized, it will shift to connect the conduit 132 and hence the output of the pump 66 and any flow passing through the one-way valve 134 to the pilot fluid conduit 104 to thereby increase the pressure in the controller 70 to decrease the displacement of the pump 66 which will in turn relieve some of the load on the engine so as to prevent the latter from stalling.
The operation of the hydraulic control system 10 is briefly stated as follows. During operation of the excavator, the control valves 12, 14, 16 and 18 will operate to divide available flow between any actuated function and the power beyond port of the valve. For example, the portion of the flow arriving at the hoe function control valve 12 which is not needed for function operation will be passed on to the left and right travel function control valves 16 and 18 via the power beyond fluid conduit 78. That portion of the flow arriving at the travel function control valves 16 and 18 which is not used for operating the travel functions is respectively passed on to the power beyond fluid conduits 80 and 82. The shuttle valve 88 will then operate in response to the greater of the fluid pressures existing in the conduits 80 and 82 to connect the losses of the fluid pressures existing in the conduits 80 and 82 to the pilot fluid conduit 104 and, hence, to the displacement controller 70 of the pump 66. The controller 70 operates in response to the pressure in the fluid conduit 104 to establish a displacement calculated to result in only slightly more fluid being pumped by the pump 66 than is needed to operate the hoe and/or travel functions being actuated.
Meanwhile, that portion of the flow arriving at the swing function control valve 14 which is not needed for operating the swing function is passed on to the power beyond fluid conduit 108. The shuttle valve 112 operates in response to the pressure of the fluid in the pilot fluid conduit 104 and the pressure of the fluid in the power beyond fluid conduit 108 to connect the lesser of the two pressures to the pilot fluid conduit 118 and, hence, to the displacement controller 72 of the pump 68. If the pressure in the conduit 108 is greater than the pressure in the conduit 118, the one-way valve 134 will open to join the flow from the power beyond fluid conduit 108 with the flow from the pump 66. In this way, the pump 68 may at some time operate to aid the pump 66 in supplying an unusual demand from the hoe and travel functions. This permits the pump 66 to have a smaller displacement than would otherwise be the case.
It is here noted, that for some applications the displacement of the pump 66 may be adequate under all conditions to supply the needs of the hoe and travel functions and in such an application the bypass circuit and the shuttle valve 112 could be eliminated with the power beyond fluid conduit 108 being connected directly to the displacement controller 72.
The operation of the lead compensators 136 and 138 and the power limiting valve 172 are thought to be evident from the description thereof set forth above and for the sake of brevity are not repeated here. | The displacement controllers of a first variable displacement pump supplying fluid for hoe and travel functions of an excavator and a second pump supplying fluid for the excavator house swing function are connected to shuttle valves which operate to couple to the controllers the lesser of the power beyond fluid pressures emanating from travel function and swing function control valves. A bypass circuit is arranged to couple power beyond flow from the swing function control valve to join the flow being outputed from the first pump when the pressure of the last-named power beyond flow exceeds the lesser of that emanating from the travel control functions. Lead compensators are provided to make the controllers more responsive to circuit demands and a power limiting valve is provided for automatically connecting pressure for destroking the pumps to relieve engine load when the engine speed falls to a predetermined minimum. | 4 |
BACKGROUND OF THE INVENTION
This invention relates generally to utility and hygienic paper towels and, more specifically, to the use of special emulsions as impregnating and softening compositions.
The generic term “paper” encompasses about 3000 different types and articles which can differ, sometimes considerably, in their applications and their properties. Their production involves the use of numerous additives among the most important of which are fillers (for example chalk or kaolin) and binders (for example starch). For tissues and hygienic papers, which come into relatively close contact with the human skin, there is a particular need for an agreeable soft feel which is normally given to the paper by careful selection of the fibers and, in particular, by a high percentage of fresh mechanical wood pulp or cellulose. However, in the interests of economic paper manufacture and from the ecological viewpoint, it is desirable to use large amounts of inferior-quality deinked wastepaper. Unfortunately, this means that the softness of the paper is significantly reduced which is troublesome in practice and can even lead to irritation of the skin, particularly with frequent use.
Accordingly, there has been no shortage of attempts in the past to treat tissue papers by impregnation, coating or other surface treatments in such a way that a more agreeable soft feel is achieved. International patent application WO 95/35411 (Procter & Gamble) relates to tissue papers coated with softening compositions which contain 20 to 80% by weight of a water-free emulsifier (mineral oils, fatty acid esters, fatty alcohol ethoxylates, fatty acid ethoxylates, fatty alcohols and mixtures thereof), 5 to 95% by weight of a carrier (fatty alcohols, fatty acids or fatty alcohol ethoxylates containing 12 to 22 carbon atoms in the fatty group) and 1 to 50% by weight of surfactants with an HLB value of preferably 4 to 20. The Examples mentioned in this document all contain petrolatum as emulsifier. International patent application WO 95/35412 discloses similar tissue papers where water-free mixtures of (a) mineral oils, (b) fatty alcohols or fatty acids and (c) fatty alcohol ethoxylates are used as softeners. International patent application WO 95/16824 (Procter & Gamble) describes softening compositions for tissue papers containing mineral oil, fatty alcohol ethoxylates and nonionic surfactants (sorbitan esters, glucamides). In addition, International patent application WO 97/30216 (Kaysersberg) describes softening compositions for paper handkerchiefs which contain (a) 35 to 90% by weight of long-chain fatty alcohols, (b) 1 to 50% by weight of wax esters containing 24 to 48 carbon atoms, (c) 0 to 20% by weight of nonionic emulsifiers and (d) 0 to 50% by weight of mineral oil. From the applicational standpoint, however, the softness and feel of the treated papers are still in need of improvement.
Accordingly, the problem addressed by the present invention was to provide compositions with which dry utility papers, more particularly tissue papers, and tissue cloths having a particularly agreeable soft feel and excellent skin-care properties could even be produced using raw materials comprising a high percentage of recycled paper. At the same time, only readily biodegradable auxiliaries would be used and the compositions would penetrate easily into the tissue, would be uniformly dispersed therein and, even in highly concentrated form, would have such a low viscosity that they would be easy to process.
DESCRIPTION OF THE INVENTION
The present invention relates to the use of emulsions containing
a) polyol poly-12-hydroxystearates,
b) wax esters and
c) waxes
as impregnating and softening compositions for papers, nonwovens and cloths, preferably for treating the skin.
It has surprisingly been found that compositions of the type mentioned above are capable of imparting an agreeable soft feel, even to particularly critical tissue paper comprising up to 95% by weight recycled paper and tissue cloth. The emulsions have low viscosities, even in highly concentrated form, so that they are easy to process. By virtue of their small droplet size, the emulsions penetrate very quickly into the tissues and are uniformly dispersed therein. Another advantage is that the substantially odorless compositions are ecotoxicologically safe and, in particular, are readily biodegradable.
Polyol Poly-12-Hydroxystearates
The polyol poly-12-hydroxystearates which form component (a) are known substances which are marketed by Henkel KGaA of Düsseldorf, FRG, for example under the names of “Dehymuls® PGPH” and “Eumulgin® VL 75” (mixture with Coco Glucosides in a ratio by weight of 1:1). Reference is also made in this connection to International patent application WO 95/34528 (Henkel). The polyol component of the emulsifiers may be derived from substances which contain at least 2, preferably 3 to 12 and more preferably 3 to 8 hydroxyl groups and 2 to 12 carbon atoms. Typical examples are
(a) glycerol and polyglycerol; (b) alkylene glycols such as, for example, ethylene glycol, diethylene glycol, propylene glycol; (c) methylol compounds such as, in particular, trimethylol ethane, trimethylol propane, trimethylol butane, pentaerythritol and dipentaerythritol; (d) alkyl oligoglucosides containing 1 to 22, preferably 1 to 8 and more preferably 1 to 4 carbon atoms in the alkyl group such as, for example, methyl and butyl glucoside; (e) sugar alcohols containing 5 to 12 carbon atoms such as, for example, sorbitol or mannitol, (f) sugars containing 5 to 12 carbon atoms such as, for example, glucose or sucrose; (g) amino sugars such as, for example, glucamine.
Among the emulsifiers suitable for use in accordance with the invention, reaction products based on polyglycerol are particularly important by virtue of their excellent applicational properties. It has proved to be of particular advantage to use selected polyglycerols which have the following homolog distribution (the preferred ranges are shown in brackets):
glycerol 5 to 35 (15 to 30) % by weight diglycerols 15 to 40 (20 to 32) % by weight triglycerols 10 to 35 (15 to 25) % by weight tetraglycerols 5 to 20 (8 to 15) % by weight pentaglycerols 2 to 10 (3 to 8) % by weight oligoglycerols to 100% by weight
Wax Esters
Wax esters used as component (b) are generally understood to be substances which correspond to formula (I):
R 1 COO—R 2 (1)
in which R 1 CO is a linear or branched acyl group containing 6 to 22 carbon atoms and 0 and/or 1 to 3 double bonds and R 2 is a linear or branched alkyl and/or alkenyl group containing 6 to 22 carbon atoms, with the proviso that the number of carbon atoms in the ester is at least 20. Typical examples of such substances are myristyl myristate, myristyl palmitate, myristyl stearate, myristyl isostearate, myristyl oleate, myristyl behenate, myristyl erucate, cetyl myristate, cetyl palmitate, cetyl stearate, cetyl isostearate, cetyl oleate, cetyl behenate, cetyl erucate, stearyl myristate, stearyl palmitate, stearyl stearate, stearyl isostearate, stearyl oleate, stearyl behenate, stearyl erucate, isostearyl myristate, isostearyl palmitate, isostearyl stearate, isostearyl isostearate, isostearyl oleate, isostearyl behenate, isostearyl oleate, oleyl myristate, oleyl palmitate, oleyl stearate, oleyl isostearate, oleyl oleate, oleyl behenate, oleyl erucate, behenyl myristate, behenyl palmitate, behenyl stearate, behenyl isostearate, behenyl oleate, behenyl behenate, behenyl erucate, erucyl myristate, erucyl palmitate, erucyl stearate, erucyl isostearate, erucyl oleate, erucyl behenate and erucyl erucate. Unsaturated wax esters, for example oleyl oleate and oleyl erucate, are preferably used.
Waxes
Waxes which are used as component (c) are natural or synthetic substances which are kneadable at 20° C., solid to fragile and hard, coarsely to finely crystalline, transparent to opaque, but not glass-like, melt without decomposing above 40° C. and are of comparatively low viscosity and non-stringing even just above their melting point. The waxes suitable for use in accordance with the invention differ from resins, for example, in the fact that they change into a molten low-viscosity state at temperatures of generally about 50 to 90° C., in exceptional cases even as high as 200° C., and are substantially free from ash-forming compounds. The waxes are divided into the following three groups according to their origin: natural waxes such as, for example, candelilla wax, carnauba wax, Japan wax, espartograss wax, cork wax, guaruma wax, rice oil wax, sugar cane wax, ouricury wax, montan wax, beeswax, shellac wax, spermaceti, lanolin (wool wax), uropygial fat, ceresine, ozocerite (earth wax), petrolatum, paraffin waxes and microwaxes; chemically modified waxes (hard waxes) such as, for example, montan ester waxes, sasol waxes, hydrogenated jojoba waxes and synthetic waxes such as, for example, polyalkylene waxes and polyethylene glycol waxes. In this connection, natural waxes, especially vegetable waxes, are preferred.
Tissue Papers and Tissue Cloths
Tissue papers to which the present invention relates may have a single-ply or multiple-ply structure. In general, the papers have a weight per square meter of 10 to 65 and preferably 15 to 30 g and a density of 0.6 g/cm 3 or lower. Examples of tissue papers to which the use according to the invention is applicable are toilet papers, paper handkerchiefs, facial wipes, make-up removing wipes, freshening wipes, kitchen roll and the like. Depending on the particular application, the tissues may contain special active ingredients, for example moisturizers, insect repellents (after-sun wipes), dihydroxyacetone, deodorizers, surfactants, alcohols (freshening wipes), skin-care oils, anti-inflammatory agents (baby wipes) and the like. Apart from paper-based tissues, the use according to the invention is also applicable to corresponding tissue cloths made of fibers or fleeces.
Emulsions
In one preferred embodiment of the invention, the emulsions contain—again based on active substance content—
(a) 5 to 25, preferably 8 to 20 and more preferably 10 to 15% by weight of polyol poly-12-hydroxystearates, (b) 50 to 90, preferably 60 to 85 and more preferably 70 to 80% by weight of wax esters and (c) 5 to 25, preferably 8 to 20 and more preferably 10 to 15% by weight of waxes,
with the proviso that the quantities shown add up to 100% by weight. The active substance content of the emulsions may be between 0.5 and 80% by weight according to the particular application envisaged. With relatively high active substance contents, the emulsions undergo a dramatic reduction in flowability; with relatively low active substance contents, they do not develop their intended effect. Concentrates with an active substance content of 10 to 70% by weight which are designed for dilution to an in-use concentration of 1 to 15% by weight are preferably marketed. If desired, the aqueous phase may also contain polyols, preferably up to 15% by weight of glycerol.
Skin-Care Oils
In another preferred embodiment of the invention, skin-care oils are used as auxiliaries and additives. Suitable skin-care oils are, for example, Guerbet alcohols based on fatty alcohols containing 6 to 18 and preferably 8 to 10 carbon atoms, esters of hydroxycarboxylic acids with linear or branched C 6-22 fatty alcohols, more particularly dioctyl malate, esters of linear and/or branched fatty acids with polyhydric alcohols (for example propylene glycol, dimer diol or trimer triol) and/or Guerbet alcohols, triglycerides based on C 6-10 fatty acids, liquid mono-/di-/triglyceride mixtures based on C 6-18 fatty acids, esters of C 6-22 fatty alcohols and/or Guerbet alcohols with aromatic carboxylic acids, more particularly benzoic acid, esters of C 2-12 dicarboxylic acids with linear or branched alcohols containing 1 to 22 carbon atoms or polyols containing 2 to 10 carbon atoms and 2 to 6 hydroxyl groups, vegetable oils, branched primary alcohols, substituted cyclohexanes, linear and branched C 6-22 fatty alcohol carbonates, Guerbet carbonates, esters of benzoic acid with linear and/or branched C 6-22 alcohols (for example Finsolv® TN), linear or branched, symmetrical or nonsymmetrical dialkyl ethers containing 6 to 22 carbon atoms per alkyl group, ring opening products of epoxidized fatty acid esters with polyols, silicone oils and/or aliphatic or naphthenic hydrocarbons such as, for example, squalane, squalene and dialkylcyclohexanes.
Co-Emulsifiers
If desired, the compositions to be used in accordance with the invention may contain other emulsifiers, preferably nonionic, cationic or amphoteric emulsifiers, such as:
(1) C 12/18 fatty acid monoesters and diesters of adducts of 1 to 30 moles of ethylene oxide with glycerol; (2) glycerol mono/diesters, sorbitan mono/diesters and sugar mono/diesters of saturated and unsaturated fatty acids containing 6 to 22 carbon atoms or hydroxycarboxylic acids containing 2 to 6 carbon atoms, for example citric acid, malic acid or tartaric acid, and ethylene oxide adducts thereof; (3) alkyl mono- and oligoglycosides containing 8 to 22 carbon atoms in the alkyl group and ethoxylated analogs thereof; (4) adducts of 15 to 60 moles of ethylene oxide with castor oil and/or hydrogenated castor oil; (5) polyglycerol esters such as, for example, polyglycerol polyricinoleate or polyglycerol dimerate. Mixtures of compounds from several of these classes are also suitable; (6) adducts of 2 to 15 moles of ethylene oxide with castor oil and/or hydrogenated castor oil; (7) partial esters based on linear, branched, unsaturated or saturated C 6/22 fatty acids, ricinoleic acid and 12-hydroxystearic acid and glycerol, polyglycerol, pentaerythritol, dipentaerythritol, sugar alcohols (for example sorbitol), alkyl glucosides (for example methyl glucoside, butyl glucoside, lauryl glucoside) and polyglucosides (for example cellulose); (8) mono-, di and trialkyl phosphates and mono-, di- and/or tri-PEG-alkyl phosphates and salts thereof; (9) wool wax alcohols; (10) polysiloxane/polyalkyl polyether copolymers and corresponding derivatives; (11) mixed esters of pentaerythritol, fatty acids, citric acid and fatty alcohol according to DE-PS 11 65 574 and/or mixed esters of fatty acids containing 6 to 22 carbon atoms, methyl glucose and polyols, preferably glycerol or polyglycerol, (12) polyalkylene glycols and (13) glycerol carbonate.
The addition products of ethylene oxide and/or propylene oxide with glycerol monoesters and diesters and sorbitan monoesters and diesters of fatty acids or with castor oil are known commercially available products. They are homolog mixtures of which the average degree of alkoxylation corresponds to the ratio between the quantities of ethylene oxide and/or propylene oxide and substrate with which the addition reaction is carried out. C 12/18 fatty acid monoesters and diesters of adducts of ethylene oxide with glycerol are known as refatting agents for cosmetic compositions from DE-PS 20 24 051.
C 8/18 alkyl mono- and oligoglycosides, their production and their use as surfactants are known from the prior-art literature. They are produced in particular by reacting glucose or oligosaccharides with primary alcohols containing 8 to 18 carbon atoms. So far as the glycoside component is concerned, both monoglycosides where a cyclic sugar unit is attached to the fatty alcohol by a glycoside bond and oligomeric glycosides with a degree of oligomerization of preferably up to about 8 are suitable. The degree of oligomerization is a statistical mean value on which a homolog distribution typical of such technical products is based.
Other suitable emulsifiers are zwitterionic surfactants. Zwitterionic surfactants are surface-active compounds which contain at least one quaternary ammonium group and at least one carboxylate and one sulfonate group in the molecule. Particularly suitable zwitterionic surfactants are the so-called betaines, such as the N-alkyl-N,N-dimethyl ammonium glycinates, for example cocoalkyl dimethyl ammonium glycinate, N-acylaminopropyl-N,N-dimethyl ammonium glycinates, for example cocoacylaminopropyl dimethyl ammonium glycinate, and 2-alkyl-3-carboxymethyl-3-hydroxyethyl imidazolines containing 8 to 18 carbon atoms in the alkyl or acyl group and cocoacylaminoethyl hydroxyethyl carboxymethyl glycinate. The fatty acid amide derivative known under the CTFA name of Cocamidopropyl Betaine is particularly preferred. Ampholytic surfactants are also suitable emulsifiers. Ampholytic surfactants are surface-active compounds which, in addition to a C 8/18 alkyl or acyl group, contain at least one free amino group and at least one —COOH— or —SO 3 H— group in the molecule and which are capable of forming inner salts. Examples of suitable ampholytic surfactants are N-alkyl glycines, N-alkyl propionic acids, N-alkylaminobutyric acids, N-alkyliminodipropionic acids, N-hydroxyethyl-N-alkylamidopropyl glycines, N-alkyl taurines, N-alkyl sarcosines, 2-alkylaminopropionic acids and alkylaminoacetic acids containing around 8 to 18 carbon atoms in the alkyl group. Particularly preferred ampholytic surfactants are N-cocoalkylaminopropionate, cocoacylaminoethyl aminopropionate and C 12/18 acyl sarcosine. According to the invention, other suitable emulsifiers besides ampholytic surfactants are quaternary emulsifiers, those of the esterquat type, preferably methyl-quaternized difatty acid triethanolamine ester salts, being particularly preferred because they further improve softness. “Esterquats” are generally understood to be quaternized fatty acid triethanolamine ester salts. These are known substances which may be obtained by the relevant methods of preparative organic chemistry, cf. International patent application WO 91/01295 (Henkel). According to this document, triethanolamine is partly esterified with fatty acids in the presence of hypophosphorous acid, air is passed through and the reaction product is quaternized with dimethyl sulfate or ethylene oxide. In addition, German patent DE-C1 4308794 (Henkel) describes a process for the production of solid esterquats in which the quaternization of triethanolamine esters is carried out in the presence of suitable dispersants, preferably fatty alcohols. Overviews on this subject have been published, for example, by R. Puchta et al. in Tens. Surf. Det., 30, 186 (1993), by M. Brock in Tens. Surf. Det. 30, 394 (1993), by R. Lagerman et al. in J. Am. Oil. Chem. Soc., 71, 97 (1994) and by I. Shapiro in Cosm. Toil., 109, 77 (1994). The quaternized fatty acid triethanolamine ester salts correspond to formula (II):
in which R 3 CO is an acyl group containing 6 to 22 carbon atoms, R 4 and R 5 independently of one another represent hydrogen or have the same meaning as R 3 CO, R 6 is an alkyl group containing 1 to 4 carbon atoms or a (CH 2 CH 2 O) q H group, m, n and p together stand for 0 or numbers of 1 to 12, q is a number of 1 to 12 and X is halide, alkyl sulfate or alkyl phosphate. Typical examples of esterquats which may be used in accordance with the invention are products based on caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, isostearic acid, stearic acid, oleic acid, elaidic acid, arachic acid, behenic acid and erucic acid and the technical mixtures thereof obtained for example in the pressure hydrolysis of natural fats and oils. Technical C 12/18 cocofatty acids and, in particular, partly hydrogenated C 16/18 tallow or palm oil fatty acids and high-elaidic C 16/18 fatty acid cuts are preferably used. To produce the quaternized esters, the fatty acids and the triethanolamine may be used in a molar ratio of 1.1:1 to 3:1. With the performance properties of the esterquats in mind, a ratio of 1.2:1 to 2.2:1 and preferably 1.5:1 to 1.9:1 has proved to be particularly advantageous. The preferred esterquats are technical mixtures of mono-, di- and triesters with an average degree of esterification of 1.5 to 1.9 and are derived from technical C 16/18 tallow or palm oil fatty acid (iodine value 0 to 40). In performance terms, quaternized fatty acid triethanolamine ester salts corresponding to formula (II), in which R 3 CO is an acyl group containing 16 to 18 carbon atoms, R 4 has the same meaning as R 3 CO, R 5 is hydrogen, R 6 is a methyl group, m, n and p stand for 0 and X stands for methyl sulfate, have proved to be particularly advantageous. Other suitable esterquats besides the quaternized fatty acid triethanolamine ester salts are quaternized ester salts of fatty acids with diethanolalkylamines corresponding to formula (III):
in which R 3 CO is an acyl group containing 6 to 22 carbon atoms, R 4 is hydrogen or has the same meaning as R 3 CO, R 6 and R 7 independently of one another are alkyl groups containing 1 to 4 carbon atoms, m and n together stand for 0 or numbers of 1 to 12 and X stands for halide, alkyl sulfate or alkyl phosphate. Finally, another group of suitable esterquats are the quaternized ester salts of fatty acids with 1,2-dihydroxypropyl dialkylamines corresponding to formula (IV):
in which R 3 CO is an acyl group containing 6 to 22 carbon atoms, R 4 is hydrogen or has the same meaning as R 3 CO, R 8 , R 9 and R 10 independently of one another are alkyl groups containing 1 to 4 carbon atoms, m and n together stand for 0 or numbers of 1 to 12 and X stands for halide, alkyl sulfate or alkyl phosphate. So far as the choice of the preferred fatty acids and the optimum degree of esterification is concerned, the examples mentioned in regard to (II) also apply to the esterquats of formulae (III) and (IV).
Active Substances
In one particular embodiment of the invention, the emulsions contain active substances such as, for example, mild surfactants, superfatting agents, consistency factors, thickeners, polymers, silicone compounds, fats, waxes, stabilizers, biogenic agents, deodorizers, film formers, UV protection factors, antioxidants, hydrotropes, preservatives, insect repellents, self-tanning agents, solubilizers, perfume oils, dyes, germ inhibitors and the like.
Typical examples of suitable mild, i.e. dermatologically compatible, surfactants, are fatty alcohol polyglycol ether sulfates, monoglyceride sulfates, mono- and/or dialkylsulfosuccinates, fatty acid isethionates, fatty acid sarcosinates, fatty acid taurides, fatty acid glutamates, α-olefin sulfonates, ether carboxylic acids, alkyl oligoglucosides, fatty acid glucamides, alkyl amidobetaines and/or protein fatty acid condensates (preferably based on wheat proteins).
Superfatting agents may be selected from such substances as, for example, lanolin and lecithin and also polyethoxylated or acylated lanolin and lecithin derivatives, polyol fatty acid esters, monoglycerides and fatty acid alkanolamides, the fatty acid alkanolamides also serving as foam stabilizers.
The consistency factors mainly used are fatty alcohols or hydroxyfatty alcohols containing 12 to 22 and preferably 16 to 18 carbon atoms and also partial glycerides, fatty acids or hydroxyfatty acids. A combination of these substances with alkyl oligoglucosides and/or fatty acid N-methyl glucamides of the same chain length and/or polyglycerol poly-12-hydroxystearates is preferably used. Suitable thickeners are, for example, Aerosil types (hydrophilic silicas), polysaccharides, more especially xanthan gum, guar-guar, agar-agar, alginates and tyloses, carboxymethyl cellulose and hydroxyethyl cellulose, also relatively high molecular weight polyethylene glycol monoesters and diesters of fatty acids, polyacrylates (for example Carbopols® [Goodrich] or Synthalens® [Sigma]), polyacrylamides, polyvinyl alcohol and polyvinyl pyrrolidone, surfactants such as, for example, ethoxylated fatty acid glycerides, esters of fatty acids with polyols, for example pentaerythritol or trimethylol propane, narrow-range fatty alcohol ethoxylates or alkyl oligoglucosides and electrolytes, such as sodium chloride and ammonium chloride.
Suitable cationic polymers are, for example, cationic cellulose derivatives such as, for example, the quaternized hydroxyethyl cellulose obtainable from Amerchol under the name of Polymer JR 400®, cationic starch, copolymers of diallyl ammonium salts and acrylamides, quaternized vinyl pyrrolidone/vinyl imidazole polymers such as, for example, Luviquat® (BASF), condensation products of polyglycols and amines, quaternized collagen polypeptides such as, for example, Lauryldimonium Hydroxypropyl Hydrolyzed Collagen (Lamequat® L/Grünau), quaternized wheat polypeptides, polyethyleneimine, cationic silicone polymers such as, for example, Amodimethicone, copolymers of adipic acid and dimethylaminohydroxypropyl diethylenetriamine (Cartaretine®/Sandoz), copolymers of acrylic acid with dimethyl diallyl ammonium chloride (Merquat® 550/Chemviron), polyaminopolyamides as described, for example, in FR-A 2 252 840 and crosslinked water-soluble polymers thereof, cationic chitin derivatives such as, for example, quaternized chitosan, optionally in microcrystalline distribution, condensation products of dihaloalkylene, for example dibromobutane, with bis-dialkylamines, for example bis-dimethylamino-1,3-propane, cationic guar gum such as, for example, Jaguar® CBS, Jaguar®C-17, Jaguar® C-16 of Celanese, quaternized ammonium salt polymers such as, for example, Mirapol® A-15, Mirapol® AD-1, Mirapol® AZ-1 of Miranol.
Suitable anionic, zwitterionic, amphoteric and nonionic polymers are, for example, vinyl acetate/crotonic acid copolymers, vinyl pyrrolidone/vinyl acrylate copolymers, vinyl acetate/butyl maleate/isobornyl acrylate copolymers, methyl vinylether/maleic anhydride copolymers and esters thereof, uncrosslinked and polyol-crosslinked polyacrylic acids, acrylamidopropyl trimethylammonium chloride/acrylate copolymers, octylacrylamide/methyl methacrylate/tert.-butylaminoethyl methacrylate/2-hydroxypropyl methacrylate copolymers, polyvinyl pyrrolidone, vinyl pyrrolidone/vinyl acetate copolymers, vinyl pyrrolidone/dimethylaminoethyl methacrylate/vinyl caprolactam terpolymers and optionally derivatized cellulose ethers and silicones.
Suitable silicone compounds are, for example, dimethyl polysiloxanes, methylphenyl polysiloxanes, cyclic silicones and amino-, fatty acid-, alcohol-, polyether-, epoxy-, fluorine-, glycoside- and/or alkyl-modified silicone compounds which may be both liquid and resin-like at room temperature. Other suitable silicone compounds are simethicones which are mixtures of dimethicones with an average chain length of 200 to 300 dimethylsiloxane units and hydrogenated silicates. In addition, a detailed overview of suitable volatile silicones was published by Todd et al. in Cosm. Toil. 91, 27 (1976).
Metal salts of fatty acids such as, for example, magnesium, aluminium and/or zinc stearate or ricinoleate may be used as stabilizers.
In the context of the invention, biogenic agents are, for example, tocopherol, tocopherol acetate, tocopherol palmitate, ascorbic acid, deoxyribonucleic acid, retinol, bisabolol, allantoin, phytantriol, panthenol, AHA acids, amino acids, ceramides, pseudoceramides, essential oils, plant extracts and vitamin complexes.
Suitable deodorizers are, for example, antiperspirants, such as aluminium chlorhydrates. These antiperspirants are colorless hygroscopic crystals which readily deliquesce in air and which accumulate when aqueous aluminium chloride solutions are concentrated by evaporation. Aluminium chlorhydrate is used for the production of perspiration-inhibiting and deodorizing compositions and probably acts by partially blocking the sweat glands through the precipitation of proteins and/or polysaccharides [cf. J. Soc. Cosm. Chem. 24, 281 (1973)]. For example, an aluminium chlorhydrate which corresponds to the formula [Al 2 (OH) 5 Cl]*2.5H 2 O and which is particularly preferred for the purposes of the invention is commercially available under the name of Locron® from Hoechst AG of Frankfurt, FRG [cf. J. Pharm. Pharmcol. 26, 531 (1975)]. Besides the chlorhydrates, aluminium hydroxylactates and acidic aluminium/zirconium salts may also be used. Other suitable deodorizers are esterase inhibitors, preferably trialkyl citrates, such as trimethyl citrate, tripropyl citrate, triisopropyl citrate, tributyl citrate and, in particular, triethyl citrate (Hydagen® CAT, Henkel KGaA, Düsseldorf, FRG). Esterase inhibitors inhibit enzyme activity and thus reduce odor formation. The free acid is probably released through the cleavage of the citric acid ester, reducing the pH value of the skin to such an extent that the enzymes are inhibited. Other esterase inhibitors are sterol sulfates or phosphates, for example lanosterol, cholesterol, campesterol, stigmasterol and sitosterol sulfate or phosphate, dicarboxylic acids and esters thereof, for example glutaric acid, glutaric acid monoethyl ester, glutaric acid diethyl ester, adipic acid, adipic acid monoethyl ester, adipic acid diethyl ester, malonic acid and malonic acid diethyl ester, hydroxycarboxylic acids and esters thereof, for example citric acid, malic acid, tartaric acid or tartaric acid diethyl ester. Antibacterial agents which influence the germ flora and destroy or inhibit the growth of perspiration-decomposing bacteria, may also be present in stick products. Examples of such antibacterial agents are chitosan, phenoxyethanol and chlorhexidine gluconate. 5-Chloro-2-(2,4-dichlorophenoxy)phenol, which is marketed under the name of Irgasan® by Ciba-Geigy of Basel, Switzerland, has also proved to be particularly effective.
UV protection factors in the context of the invention are, for example, organic substances (light filters) which are liquid or crystalline at room temperature and which are capable of absorbing ultraviolet radiation and of releasing the energy absorbed in the form of longer-wave radiation, for example heat. UV-B filters can be oil-soluble or water-soluble. The following are examples of oil-soluble substances:
3-benzylidene camphor or 3-benzylidene norcamphor and derivatives thereof, for example 3-(4-methylbenzylidene)-camphor as described in EP-B1 0693471; 4-aminobenzoic acid derivatives, preferably 4-(dimethylamino)-benzoic acid-2-ethylhexyl ester, 4-(dimethylamino)-benzoic acid-2-octyl ester and 4-(dimethylamino)-benzoic acid amyl ester; esters of cinnamic acid, preferably 4-methoxycinnamic acid-2-ethylhexyl ester, 4-methoxycinnamic acid propyl ester, 4-methoxycinnamic acid isoamyl ester, 2-cyano-3,3-phenylcinnamic acid-2-ethylhexyl ester (Octocrylene); esters of salicylic acid, preferably salicylic acid-2-ethylhexyl ester, salicylic acid-4-isopropylbenzyl ester, salicylic acid homomethyl ester; derivatives of benzophenone, preferably 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4′-methylbenzophenone, 2,2′-dihydroxy-4-methoxybenzophenone; esters of benzalmalonic acid, preferably 4-methoxybenzalmalonic acid di-2-ethylhexyl ester; triazine derivatives such as, for example, 2,4,6-trianilino-(p-carbo-2′-ethyl-1′-hexyloxy)-1,3,5-triazine and Octyl Triazone as described in EP-A1 0818450; propane-1,3-diones such as, for example, 1-(4-tert.butylphenyl)-3-(4′-methoxyphenyl)-propane-1,3-dione; ketotricyclo(5.2.1.0)decane derivatives as described in EP-B1 0694521.
Suitable water-soluble substances are
2-phenylbenzimidazole-5-sulfonic acid and alkali metal, alkaline earth metal, ammonium, alkylammonium, alkanolammonium and glucammonium salts thereof; sulfonic acid derivatives of benzophenones, preferably 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and salts thereof; sulfonic acid derivatives of 3-benzylidene camphor such as, for example, 4-(2-oxo-3-bornylidenemethyl)-benzene sulfonic acid and 2-methyl-5-(2-oxo-3-bornylidene)-sulfonic acid and salts thereof.
Typical UV-A filters are, in particular, derivatives of benzoyl methane such as, for example, 1-(4′-tert.butylphenyl)-3-(4′-methoxyphenyl)-propane-1,3-dione, 4-tert.butyl-4′-methoxydibenzoyl methane (Parsol 1789) or 1-phenyl-3-(4′-isopropylphenyl)-propane-1,3-dione. The UV-A and UV-B filters may of course also be used in the form of mixtures. Besides the soluble substances mentioned, insoluble light-blocking pigments, i.e. finely dispersed metal oxides or salts, may also be used for this purpose. Examples of suitable metal oxides are, in particular, zinc oxide and titanium dioxide and also oxides of iron, zirconium oxide, silicon, manganese, aluminium and cerium and mixtures thereof. Silicates (talcum), barium sulfate and zinc stearate may be used as salts. The oxides and salts are used in the form of the pigments for skin-care and skin-protecting emulsions and decorative cosmetics. The particles should have a mean diameter of less than 100 nm, preferably between 5 and 50 nm and more preferably between 15 and 30 nm. They may be spherical in shape although ellipsoidal particles or other non-spherical particles may also be used. The pigments may also be surface-treated, i.e. hydrophilized or hydrophobicized. Typical examples are coated titanium dioxides, for example Titandioxid T 805 (Degussa) and Eusolex® T2000 (Merck). Suitable hydrophobic coating materials are, above all, silicones and, among these, especially trialkoxyoctylsilanes or simethicones. So-called micro- or nanopigments are preferably used in sun protection products. Micronized zinc oxide is preferably used. Other suitable UV filters can be found in P. Finkel's review in SOFW-Journal 122, 543 (1996).
Besides the two groups of primary sun protection factors mentioned above, secondary sun protection factors of the antioxidant type may also be used. Secondary sun protection factors of the antioxidant type interrupt the photochemical reaction chain which is initiated when UV rays penetrate into the skin. Typical examples are amino acids (for example glycine, histidine, tyrosine, tryptophane) and derivatives thereof, imidazoles (for example urocanic acid) and derivatives thereof, peptides, such as D,L-carnosine, D-carnosine, L-carnosine and derivatives thereof (for example anserine), carotinoids, carotenes (for example α-carotene, β-carotene, lycopene) and derivatives thereof, chlorogenic acid and derivatives thereof, liponic acid and derivatives thereof (for example dihydroliponic acid), aurothioglucose, propylthiouracil and other thiols (for example thioredoxine, glutathione, cysteine, cystine, cystamine and glycosyl, N-acetyl, methyl, ethyl, propyl, amyl, butyl and lauryl, palmitoyl, oleyl, γ-linoleyl, cholesteryl and glyceryl esters thereof) and their salts, dilaurylthiodipropionate, distearylthiodipropionate, thiodipropionic acid and derivatives thereof (esters, ethers, peptides, lipids, nucleotides, nucleosides and salts) and sulfoximine compounds (for example butionine sulfoximines, homocysteine sulfoximine, butionine sulfones, penta-, hexa- and hepta-thionine sulfoximine) in very small compatible dosages (for example pmole to μmole/kg), also (metal) chelators (for example α-hydroxyfatty acids, palmitic acid, phytic acid, lactoferrine), α-hydroxy acids (for example citric acid, lactic acid, malic acid), humic acid, bile acid, bile extracts, bilirubin, biliverdin, EDTA, EGTA and derivatives thereof, unsaturated fatty acids and derivatives thereof (for example γ-linolenic acid, linoleic acid, oleic acid), folic acid and derivatives thereof, ubiquinone and ubiquinol and derivatives thereof, vitamin C and derivatives thereof (for example ascorbyl palmitate, Mg ascorbyl phosphate, ascorbyl acetate), tocopherols and derivatives (for example vitamin E acetate), vitamin A and derivatives (vitamin A palmitate) and coniferyl benzoate of benzoin resin, rutinic acid and derivatives thereof, α-glycosyl rutin, ferulic acid, furfurylidene glucitol, carnosine, butyl hydroxytoluene, butyl hydroxyanisole, nordihydroguaiac resin acid, nordihydroguairetic acid, trihydroxybutyrophenone, uric acid and derivatives thereof, mannose and derivatives thereof, Superoxid-Dismutase, zinc and derivatives thereof (for example ZnO, ZnSO 4 ), selenium and derivatives thereof (for example selenium methionine), stilbenes and derivatives thereof (for example stilbene oxide, trans-stilbene oxide) and derivatives of these active substances suitable for the purposes of the invention (salts, esters, ethers, sugars, nucleotides, nucleosides, peptides and lipids).
In addition, hydrotropes, for example ethanol, isopropyl alcohol or polyols, may be used to improve flow behavior. Suitable polyols preferably contain 2 to 15 carbon atoms and at least two hydroxyl groups. The polyols may contain other functional groups, more especially amino groups, or may be modified with nitrogen. Typical examples are
glycerol; alkylene glycols such as, for example, ethylene glycol, diethylene glycol, propylene glycol, butylene glycol, hexylene glycol and polyethylene glycols with an average molecular weight of 100 to 1000 dalton; technical oligoglycerol mixtures with a degree of self-condensation of 1.5 to 10 such as, for example, technical diglycerol mixtures with a diglycerol content of 40 to 50% by weight; methylol compounds such as, in particular, trimethylol ethane, trimethylol propane, trimethylol butane, pentaerythritol and dipentaerythritol; lower alkyl glucosides, particularly those containing 1 to 8 carbon atoms in the alkyl group, for example methyl and butyl glucoside; sugar alcohols containing 5 to 12 carbon atoms, for example sorbitol or mannitol, sugars containing 5 to 12 carbon atoms, for example glucose or sucrose; aminosugars, for example glucamine; dialcoholamines, such as diethanolamine or 2-aminopropane-1,3-diol.
Suitable preservatives are, for example, phenoxyethanol, formaldehyde solution, parabens, pentanediol or sorbic acid and the other classes of compounds listed in Appendix 6, Parts A and B of the Kosmetikverordnung (“Cosmetics Directive”). Suitable insect repellents are N,N-diethyl-m-toluamide, pentane-1,2-diol or Insect Repellent 3535. A suitable self-tanning agent is dihydroxyacetone.
Suitable perfume oils are mixtures of natural and synthetic fragrances. Natural fragrances include the extracts of blossoms (lily, lavender, rose, jasmine, neroli, ylang-ylang), stems and leaves (geranium, patchouli, petitgrain), fruits (anise, coriander, caraway, juniper), fruit peel (bergamot, lemon, orange), roots (nutmeg, angelica, celery, cardamon, costus, iris, calmus), woods (pinewood, sandalwood, guaiac wood, cedarwood, rosewood), herbs and grasses (tarragon, lemon grass, sage, thyme), needles and branches (spruce, fir, pine, dwarf pine), resins and balsams (galbanum, elemi, benzoin, myrrh, olibanum, opoponax). Animal raw materials, for example civet and beaver, may also be used. Typical synthetic perfume compounds are products of the ester, ether, aldehyde, ketone, alcohol and hydrocarbon type. Examples of perfume compounds of the ester type are benzyl acetate, phenoxyethyl isobutyrate, p-tert.butyl cyclohexylacetate, linalyl acetate, dimethyl benzyl carbinyl acetate, phenyl ethyl acetate, linalyl benzoate, benzyl formate, ethylmethyl phenyl glycinate, allyl cyclohexyl propionate, styrallyl propionate and benzyl salicylate. Ethers include, for example, benzyl ethyl ether while aldehydes include, for example, the linear alkanals containing 8 to 18 carbon atoms, citral, citronellal, citronellyloxyacetaldehyde, cyclamen aldehyde, hydroxycitronellal, lilial and bourgeonal. Examples of suitable ketones are the ionones, α-isomethylionone and methyl cedryl ketone. Suitable alcohols are anethol, citronellol, eugenol, isoeugenol, geraniol, linalool, phenylethyl alcohol and terpineol. The hydrocarbons mainly include the terpenes and balsams. However, it is preferred to use mixtures of different perfume compounds which, together, produce an agreeable fragrance. Other suitable perfume oils are essential oils of relatively low volatility which are mostly used as aroma components. Examples are sage oil, chamomile oil, clove oil, melissa oil, mint oil, cinnamon leaf oil, lime-blossom oil, juniper berry oil, vetiver oil, olibanum oil, galbanum oil, labolanum oil and lavendin oil. The following are preferably used either individually or in the form of mixtures: bergamot oil, dihydromyrcenol, lilial, lyral, citronellol, phenylethyl alcohol, α-hexylcinnamaldehyde, geraniol, benzyl acetone, cyclamen aldehyde, linalool, Boisambrene Forte, Ambroxan, indole, hedione, sandelice, citrus oil, mandarin oil, orange oil, allylamyl glycolate, cyclovertal, lavendin oil, clary oil, β-damascone, geranium oil bourbon, cyclohexyl salicylate, Vertofix Coeur, Iso-E-Super, Fixolide NP, evernyl, iraldein gamma, phenylacetic acid, geranyl acetate, benzyl acetate, rose oxide, romillat, irotyl and floramat.
Suitable dyes are any of the substances suitable and approved for cosmetic purposes as listed, for example, in the publication “Kosmetische Färbemittel” of the Farbstoffkommission der Deutschen Forschungsgemeinschaft, Verlag Chemie, Weinheim, 1984, pages 81 to 106. These dyes are normally used in concentrations of 0.001 to 0.1% by weight, based on the mixture as a whole.
Typical examples of germ inhibitors are preservatives which act specifically against gram-positive bacteria such as, for example, 2,4,4′-trichloro-2′-hydroxydiphenyl ether, chlorhexidine (1,6-di-(4-chlorophenylbiguanido)-hexane) or TCC (3,4,4′-trichlorocarbanilide). Numerous perfumes and essential oils also have antimicrobial properties. Typical examples are the active substances eugenol, menthol and thymol in nettle, mint and thyme oil. An interesting natural deodorant is the terpene alcohol farnesol (3,7,11-trimethyl-2,6,10-dodecatrien-1-ol) which is present in linden blossom oil and which smells of lily-of-the-valley. Glycerol monolaurate has also been successfully used as a bacteriostatic agent. The percentage content of the additional germ inhibitors is normally about 0.1 to 2% by weight, based on the solids component of the formulations.
The total percentage content of auxiliaries and additives may be from 1 to 50% by weight and is preferably from 5 to 40% by weight, based on the particular composition. The compositions may be produced by standard hot or cold processes and are preferably produced by the phase inversion temperature method.
Treatment of the Tissue Papers with the Softening Compositions
The treatment of the tissue papers with the softening compositions may be carried out in known manner, the solution being applied to at least one side of the papers. Basically, any known method by which liquids or melts can be applied to more or less hard surfaces may be used for this purpose, including for example spraying, printing (for example flexographic printing), coating (gravure coating), extrusion and combinations of these methods. The papers/tissues may also be impregnated with the compositions. Application of the compositions is generally followed by a brief drying step. Processes for treating tissue papers with softening compositions are described in detail in the above-cited documents WO 95/35411 and WO 97/30216 to which reference is hereby specifically made.
EXAMPLES
To test performance properties, commercially available three-ply tissue papers with a recycled paper content of 95% and a weight of 18 g/m 2 were treated with emulsions 1 to 5 according to the invention and with the two comparison compositions C1 and C2 in quantities of 2.5 g/m 2 . The papers were then dried for 30 minutes at 30° C., after which their softness was evaluated by a panel of six experienced testers on a scale of (+++) very soft to (+) hard. The sensorial feeling on touching the tissues was also evaluated. The results which represent the averages of three test series are set out in Table 1.
TABLE 1
Softness of tissue papers using emulsions
Composition/
performance
1
2
3
4
5
C1
C2
Polyglyceryl-2-
8.0
10.0
8.0
8.0
10.0
−
−
Dipolyhydro-
xystearate
Glyceryl Oleate
−
−
−
−
−
8.0
10.0
Oleyl Erucate
60.0
65.0
−
−
55.0
60.0
65.0
Oleyl Oleate
−
−
60.0
−
−
−
−
Candelilla wax
7.0
6.0
−
65.0
−
7.0
5.0
Carnauba wax
−
−
7.0
5.0
−
−
−
Bees Wax
−
−
−
−
5.0
−
−
Water
to 100
Softness
+++
+++
+++
++
++
+
+
Sensorial
Moist
Moist
Moist
Moist
Moist
Flat
Flat
evaluation | A process for making paper substrates having a soft feel involving: (a) providing a paper substrate; (b) providing an emulsion containing: (i) a polyol poly-12-hydroxystearate; (ii) a wax ester; and (iii) a wax; and (c) impregnating the paper substrate with the emulsion. | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of U.S. application Ser. No. 10/358,652, filed Feb. 5, 2003, now U.S. Pat. No. 7,157,578, which is a continuation of U.S. application Ser. No. 10/092,312, filed Mar. 6, 2002, now abandoned, which claims the benefit of U.S. Application No. 60/275,403, filed Mar. 13, 2001, the contents all of which are incorporated herein by reference.
FIELD OF THE INVENTION
This invention relates to a treatment of psychiatric disorders and neurological diseases including major depression, anxiety-related disorders, post-traumatic stress disorder, supranuclear palsy and feeding disorders as well as treatment of immunological, cardiovascular or heart-related diseases and colonic hypersensitivity associated with psycho-pathological disturbances and stress, by administration of 4-(2-Butylamino)-2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)pyrazolo-[1,5-a]-1,3,5-triazine, its enantiomer and pharmaceutically acceptable salts as a corticotropin releasing factor receptor ligand.
BACKGROUND OF THE INVENTION
Corticotropin releasing factor (herein referred to as CRF), a 41 amino acid peptide, is the primary physiological regulator of proopiomelanocortin (POMC)-derived peptide secretion from the anterior pituitary gland [J. Rivier et al., Proc. Nat. Acad Sci . ( USA ) 80:4851 (1983); W. Vale et al., Science 213:1394 (1981)]. In addition to its endocrine role at the pituitary gland, immunohistochemical localization of CRF has demonstrated that the hormone has a broad extrahypothalamic distribution in the central nervous system and produces a wide spectrum of autonomic, electrophysiological and behavioral effects consistent with a neurotransmitter or neuromodulator role in brain [W. Vale et al., Rec. Prog. Horm. Res. 39:245 (1983); G. F. Koob, Persp. Behav. Med. 2:39 (1985); E. B. De Souza et al., J. Neurosci. 5:3189 (1985)]. There is also evidence that CRF plays a significant role in integrating the response of the immune system to physiological, psychological, and immunological stressors [J. E. Blalock, Physiological Reviews 69:1 (1989); J. E. Morley, Life Sci. 41:527 (1987)].
Clinical data provide evidence that CRF has a role in psychiatric disorders and neurological diseases including depression, anxiety-related disorders and feeding disorders. A role for CRF has also been postulated in the etiology and pathophysiology of Alzheimer's disease, Parkinson's disease, Huntington's disease, progressive supranuclear palsy and amyotrophic lateral sclerosis as they relate to the dysfunction of CRF neurons in the central nervous system [for review see E. B. De Souza, Hosp. Practice 23:59 (1988)].
In affective disorder, or major depression, the concentration of CRF is significantly increased in the cerebrospinal fluid (CSF) of drug-free individuals [C. B. Nemeroff et al., Science 226:1342 (1984); C. M. Banki et al., Am. J. Psychiatry 144:873 (1987); R. D. France et al., Biol. Psychiatry 28:86 (1988); M. Arato et al., Biol Psychiatry 25:355 (1989)]. Furthermore, the density of CRF receptors is significantly decreased in the frontal cortex of suicide victims, consistent with a hypersecretion of CRF [C. B. Nemeroffet al., Arch. Gen. Psychiatry 45:577 (1988)]. In addition, there is a blunted adrenocorticotropin (ACTH) response to CRF (i.v. administered) observed in depressed patients [P. W. Gold et al., Am J. Psychiatry 141:619 (1984); F. Holsboer et al., Psychoneuroendocrinology 9:147 (1984); P. W. Gold et al., New Eng. J. Med. 314:1129 (1986)]. Preclinical studies in rats and non-human primates provide additional support for the hypothesis that hypersecretion of CRF may be involved in the symptoms seen in human depression [R. M. Sapolsky, Arch. Gen. Psychiatry 46:1047 (1989)]. There is preliminary evidence that tricyclic antidepressants can alter CRF levels and thus modulate the numbers of CRF receptors in brain [Grigoriadis et al., Neuropsychopharmacology 2:53 (1989)].
It has also been postulated that CRF has a role in the etiology of anxiety-related disorders. CRF produces anxiogenic effects in animals and interactions between benzodiazepine/non-benzodiazepine anxiolytics and CRF have been demonstrated in a variety of behavioral anxiety models [D. R. Britton et al., Life Sci. 31:363 (1982); C. W. Berridge and A. J. Dunn Regul. Peptides 16:83 (1986)]. Preliminary studies using the putative CRF receptor antagonist a-helical ovine CRF (9-41) in a variety of behavioral paradigms demonstrate that the antagonist produces “anxiolytic-like” effects that are qualitatively similar to the benzodiazepines [C. W. Berridge and A. J. Dunn Horm. Behav. 21:393 (1987), Brain Research Reviews 15:71 (1990)].
Neurochemical, endocrine and receptor binding studies have all demonstrated interactions between CRF and benzodiazepine anxiolytics, providing further evidence for the involvement of CRF in these disorders. Chlordiazepoxide attenuates the “anxiogenic” effects of CRF in both the conflict test [K. T. Britton et al., Psychopharmacology 86:170 (1985); K. T. Britton et al., Psychopharmacology 94:306 (1988)] and in the acoustic startle test [N. R. Swerdlow et al., Psychopharmacology 88:147 (1986)] in rats. The benzodiazepine receptor antagonist (Ro15-1788), which was without behavioral activity alone in the operant conflict test, reversed the effects of CRF in a dose-dependent manner while the benzodiazepine inverse agonist (FG7142) enhanced the actions of CRF [K. T. Britton et al., Psychopharmacology 94:306 (1988)].
The mechanisms and sites of action through which the standard anxiolytics and antidepressants produce their therapeutic effects remain to be elucidated. It has been hypothesized however, that they are involved in the suppression of the CRF hypersecretion that is observed in these disorders. Of particular interest is that preliminary studies examining the effects of a CRF receptor antagonist (a-h elical CRF9-41) in a variety of behavioral paradigms have demonstrated that the CRF antagonist produces “anxiolytic-like” effects qualitatively similar to the benzodiazepines [for review see G. F. Koob and K. T. Britton, In: Corticotropin - Releasing Factor: Basic and Clinical Studies of a Neuropeptide , E. B. De Souza and C. B. Nemeroff eds., CRC Press p221 (1990)].
It has been further postulated that CRF has a role in cardiovascular or heart-related diseases as well as gastrointestinal disorders arising from stress such as hypertension, tachycardia and congestive heart failure, stroke, irritable bowel syndrome post-operative ileus and colonic hypersensitivity associated with psychopathological disturbance and stress [for reviews see E. D. DeSouza, C. B. Nemeroff, Editors; Corticotropin - Releasing Factor: Basic and Clinical Studies of a Neuropeptide , E. B. De Souza and C. B. Nemeroff eds., CRC Press p221 (1990) and C. Maillot, M. Million, J. Y. Wei, A. Gauthier, Y. Tache, Gastroenterology, 119, 1569-1579 (2000)].
Over-expression or under-expression of CRF has been proposed as an underlying cause for several medical disorders. Such treatable disorders include, for example and without limitation: affective disorder, anxiety, depression, headache, irritable bowel syndrome, post-traumatic stress disorder, supranuclear palsy, immune suppression, Alzheimer's disease, gastrointestinal diseases, anorexia nervosa or other feeding disorder, drug addiction, drug or alcohol withdrawal symptoms, inflammatory diseases, cardiovascular or heart-related diseases, fertility problems, human immunodeficiency virus infections, hemorrhagic stress, obesity, infertility, head and spinal cord traumas, epilepsy, stroke, ulcers, amyotrophic lateral sclerosis, hypoglycemia, hypertension, tachycardia and congestive heart failure, stroke, osteoporosis, premature birth, psychosocial dwarfism, stress-induced fever, ulcer, diarrhea, post-operative ileus and colonic hypersensitivity associated with psychopathological disturbance and stress [for reviews see J. R. McCarthy, S. C. Heinrichs and D. E. Grigoriadis, Cuur. Pharm. Res., 5, 289-315 (1999); P. J. Gilligan, D. W. Robertson and R. Zaczek, J. Medicinal Chem., 43, 1641-1660 (2000), G. P. Chrousos, Int. J. Obesity, 24, Suppl. 2, S50-S55 (2000); E. Webster, D. J. Torpy, I. J. Elenkov, G. P. Chrousos, Ann. N.Y. Acad. Sci., 840, 21-32 (1998); D. J. Newport and C. B. Nemeroff, Curr. Opin. Neurobiology, 10, 211-218 (2000); G. Mastorakos and I. Ilias, Ann. N.Y. Acad. Sci., 900, 95-106 (2000); M. J. Owens and C. B. Nemeroff, Expert Opin. Invest. Drugs, 8, 1849-1858 (1999); G. F. Koob, Ann. N.Y. Acad. Sci., 909, 170-185 (2000)].
The following publications each describe CRF antagonist compounds; however, none disclose the compounds provided herein: WO95/10506; WO99/51608; WO97/35539; WO99/01439; WO97/44308; WO97/35846; WO98/03510; WO99/11643; PCT/US99/18707; WO99/01454; and, WO00/01675.
SUMMARY OF THE INVENTION
In accordance with one aspect, the present invention provides a novel compound, pharmaceutical compositions and methods which may be used in the treatment of affective disorder, anxiety, depression, irritable bowel syndrome, post-traumatic stress disorder, supranuclear palsy, immune suppression, Alzheimer's disease, gastrointestinal disease, anorexia nervosa or other feeding disorder, drug or alcohol withdrawal symptoms, drug addiction, inflammatory disorder, fertility problems, disorders, the treatment of which can be effected or facilitated by antagonizing CRF, including but not limited to disorders induced or facilitated by CRF, or a disorder selected from inflammatory disorders such as rheumatoid arthritis and osteoarthritis, pain, asthma, psoriasis and allergies; generalized anxiety disorder; panic, phobias, obsessive-compulsive disorder; post-traumatic stress disorder; sleep disorders induced by stress; pain perception such as fibromyalgia; mood disorders such as depression, including major depression, single episode depression, recurrent depression, child abuse induced depression, and postpartum depression; dysthemia; bipolar disorders; cyclothymia; fatigue syndrome; stress-induced headache; cancer, human immunodeficiency virus (HIV) infections; neurodegenerative diseases such as Alzheimer's disease, Parkinson's disease and Huntington's disease; gastrointestinal diseases such as ulcers, irritable bowel syndrome, Crohn's disease, spastic colon, diarrhea, and post operative ilius and colonic hypersensitivity associated by psychopathological disturbances or stress; eating disorders such as anorexia and bulimia nervosa; hemorrhagic stress; stress-induced psychotic episodes; euthyroid sick syndrome; syndrome of inappropriate antidiarrhetic hormone (ADH); obesity; infertility; head traumas; spinal cord trauma; ischemic neuronal damage (e.g. cerebral ischemia such as cerebral hippocampal ischemia); excitotoxic neuronal damage; epilepsy; cardiovascular and heart related disorders including hypertension, tachycardia and congestive heart failure; stroke; immune dysfunctions including stress induced immune dysfunctions (e.g., stress induced fevers, porcine stress syndrome, bovine shipping fever, equine paroxysmal fibrillation, and dysfunctions induced by confinement in chickens, sheering stress in sheep or human-animal interaction related stress in dogs); muscular spasms; urinary incontinence; senile dementia of the Alzheimer's type; multiinfarct dementia; amyotrophic lateral sclerosis; chemical dependencies and addictions (e.g., dependencies on alcohol, cocaine, heroin, benzodiazepines, or other drugs); drug and alcohol withdrawal symptoms; osteoporosis; psychosocial dwarfism; and hypoglycemia in a mammal.
The present invention provides a novel compound that binds to corticotropin releasing factor receptors, thereby altering the anxiogenic effects of CRF secretion. The compound of the present invention is useful for the treatment of psychiatric disorders and neurological diseases, anxiety-related disorders, post-traumatic stress disorder, supranuclear palsy and feeding disorders as well as treatment of immunological, cardiovascular or heart-related diseases and colonic hypersensitivity associated with psychopathological disturbance and stress in a mammal.
According to another aspect, the present invention provides a novel compound of Formula (I) (described below) which is useful as an antagonist of the corticotropin releasing factor. The compound of the present invention exhibits activity as a corticotropin releasing factor antagonist and appears to suppress CRF hypersecretion. The present invention also includes pharmaceutical compositions containing such a compound of Formula (I), and methods of using such a compound for the suppression of CRF hypersecretion, and/or for the treatment of anxiogenic disorders.
The use of competitive binding assays is considered particularly valuable for screening candidates for new drugs, e.g. to identify new CRF ligands or other compounds having even greater or more selective binding affinity for CRF receptors, which candidates would therefore be potentially useful as drugs. In the assay, one determines the ability of the candidate ligand to displace the labelled compound.
Therefore, another embodiment of the invention includes the use of a compound of the invention is a binding assay, wherein one or more of the compounds may be joined to a label, where the label can directly or indirectly provide a detectable signal. Various labels include radioisotopes, fluorescers, chemiluminescers, specific binding molecules, particles, e.g. magnetic particles, and the like.
Another embodiment of the invention is directed to the use of the compounds of the invention (particularly labeled compounds of this invention) as probes for the localization of receptors in cells and tissues and as standards and reagents for use in determining the receptor-binding characteristics of test compounds. Labeled compounds of the invention may be used for in vitro studies such as autoradiography of tissue sections or for in vivo methods, e.g. PET or SPECT scanning. Particularly, preferred compounds of the invention are useful as standards and reagents in determining the ability of a potential pharmaceutical to bind to the CRF1 receptor.
DETAILED DESCRIPTION OF THE INVENTION
[1] In a first embodiment, the present invention provides a compound of Formula (I):
and stereoisomeric forms thereof, or mixtures of stereoisomeric forms thereof, and pharmaceutically acceptable salt or pro-drug forms thereof.
[2] In another embodiment, the present invention provides a compound of embodiment [1], isomers thereof, stereoisomeric forms thereof, mixtures of stereoisomeric forms thereof, pharmaceutically acceptable prodrugs thereof, or pharmaceutically acceptable salt forms thereof, wherein said compound is 4-((R)-2-butylamino)2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-1,3,5-triazine.
[3] In another embodiment, the present invention provides a compound of any one of embodiments [1] to [2], pharmaceutically acceptable prodrugs thereof, or pharmaceutically acceptable salt forms thereof, wherein said compound is substantially free of its (S) stereoisomer.
[4] In another embodiment, the present invention provides a compound of embodiment [1], wherein said compound is 4-(2-butylamino)2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-1,3,5-triazine.
[5] In another embodiment, the present invention provides a compound of embodiment [1], wherein said compound is 4-((R)-2-butylamino)2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-1,3,5-triazine.
[6] A pharmaceutical composition comprising a pharmaceutically acceptable carrier and a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
[7] In another embodiment, the present invention provides a method of antagonizing a CRF receptor in a mammal, comprising administering to the mammal, a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
[8] In another embodiment, the present invention provides a method of treating a disorder manifesting hypersecretion of CRF in a warm-blooded animal, comprising administering to the animal a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
[9] In another embodiment, the present invention provides a method for the treatment of a disorder, the treatment of which can be effected or facilitated by antagonizing CRF, comprising administering to the mammal a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
[10] In another embodiment, the present invention provides a method of antagonizing a CRF receptor in a mammal, comprising administering to the mammal, a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
[11] In another embodiment, the present invention provides a method of treating anxiety or depression in mammals, comprising administering to the mammal a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
[12] In another embodiment, the present invention provides a method for screening for ligands for CRF receptors, which method comprises:
a) carrying out a competitive binding assay with a CRF receptor, a compound of any one of embodiments [1] to [5] which is labelled with a detectable label, and a candidate ligand; and b) determining the ability of said candidate ligand to displace said labelled compound.
[13] In another embodiment, the present invention provides a method for detecting CRF receptors in tissue comprising:
a) contacting a compound of any one of embodiments [1] to [5], which is labelled with a detectable label, with a tissue, under conditions that permit binding of the compound to the tissue; and b) detecting the labelled compound bound to the tissue.
[14] In another embodiment, the present invention provides a method of inhibiting the binding of CRF to a CRF-1 receptor, comprising contacting a compound of any one of embodiments [1] to [5] with a solution comprising cells expressing the CRF1 receptor, wherein the compound is present in the solution at a concentration sufficient to inhibit the binding of CRF to the CRF-1 receptor.
[15] In another embodiment, the present invention provides an article of manufacture comprising:
a) a packaging material; b) a compound of any one of embodiments [1] to [5]; and
a label or package insert contained within said packaging material indicating that said compound is effective for treating anxiety or depression.
[16] The present invention also comprises a method of treating affective disorder, anxiety, depression, headache, irritable bowel syndrome, post-traumatic stress disorder, supranuclear palsy, immune suppression, Alzheimer's disease, gastrointestinal diseases, anorexia nervosa or other feeding disorder, drug addiction, drug or alcohol withdrawal symptoms, inflammatory diseases, cardiovascular or heart-related diseases, fertility problems, human immunodeficiency virus infections, hemorrhagic stress, obesity, infertility, head and spinal cord traumas, epilepsy, stroke, ulcers, amyotrophic lateral sclerosis, hypoglycemia or a disorder the treatment of which can be effected or facilitated by antagonizing CRF, including but not limited to disorders induced or facilitated by CRF, in mammals comprising administering to the mammal a therapeutically effective amount of a compound of any one of embodiments [1] to [5].
Definitions
As used herein, the term “pharmaceutically acceptable salts” refers to salts prepared from pharmaceutically acceptable non-toxic acids, including inorganic acids and organic acids. Suitable non-toxic acids include inorganic and organic acids of basic residues such as amines, for example, acetic, benzenesulfonic, benzoic, amphorsulfonic, citric, ethenesulfonic, fumaric, gluconic, glutamic, hydrobromic, hydrochloric, isethionic, lactic, maleic, malic, mandelic, methanesulfonic, mucic, nitric, pamoic, pantothenic, phosphoric, succinic, sulfuric, tartaric acid, p-toluenesulfonic and the like; and alkali or organic salts of acidic residues such as carboxylic acids, for example, alkali and alkaline earth metal salts derived from the following bases: sodium hydride, sodium hydroxide, potassium hydroxide, calcium hydroxide, aluminum hydroxide, lithium hydroxide, magnesium hydroxide, zinc hydroxide, ammonia, trimethylammonia, triethylammonia, ethylenediamine, n-methyl-glucamine, lysine, arginine, ornithine, choline, N,N′-dibenzylethylenediamine, chloroprocaine, diethanolamine, procaine, n-benzylphenethylamine, diethylamine, piperazine, tris(hydroxymethyl)-aminomethane, tetramethylammonium hydroxide, and the like.
Pharmaceutically acceptable salts of the compounds of the invention can be prepared by reacting the free acid or base forms of these compounds with a stoichiometric amount of the appropriate base or acid in water or in an organic solvent, or in a mixture of the two; generally, nonaqueous media like ether, ethyl acetate, ethanol, isopropanol, or acetonitrile are preferred. Lists of suitable salts are found in Remington's Pharmaceutical Sciences, 17th ed., Mack Publishing Company, Easton, Pa., 1985, p. 1418, the disclosure of which is hereby incorporated by reference.
“Pharmaceutically acceptable prodrugs” as used herein means any covalently bonded carriers which release the active parent drug of Formula (I) in vivo when such prodrug is administered to a mammalian subject. Prodrugs of the compounds of Formula (I) are, within the scope of sound medical judgment, suitable for use in contact with the tissues of humans and lower animals with undue toxicity, irritation, allergic response, and the like, commensurate with a reasonable benefit/risk ratio, and effective for their intended use, as well as the zwitterionic forms, where possible, of the compounds of the invention. The term “prodrug” means compounds that are rapidly transformed in vivo to yield the parent compound of formula (I), for example by hydrolysis in blood. Functional groups which may be rapidly transformed, by metabolic cleavage, in vivo form a class of groups reactive with the carboxyl group of the compounds of this invention. They include, but are not limited to such groups as alkanoyl (such as acetyl, propionyl, butyryl, and the like), unsubstituted and substituted aroyl (such as benzoyl and substituted benzoyl), alkoxycarbonyl (such as ethoxycarbonyl), trialkylsilyl (such as trimethyl- and triethysilyl), monoesters formed with dicarboxylic acids (such as succinyl), and the like. Because of the ease with which the metabolically cleavable groups of the compounds useful according to this invention are cleaved in vivo, the compounds bearing such groups act as pro-drugs. The compounds bearing the metabolically cleavable groups have the advantage that they may exhibit improved bioavailability as a result of enhanced solubility and/or rate of absorption conferred upon the parent compound by virtue of the presence of the metabolically cleavable group. A thorough discussion of prodrugs is provided in the following: Design of Prodrugs, H. Bundgaard, ed., Elsevier, 1985; Methods in Enzymology, K. Widder et al, Ed., Academic Press, 42, p. 309-396, 1985; A Textbook of Drug Design and Development, Krogsgaard-Larsen and H. Bundgaard, ed., Chapter 5; “Design and Applications of Prodrugs” p. 113-191, 1991; Advanced Drug Delivery Reviews, H. Bundgard, 8, p. 1-38, 1992; Journal of Pharmaceutical Sciences, 77, p. 285, 1988; Chem. Pharm. Bull., N. Nakeya et al, 32, p. 692, 1984; Pro-drugs as Novel Delivery Systems, T. Higuchi and V. Stella, Vol. 14 of the A.C.S. Symposium Series, and Bioreversible Carriers in Drug Design, Edward B. Roche, ed., American Pharmaceutical Association and Pergamon Press, 1987, which are incorporated herein by reference.
“Prodrugs” are considered to be any covalently bonded carriers which release the active parent drug of Formula (I) in vivo when such prodrug is administered to a mammalian subject. Prodrugs of the compounds of Formula (I) are prepared by modifying functional groups present in the compounds in such a way that the modifications are cleaved, either in routine manipulation or in vivo, to the parent compounds. Prodrugs include compounds wherein hydroxy, amine, or sulfhydryl groups are bonded to any group that, when administered to a mammalian subject, cleaves to form a free hydroxyl, amino, or sulfhydryl group, respectively. Examples of prodrugs include, but are not limited to, acetate, formate and benzoate derivatives of alcohol and amine functional groups in the compounds of Formula (I), and the like.
As used herein to describe a compound, the term “substantially free of its (S) stereoisomer” means that the compound is made up of a significantly greater proportion of its (R) stereoisomer than of its optical antipode (i.e., its (S) stereoisomer). In a preferred embodiment of the invention, the term “substantially free of its (S) stereoisomer” means that the compound is made up of at least about 90% by weight of its (R) stereoisomer and about 10% by weight or less of its (S) stereoisomer.
In a more preferred embodiment of the invention, the term “substantially free of its (S) stereoisomer” means that the compound is made up of at least about 95% by weight of its (R) stereoisomer and about 5% by weight or less of its (S) stereoisomer. In an even more preferred embodiment, the term “substantially free of its (S) stereoisomer” means that the compound is made up of at least about 99% by weight of its (R) stereoisomer and about 1% or less of its (S) stereoisomer. In another preferred embodiment, the term “substantially free of its (S) stereoisomer” means that the compound is made up of nearly 100% by weight of its (R) stereoisomer. The above percentages are based on the total amount of the combined stereoisomers of the compound.
The term “therapeutically effective amount” of a compound of this invention means an amount effective to antagonize abnormal level of CRF or treat the symptoms of affective disorder, anxiety or depression in a host.
As used herein, the term “labeled” is meant that the compound is either directly or indirectly labeled with a label which provides a detectable signal, e.g. radioisotope, fluorescers, enzyme, antibodies, particles such as magnetic particles, chemiluminescer, P 32 , I 131 , and At 211 , etc.
Syntheses
Many organic compounds exist in optically active forms, i.e., they have the ability to rotate the plane of plane-polarized light. In describing an optically active compound, the prefixes D and L or R and S are used to denote the absolute configuration of the molecule about its chiral center(s). The prefixes d and l or (+) and (−) are employed to designate the sign of rotation of plane-polarized light by the compound, with (−) or l meaning that the compound is levorotatory. A compound prefixed with (+) or d is dextrorotatory. For a given chemical structure, these compounds, called stereoisomers, are identical except that they are mirror images of one another. A specific stereoisomer may also be referred to as an enantiomer, and a mixture of such isomers is often called an enantiomeric mixture. A 50:50 mixture of enantiomers is referred to as a racemic mixture.
The present invention includes all stereoisomeric forms of the compounds of the formula I. Centers of asymmetry that are present in the compounds of formula I can all independently of one another have S configuration or R configuration. The prefixes d and l or (+) and (−) are employed to designate the sign of rotation of plane-polarized light by the compound, with (−) or l meaning that the compound is levorotatory. A compound prefixed with (+) or d is dextrorotatory. The invention includes all possible enantiomers and diastereomers and mixtures of two or more stereoisomers, for example mixtures of enantiomers and/or diastereomers, in all ratios. Thus, enantiomers are a subject of the invention in enantiomerically pure form, both as levorotatory and as dextrorotatory antipodes, in the form of racemates and in the form of mixtures of the two enantiomers in all ratios. In the case of a cis/trans isomerism the invention includes both the cis form and the trans form as well as mixtures of these forms in all ratios. The preparation of individual stereoisomers can be carried out, if desired, by separation of a mixture by customary methods, for example by chromatography or crystallization, by the use of stereochemically uniform starting materials for the synthesis or by stereoselective synthesis. Optionally a derivatization can be carried out before a separation of stereoisomers. The separation of a mixture of stereoisomers can be carried out at the stage of the compounds of the formula I or at the stage of an intermediate during the synthesis. The present invention also includes all tautomeric forms of the compounds of formula (I).
The compound of Formula (I) may be prepared from using the procedures outlined in Scheme 1.
A compound of Formula (II), where X=F, may be treated with a metal alkoxide (e.g. sodium methoxide, potassium methoxide; pre-formed or generated in situ) in an inert solvent to generate an intermediate of Formula (III). Inert solvents may include, but are not limited to, alkyl alcohols (1 to 8 carbons, preferably methanol or ethanol), lower alkanenitriles (1 to 6 carbons, preferably acetonitrile), water, dialkyl ethers (preferably diethyl ether), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one), dialkylsulfoxides (preferably dimethylsulfoxide) or aromatic hydrocarbons (preferably benzene or toluene). Preferred reaction temperatures range from 0° C. to 100° C.
Alternatively, a compound of Formula (II), where X=OH, may be treated with an alkylating agent in the presence of a base in an inert solvent to generate an intermediate of Formula (III). Alkylating agents include, but are not limited to, haloalkanes (e.g. CH 3 I), dialkyl sulfates (e.g. Me 2 SO 4 ) or alkyl trifluoro-sulfonates (e.g. CH 3 O 3 SCF 3 ).
Bases may include, but are not limited to, alkali metals, alkali metal hydrides (preferably sodium hydride), alkali metal alkoxides (1 to 6 carbons)(preferably sodium methoxide or sodium ethoxide), alkaline earth metal hydrides, alkali metal carbonates, alkaline metal carbonates, transition metal carbonates (e.g. silver carbonate), alkali metal dialkylamides (preferably lithium di-isopropylamide), alkali metal bicarbonates, alkali metal hydroxides, alkali metal bis(trialkylsilyl)amides (preferably sodium bis(trimethylsilyl)amide), trialkyl amines (preferably N,N-di-isopropyl-N-ethyl amine) or aromatic amines (preferably pyridine).
Inert solvents may include, but are not limited to, halocarbons (1 to 8 carbons, 1 to 8 halogens), lower alkanenitriles (1 to 6 carbons, preferably acetonitrile), water, dialkyl ethers (preferably diethyl ether), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one), dialkylsulfoxides (preferably dimethylsulfoxide) or aromatic hydrocarbons (preferably benzene or toluene). Preferred reaction temperatures range from 50° C. to 150° C.
A compound of Formula (III) may be transformed to a compound of Formula (IV) by reaction with a brominating agent in the presence or absence of an additive in an inert solvent. Brominating agents include, but are not limited to, N-bromosuccinimide-2,2′-azobisisobutyro-nitrile (AIBN), N-bromophthalimide-2,2′-azobisiso-butyronitrile (AIBN)), bromine. Additives include, but are not limited to, alkali metal phosphates (e.g. K 3 PO 4 , Na 3 PO 4 ), alkali metal hydrogen phosphates (e.g. Na 2 HPO 4 , K 2 HPO 4 ), alkali metal dihydrogen phosphates (e.g. NaH 2 PO 4 , KH 2 PO 4 ). Inert solvents include, but are not limited to, halocarbons (1 to 6 carbons, 1 to 6 halogens (preferably chlorine), water, N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one). Reaction temperatures range from 0° C. to 200° C. (preferably 20° C. to 120° C.).
A compound of Formula (IV) may be converted to a compound of Formula (V) by sequential reactions with (1) an alkyl lithium in an inert solvent at temperatures ranging from −100° C. to 50° C.; (2) a compound of the Formula B(OR a ) 3 (where R a is branched or straight chain alkyl of 1 to 20 carbons) at temperatures ranging from −100° C. to 50° C. and (3) an acid in the presence or absence of water at temperatures ranging from −100° C. to 100° C. Alkyl lithiums may be branched or straight chain compounds containing 1 to 20 carbons. Inert solvents include, but are not limited to, dialkyl ethers (preferably diethyl ether), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), or aromatic hydrocarbons (preferably benzene or toluene).
Acids may include, but are not limited to, alkanoic acids of 2 to 10 carbons (preferably acetic acid), haloalkanoic acids (2-10 carbons, 1-10 halogens, such as trifluoroacetic acid), arylsulfonic acids (preferably p-toluenesulfonic acid or benzenesulfonic acid), alkanesulfonic acids of 1 to 10 carbons (preferably methanesulfonic acid), hydrochloric acid, sulfuric acid or phosphoric acid.
A compound of Formula (VII) may be produced by reaction of a compound of Formula (V) with a compound of Formula (VI) in the presence of a complex or salt of palladium or nickel, a base and an inert solvent. Complexes of palladium or nickel include, but are not limited to, phosphine complexes such as Pd(PPh 3 ) 4 , PdCl 2 (PPh 3 ) 2 , NiCl 2 (PPh 3 ) 2 , or [1,1-bis(diphenylphosphino)ferrocene]-dichloropalladium. Bases may include, but are not limited to, alkali metals, alkali metal hydrides (preferably sodium hydride), alkali metal alkoxides (1 to 6 carbons)(preferably sodium methoxide or sodium ethoxide), alkali metal carbonates, alkaline metal carbonates (e.g. barium carbonate), transition metal carbonates (e.g. silver carbonate) or trialkyl amines (e.g. triethyl amine). Inert solvents may include, but are not limited to, dialkyl ethers (preferably diethyl ether), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), or aromatic hydrocarbons (preferably benzene or toluene). Preferred reaction temperatures range from −100° C. to 100° C.
An intermediate of Formula (VII) may be reacted with a base in the presence of an inert solvent to afford a compound of Formula (VIII), where M is an alkali metal cation (e.g. sodium or potassium). Bases may include, but are not limited to, alkali metal hydroxides (e.g. NaOH or KOH), alkali metal alkoxides (1 to 6 carbons) (preferably sodium methoxide or sodium ethoxide) or alkaline earth metal hydroxides. Inert solvents may include, but are not limited to, alkyl alcohols (1 to 6 carbons), lower alkanenitriles (1 to 6 carbons, preferably acetonitrile), water, cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one), dialkylsulfoxides (preferably dimethylsulfoxide). Preferred reaction temperatures range from 0° C. to 150° C.
Compounds of Formula (VIII) may be treated with hydrazine-hydrate in the presence of an acid and an inert solvent at temperatures ranging from 0° C. to 200° C., preferably 70° C. to 150° C., to produce compounds of Formula (IX). Acids may include, but are not limited to, alkanoic acids of 2 to 10 carbons (preferably acetic acid), haloalkanoic acids (2-10 carbons, 1-10 halogens, such as trifluoroacetic acid), arylsulfonic acids (preferably p-toluenesulfonic acid or benzenesulfonic acid), alkanesulfonic acids of 1 to 10 carbons (preferably methanesulfonic acid), hydrochloric acid, sulfuric acid or phosphoric acid.
Inert solvents may include, but are not limited to, water, alkyl alcohols (1 to 8 carbons, preferably methanol or ethanol), lower alkanenitriles (1 to 6 carbons, preferably acetonitrile), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one), dialkylsulfoxides (preferably dimethylsulfoxide) or aromatic hydrocarbons (preferably benzene or toluene).
A compound of Formula (IX) may be reacted with compounds of Formula H 3 C(C═NH)OR c (where R c is alkyl (1-6 carbons)) in the presence or absence of an acid in the presence of an inert solvent at temperatures ranging from 0° C. to 200° C. to produce a compound of Formula (X). Acids may include, but are not limited to alkanoic acids of 2 to 10 carbons (preferably acetic acid), haloalkanoic acids (2-10 carbons, 1-10 halogens, such as trifluoroacetic acid), arylsulfonic acids (preferably p-toluenesulfonic acid or benzenesulfonic acid), alkanesulfonic acids of 1 to 10 carbons (preferably methanesulfonic acid), hydrochloric acid, sulfuric acid or phosphoric acid. Stoichiometric or catalytic amounts of such acids may be used.
Inert solvents may include, but are not limited to, water, alkanenitriles (1 to 6 carbons, preferably acetonitrile), halocarbons of 1 to 6 carbons and 1 to 6 halogens (preferably dichloroethane or chloroform), alkyl alcohols of 1 to 10 carbons (preferably ethanol), dialkyl ethers (4 to 12 carbons, preferably diethyl ether or di-isopropylether) or cyclic ethers such as dioxan or tetrahydrofuran. Preferred temperatures range from 0° C. to 100° C.
A compound of Formula (X) may be converted to an intermediate compound of Formula (XI) by treatment with compounds C═O(R d ) 2 (where R d is halogen (preferably chlorine), alkoxy (1 to 4 carbons) or alkylthio (1 to 4 carbons)) in the presence or absence of a base in an inert solvent at reaction temperatures from −50° C. to 200° C. Bases may include, but are not limited to, alkali metal hydrides (preferably sodium hydride), alkali metal alkoxides (1 to 6 carbons) (preferably sodium methoxide or sodium ethoxide), alkali metal carbonates, alkali metal hydroxides, trialkyl amines (preferably N,N-di-isopropyl-N-ethyl amine or triethylamine) or aromatic amines (preferably pyridine).
Inert solvents may include, but are not limited to, alkyl alcohols (1 to 8 carbons, preferably methanol or ethanol), lower alkanenitriles (1 to 6 carbons, preferably acetonitrile), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one), dialkylsulfoxides (preferably dimethylsulfoxide) or aromatic hydrocarbons (preferably benzene or toluene).
A compound of Formula (XD may be treated with a halogenating agent in the presence or absence of a base in the presence or absence of an inert solvent at reaction temperatures ranging from −80° C. to 250° C. to give a halogenated intermediate (XII) (where X is halogen). Halogenating agents include, but are not limited to, SOCl 2 , POCl 3 , PCl 3 , PCl 5 , POBr 3 , PBr 3 or PBr 5 . Bases may include, but are not limited to, trialkyl amines (preferably N,N-di-isopropyl-N-ethyl amine or triethylamine) or aromatic amines (preferably N,N-diethylaniline).
Inert solvents may include, but are not limited to, N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one) or aromatic hydrocarbons (preferably benzene or toluene). Preferred reaction temperatures range from 20° C. to 200° C.
A compound of Formula (XII) may be reacted with an alkyl amine in the presence or absence of a base in the presence or absence of an inert solvent at reaction temperatures ranging from −80 ° to 250° C. to generate compounds of Formula (I). Bases may include, but are not limited to, alkali metal hydrides (preferably sodium hydride), alkali metal alkoxides (1 to 6 carbons) (preferably sodium methoxide or sodium ethoxide), alkaline earth metal hydrides, alkali metal dialkylamides (preferably lithium di-isopropylamide), alkali metal carbonates, alkali metal bicarbonates, alkali metal bis(trialkylsilyl)amides (preferably sodium bis(trimethylsilyl)amide), trialkyl amines (preferably N,N-di-isopropyl-N-ethyl amine) or aromatic amines (preferably pyridine).
Inert solvents may include, but are not limited to, alkyl alcohols (1 to 8 carbons, preferably methanol or ethanol), lower alkanenitriles (1 to 6 carbons, preferably acetonitrile), dialkyl ethers (preferably diethyl ether), cyclic ethers (preferably tetrahydrofuran or 1,4-dioxane), N,N-dialkylformamides (preferably dimethylformamide), N,N-dialkylacetamides (preferably dimethylacetamide), cyclic amides (preferably N-methylpyrrolidin-2-one), dialkylsulfoxides (preferably dimethylsulfoxide), aromatic hydrocarbons (preferably benzene or toluene) or haloalkanes of 1 to 10 carbons and 1 to 10 halogens (preferably dichloroethane). Preferred reaction temperatures range from 0° C. to 140° C.
The compounds of the invention may be prepared as radiolabeled compounds by carrying out their synthesis using precursors comprising at least one atom that is a radioisotope. The radioisotope is preferably selected from of at least one of carbon (preferably 14 C), hydrogen (preferably 3 H), sulfur (preferably 35 S), or iodine (preferably 125 I). Such radiolabeled probes are conveniently synthesized by a radioisotope supplier specializing in custom synthesis of radiolabeled probe compounds. Such suppliers include Amersham Corporation, Arlington Heights, Ill.; Cambridge Isotope Laboratories, Inc. Andover, Mass.; SRI International, Menlo Park, Calif.; Wizard Laboratories, West Sacramento, Calif.; ChemSyn Laboratories, Lexena, Kans.; American Radiolabeled Chemicals, Inc., St. Louis, Mo.; and Moravek Biochemicals Inc., Brea, Calif.
Tritium labeled probe compounds may also conveniently be prepared catalytically via platinum-catalyzed exchange in tritiated acetic acid, acid-catalyzed exchange in tritiated trifluoroacetic acid, or heterogeneous-catalyzed exchange with tritium gas. Such preparations are also conveniently carried out as a custom radiolabeling by any of the suppliers listed in the preceding paragraph using the compound of the invention as substrate. In addition, certain precursors may be subjected to tritium-halogen exchange with tritium gas, tritium gas reduction of unsaturated bonds, or reduction using sodium borotritide, as appropriate.
Receptor autoradiography (receptor mapping) may be carried out in vitro as described by Kuhar in sections 8.1.1 to 8.1.9 of Current Protocols in Pharmacology (1998) John Wiley & Sons, New York, using radiolabeled compounds of the invention.
EXAMPLES
Analytical data were recorded for the compounds described below using the following general procedures. Proton NMR spectra were recorded on a Varian VXR or Unity 300 FT-NMR instruments (300 MHz); chemical shifts were recorded in ppm (δ) from an internal tetramethysilane standard in deuterochloroform or deuterodimethylsulfoxide as specified below. Mass spectra (MS) or high resolution mass spectra (HRMS) were recorded on a Finnegan MAT 8230 spectrometer or a Hewlett Packard 5988A model spectrometer (using chemi-ionization (CI) with NH 3 as the carrier gas, electrospray (ESI), atmospheric pressure chemi-ionization (APCI) or gas chromatography (GC)). Melting points were recorded on a MelTemp 3.0 heating block apparatus and are uncorrected. Boiling points are uncorrected. All pH determinations during workup were made with indicator paper.
Reagents were purchased from commercial sources and, where necessary, purified prior to use according to the general procedures outlined by D. Perrin and W. L. F. Armarego, Purification of Laboratory Chemicals, 3rd ed., (New York: Pergamon Press, 1988). Chromatography was performed on silica gel using the solvent systems indicated below. For mixed solvent systems, the volume ratios are given. Otherwise, parts and percentages are by weight. Commonly used abbreviations are: DMF (N,N-dimethylformamide), EtOH (ethanol), MeOH (methanol), EtOAc (ethyl acetate), HOAc (acetic acid), DME (1,2-diethoxyethane) and THF (tetrahydrofuran).
The following examples are provided to describe the invention in further detail. These examples, which set forth the best mode presently contemplated for carrying out the invention, are intended to illustrate and not to limit the invention.
Example 1
Preparation of 2,7-dimethyl-8(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-[1,3,5]-triazin-4(3H)-one
A. 2-Methoxy-6-methylpyridine
Sodium (31.0 g, 1.35 mol) was added portionwise to methanol (500 mL) over 30 min with stirring in a flask equipped with a reflux cindenser. After the addition was complete, the reaction mixture was allowed to cool to ambient temperature. 2-Fluoro-6-methylpyridine (50 g, 450 mmol) was added portionwise with stirring. The reaction mixture was then heated to reflux temperature and stirred for 48 h. The mix was then cooled to ambient temperature and solvent was removed in vacuo to provide a yellow oil. The residue was taken up in water (500 mL) and three extractions with ether (200 mL) were performed. The combined organic layers were dried over MgSO 4 , filtered and solvent was removed in vacuo from the filtrate to give a yellow liquid: 1 H-NMR(CDCl 3 , 300 MHz): δ 7.44 (dd, 1H, J=8, 7), 6.71 (d, 1H, J=7), 6.53 (d, 1H, J=8), 3.91 (s, 3H), 2.45 (s, 3H).
B. 2-Methoxy-6-methylpyridine
A mixture of 2-hydroxy-6-methylpyridine (6.85 g, 62.8 mmol), silver carbonate (22.5 g, 81.6 mmol), iodomethane (39.1 mL, 628 mmol) and chloroform (200 mL) was stirred at ambient temperature for 40 h in the dark. The reaction mixture was filtered through celite. The collected solid was washed with ether. The combined filtrates were concentrated in vacuo to give a liquid (6.25 g), which was identical to the product from Part A.
C. 6-Methoxy-3-bromo-2-methylpyridine
A mixture of 2-methoxy-6-methylpyridine (17.0 g, 138 mmol) and a solution of disodium hydrogen phosphate (0.15M in water, 250 mL) was stirred at room temperature. Bromine (7.1 mL, 138 mmol) was added dropwise over 15 min via an addition funnel. The reaction mixture was then stirred at room temperature for 4 h. The clear colorless solution was diluted with water (500 mL) and extracted with dichloromethane (200 mL) three times. The combined organic layers were dried over MgSO 4 , filtered and solvent was removed in vacuo from the filtrate to give a yellow liquid. Flash chromatography on silica gel (EtOAc:hexane::1:20) and removal of solvent from the desired combined fractions afforded a clear colorless liquid (15.4 g): 1 H-NMR(CDCl 3 , 300 MHz): δ 7.60(d, 1H, J=8), 6.46 (d, 1H, J=8), 3.89 (s, 3H), 2.54 (s, 3H).
D. 6-Methoxy-2-methylpyridine-3-boronic acid
A solution of 6-methoxy-3-bromo-2-methylpyridine (59.8 g, 296 mmol) in dry THF (429 mL) was cooled with stirring to ˜−78° C. under a nitrogen atmosphere. A solution of n-butyl lithium (2.5 M, 130.4 mL, 326 mmol) in hexane was added dropwise over 30 min. The reaction mixture was stirred for 3 h at ˜−78° C. A solution of tri-isopropyl borate (102.7 mL, 445 mmol) in dry THF (100 mL) was added dropwise over 30 min. The reaction mixture was warmed to ambient temperature with stirring over 16 h. Acetic acid (37.35 g, 622 mmol), then water (110 mL) were added to the reaction mixture with stirring. After 2 h, the layers were separated and the organic layer was concentrated in vacuo. The residue was taken up in 2-propanol (750 mL) and solvent was removed on a rotary evaporator (bath temperature ˜50° C). The residue was triturated with ether. The product was collected by filtration and dried in vacuo (48.4 g): mp>200° C.; 1 H-NMR(CD 3 OH, 300 MHz): δ 7.83 (d, 1H, J=8), 6.56 (d, 1H, J=8), 3.85 (s, 3H), 2.44 (s, 3H); GC-MS: 168 (M + +H).
E. 2-Methyl-3-(5-methylisoxazol-4-yl)-6-methoxypyridine
A mixture of 4-iodo-5-methylisoxazole (18.2 g, 87 mmol), 6-methoxy-2-methylpyridine-3-boronic acid (14.6 g, 87 mmol), sodium bicarbonate (22.0 g, 262 mmol), water (150 mL) and DME (150 mL) was degassed three times with stirring by the application of a vacuum and then introduction of a nitrogen atmosphere. [1,1-Bis(diphenylphosphino)ferrocene]-dichloropalladium (II) (2.14 g, 2.6 mmol) was added in one portion. The reaction mixture was degassed as before. The reaction mixture was then stirred at 80° C. for 4 h, then it was cooled to ambient temperature. Three extractions with EtOAc, drying the combined organic layers over MgSO 4 , filtration and removal of solvent in vacuo afforded an oil. Flash chromatography (EtOAc:hexane::1:9) and removal of solvent in vacuo from the desired fractions gave the product (7.15 g): 1 H-NMR(CDCl 3 , 300 MHz): δ 8.16 (s, 1H), 7.33 (d, 1H, J=8), 6.63 (d, 1H, J=8), 3.95 (s, 3H), 2.35 (s, 6H); APCI + -MS: 205 (M + +H).
F. 1-Cyano-1-(2-methyl-6-methoxypyrid-3-yl)propan-2-one, Sodium Salt
A mixture of sodium methoxide (25% w/w, 13 mL, 70 mmol), 2-methyl-3-(5-methylisoxazol-4-yl)-6-methoxypyridine (7.15 g, 35 mmol) and methanol (50 mL) was stirred at room temperature for 16 h. Solvent was removed in vacuo to give a yellow oil. Trituration with ether, filtration and drying in vacuo afforded the crude product as a white solid (9.3 g).
G. 5-Amino-4-(2-methyl-6-methoxypyrid-3-yl)-3-methylpyrazole
A mixture of 1-cyano-1-(2-methyl-6-methoxypyrid-3-yl)propan-2-one, sodium salt (9.3 g), hydrazine-hydrate (6 mL, 123.3 mmol) and glacial acetic acid (150 mL) was stirred at room temperature for 4 h. The reaction mixture was concentrated in vacuo. The residue was dissolved in 1N HCl and the resulting solution was extracted with EtOAc two times. A 1N NaOH solution was added to the aqueous layer until pH=12. The resulting semi-solution was extracted three times with ethyl acetate. The combined organic layers were dried over MgSO 4 and filtered. Solvent was removed in vacuo to give a viscous oil (5.8 g): 1 -NMR (CDCl 3 , 300 MHz): 7.37 (d, 2H, J=8), 6.62 (d, 2H, J=8), 3.95 (s, 3H), 2.36 (s, 3H), 2.08 (s, 3H); APCI + -MS: 219 (M + +H); 260 (M + +CH 3 CN).
H. 5-Acetamidino-4-(2-methyl-6-methoxypyrid-3-yl)-3-methylpyrazole, acetic acid salt
Ethyl acetamidate hydrochloride (6.46 g, 52.2 mmol) was added quickly to a rapidly stirred mixture of potassium carbonate (6.95 g, 50.0 mol), dichloromethane (60 mL) and water (150 mL). The layers were separated and the aqueous layer was extracted with dichloromethane (2×60 mL). The combined organic layers were dried over MgSO 4 and filtered. Solvent was removed by simple distillation and the pot residue, a clear pale yellow liquid, was used without further purification.
Glacial acetic acid (1.0 mL, 17.4 mmol) was added to a stirred mixture of 5-amino-4-(2-methyl-6-methoxypyrid-3-yl)-3-methylpyrazole (3.8 g, 17.4 mmol), ethyl acetamidate free base and dichloromethane (100 mL). The resulting reaction mixture was stirred at room temperature for 16 h; at the end of which time, it was concentrated in vacuo. The residue was triturated with ether, the product was filtered and washed with copious amounts of ether. The white solid was dried in vacuo (5.4 g): 1 H-NMR (CD 3 OH, 300 MHz): 7.43 (d, 2H, J=8), 6.69 (d, 2H, J=8), 4.9 (br s, 2H), 3.93 (s, 3H), 2.31 (s, 3H), 2.24 (s, 3H), 2.13 (s, 3H), 1.88 (s, 3H); APCI + -MS: 260 (M + +H).
I. 2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-[1,3,5]-triazin-4(3H)-one
Sodium pellets (3.9 g, 169 mmol) were added portionwise to ethanol (200 mL) with vigorous stirring. After all the sodium reacted, 5-acetamidino-4-(2-methyl-6-methoxypyrid-3-yl)-3-methylpyrazole, acetic acid salt (5.4 g, 16.9 mmol) and diethyl carbonate (16.4 mL, 135.3 mmol) were added. The resulting reaction mixture was heated to reflux temperature and stirred for 18 hours. The mix was cooled to room temperature and solvent was removed in vacuo. The residue was dissolved in water and a 1N HCl solution was added slowly until pH˜6. The aqueous layer was extracted with EtOAc three times; the combined organic layers were dried over MgSO 4 and filtered. Solvent was removed in vacuo to give a solid. Trituration with ether, filtration and drying in vacuo afforded a white solid (3.9 g): 1 H-NMR (CD 3 OH, 300 MHz): 7.49 (d, 2H, J=8), 6.69 (d, 2H, J=8), 3.93 (s, 3H), 2.35 (s, 3H), 2.28 (s, 3H), 2.24 (s, 3H); APCI + -MS: 286 (M + +H).
Example 2
Preparation of 4-((R)-2-butylamino)2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-1,3,5-triazine
A. 4-Chloro-2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolotriazine
A mixture of 2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-1,3,5-triazin-4-one (Example 1, 3.9 g, 13.7 mmol), di-isopropyl-ethylamine (9.5 mL, 54.7 mmol), phosphorus oxychloride (5.1 mL, 54.7 mmol) and toluene (75 mL) was stirred at reflux temperature for 4 h. The volatiles were removed in vacuo. The residue was loaded on a pad of silica gel on celite and eluted with a 1:1 mixture of EtOAc and hexane. Solvent was removed in vacuo from the filtrate to give an oil.
B. 4-((R)-2-butylamino)2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolo-1,3,5-triazine
A mixture of 4-chloro-2,7-dimethyl-8-(2-methyl-6-methoxypyrid-3-yl)[1,5-a]-pyrazolotriazine, (R)-2-butylamine (2.0 mL, 20.5 mmol), di-isopropyl-ethylamine (9.5 mL, 54.7 mmol) and dry THF (25 mL) was stirred at ambient temperature for 18 hours. Solvent was removed in vacuo. Column chromatography of the residue (first using EtOAc:hexane::1:2, then using EtOAc:hexane::1:4) afforded the product. Removal of solvent in vacuo gave a white solid (2.3 g): mp=118.3° C.; 1 H-NMR (CDCl 3 , 300 MHz): δ 7.41 (d, 1H, J=8), 6.63 (d, 1H, J=8), 6.25 (br d, 1H, J=9), 4.35-4.30 (m, 1H), 3.95 (s, 3H), 2.49 (s, 3H), 2.35 (s, 3H), 2.30 (s, 3H), 1.76-1.66 (m, 2H), 1.34 (d, 3H, J=7), 1.02 (t, 3H, J=7); 13 C-NMR (CDCl 3 , 100.52 MHz): δ 163.8, 163.0, 155.7, 153.7, 147.8, 146.6, 141.6, 118.5, 107.4, 106.6, 53.3, 48.2, 29.7, 26.1, 22.9, 20.4, 13.1, 10.3; IR (neat, KBr, cm −1 ): 3380 (m), 3371 (m), 2968 (m), 2928 (m), 2872 (w), 1621 (s), 1588 (s), 1544 (s), 1489 (s), 1460 (s), 1425 (s), 1413 (s), 1364 (s), 1346 (m), 1304 (s) 1275 (s), 1247 (s), 1198 (m), 1152 (m), 1134 (m), 1112 (m), 1034 (s), 1003 (m); ESI(+)-HRMS: Calcd for C 18 H 24 N 6 O: 341.2089. Found: 341.2093 (M + +H). Anal. Calcd for C 18 H 24 N 6 O: C, 63.51; H, 7.12; N, 24.69. Found: C, 63.67; H, 7.00; N, 24.49.
Utility
Rat CRF Receptor Binding Assay for the Evaluation of Biological Activity.
Receptor binding affinity to rat cortical receptors was assayed according to the published methods (E. B. De Souza, J. Neuroscience, 7: 88 (1987).
Curves of the inhibition of [ 125 I-Tyr 0 ]-o-CRF binding to cell membranes at various dilutions of test drug were analyzed by the iterative curve fitting program LIGAND [P. J. Munson and D. Rodbard, Anal. Biochem. 107:220 (1980), which provides Ki values for inhibition which are then used to assess biological activity.
Inhibition of CRF-Stimulated Adenylate Cyclase Activity
Inhibition of CRF-stimulated adenylate cyclase activity can be performed as described by G. Battaglia et al. Synapse 1:572 (1987). Briefly, assays are carried out at 37° C. for 10 min in 200 ml of buffer containing 100 mM Tris-HCl (pH 7.4 at 37° C.), 10 mM MgCl 2 , 0.4 mM EGTA, 0.1% BSA, 1 mM isobutylmethylxanthine (IBMX), 250 units/ml phosphocreatine kinase, 5 mM creatine phosphate, 100 mM guanosine 5′-triphosphate, 100 nM oCRF, antagonist peptides (concentration range 10 −9 to 10 −6m ) and 0.8 mg original wet weight tissue (approximately 40-60 mg protein). Reactions are initiated by the addition of 1 mM ATP/ 32 P]ATP (approximately 2-4 mCi/tube) and terminated by the addition of 100 ml of 50 mM Tris-HCL, 45 mM ATP and 2% sodium dodecyl sulfate. In order to monitor the recovery of cAMP, 1 μl of [ 3 H]cAMP (approximately 40,000 dpm) is added to each tube prior to separation. The separation of [ 32 P]cAMP from [ 32 P]ATP is performed by sequential elution over Dowex and alumina columns.
In Vivo Biological Assay
The in vivo activity of a compound of the present invention can be assessed using any one of the biological assays available and accepted within the art. Illustrative of these tests include the Acoustic Startle Assay, the Stair Climbing Test, and the Chronic Administration Assay. These and other models useful for the testing of compounds of the present invention have been outlined in C. W. Berridge and A. J. Dunn Brain Research Reviews 15:71 (1990).
A compound may be tested in any species of rodent or small mammal.
A compound of this invention has utility in the treatment of imbalances associated with abnormal levels of corticotropin releasing factor in patients suffering from depression, affective disorders, and/or anxiety.
A compound of this invention can be administered to treat these abnormalities by means that produce contact of the active agent with the agent's site of action in the body of a mammal. The compounds can be administered by any conventional means available for use in conjunction with pharmaceuticals either as individual therapeutic agent or in combination of therapeutic agents. It can be administered alone, but will generally be administered with a pharmaceutical carrier selected on the basis of the chosen route of administration and standard pharmaceutical practice.
The dosage administered will vary depending on the use and known factors such as pharmacodynamic character of the particular agent, and its mode and route of administration; the recipient's age, weight, and health; nature and extent of symptoms; kind of concurrent treatment; frequency of treatment; and desired effect. For use in the treatment of said diseases or conditions, a compound of this invention can be orally administered daily at a dosage of the active ingredient of 0.002 to 200 mg/kg of body weight. Ordinarily, a dose of 0.01 to 10 mg/kg in divided doses one to four times a day, or in sustained release formulation will be effective in obtaining the desired pharmacological effect.
Dosage forms (compositions) suitable for administration contain from about 1 mg to about 100 mg of active ingredient per unit. In these pharmaceutical compositions, the active ingredient will ordinarily be present in an amount of about 0.5 to 95% by weight based on the total weight of the composition.
The active ingredient can be administered orally in solid dosage forms, such as capsules, tablets and powders; or in liquid forms such as elixirs, syrups, and/or suspensions. The compounds of this invention can also be administered parenterally in sterile liquid dose formulations.
Gelatin capsules can be used to contain the active ingredient and a suitable carrier such as but not limited to lactose, starch, magnesium stearate, steric acid, or cellulose derivatives. Similar diluents can be used to make compressed tablets. Both tablets and capsules can be manufactured as sustained release products to provide for continuous release of medication over a period of time. Compressed tablets can be sugar-coated or film-coated to mask any unpleasant taste, or used to protect the active ingredients from the atmosphere, or to allow selective disintegration of the tablet in the gastrointestinal tract.
Liquid dose forms for oral administration can contain coloring or flavoring agents to increase patient acceptance.
In general, water, pharmaceutically acceptable oils, saline, aqueous dextrose (glucose), and related sugar solutions and glycols, such as propylene glycol or polyethylene glycol, are suitable carriers for parenteral solutions. Solutions for parenteral administration preferably contain a water soluble salt of the active ingredient, suitable stabilizing agents, and if necessary, butter substances. Antioxidizing agents, such as sodium bisulfite, sodium sulfite, or ascorbic acid, either alone or in combination, are suitable stabilizing agents. Also used are citric acid and its salts, and EDTA. In addition, parenteral solutions can contain preservatives such as benzalkonium chloride, methyl- or propyl-paraben, and chlorobutanol.
Suitable pharmaceutical carriers are described in “Remington's Pharmaceutical Sciences”, A. Osol, a standard reference in the field.
Useful pharmaceutical dosage-forms for administration of the compounds of this invention can be illustrated as follows:
Capsules
A large number of units capsules are prepared by filling standard two-piece hard gelatin capsules each with 100 mg of powdered active ingredient, 150 mg lactose, 50 mg cellulose, and 6 mg magnesium stearate.
Soft Gelatin Capsules
A mixture of active ingredient in a digestible oil such as soybean, cottonseed oil, or olive oil is prepared and injected by means of a positive displacement was pumped into gelatin to form soft gelatin capsules containing 100 mg of the active ingredient. The capsules were washed and dried.
Tablets
A large number of tablets are prepared by conventional procedures so that the dosage unit was 100 mg active ingredient, 0.2 mg of colloidal silicon dioxide, 5 mg of magnesium stearate, 275 mg of microcrystalline cellulose, 11 mg of starch, and 98.8 mg lactose. Appropriate coatings may be applied to increase palatability or delayed adsorption.
The compounds of this invention may also be used as reagents or standards in the biochemical study of neurological function, dysfunction, and disease.
Although the present invention has been described and exemplified in terms of certain preferred embodiments, other embodiments will be apparent to those skilled in the art. The invention is, therefore, not limited to the particular embodiments described and exemplified, but is capable of modification or variation without departing from the spirit of the invention, the full scope of which is delineated by the appended claims. | Corticotropin releasing factor (CRF) antagonists of Formula (I):
and its use in treating anxiety, depression, and other psychiatric, neurological disorders as well as treatment of immunological, cardiovascular or heart-related diseases and colonic hypersensitivity associated with psychopathological disturbance and stress. | 0 |
RELATED APPLICATION INFORMATION
This application claims the benefit of and is a continuation of U.S. application Ser. No. 12/406,601, filed on Mar. 18, 2009, which application, in turn, claims the benefit of U.S. Provisional Application No. 61/037,759, filed Mar. 19, 2008, the disclosures of which are incorporated herein by reference in its entirety.
BACKGROUND
Portable controlling devices, such as for example universal remote controls, and the features and functions offered by such devices are well known in the art. Increasingly, implementations of these devices incorporate technologies such as color touch screens supporting graphical user interfaces, wireless home network compatibility, command relay stations positioned to control appliances not situated in line of sight of the controlling device, etc.
Contemporaneously, personal communication, productivity, and entertainment devices such as cellular phones, portable email devices, music players, hand-held games, etc. are also increasingly offering features such as graphical user interfaces (“GUI”) on color touch screens, wireless Internet capability, etc. Recently, manufacturers of such platforms have begun to encourage the development of native third party applications which enhance the utility of these devices.
SUMMARY OF THE INVENTION
This invention relates generally to a system and method for enabling control of consumer electronic appliances via a graphical user interface implemented on touch screen equipped personal communication or entertainment devices which include wireless local network capability, such as for example the iPhone® or iPod Touch® products from Apple®. Since such devices do not inherently provide a capability to directly communicate commands to the appliances to be controlled, a network connected relay station is provided which receives control requests from a software application installed on a personal communication or entertainment device and converts these requests into appliance compatible infrared (“IR”) or radio frequency (“RF”) command transmissions.
In this regard, Apple has recently released a software development kit (“SDK”) for developing and distributing custom third party applications for the iPhone and iPod Touch devices. This SDK provides a full featured and supported environment for developing software that runs on the devices, allowing accessory applications that leverage the features built into these devices, such as integrated Wi-Fi connectivity, multi-point touch screen interface with gesture recognition, location services, audio and video capabilities, 3-axis accelerometer, proximity sensor, etc. Where necessary for a complete understanding of the invention disclosed herein, exemplary embodiments may be described in terms of the Apple products and SDK. However, it will be appreciated that other personal communication or entertainment devices which offer similar feature sets and application support may be equally suitable as platforms upon which to host comparable features to those described herein, and accordingly any references to specific Apple products herein are not intended to be limiting.
In the exemplary embodiments described herein, the universal remote control GUI is implemented as a native application, i.e., designed to run in the computer and operating system environment of a specific personal communication or entertainment device or family of devices, collectively referred to hereafter as a “smartphone,” thus enabling the full capabilities of platform specific features such as for example multi-point touch screen interface, motion based gestures, etc., and thereby providing a robust and high quality user experience. This is as opposed to a so-called “web app,” for example one based on HTML pages served to an embedded browser such as described for example in co-pending U.S. patent application Ser. No. 12/147,770 “System and Method for Ubiquitous Appliance Control,” of like assignee and incorporated herein by reference in its entirety. While such web apps are useful when a broad spectrum of different host device types are to be supported, in general they may not be able to fully leverage device unique features in the manner described herein.
A better understanding of the objects, advantages, features, properties and relationships of such a portable controlling device system having control capabilities will be obtained from the following detailed description and accompanying drawings which set forth illustrative embodiments and which are indicative of the various ways in which the principles of the system so described may be employed.
BRIEF DESCRIPTION OF THE DRAWINGS
For a better understanding of the various aspects of the portable controlling device system having control capabilities described hereinafter, reference may be had to preferred embodiments shown in the attached drawings in which:
FIG. 1 illustrates an exemplary system in which exemplary personal communication device or entertainment devices may be used as controlling devices;
FIG. 2 illustrates in block diagram form an exemplary command relay device of the type used in the exemplary system of FIG. 1 ;
FIG. 3 a through 3 d illustrate exemplary touch screen displays of a personal communication device executing an exemplary remote control application;
FIGS. 4 and 5 illustrate the operation of the exemplary remote control application of FIG. 3 in flow chart form;
FIG. 6 further illustrates the operation of an exemplary remote control application when issuing a request to an exemplary command relay device; and
FIG. 7 illustrates the operation of an exemplary command relay device when processing a request received from an exemplary remote control application.
DETAILED DESCRIPTION
With reference to FIG. 1 , according to the teachings set forth in greater detail below an appliance command relay device 100 is provided which receives control request transmissions 120 from a GUI application 130 loaded on a smartphone or similar device 102 , via a local network. Control requests 120 are transmitted wirelessly from the smartphone 102 , for example via a WiFi local network 110 . These requests may be received directly by a command relay device 100 equipped with a compatible wireless network interface, or may be received by, for example, a wireless router 112 and forwarded to a command relay device 100 ′ via a wired connection 114 , for example an Ethernet link. In either case, the command relay device decodes the received control request transmission, ascertains from it a target appliance, for example TV 108 , set top box 106 , or AV receiver 104 , and issues a control command 122 in a form recognizable by that appliance, for example an IR or RF signal of the format used by that appliance's remote control device. In this manner, command relay devices 100 and 100 ′ provide a conduit for the GUI application 130 resident in smartphone device 102 to issue operational commands to appliances 108 , 106 , 104 and 108 ′, 106 ′ respectively.
While illustrated in the context of a television 108 , an STB 106 , and an AV receiver 104 , it is to be understood that controllable appliances may include, but are not limited to, televisions, VCRs, DVRs, DVD players, cable or satellite converter set-top boxes (“STBs”), amplifiers, CD players, game consoles, home lighting, drapery, fans, HVAC systems, thermostats, personal computers, etc. Further, while the exemplary embodiments presented preferably utilize WiFi-based communication from smartphone device 102 , it will be appreciated that in other embodiments different wireless communication protocols such as for example Bluetooth, Zigbee, Z-wave, etc., may be employed as appropriate.
Turning now to FIG. 2 , the architecture of an exemplary command relay device is illustrated in block diagram form. For use in commanding the functional operations of one or more appliances in response to messages received via a wired or wireless network connection, a command relay device 100 may include, as needed for a particular application, a processor 200 coupled to a ROM memory 204 , a RAM memory 202 , a non-volatile read/write memory 206 , circuit(s) 208 for transmission of operating commands to appliances (e.g., IR and/or RF), a wireless network transceiver 210 (e.g., WiFi, Bluetooth, etc.) and/or a wired network interface 212 (e.g., Ethernet) for communication with a local network, a means 214 to provide feedback to the user (e.g., one or more LEDs, LCD display, speaker, and/or the like), and a power source 216 .
As will be understood by those skilled in the art, some or all of the memories 202 , 204 , 206 may include executable instructions (collectively, the program memory) that are intended to be executed by the processor 200 to control the operation of the command relay device 100 , as well as data that serves to define appliance control protocols and command values to the operational software (the appliance code data). In this manner, the processor 200 may be programmed to control the various electronic components within the command relay device 100 and process the input and output data thereof, for example, to receive and transmit data via network interfaces 210 and/or 212 , to act upon commands and requests embodied in such data, to cause the transmission of appliance command signals via transmission circuits(s) 208 to appliances to be controlled, to control visual feedback device(s) 214 , etc. While the memory 204 is illustrated and described as a ROM memory, memory 204 may also be comprised of any type of readable media, such as ROM, FLASH, EEPROM, or the like. Preferably, the memories 204 and 206 are non-volatile or battery-backed such that data is not required to be reloaded after power interruptions. In addition, the memories 202 , 204 , and 206 may take the form of a chip, a hard disk, a magnetic disk, an optical disk, and/or the like. Still further, it will be appreciated that some or all of the illustrated memory devices may be physically incorporated within the same IC chip as the microprocessor 200 (a so called “microcontroller”) and, as such, they are shown separately in FIG. 2 only for the sake of clarity.
To cause the command relay device 100 to perform an action, command relay device 100 is adapted to be responsive to events, such as a received signal from network interface port 210 or 212 . In response to an event, appropriate instructions within the program memory (hereafter the “operating program”) may be executed. For example, receipt of a control request message from smartphone device 102 may result in the retrieval from the appliance code data the command value and control protocol appropriate for an intended target device and a resulting transmission of the requested command to the intended target appliance, e.g., the STB 106 , in a format recognizable by the intended target appliance.
For selecting a set of appliance code data to be associated with an appliance to be controlled, data may be provided to the command relay device 100 that serves to identify an intended target appliance by its type and command protocol. Such data, provided as part of or separately from a command request, may allow the command relay device 100 to identify the appropriate appliance code data elements within a preprogrammed library of appliance code data, to be used to transmit recognizable commands in a format appropriate for such identified appliances. Alternatively, either in place of or in addition to a pre-stored library, appliance code data may be downloaded into command relay device 100 via a network interface(s) 210 , 212 either during an initialization phase or on an as required basis.
Operation of the Remote Control Application.
Turning now to FIG. 3 , a third party remote control application may be provided for purchase and download into a smartphone, for example through Apple's iPhone App Store—apple.com/iphone/appstore. Once downloaded and installed, the availability of an exemplary remote control application may be represented on a smartphone home screen 300 (such as shown in FIG. 3 a ) by the presence of an icon 302 . Activation of icon 302 , i.e., execution of the remote control application, may result in a GUI screen 304 such as illustrated in FIG. 3 b . This GUI may comprise selection icons 306 representative of the appliances that the application and its associated command relay station are currently configured to control, together with configuration icon 308 activatable to add or reconfigure controlled devices and icon 310 activatable to return to the smartphone home screen 300 . Activation of a device icon 306 , for example the icon labeled “TV,” may result in the presentation of a set of appliance control icons 320 such as illustrated in FIG. 3 c . The specific set of appliance control icons presented may be dependent on the device type selected. In the event more device control functions are available than can reasonably be presented in a single display page, additional display pages may be provided, accessible via the smartphone device's usual page scrolling functionality (for example, a horizontal swipe of a finger in the case of an Apple iPhone.)
The functionality of various icons illustrated in FIGS. 3 b through 3 d will now be described in greater detail in conjunction with the flowcharts of FIGS. 4 and 5 , which are representative of the processing performed by an exemplary remote control application, commencing at step 400 when an event such as a screen touch, accelerometer output, proximity sensor, timer expiry, etc., is detected by the smartphone operating system and presented to the exemplary remote control application for processing. It will be appreciated that in these and other flowcharts presented herein by way of illustration, steps associated with common housekeeping functionality as is well known in the art, for example low battery detection, display timeouts, error conditions, etc., may be omitted for clarity. First, at step 402 it is determined if the event is an incoming phone call. If so, at step 404 the current status of the remote control application is saved in order to allow the application to return to the same operational screen when re-launched, for example at the conclusion of a phone conversation. Next, at step 406 it is determined if the automatic mute/pause feature (a user option in the exemplary embodiment) is enabled. If so, at step 408 a “mute” command request targeted to the volume control appliance and/or a “pause” command request targeted to the media playback appliance may be issued to the command relay station, after which at step 440 the exemplary remote control application relinquishes smartphone device control to the phone mode.
If the event is not an incoming call, at step 410 it is determined if the event is the result of a user interaction with the device such a button tap, finger swipe, accelerometer based input, proximity sensor input, etc. If so, it is next determined at step 412 if the current status of the remote application is gesture mode. If so, processing continues at step 500 in FIG. 5 , as will described hereafter. If the status of the remote control application is not gesture mode, it is next determined at step 414 if the event was activation of a button icon. If so, at step 416 it is determined if the activated icon was a “close” icon 310 or 326 . If so the exemplary remote control application closes and relinquishes smartphone device control to the default phone mode of operation. If a “close” icon was not activated, it is next determined at step 418 if the activated icon was one of the appliance selection icons 306 . If so, at step 436 the current appliance to be controlled is set as indicated by the particular appliance selection icon activated, and the first page of command icons applicable to the selected appliance is retrieved and displayed. By way of example, if the selected appliance is a TV, the displayed page may be as illustrated at 320 in FIG. 3 c . It will be appreciated that the contents of this first, initially displayed, page may vary with appliance type—for example while a TV appliance page may be as illustrated, a DVD appliance first page may comprise transport controls (play, pause, fast forward, etc.), a cable STB first page may comprise program guide navigation and selection controls, etc.
If the event is not an appliance selection, at step 420 it is next determined if the activated icon is a request to perform an operation internal to the remote control application, for example, via activations of icons 322 for scrolling to a control page for a different type of appliance, icon 324 for returning to the remote control “home” page (for example, appliance selection page 304 ), icon 326 for exiting the remote control application, etc. If so, at step 422 the requisite action is performed.
If the activated icon is not to result in the performance of an internal operation, the icon activation may represent an appliance command operation, for example a request to issue a TV “power” command initiated via icon 328 . If so, at step 432 the requested command function is determined and at step 434 an appropriate command request is issued to command relay device 100 . The requested command function may also be internally stored by the remote control application for future reference.
If the event is not an icon activation, at step 428 it is next determined if the event comprises a shake, i.e. rapid movement along two or more axes as reported by the accelerometer hardware of the smartphone device. If so, in an exemplary embodiment this action by the user is interpreted as a request to repeat the last appliance command issued. In this case, at step 430 the command previously stored at step 434 above is retrieved and a request for that command issued to command relay device 100 .
If not a shake, at step 436 it is next determined if the event comprises a touch screen gesture by the smartphone user. If so, this event is processed as will be described hereafter in conjunction with FIG. 5 . If not, no recognizable event has occurred, and the remote control application terminates current processing at step 438 .
If the detected event is not an incoming call or a user interaction, at step 424 it is determined if the event is a timer expiry. If not, no recognizable event has occurred, and the remote control application terminates current processing at step 438 . If so, at step 426 any gesture mode status and screen overlay display(s) are cleared. By way of explanation, during certain gesture activities a semi-transparent overly may be displayed as described in greater detail hereafter in conjunction with FIG. 5 . While this display is present, a time-out may be established in order to remove the display overlay after a predetermined period of inactivity.
Turning now to FIG. 5 , if at step 436 it was determined that the user input constituted a gesture (i.e., a touch screen interaction of a particular type, as detectable by the smartphone vendor-supplied operating system), at step 506 it is determined if the gesture was a simple scroll request, for example a horizontal swipe which may be interpreted as a request to scroll to the next page of appliance command icons in instances where multiple pages of command functions exist for a particular appliance type. If so, the request is processed at step 518 and the remote control application thereafter terminates current processing at step 516 . If not a scroll request, at step 508 it is next determined if the gesture comprised a two finger double tap. If so, in the exemplary embodiment this may be interpreted as a user request to enter into a volume and channel control mode. Additionally, in the exemplary embodiment, repeat of a mode setting gesture while already in that mode may be interpreted as a request to terminate that mode of operation. Accordingly, at step 520 it is first determined if the remote control application is already operating in the volume and channel control mode. If so, processing continues at step 426 to clear that mode. If not, at step 522 the gesture mode status is set to “Vol/Chan control,” at step 524 a semi-transparent overlay, for example as illustrated at 330 of FIG. 3 d , is displayed to indicate the mode of operation, and at step 540 a gesture mode timer is started (or restarted, if the remote control application was already operating in one of the gesture modes), after which processing of the current event completes at step 516 .
If not a two finger double tap, at step 510 it is determined if the event comprised a three finger double tap. If so, in the exemplary embodiment this may be interpreted as a user request to enter into a transport control mode, i.e., offering control of the “play”, “pause”, “fast forward”, “rewind”, etc. functions of a media playback appliance, and at steps 526 through 530 the request is processed in a similar manner to that previously described, resulting in the display of a transport function semi-transparent overlay (not illustrated).
If not a three finger double tap, at step 512 it is determined if the event comprised a pinch close gesture (two digits, typically a finger and thumb, placed in contact with the touch sensitive surface and moved in opposing directions towards one another). If so, in the exemplary embodiment this may be interpreted as a user request to enter into a menu navigation mode, i.e., offering control of the “select”, “up”, “down”, “left”, “right,” etc. functions of an appliance, and at steps 532 through 536 the request is processed in a similar manner to that previously described, resulting in the display of a menu navigation function semi-transparent overlay (not illustrated).
If not a pinch close gesture, at step 514 it is next determined if the event comprised a two finger vertical swipe. If so, in the exemplary embodiment this may be interpreted as a user request to issue a mute command to the current audio rendering appliance, and at step 538 the requested appliance command is set for issuance to command relay station 100 . If not a two finger vertical swipe, no recognizable event has occurred, and the remote control application terminates current processing at step 516 .
When the remote control application status indicates that it is operating in the gesture mode (i.e., a mode previously set at one of steps 522 , 528 or 534 and not dismissed or timed out) receipt of a user interaction event at step 412 causes processing to continue at step 500 where it is determined if the event is a horizontal or vertical finger swipe. If so, the appropriate appliance command is selected at step 504 and a request issued to command relay device 100 via step 434 . Selection of appliance type and command is based on the current gesture status, for example an upward swipe may indicate “channel up” if in volume/channel control mode, “stop” if in transport control mode, “menu up” if in menu navigation mode, etc. If not a finger swipe, at step 501 it is next determined if the event is a finger tap in the central portion of the screen. If so, processing continues at step 504 with the selection of an appropriate command (for example “mute”, “pause”, or “select” dependent once again on the current gesture status.) If not, at step 502 it is determined if the event is activation of dismiss icon 332 , indicating that the user wishes to exit gesture mode. If so processing continues at step 426 where the gesture mode status and screen overlay display are cleared. If not processing continues at step 508 as previously described.
It will be appreciated that additional or alternative gestures and/or command functions may be implemented in this or other embodiments dependent on the gesture recognition capabilities of specific smartphone or entertainment device platforms, including those that may comprise two or more types of gestures performed simultaneously or in concert with one another in order to accomplish more complex command functions. By way of example, in one embodiment of the present invention a ramping fast forward or reverse function may be enabled via a single button press and hold input on the touch screen, during which accelerometer based input (e.g., tilting the smartphone to the right or left) gradually increases or decreases the rate at which media is fast-forwarded or reversed. Furthermore, in some embodiments the assignment of particular gestures to specific command functions may configurable at user option. Accordingly, it is to be understood that the gesture functionality presented in the foregoing paragraphs is by way of example only and not intended to be limiting.
Request Protocol Between Remote Control Application and Command Relay Device.
In an exemplary embodiment command request and response data packets of the format described below may be exchanged between a remote control application and a command relay device via a wireless 110 and/or wired 114 local area network.
A command request from remote control application to a command relay device comprises the following data fields (values in parentheses after each field name represent the size of that field in bytes, i.e., the number of digits or characters):
SystemID(4), SpecRevision(4), RcdLength(2), RequestType(1), ApplianceType(2), ApplianceNum(4), CommandCode(2), KeyFlag(1)
Where:
SystemID may be a unique system identification number established for example during an initial discovery and pairing process between a remote control application and a command relay device with which it is to be associated.
SpecRevision may be a version/revision indicator of the interface specification to which this data packet format conforms, for example to ensure compatibility between devices or for determining data packet field locations and values.
RcdLength may be the number of data characters following this field (i.e., excluding itself)—“10” in the case of this exemplary command request packet.
RequestType may be the type of request—In the example presented, “01” may represent a request to commence transmitting an appliance command, “02” may represent a request to continue transmitting an appliance command, and “00” may represent a request to cease transmitting an appliance command. See the narrative below regarding the KeyFlag field for further insight regarding this aspect of the request protocol between the exemplary remote control application and the command relay device.
Appliance Type may be the type of appliance to be commanded, for example according to the following table:
TABLE 1
Exemplary appliance types.
Appliance Type
Device Name
00
TV
01
Cable STB
02
Video Accessory
03
Satellite STB
04
VCR
05
Laser Disk
06
DVD
07
Tuner/AV Receiver
08
Amplifier
09
CD
10
Home Control
11-31
Reserved
ApplianceNum may be a four digit number which identifies a set of command data and transmission format information, i.e., the appliance code data, required to control a particular appliance or family of appliances. This may for example represent a set up code or appliance identifier as is well known in the universal remote control art, see for example “ATLAS OCAP 5-Device Remote Control” user manual, Revision 3.0, by Universal Electronics Inc., incorporated herein by reference in its entirety.
CommandCode may be a two digit identifier of the specific command requested, for example according to the following table:
TABLE 2
Exemplary appliance command functions
Standard
Command #
Function
01
POWER TOGGLE
02
POWER ON
03
POWER OFF
04
CHANNEL UP
05
CHANNEL DOWN
06
VOLUME UP
07
VOLUME DOWN
08
MUTE
09
DIGIT 1
10
DIGIT 2
11
DIGIT 3
12
DIGIT 4
13
DIGIT 5
14
DIGIT 6
15
DIGIT 7
16
DIGIT 8
17
DIGIT 9
18
DIGIT 0
19
CHANNEL ENTER
20
+100
21
LAST CHANNEL
22
INPUT
23
EXIT
25
STOP
26
PAUSE
27
REWIND
28
FAST FORWARD
29
RECORD
30
SKIP FWD
31
SKIP REVERSE
32
LIVE
33
SOURCE MENU
34
DEVICE MENU
35
GUIDE
36
EXIT
37
BACK
38
CURSOR UP
39
CURSOR DOWN
40
CURSOR LEFT
41
CURSOR RIGHT
42
MENU SELECT
43
PAGE UP
44
PAGE DOWN
45
FAVORITE
46
DISPLAY
47-99
Reserved
KeyFlag may be a directive which may control the style of command transmission to the appliance. By way of example, in an exemplary embodiment KeyFlag=“1” may request that the appliance command be issued once by the command relay device, while KeyFlag=“0” may request that the appliance command be continuously transmitted by the command relay device until an explicit “cease transmitting” request is received—used, for example, in the case of ramping functions such as volume control where a command transmission should be continuously repeated for as long as a user keeps a key depressed, a channel surfing function in which channels are to be incrementally viewed, etc.
A response from a command relay device to a remote control application may comprise the following fields:
SystemID(4), SpecRevision(4), RcdLength(2), RequestType(1), ApplianceType(2), ApplianceNum(4), CommandCode(2), Status(2)
Wherein the first seven fields may be as described above and may comprise an echo of the received request by way of confirmation, and the final Status field may comprise one of the values shown in Table 3 below, representing the completion status of the command request.
TABLE 3
Exemplary status response values
Status value
Message
00
Completed without error
01
Invalid appliance type
02
Invalid appliance number
03
Invalid request type
04
Invalid command code
05
No command data available
06
Data Packet Format Error
07
Continuous command transmission aborted by
timeout
08-99
Reserved
Turning now to FIG. 6 , the steps performed by an exemplary embodiment of a remote control application in issuing a command request in accordance with the exemplary data protocols above will be described in further detail, i.e., a series of steps which may correspond to the process of step 434 of FIG. 4 . First at step 602 exemplary packet header data is initialized, comprising for example appropriate SystemID, SpecRevision, and RcdLength fields together with a RequestType field value of “01” (commence transmitting a command). Next, at steps 604 and 606 , exemplary ApplianceType, ApplianceNum, and CommandCode fields are populated according to the indicated appliance and function request. At step 608 the requested command is also saved locally for possible future use in processing a possible “repeat last command” request as previously described in conjunction with FIG. 4 . At step 610 it is determined if the requested is for a ramping function. By way of example, when an exemplary remote control application is operating in the volume/channel gesture input mode illustrated in FIG. 3 d , a left to right finger swipe terminating with the finger removed from contact with the touch sensitive surface may be interpreted as a request to issue a single instance of a “volume up” command to the designated appliance, i.e., a non-ramping function, whereas a left to right finger swipe terminating with the finger remaining in stationary contact with the touch sensitive surface may be interpreted as a request to continuously issue “volume up” commands to the designated appliance until such time as the finger is lifted, i.e., a ramping function. At steps 612 and 614 the KeyFlag field value is set according to this determination. At step 616 , the completed request data packet is forwarded to an exemplary command relay device via wireless local area network 110 . As will be appreciated, the data packet may be encapsulated for transmission purposes within further header fields, control parameters, error detection and/or correction data, etc., as appropriate for the wireless protocol being employed, for example WiFi, Buetooth, Zigbee, Zensys, etc., all as well known in the art.
After transmission of the request data packet, at steps 618 , 620 and 622 the remote control application waits for a response from the exemplary command relay device. If the received response is negative, i.e., any value other than “00” in the example presented, or if no response is received within a predetermined amount of time, an error condition exists and is processed at step 652 . The exact actions taken may depend upon both the type of error and the activity currently being requested. By way of example without limitation, a timeout or receipt of a status code such as 06 “data packet format error” may result in re-transmission of the request packet; receipt of status code 05 “no command data available” may result in graying out of particular button icons in certain display pages; receipt of status code 02 “invalid appliance number” may result in a message to the user suggesting re-initialization of appliance settings within the smartphone device and/or downloading of additional code data to command relay station 100 ; while other error status codes may result in display of error messages requesting possible action by the user such as reconfiguring or reinitializing devices, etc.
If a good status response is received, at step 624 the remote control application next determines if the KeyFlag value of the acknowledged request was “01.” If so, the function requested was the transmission of a single instance of the appliance command represented by CommandCode, and processing is complete. If not, the request is for a continuous transmission of the appliance command for as long as the key or other user input remains activated. In that case, at step 626 a predetermined key timeout is first initiated as a precaution in the event that the continued key activation is not the result of a user action but rather an error condition—for example a smartphone device has become lodged between couch cushions, an object has been inadvertently placed on or has fallen onto the touch screen surface, etc. Should this timeout expire, the remote control application will subsequently act as if the key had been released regardless of its activated state. Then, at step 628 it is determined if the key or input is in fact still activated and if so, provided the above referenced key timeout has not expired (step 630 ), at steps 632 and 634 a further request packet is transmitted to the exemplary command relay device, with RequestType set to “02—continue transmitting.” As will be detailed hereafter, in certain embodiments an exemplary command relay device which is transmitting a command continuously may require periodic receipt of such “continue transmitting” requests from the remote control application in order to sustain the transmission, this representing a safety feature to prevent runaway of an appliance adjustment function in the event that communication between the remote control application and the command relay device is interrupted prior the issuance of a “cease transmitting” request.
Upon completion of transmission of the packet, the remote application once again waits for a response from the exemplary command relay device. If a bad response or timeout occurs, the error condition is processed at step 652 as previously described. If a good response is received, the sequence is repeated starting at 628 until such time as the key or input is no longer activated or the key timer times out. Upon occurrence of either of these events, at steps 642 and 644 a request packet is transmitted to the exemplary command relay device, with RequestType set to “00—cease transmitting”, the ensuing response is evaluated at steps 646 , 648 and 650 , and processing is complete.
Operation of the Command Relay Device.
Turning now to FIG. 7 , the steps performed by an exemplary embodiment of a command relay device in processing a command request in accordance with the exemplary data protocols above will be described in further detail. Upon receipt of a command request data packet in conformance with the protocol described previously, at initial step 702 the packet header data is examined. For example, the exemplary SystemID and SpecRevision fields may be inspected to determine if they match expected values. An exemplary RcdLength field may also be evaluated at this step to determine if a complete data packet has been received. If any of these tests fail, a data packet that is broken and/or of unknown format has been received, and accordingly at step 704 a status “data packet format error” is set whereafter the balance of the received packet fields are ignored, a response containing that status is returned to the originating remote control application at step 750 , and processing is complete.
Next, at step 706 an exemplary RequestType field is examined to determine if the received data packet is a “00—cease transmitting” request. If so, at step 732 and 733 a status “good completion” is set and any timeout timer is cleared, whereafter any ongoing appliance command transmission is cancelled at step 746 , a response containing the good status is returned to the originating remote control application at step 750 , and processing is complete.
If the exemplary RequestType field is not a cease transmitting request, at step 708 it is determined if the received RequestType field is a “02—continue transmitting” request. If so, at step 709 a status “good completion” is set, whereafter at step 748 an exemplary transmission timeout is reset, a response containing the good status is returned to the originating remote control application at step 750 , and processing is complete.
If the exemplary RequestType field is not a continue transmitting request, at step 710 it is determined if the received RequestType field is a “01—transmit command” request. If not, other type of requests may be processed at step 712 . By way of example these may include device discovery and pairing transactions, initial and setup and configuration communications, etc. without limitation, as required by particular embodiments.
If the request is for a command transmission, at step 714 the exemplary ApplianceType and ApplianceNum fields are evaluated. If the requested appliance type and/or number are invalid, i.e., do not correspond to an identifiable portion of the appliance code data currently stored in the memories 202 , 204 , 206 of command relay device 100 , an appropriate error status is set at step 716 and processing continues at step 750 as previously described.
If the requested appliance type and number are valid, at step 718 these are registered as the appliance to be controlled, for example by establishing a pointer to the appropriate portion of stored appliance code data. At step 720 , the contents of the exemplary CommandCode field are then examined. If there is not a recognizable command code, an error status is set at step 722 and processing continues at step 750 as previously described. If a valid command code is present, at step 724 and 726 the entry within the stored appliance code data which corresponds to the request appliance type, number, and command is examined. If no data is available, an error status is set at step 728 and processing continues at step 750 as previously described. By way of explanation, not all appliances necessarily support every function defined in the universe of possible appliance commands. By way of specific example, a particular appliance may not support a discrete “power on” function even though in the exemplary embodiment illustrated in Table 2 this is a permissible command (“02”), in which case the appliance code data entry corresponding to that appliance type/number/command may be null, resulting in the “no command data available” status of step 728 .
If valid data is present, then at steps 730 and 732 the software driver associated with IR or RF transmitter 208 is initialized using the stored formatting information corresponding to the selected appliance type and number. Such formatting information may include for example a carrier frequency, duty cycle, encoding schema, frame length, etc., as well known in the art. Thereafter, at steps 738 and 740 the command data is retrieved and transmission commenced. Once command transmission is initiated, the response status is set to “good” at step 742 .
The exemplary KeyFlag field is then examined at step 744 . If the content is non-zero, processing continues at step 746 and command transmission is stopped after completion of a single instance. In this regard, it will be appreciated that a single instance of a command may comprise transmission of more than one frame of data, depending on the appliance protocol is use. By way of specific example, the error detection mechanism of a certain manufacturer's IR command protocol may require that a frame of command data be repeated multiple times for comparison purposes before it will acted upon. Accordingly it is to be understood that at step 746 transmission will only cease after completion of all requirements of the particular appliance command protocol currently in use. Once complete, processing continues at step 750 by issuing a completion response to the requesting smartphone device, after which processing is complete.
If the content of the exemplary KeyFlag field is zero, the requesting smartphone device wishes to initiate a ramping function, and accordingly at step 748 an exemplary transmit timeout is initiated, whereafter a completion status is returned to the requesting smartphone device and processing completes with command transmission ongoing.
As mentioned previously, the purpose of the timeout initiated at step 748 is to prevent a runaway command situation in the event that communication between smartphone 102 and command relay device 100 is interrupted and a timely “Cease transmitting” request is not received by the command relay device. Accordingly, if this timeout expires prior to receipt of any “Continue transmitting” or “Cease transmitting” request from the smartphone device, at step 734 a response status “Aborted by timeout” is set, after which any ongoing command transmission is terminated and that status is communicated to the smartphone device.
Initialization of the System.
A newly-installed remote control application when run for the first time on a smartphone device may initiate a discovery process to locate and pair with a command relay device 100 attached to the local wireless network. In certain embodiments, upon discovering a command relay device the remote control application will instruct that command relay device to visually or audibly signal the user, for example using status indicator 214 , and then prompt the user for a confirmation input, for example via the touch screen. If no user confirmation is received within a predetermined period of time the remote control application may resume the discovery process after flagging the current command relay device so as to not identify it again during the current run instance. In this manner allowance may be made for the presence of more than one command relay device on the same local network.
Once paired with a command relay device, in certain embodiments the remote control application may immediately enter an “add device” mode soliciting user configuration of the appliance types, brands and/or models to be controlled. Alternatively, the remote control application may simply display a blank home screen (similar to screen 304 sans appliance selection icons 306 ) awaiting manual user initiation of an add device mode, for example via activation of icon 308 . In either event, multiple methodologies for identification of appliances to be controlled, whether performed locally or by interaction with a Web-based service are well known in the art, by way of example without limitation, as may be found described in U.S. Pat. No. 4,959,810 “Universal Remote Control Device” or U.S. Pat. No. 7,218,243 “System and Method for Automatically Setting Up a Universal Remote Control,” both of like assignee and incorporated herein by reference in their entirety. In some embodiments, appliance identification may be performed by interacting with a web-based service which may convert user-supplied appliance brand and model information into appliance type and number values suitable for use by the smartphone application. In some instances, supplemental appliance code data not already present in the memories of command relay device 100 may be downloaded into the device via network connections 114 or 120 . In certain embodiments this may occur based on a web service's prior knowledge of the current library of appliance code data in command relay device 100 , while in other embodiments this may be triggered, for example, by a smartphone application upon receipt of an “Invalid appliance number” or “Invalid appliance type” status response from command relay device 100 .
In some embodiments, various further options may be configurable within the remote control application either during the initialization process or separately thereafter, for example the optional pause and/or mute features illustrated at steps 406 and 408 of FIG. 4 may be enabled or disabled, individually or jointly. Additionally the assignment of appliance type, command functions and/or remote control application local functions to specific gestures may be user configurable. It will be appreciated that in certain embodiments, the device type to be associated with a specific gesture may be globally assignable, i.e., effective without regard to the currently selected device of the remote control application (for example, the volume control functions may be globally assigned to TV 104 , while channel up/down functions may be globally assigned to set top box 106 ), while in other embodiments the device type may be that currently selected within the remote control application. In this connection, functions represented by conventional button icons which have also been assigned a gesture, for example the channel up icon 340 and channel down icon 342 of FIG. 3 c may be visually identified as such by the addition of a badge or tag 344 appended to or placed in the proximity of that function icon.
While various concepts have been described in detail, it will be appreciated by those skilled in the art that various modifications and alternatives to those concepts could be developed in light of the overall teachings of the disclosure. For example, it will be appreciated that alternative and/or additional gestures may be utilized in various embodiments of the invention, and that the GUI displays and functionality presented herein are illustrative only. For example, in certain embodiments icons 322 , 324 and 326 may be utilized to access user-assignable favorite channels rather than the internal functions described herein. Further, certain embodiments of the remote control application may take advantage of additional capabilities of the smartphone platform in which they are resident. For example a remote control application resident in a smartphone platform capable of spatial awareness (e.g., via GPS, wireless network detection, or other location based technology) may automatically select appropriate appliances to be controlled as a user moves from room to room and/or to automatically alter which appliance is assigned to various gestures. Additionally, while combination gestures (for example a finger swipe followed by a tap, tilt, shake, etc.) may be presented in the exemplary embodiments illustrated herein as being fully interpreted within a smartphone platform, it will be appreciated that in alternative embodiments each of the individual gesture component actions may be separately reported to a command relay device and interpreted thereat.
While described in the context of functional modules and illustrated using block diagram and flow chart formats, it is to be understood that, unless otherwise stated to the contrary, one or more of the described functions and/or features may be integrated in a single physical device and/or a software module, or one or more functions and/or features may be implemented in separate physical devices or software modules. It will also be appreciated that a detailed discussion of the actual implementation of each module is not necessary for an enabling understanding of the invention. Rather, the actual implementation of such modules would be well within the routine skill of an engineer, given the disclosure herein of the attributes, functionality, and inter-relationship of the various functional modules in the system. Therefore, a person skilled in the art, applying ordinary skill, will be able to practice the invention set forth in the claims without undue experimentation. It will be additionally appreciated that the particular concepts disclosed are meant to be illustrative only and not limiting as to the scope of the invention which is to be given the full breadth of the appended claims and any equivalents thereof.
All patents cited within this document are hereby incorporated by reference in their entirety. | A system for use in controlling operating functions of a controllable device includes a hand-held device and an intermediate device in communication with the hand-held device and the controllable device. The hand-held device is adapted to receive a gesture based input and to transmit a signal having data representative of the gesture based input. The intermediate device has programming for translating the data representative of the gesture based input in a signal received from the hand-held device into a command signal to be communicated to the controllable device wherein the command signal has a format appropriate for controlling an operating function of the controllable device that is associated with the gesture based input. | 7 |
BACKGROUND OF THE INVENTION
This invention relates to the cleaning of deposits from the walls of a refractory furnace. More particularly, the invention relates to a device containing rotating scrapers to remove deposits from the furnace walls.
Refractory furnaces such as coke, ovens, carbon baking furnaces and the like require periodic cleaning to remove deposits of carbon and other materials on the furnace walls. This can be done manually after first cooling the furnace by a crew of laborers who chip and scrape at the deposits, usually with hand tools. The work is tedious, dirty and, to some extent, a health hazard due to the extreme dust conditions which necessitate the wearing of protective devices such as goggles and masks.
The desire to automate this cleaning operation has lead to the proposing of elaborate devices which attempt to duplicate the manual effort to remove as much of the deposits as possible. Unfortunately, elaborate schemes such as, for example, proposed in Evrard et al, U.S. Pat. No. 4,279,052, can result in the creation of machinery maintenance problems which merely shift the manual labor to the cleaning, maintaining and repairing of equipment. This patent discloses the use of a plurality of chain-driven rotating screw-type cutters against each of two opposing walls of a furnace. The rotating scrapers are linked by a chain to a rotation source and are connected together by universal joints. The use of a plurality of scrapers is said to be necessary in the event that the built-up deposits are thicker on some areas of the walls.
While the described device will apparently permit automation of the cleaning job, the motors, chains and universal joints are all susceptible to maintenance problems because of the carbon deposits generated during the cleaning process. Furthermore, the screw-type scraper blades may have to be periodically replaced as the scraping surface is worn away.
It would, therefore, be desirable to provide a device with a minimum of moving parts exposed to dirt and dust conditions. It would also be desirable to provide a scraping apparatus means not necessitating complete removal for maintenance or renewing of the cutting surface.
SUMMARY OF THE INVENTION
It is, therefore, an object of the invention to provide a simplified cleaning apparatus for cleaning deposits from furnace walls.
It is another object of the invention to provide self-contained rotational means on the cleaning apparatus for removing deposits from furnace walls with a minimum exposure of the rotational driving means to the resultant dust and dirt attendant with the removal.
It is yet another object of the invention to provide simplified means for renewing the cutting surfaces of the rotational means without removal of the rotational means.
It is a further object of the invention to provide a device for cleanihg and removing deposits from furnace walls which provide a single control for rotating a deposit removal means against the furnace walls and for urging the removal means against the furnace wall.
These and other objects of the invention will be apparent from the accompanying description and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an isometric view of the apparatus.
FIG. 2 is a partially sectioned side view of the apparatus.
FIG. 3 is a further cutaway view of FIG. 2 showing inside the inner and outer motor casing.
FIG. 4 is a cutaway end section of FIG. 3 taken along lines III--III.
FIG. 5 is a side view of a portion of the outer surface of the drum.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Turning now to FIG. 1, the furnace cleaning apparatus, generally indicated at 2, comprises a bar 10 having a handle 20 thereon which can be grasped by the hook of an overhead crane and two rotatable cleaning drums 100 and 110 which are mounted to bar 10 via arms 40-46 which depend therefrom.
Arms 40 and 42 are pivotally mounted at 12 to one end of bar 10. Arms 44 and 46 are pivotally mounted at 14 to the opposite end of bar 10.
As seen more clearly in FIG. 2, drum 110 is rotatably mounted to arms 42 and 46. The attachment of drum 110 to arm 46 is via a bearing 56 on arm 46 through which a shaft extension 112a on drum 110 is journalled, as will be described below. Drum 110 is carried by arm 42 via air-driven motor assembly 160. Drum 110 comprises a hollow cylinder having an inner diameter slightly smaller than the outer diameter of outer shell 162 of air motor 160. A round plate or spider 114 is mounted within drum 110, preferably in a removable manner as by set screws passing through drum 110 into plate or spider 114. Shaft 112 is centrally welded to spider 114 coaxially with drum 110.
Shaft 112 passes through a bearing 156 mounted to the outer shell 162 of air motor assembly 160. Shaft 112 is coupled to air motor 160 via a spline arrangement, as will be described below.
Outer casing 162 of air motor assembly 160 is, in turn, secured at 161, as by welding or the like, to a mounting plate 180 which is bolted to arm 42 by bolts 182.
Spider 114a, having shaft 112a coaxially secured thereto, is mounted inside the opposite end of drum 110 in similar fashion except that it may be mounted closer to the end of drum 110. Shaft 112a passes through bearing 56 which is mounted as by welding to plate 180a, which is secured by bolts 182 to arm 46.
Turning now to the cutaway view of motor assembly 160 shown in FIG. 3, air motor 170 is mounted to an inner casing 168 by bolts 178. Motor shaft 172 is coupled to shaft 112 by spline assembly 174 which permits easy disengagement of motor 170 should removal of motor 170 be desired.
As best seen in FIG. 1, inner casing 168 is secured to outer casing 162 by set screws 164, which may be accessed through openings 118 provided in drum 110. Two set screws are used in the illustrated embodiment spaced 180° apart.
Motor 170 and inner casing 162 may be removed from the apparatus as a unit after removal of set screws 164 via an opening 184 provided in plate 180. Opening 184 also provides ingress for air line 200 which provides compressed air to air motor 170. Air line 200 is routed along arm 42 to bar 10 where it joins a second air line (not shown) which feeds a similar motor powering drum 100. The construction and interrelationship of arms 40 and 44 with drum 100 is the same as that already described for arms 42 and 46 and drum 110. The use of a single supply of air (and at the same pressure) for the identical air motor respectively powering drums 100 and 110 insures that both will rotate at the same speed as the apparatus is raised or lowered by the crane operator.
It should also be noted here that the mounting of air motor assembly 160 within drum 110 shields the air motor assembly from the dust and particles abraded from the furnace walls which might otherwise clog the moving parts, thus requiring more maintenance and downtime. In fact, the egress of the air through the end of drum 110 will actually tend to purge the motor area of dirt particles.
Air line 200, in addition to junctioning with a similar air line for the motor powering drum 100, junctions at 210 with an air line 220, which passes through an air regulator 230 to reduce its pressure. The amount of pressure reduction is preselected to permit sufficient urging of the drums against the furnace walls without stalling the air motors by excessive force against the furnace walls. Air line 224 from air regulator 230 branches into lines 226 and 226a, which respectively feed air cylinders 80 and 82.
After the crane operator has lowered furnace cleaning apparatus 2 into a furnace, air line 200 is activated by solenoid 240 in the crane which feeds air pressure from the crane into air line 200. Air feeding from line 200 through regulator 230, line 226 and line 226a to air cylinders 80 and 82 urge the opposing arms 40,42 and 44,46 apart to bring drums 100 and 110 into contact with the furnace walls. At the same time, air line 200 feeds air into air motor 170 and its counterpart in drum 110 to rotate both drums. It should be noted in this regard that the air motor in drum 100 is mounted in the opposite end from the mounting of air motor 170 in drum 110 to impart counter rotation by the two drums which permits even travel of the apparatus up and down the furnace walls.
Thus, a single source of air activated by a single switch by the crane operator simultaneously operates all the air cylinders and air motors on the apparatus obviating any need for additional manual operations conducted by personnel within or adjacent to the furnace, as in the prior art, as illustrated, for example, in the aforementioned Evrard et al patent.
Drums 100 and 110 are provided with a renewable cutting surface by mounting a flat wire belt 260 to the surface of the drum. In the preferred embodiment, belt 260 is a 1"×1" flat wire belt, picket size 3/8"×0.046 flat high carbon steel with 11 gauge (0.120) connector pins.
Belt 260 is rotationally secured to drum 110 by a series of 3/8" nuts 280 which are positioned circumferentially around drum 110. As best seen in FIG. 5, in a preferred embodiment, a series of nuts is radially positioned around drum 110 to fit into every opening adjacent the end of the drum and every other opening in the next set of pickets. As shown in the drawing, three nuts are then spaced 120° apart in every sixth row of pickets to the other end of drum 110 where the arrangement at the first end is repeated. The belt is then cut to fit the circumference of drum 110, and the ends of the belt are crimped or welded together at the seam. Should the belt wear down or break, it thus is easily removed from the drum and a new belt put in place. The seam merely holds the belt together while the cog wheel action of the nuts in the belt openings serve to secure the belt rotationally to the drum. This type of cutting surface thus provides many scraping edges which reduce the point contact pressure, which provides longer life for the cutting edges as well as lowering refractory damage to the walls of the furnace.
Thus, there is provided an apparatus for cleaning furnaces which is simple to operate by one man, requires little maintenance due to the location of the driving parts within the rollers where they are shielded from the dust which will be produced by the operation, and which uses a single supply of air with a single control operating all air tools. The apparatus of the invention is further characterized by an easily renewable cutting surface which also contributes to lower maintenance and downtime. | An improved and simplified device for removal of deposits on furnace walls is disclosed which can be operated by a single individual. The device is characterized by rotating scrapers driven by internally-contained air-powered motors. The horizontally opposed scrapers are journalled on each end to pairs of arms which are connected together at a pivot spaced from the journals. Air cylinders, powered from a common source with the air motors, spread the arms apart simultaneously with activation of the air motors to bring the rotating scrapers in contact with the furnace walls. | 5 |
BACKGROUND OF THE INVENTION
The present invention relates to a device for associating a pair of planar parallel panels of any thickness, particularly to provide walls for exhibition stands and the like.
As is known, in the above specified field there is generally the need to divide the exhibition area by means of dividing walls made of panels which can also be used as support for drawings, posters and the like. Such panels must be suitable to form walls of different dimensions and geometries according to the requirements of the exhibition. Furthermore, in order to reduce setup costs, it is obviously necessary that said panels be easy and rapid to assemble and disassemble. The systems currently in use to provide said diving walls do not entirely meet these requirements.
SUMMARY OF THE INVENTION
The aim of the present invention is to provide a device for associating in a simple and rapid manner pairs of planar parallel panels so as to make walls of any type of configuration.
Within this aim, an object of the present invention is to provide a device which is simple in concept, easy, reliable and versatile in use and relatively economical in its cost.
This aim and this object are both achieved, according to the invention, by a device for associating a pair of planar parallel panels, particularly to provide walls for exhibition stands and the like, comprising a pair of profiled elements and a spacer block arranged between said profiled elements and connected therewith, each profiled element comprising a plate having a right angle and an outer edge extending along two sides of said plate enclosing said right angle, said plate and edge defining a groove into which a corner of said panels engages, said spacer block including a seat and a sylinder being rotatably accommodated in said seat according to an axis perpendicular to said plates, said cylinder being provided with means for anchoring one end of a tensioning member extending between said pair of panels and having the opposite end associated to a similar device applied in diagonally opposite corners of said panels.
BRIEF DESCRIPTION OF THE DRAWINGS
The details of the invention will become apparent from the detailed description of a preferred embodiment of the device for mutually associating a pair of planar parallel panels, illustrated by way of non-limitative example in the accompanying drawing, wherein:
FIG. 1 is a perspective view of a pair of panels associated by means of the device according to the invention;
FIG. 2 is a side view of the device taken on the plane II--II of FIG. 4;
FIG. 3 is sectional view of the device, taken on the plane III--III of FIG. 4 and illustrating in spaced position means for coupling a pair of adjacent walls;
FIG. 4 is a sectional view of the device taken on the plane IV--IV of FIG. 3.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to the above described figures, the numeral 1 generally indicates the device intended, according to the invention, to mutually associate a pair of planar parallel panels 2 to form a wall.
The device 1 comprises a pair of profiled elements 3 adapted to be respectively applied at the corners of the panels 2 and mutually associated by means of a spacer block 4. The spacer block 4 is associated to a tension member 5, adapted to rigidly couple the device 1 with a similar device applied in an diagonally opposite position of the panels 2.
More in detail, each profiled element 3 has a sort of groove 3a which is defined between an edge 6, on the outer side of the device, and a plate 7 on the inner side. The plate 7, has a rectangular form and the edge 6 extends along two sides of the plate to define L-shaped grooves 3a.
The spacer block 4 is constituted by a body having a significantly flattened parallelepipedal shape and is fixed, by means of a plurality of rivets 8, between the profiled elements 3, so as to set their mutual distance. The spacer block 4 is centrally provided with a seat 4a housing a cylinder 9 the axis whereof is perpendicular to the walls plates 7 of the profiled elements 3. The tension member 5 has a terminal portion 10 inserted diametrally in the cylinder 9 and can be moved axially by means of a screw element 11 to tension said tension element. A dowel 12 acts on a flattened portion 10a of the terminal 10 in order to prevent its rotation when the screw 11 is screwed. The dowel 12 is accessible through a central opening 7a in the walls 7.
The tension member 5 protrudes diagonally from the device 1 through a cavity 13 provided on the middle plane of the spacer block 4. The screw 11 is actuatable by means of an appropriate tool through a further cavity 14 which is diametrally opposite to the preceding one with respect to the cylinder 9.
The spacer block 4 furthermore has means for locking the panels 2 within grooves 3a of the profiled elements 3. Said locking means, which have the purpose of compensating different thicknesses of the panels with respect to the width of the grooves 3a, are substantially constituted by a pair of mutually superimposed plates 15, 16 coaxially rotatable in opposite directions about a pivot 17. The plates 15, 16 have a symmetrically trapezoidal shape so to press, at one end, respectively on one of the panels 2 through an opening 18 provided in the wall of the profiled elements 3. The angular rotation of the plates 15, 16 is determined by the translatory motion of a shank 19 which slideably engages respective mutually oblique elongated slots 20, 21 of said plates. The shank 19 has a portion provided with a female thread 22 which is coupled to a threaded stem 23 and is movable within a seat 24 provided in the spacer block 4. The stem 23 is provided, at one end, with a diametral notch 25, accessible through the cavity 14, for the engagement of an appropriate tool.
Thus, by rotating the stem 23 the shank 19 can be displaced along the seat 24 and the plates 15, 16 owing to the oblique slots 20, 21 are caused to rotate in opposite directions thus pressing the panels 2 against the outer edge 6 of the profiled elements 3, as indicated in broken lines 2a in FIG. 4.
Each pair of planar parallel panels 2 is thus positioned at its corners by means of respective devices 1 and rigidly associated by means of a pair of crossed tension members 5 which thus clamp, when tensioned, the pair of panels with a compressed action in a diagonal direction.
Said pair of panels is intended to be connected, in order to form a dividing wall, to similar pairs of panels by means of coupling means such as that indicated by the reference numeral 26 in FIGS. 3 and 4.
The coupling means 26 comprises a profiled element having a U-shaped cross section which has, at its opposite ends, respective wings 27 which extend from its longitudinal edges. The wings 27 are adapted to insert within corresponding recesses 28 provided in the spacer block 4 adjacent to the plates 7.
The profiled element illustrated in the drawing is obviously adapted for coupling two pairs of horizontally flanking and co-planar panels, its wings 27 inserting in the spacer blocks 4 of respective adjacent devices 1. Corner-shaped and cross-shaped simple or double profiled elements, equally having said pair of wings at the ends of their related arms, are however also provided for the horizontal and vertical coupling of the panels according to different geometries.
A connecting profiled element is furthermore provided, constituted by a single pair of wings and having, for its coupling to a pair of vertically adjacent panels, a hole for the passage of screw means which screw in a threaded hole 29 provided in the body of the spacer 4. The mounting of appropriate feet is provided at the base of the dividing wall, said feet screwing, according to the instances, in nuts 30 arranged at holes provided centrally to said profiled elements or in the threaded hole 29 provided in the spacer block 4.
In the practical embodiment of the invention, the materials employed, as well as the shapes and dimensions, may be any according to the requirements. | Device for associating a pair of planar parallel panels, particularly for producing walls for exhibition stands and the like, includes a pair of L-shaped profiled elements arranged side by side and adapted to be respectively applied at the corners of corresponding panels, spacer means adapted to mutually associate the profiled elements, tension elements rigidly associated with the spacer means and adapted to rigidly associate the device with a similar device applied in a position which is angularly opposite to the pair of panels. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention pertains to roof platforms, and more particularly to portable and readily adjustable roof platforms that do not damage the roof surface.
2. Description of the Prior Art
The purpose of a roof platform is to provide a relatively horizontal surface on which a person may comfortably stand while working on a sloped roof. To that end, several designs of adjustable roof platforms have been developed. U.S. Pat. Nos. 955,159; 2,320,538; and 3,866,715 are examples of swingable platforms that lock in discrete positions by means of pins and corresponding holes. Each of the above three patented platforms utilizes spikes or barbs which imbed into the roof to hold the platform in place. Using a spiked holding means is undesirable on asphalt and shake roofs because of potential damage to the roofing material. Furthermore, spiked holding means are not suitable for slate roofs. U.S. Pat. No. 3,164,353 discloses a roof bracket that is infinitely adjustable through its range. The bracket is secured to the roof by nailing plates and nails. The disadvantages of nailing the bracket to a finished roof are apparent.
In addition to not damageing the roof surface, a desireable feature of a roof platform is ease of operation. In some applications, time and weather conditions impose severe constraints on the set-up procedures of a roof platform. For example, fire-fighting personnel require a platform that may quickly be put in to use in all kinds of weather. Moreover, the platform must be rapidly and conveniently operated by personnel wearing heavy mittens. A roof platform that rests on the rungs of a roof ladder does not damage a finished roof. U.S. Pat. No. 2,848,282 illustrates a platform that is supported by a roof ladder. However, rapid and efficient set-up of the 2,848,282 platform is precluded because of the necessity of loosening and tightening or otherwise handling relatively small fasteners, which may easily be lost under adverse conditions. Thus, a need exists for an adjustable roof platform that does not damage a completed roof and that can be employed quickly and safely under emergency conditions.
SUMMARY OF THE INVENTION
The present invention provides an adjustable roof platform that is easily and rapidly adjustable through its range and that does not damage the roof. The adjustable roof platform includes a base which is adapted to engage the rungs of a roof ladder. To accomplish that purpose, the base incorporates at least one notch, which may be shaped in the form of an L, to hook onto a ladder rung to positively and safely secure the platform to the ladder. As adjustable step is pivotably connected to the base. Pivotable adjustment of the step relative to the base is accomplished by a toggle mechanism actuated by toggle actuating means, which may comprise a screw and thrust bearing arrangement. The screw may be rotated by means of a handle located in a convenient and accessable location. The step is preferrably pivotable relative to the base from a parallel side-by-side relation through an angle of about 45°.Further important features include light weight, a slip-proof step surface, and convenient portablity.
BRIEF DESCRIPTION OF THE DRAWINGS
While the specification concludes with claims particularly pointing out and distinctly claiming the subject matter regarded as forming the present invention, it is believed this invention will be better understood from the following detailed description taken in connection with the accompanying drawings, in which:
FIG. 1 is a perspective view of the portable adjustable platform of the present invention in operative position on a roof ladder;
FIG. 2 is a side view, partially broken, of the roof platform in an opened position; and
FIG. 3 is a side view of the roof platform in the closed position.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, reference numeral 1 indicates the portable adjustable roof platform of the present invention. In the illustrated embodiment, the platform is designed for use on sloped roofs, such as shown at 3, having pitches of up to about 45° with the horizontal. Reference numeral 5 represents a roof ladder conventionally constructed for the task at hand. For example, the roof ladder may be of the type commonly employed by fire-fighting personnel wherein spring actuated hooks engage the apex of the roof. It will be understood, however, that the use of the roof platform of the present invention is not limited to a particular occupation. For instance, the present platform is eminently suitable for carpenters working on building dormers.
In accordance with the present invention, the roof platform includes a base 7 adapted to engage rungs 9, 11 of the ladder 5. The base is preferably constructed of a generally U-shaped member having a flat frame portion 12 and a pair of downwardly extending support walls 14. It is anticipated that the platform will be employed with commonly used roof ladders having a relatively standard construction. Thus, it is expected that the depth of the ladder rails 13, the spacing between the rails, the diameter of the rungs, and spacings between the rungs will lie within relatively narrow ranges. A single width between the walls 14 and a single height of the walls should therefore suit the great majority of ladders commonly used on roofs.
To securely lock the base 7 onto the ladder rung 9, each support wall is formed with at least one notch, which is preferably L-shaped as indicated by reference numeral 15, FIG. 2. Upper surfaces 17 of notches 15 are preferrably of semi-circular shape, FIG. 3. The width of notch opening 21 and the diameter of upper surface 17 are sized to accommodate most ladder rungs; a dimension of about 1.50 inches in both instances is considered satisfactory. It is readily apparent that the weight of the platform as well as a person standing on it will tend to increase the engaging force of the base onto the ladder. To support the lower end 18 of the platform on ladder rung 11, the walls 14 may be formed with lower notches 19, which may be of a generally rectangular shape. The spacing between the openings 21 and the lower portions 22 of notches 19 may be about 14 inches, as that dimension will accommodate a standard spacing between adjacent rungs 9, 11. This and other dimensions specified herein are not considered to be critical. Indeed, although the invention is described in connection with a preferred embodiment, it will be understood that it is not intended to limit the invention to that embodiment. On the contrary, it is entended to cover all alternatives, modifications, and equivalents as may be included within the spirit and broad scope of the invention as defined in the appended claims.
Pursuant to the invention, lower surfaces 23 of the support walls 14 are preferrably spaced only a slight distance, perhaps on the order of 0.25 inches, from the roof when the base is in place on a ladder. The reason for the minimal spacing will be fully explained hereinafter.
To provide a working surface for use on a pitched roof, the adjustable platform of this invention includes a step 25, FIG. 1. In the particular platform illustrated, the step is fabricated as a generally rectangular frame 31. The frame is preferrably composed of suitable angles 33 together with a center support 35, as that design provides adequate strength with minimum weight. The preferrably employs a slip-proof working surface. For light weight, this is accomplished in the present instance by securing an expanded metal grating 37 to the top of the frame angles 33. Any suitable securing means, such as welding, may be used to fabricate the angles, support bar, and grating into a rigid unitary structure.
For allowing pivotable motion of step 25 relative to the base 7, the base may be constructed with a pair of vertical lugs 27, FIG. 2. Suitable coaxial pins 29 fixed within the lugs rotatively couple corresponding holes in the frame 31. To raise and lower the step relative to the base, the present invention incorporates a toggle mechanism 41. The toggle mechanism includes a pair of upper links 43. Each upper link is rotatably connected at its upper end by a pin 44 to a lug 45 projecting downwardly from the support bar 35. Each of the pair of lower links 47 is rotatably connected at its lower end by a pin 48 to a bracket 49 in the base. The lower links pass through a suitable opening 51 in the flat frame portion 12. The lower end of each upper link is mounted onto a hub 53 of a support bar 55 adjacent to the upper end of the corresponding lower link. Cotter pins, not shown, may be utilized to hold the links on the support bar.
Further in accordance with the present invention, the toggle mechanism is actuated by a toggle actuating means 56. The toggle actuating means may be any suitable device, such as a piston and cylinder arrangement. In the preferred embodiment, the toggle actuating means includes an elongated screw 59 and supporting structure 58. The upper end 60 of the screw engages corresponding threads in the support bar 55. The lower end 62 of the screw is supported for rotation in a journal 61 formed in bearing block 63. The bearing block may be be formed with a pair of opposed cylindrical hubs. 67. The hubs are rotatably supported in cooperating apertures in a pair of bearing supports 69. The bearing supports may be fastened to the base 7 by any appropriate method. The lower end of the screw, which is supported in the journal 61, is preferrably threaded. Washers 71 may be interposed between the bearing block and a pair of nuts 73 threaded onto the screw on either side of the bearing block, thus forming a pair of opposed thrust bearings. The illustrated toggle actuating means constitutes a non-overriding structure. The screw does not rotate to lower the step 25 when weight is applied to the step. Override is prevented by employing a screw having a diameter of about 0.75 inches and having about 12 threads per inch. To turn the screw and thereby actuate the toggle mechanism, a handle 75 of conventional construction may be permantently attached to the lower end of the screw by suitable means, such as a pin, not shown.
One of the features of the present invention is that it is readily transportable. For that purpose, the base 7, step 25, connecting links 43 and 47, bearing supports 69, and bearing block 63 are preferrably fabricated from aluminum. To further enhance portability, the support walls 14 may be constructed with generally oval openings 79. The openings serve as hand-holds, and they may be sized to accomodate a mittened hand. For ease of storage as well as transportation, the platform fully folds so that the base and the step lie in parallel side-by-side relationship, as shown in FIG. 3. As a result of the ease with which the instant roof platform may be carried, it is anticipated that a fire-fighter can easily carry it to a roof on the first response. Normally, a second fire-fighter would carry and set up the roof ladder.
To use the adjustable roof platform of the present invention, it will be assumed that the platform is carried to the roof in the closed position. Openings 21 of notches 15 are placed over a selected ladder rung, as at 9. The platform is lowered onto the rung, and then it is slid along the rung until the upper surface 17 engages the rung. Simultaneously, the lower notch 19 is lowered onto and slid along rung 11. Handle 75 is then rotated so that support bar 55 moves linearly toward the upper end 60 of the screw 59, thus causing the links 43, 47 to open the step 25 relative to the base 7. Rotating the handle in the opposite direction will cause the step to close. It is manifest that the platform of the present invention may be deployed quickly and efficiently under adverse conditions. Moreover, the platform step may be positioned and will remain in the desired position without the necessity of handling small pins or threaded fasteners.
It is a feature of the invention that the platform may be utilized with the notches 15, 19 of only one support wall 14 in engagement with rungs 9, 11, respectively. Thus, if desireable, the walls may straddle a ladder rail 13, with surface 23 of one wall resting on the roof. A fire-fighter would find this arrangement particularly useful when he is cutting a hole in the roof with a power cutting tool; he could conveniently cut the hole higher on the roof than the step 25 and adjacent the ladder 5.
Without further description, it is thought that the advantages to be gained from the disclosed embodiment of my portable adjustable roof platform will be apparent to those skilled in the art. It is contemplated that various modifications and changes may be made to the portable adjustable roof platform of the present invention within the scope of the appended claims without departing from the spirit of the invention. | A portable adjustable roof platform for use with a roof ladder so as not to damage a sloped roof surface. The roof platform may be quickly engaged with the roof ladder and adjusted to the horizontal position without handling small locating or fastening parts. The roof platform folds into a compact closed configuration for ease of transportation. | 4 |
BACKGROUND OF THE INVENTION
The present invention relates to systems for detecting the passage of a mobile at a predetermined point on its guided displacement along a track, and it has a particularly important, although not limiting, application to automatically controlled public transport installations.
Detection systems are already known of the type that comprises an interrogation assembly and a passive responder, (i.e. having no electrical power supply of its own, neither by means of a battery or storage battery, nor by means of connection to a power supply network), one being carried by the mobile and the other carried by the track, in which:
the interrogation assembly includes firstly a low frequency transmitter and secondly a medium frequency transmitter designed to operate continuously, the transmitters having respective antennas transmitting towards a zone that is predetermined relative to the antennas and through which the responder passes during displacement of the mobile, and secondly a unit that is responsive to the characteristics of the responder when the latter is in the zone, said interrogation assembly being arranged to be connected to an electrical power supply; and
the responder comprises a circuit for receiving the medium frequency signal and a circuit for receiving the low frequency signal which is arranged to control the medium frequency circuit.
Among existing systems, particular mention may be made of those in which each responder comprises two members which, when a mobile passes, generate medium frequency signals and which are offset along the track so that the sum of signals received by the interrogation assembly is subjected to a sudden variation as a mobile passes a determined point of the zone.
In general, the passive responder is carried by the track, but it could be carried by the mobile; it is often designated by the term "marker" or "beacon". Since it does not need any electrical power supply and since it is cheap, it is possible to distribute a large number of responders along a track which are single-piece non-reparable units.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a system enabling the cost and complexity of responders to be reduced even further in comparison with existing responders.
To this end, the invention provides, in particular, a system of the hereinbefore defined type wherein said low and medium frequency circuits of the responder comprise respective tuned radiating circuits and are associated in such a manner that the low frequency signal that is induced in the low frequency circuit by the low frequency transmitter of the interrogation assembly short-circuits the medium frequency resonance circuit at the low frequency rate, and wherein said interrogation assembly is responsive to disturbances of the medium frequency transmitter caused by the short-circuiting of the medium frequency tuned radiating circuit of the responder. The responder may easily be implemented so as to be programmable in situ.
In a particularly simple embodiment, the responder may be considered as being analog: The low frequency circuit short-circuits the medium frequency resonant circuit whenever it receives a low frequency magnetic field at a high enough level from the interrogation assembly, at the low frequency rate. The processor unit of the interrogation assembly detects medium frequency resonant circuit short-circuiting (i.e. its active or inhibited state, as the case may be), which changes the characteristics of the medium frequency transmitter due to the magnetic coupling between the medium frequency antenna of the interrogation assembly and the medium frequency tuned circuit of the responder. In practice, the processor unit merely determines whether the transmission medium frequency current is above or below a threshold.
In a more sophisticated embodiment, the responder may be considered as being digital. It further includes a logic unit designed, when enabled, to provide a serial digital message that is modulated at the low frequency rate, and said logic unit short-circuits the medium frequency resonant circuit of the responder only for a predetermined value of a digital message constituted by phase-modulated bits at the low frequency rate, which constitutes a clock signal. The message may differ for each responder. It is reconstructed by processing in the interrogation assembly. The electrical power required for operating the logic unit is generated by rectifying the low frequency signal induced in the low frequency tuned radiating circuit.
In such a responder, that may be referred to as "digital", the digital messages may be sent by phase shift keying (+π/4, -π/4), at the rate of the induced low frequency.
The use of a low frequency magnetic field link whose propagation and energy transfer can both be controlled constitutes an intrinsic safety factor as compared with arrangements in which the beacon is responsive to a much more disturbed electro-magnetic field and, at least at high frequency, is subject to parasitic excitation, in particular due to reflections.
The invention will be better understood on reading the following description of particular embodiments, given by way of non-limiting examples. The description refers to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of the system;
FIG. 2 is a block diagram of a passive network for amplifying phase difference, suitable for use in an interrogation assembly of the system of FIG. 1;
FIG. 3 shows a variant of FIG. 2;
FIG. 4 is a block diagram showing how the medium frequency antenna is short-circuited in the responder of the system of FIG. 1;
FIG. 5 shows how an LF antenna may be constituted for measuring speed;
FIG. 6 is a block diagram of a system according to a particular embodiment of the invention, having a digital responder; and
FIG. 7 and 8 are wave-form diagrams showing the appearance of the signals that appear in the interrogation assembly and in the responder, respectively.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The embodiments of the invention described below are applicable, in particular, to rail transport installations in which each responder constitutes a marker or beacon that is stationary relative to the track. The system is suitable for use in cooperation with automatic safety systems for driving transport vehicles of the kind already implemented in the VAL system and which therefore require no further description.
The interrogation assembly may be split into two portions; firstly the antennas placed beneath the mobile so as to have an effect on the antennas of the responder, and secondly the electronic circuit assembly that may be offset by a distance of several meters so as to be located in a protected zone. As explained below, the presence of a connecting cable between the antennas and the electronics may be used for the purpose of amplifying the phase offset used for detection purposes.
Whatever the embodiment, the detection system has the basic structure shown in FIG. 1. It comprises an interrogation assembly 10 and a responder 12 between which two magnetic field links are established in operation:
a low frequency link, e.g. at 128 kHz, that provides the power required for powering the responder 12 and that sets the modulation frequency of the response (and also the synchronization clock for the return message in the event of a digital responder); and
a higher frequency link, generally in the medium frequency band, e.g. in the range 5 MHz to 80 MHz, that can be considered as constituting a return path back to the interrogation assembly.
The principle on which the system operates is then as follows: by continuously analyzing the impedance of an antenna resonator 14 tuned to the medium frequency and connected to a continuously operating medium frequency oscillator 16, it is possible to detect when the medium frequency tuned resonant circuit 18 is short-circuited at the low frequency on receiving the low frequency signal via an LF receiver 20 in the responder.
When the interrogation assembly is located over a responder and the MF resonant circuit 18 is not short-circuited, the antenna resonator 14 becomes de-tuned by magnetic coupling, thereby causing the MF current through the MF resonator 14 to vary. A unit 22 in the interrogation assembly serves to detect this condition by monitoring:
either the phase shift of the MF current relative to a reference that is insensitive to environnement (such as an amplifier output voltage);
or else the amplitude of the antenna current, which varies at the rate at which the resonant circuit 18 is short-circuited, i.e. at the low frequency rate (and also in response to an identification message contained in a read only memory 24 if the responder is a digital responder).
The low frequency link to the LF receiver 20 is provided from the interrogation assembly by means of an LF oscillator 26 that runs continuously in use, and via an LF antenna 28.
A phase or amplitude change due to passing over a responder 12, having its resonant circuit 18 short-circuited at the low frequency rate, is detected, preferably by means of a passive network for amplifying phase or amplitude difference as presented periodically by the MF current delivered by the antenna resonator 14. In particular, the passive network may make use of the properties of unmatched transmission lines that give rise to standing waves. Such a network includes a length of line that is sufficient for even a small amount of unmatching at the end of the line to give rise to a usable effect on the source. The effect appears as a change in the complex impedance as seen from the MF oscillator 16. It gives rise to a voltage/current phase shift or to a change in the amplitude of the current.
In practice, the length of the line will be equal to (2k+1)λ/2, where k is an integer greater than 1 and λ is the wave length of the medium frequency signal.
In the embodiment shown in FIG. 2, the line 30 is constituted by a length l of cable of known characteristic impedance. The current I in the cable is sensed with a current transformer represented by a loop 32.
In the example shown in FIG. 3, the line of length l is synthetized by a cascade of elementary quadriple cells 34 (R, L, C, G). The number of cells used is sufficient to represent a length of line that is longer than the wave length of the medium frequency signal and that is an odd multiple of a half-wavelength. The current I is again sensed from one of the line conductors and the voltage V is taken across the conductors, at the input of the unit 20, as seen from the antenna. There is no need to describe the LF oscillator 26 which may be of conventional design. The antennas 14 and 28 may both be constituted by flat coils and they may be superposed or even wound on a common insulating support.
The receiver 20 of the responder for short-circuiting the MF resonant circuit 18 is of different structure depending on whether the responder is an analogue responder or a digital responder. In all cases, control may rely on a change in the dynamic impedance of a diode, e.g. constituted by a PN junction, responsive to the current flowing through it. Such dynamic impedance may be considered as being a resistance rd that varies, responsive to the low frequency current Ie flowing through it, in accordance with the relationship:
rd=(kT/q)·(1/Ie)
where kT/q is the thermo-dynamic potential, of about 25 mV at 20° C.
The medium frequency link must give rise to a current Ie whose extreme values are sufficient when the interrogation assembly passes over the responder, to give rise to a significant change in rd, enabling the responder to be detected.
The use of the dynamic impedance of a diode as the switching element confers a major advantage from the point of view of intrinsic safety. In this context, it must be recalled that safety requires that there is no excitation of a responder by a mobile or any source other than a mobile travelling over the responder (e.g. to avoid an erroneous indication that a vehicle leaves a block on a railway track). In contrast, failure to detect passage over a responder generally gives rise to consequences that are much less severe, since safety must rather result in failure to detect.
As shown above, the resistance rd of the diode is an inverse function of the current flowing through it. Any reduction in the current flowing through the diode below a threshold will give rise to a diode resistance that remains high enough to ensure that there is no finding or short-circuiting. Consequently, the magnetic coupling with the medium frequency resonant circuit 36 is degraded.
If the responder is an analogue responder, the method of control may be as shown diagrammatically in FIG. 4: a diode 38 is connected in parallel across the output of the antenna 36 of the receiver 20. This output is connected to the MF resonator 18 of the responder via a filter 40, for the purpose of eliminating transients and a part of the noise.
If the marker is a digital marker, the receiver also includes a PROM 24 for controlling the current Ie in such a manner as to build up a serial message that may be decoded by unit 22.
An embodiment of the invention that enables the displacement speed of the mobile to be measured under conditions of intrinsic safety, makes use of a low frequency antenna 28 that comprises three components that are offset in the displacement direction and that are powered differently. In practice, the low frequency antenna may then comprise three coils 28a, 28b, 28c that are powered in phase opposition (0, π, 0) by the LF oscillator 26 (FIG. 5).
As before, the unit 22 can sense changes of current with intrinsic safety by applying envelope detection to the MF current. However, in this case, phase inversions--that occur when the interrogation assembly travels over the responder--are detected at the same times as the instants at which they occur thereby making it possible to calculate speed. With a digital responder, demodulation of the digital signal representative of the identification message must take the phase inversions (0, π) of the low frequency signal into account.
As explained above, the phase inversions of the low frequency signal can be processed safely by using safety electronics of known type, such as that used in the automatic on-board controllers in the VAL transport system, where the same function is required for detecting passages over the servo-control lines of the transmission mat placed on the crossings of the track.
When necessary, it is also possible to establish a low data rate communication link between the interrogation assembly and the marker. To do this, the low frequency signal can be phase modulated at a low modulation rate of about 1 Kb/s. That modulation may be used as a return channel, which is advantageous in certain responder locations, e.g. in a station. Such a link can be established without requiring an additional antenna on the interrogation assembly.
It is possible to use responders having lengths in the track direction which depend on their locations. It is generally desirable to have short responders in the ordinary portions of the track. In contrast, it may be desirable to use long responders, e.g. having tuned circuits that extend over a length of 1 m to 3 m, in stations. Safety reasons often require vehicle doors to open only when the interrogation assembly of the vehicle is located over a marker. The accuracy with which vehicles are stopped often does not enable this condition to be satisfied if the responders have the short length that is acceptable in an ordinary portion of the track.
Like the responders in an ordinary portion, such responders are compatible with low data rate transmission of a signal via the low frequency channel.
A detection system having a digital responder enabling speed to be measured will now be described as a particular embodiment.
The overall structure of this system is shown in FIG. 6 where elements corresponding to elements in the preceding figures are designated by the same reference numerals.
As mentioned above, the interrogation assembly 10 includes an LF oscillator 26 which feeds the LF antenna 28 via a tuning circuit 42. A second output of the LF oscillator 26 feeds a phase demodulator 52 and a safety phase comparator 44 belonging to the processor unit 22 and described below.
The MF transmitter 16 drives the MF antenna 14 via a cable compensation network 46 and a tuning circuit 42. To limit overall size, the antennas may be constructed as concentric flat radiating coils. The Q-factor of the LF antenna must be high enough to ensure coupling that will generate a significant signal in the responder 12. In a railway application, it is possible to use an LF oscillator 26 at 128 kHz, that provides a sine wave signal having a RMS power of 10 W at the LF antenna 20. The tuning circuit may be connected to the electronics by means of a cable having a characteristic impedance close to 50 Ω.
The MF oscillator may deliver an RMS power of about 1 W to the antenna via a cable having a characteristic impedance of 50 Ω at a frequency of 10 MHz. The compensation network 46 is such that the link is of sufficient length for the MF current at the output from the oscillator 16 to be responsive to the de-tuning caused by the presence of the medium frequency resonant circuit of the responder.
The unit 22 shown by way of example retrieves the low frequency component of the MF current modulation at the output from the oscillator 16. The pass band of the unit must be sufficient to avoid distorting the digital message provided by the programmable read only memory 24 of the marker. For a low frequency of 128 kHz, an acceptable pass band is about 300 kHz.
The unit 22 includes a functional path that is necessary and a safety path that is merely optional. The functional path comprises an envelope detector 50 for recovering the LF signal and a phase demodulator 52 for recovering the PSK coded digital message. The detector 50 may include a diode rectifier in conventional manner.
The safety envelope detector 54 of the safety path operates on the same principle as the detector 50, with a narrower pass band. The safety path does not need to recover a message, it merely has to identify the 128 kHz spectral peak and phase inversions on passing from coil 28a to coil 28b, and from coil 28b to coil 28c. The circuit shown in FIG. 6 further makes it possible to perform safety speed measurements. The function of the detector 54 is to recover the low frequency transmitted by the interrogation assembly and to enable the signal phase (0, π), to be recognized, which phase depends on which one of the coils (FIG. 5) is beneath the LF antenna 28. The safety phase comparator 44 determines phase rotations (0, π) in the low frequency signal and may be constructed to be secure, as is the case for the circuits used in the VAL systems.
Also advantageously, the responder 12 includes antennas constituted by concentric coils, the MF resonant circuit having a Q-factor that is high enough for the magnetic coupling effect with the antenna resonator 14 to generate a detectable disturbance.
The resonator also includes a rectifier network 54 which provides the necessary power supplies from the low frequency power induced in the antenna 56 of the low frequency receiver 20. A second circuit 58 extracts a clock signal from the low frequency signal. The rectified signal is applied to a logic unit 60 connected to the read only memory 24. The logic unit also includes a phase modulator for PSK encoding of the digital signal from the read only memory at the low frequency rate provided by the clock circuit 58.
The MF resonant circuit 18 is short-circuited by a diode 38 that is current driven from a control circuit 62, whose switching element may be a bipolar transistor. A network 64 matches the impedance of the control circuit to that of the MF resonant circuit 18.
By way of example, FIG. 7 shows the appearance of signals in the interrogation assembly at points marked in FIG. 6 by letters that correspond to the lines of FIG. 7. Time interval 66 corresponds to operation during the period when the interrogator is not moving over a responder. Time interval 68 corresponds to the first coil of an antenna of the kind shown in FIG. 5 passing over the responder. Time t corresponds to a phase inversion that occurs when the second coil is coupled with the responder. At the end of the second stage 70, a third stage occurs (not shown) during which the phase is the same as it was during the first stage.
FIG. 8 shows the appearance of signals in the responder 12 at points marked by letters in FIG. 6, for a digital marker (ligne M) and for an analog marker (line N).
The signal K is generated only in a digital responder. In a digital responder, the signal M corresponds to the MF resonant circuit 18 being opened and short-circuited. In an analog responder, the resonant circuit is opened and closed merely at the rate of the low frequency. Due to rectification, the signal J gives rise to a magnifying effect. | The system comprises an interrogation assembly and a passive responder. One is carried by a mobile and the other by a track. The interrogation assembly includes continuously operating low frequency and medium frequency transmitters. The transmitters have respective antennas directed towards a predetermined zone with respect to the antennas, which is traversed by the responder during movement of the mobile. It further has a unit which is responsive to the characteristics of the responder when the responder is in the zone. The responder has a low frequency reception circuit which controls a medium frequency circuit. Both circuits have radiating circuits which are tuned and the low frequency signal generated in the low frequency circuit is used to short-circuit the medium frequency tuned circuit of the responder, at the rate of low frequency rate. | 1 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Patent Application No. 61/492,781 filed Jun. 2, 2011 which is incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates generally to an apparatus for securing rail seals to a rail. Particularly, the present invention relates to a rail seal clip for use in rail crossings or road level railbeds.
BACKGROUND OF THE INVENTION
Rail crossings are places where roads, footpaths, or other rights of way cross railway tracks. Crossings are a source of ongoing conflict between the needs of the railways and the needs of rail crossing users. Pedestrians, drivers, animals and other users prefer that the crossings be as similar to or as consistent with the road surface as possible. Similarly, in road level railbeds such as those used for light rail, it is desirous to have the railbed and the road form as continuous a surface as possible. However, trains and other rail equipment require a space, called a flangeway gap, between the inner edge of the rail and the crossing surface sufficient to allow the wheels of the train or other rail equipment to pass through. The flangeway gap can cause issues for non-rail users and is also an area where there is frequent accumulation of water and debris, accelerating wear and tear on the crossing and adding to maintenance requirements.
Rail seals such as those described in U.S. Pat. Nos. 4,606,498 and 8,100,342 are designed to fill the flangeway gap while still allowing the train to pass. They fit snugly against the rail on gage and field sides, easing rail crossings and road level railbeds and preventing moisture and debris from filling the gaps between the rail and the crossing material.
In order to function properly, rail seals need to be firmly held against the sides of the rail. Typically, rail seals are held in place using spikes as in U.S. Pat. No. 4,606,498 or rail clips as in U.S. Pat. No. 6,213,407. Bending partially driven spikes to hold the rail seals in place can be dangerous and can damage the cross ties. Traditional spring-clips require special tools to install them correctly. There is therefore a need in the art for rail clips that are easy to install and do not require special tools for installation.
SUMMARY OF THE INVENTION
The following summary is intended to highlight and introduce some aspects of the disclosed embodiments, but not to limit the scope of the claims. Thereafter, a detailed description of illustrated embodiments is presented, which will permit one skilled in the relevant art to make and use various embodiments. The summary is directed to rail clips that may be used to hold rail seals or other flangeway fillers in place and methods for installing such rail clips.
The rail clip as described herein is a metal bracket of a generally U-shaped configuration. In one embodiment the rail clip may be formed by joining a J shaped bracket with a reversed C shaped bracket with an elongated arm formed by the back of the J shaped bracket. In another embodiment the rail clip may be formed by joining a reverse J shaped bracket with a C shaped bracket with an elongated arm formed by the back of the J shaped bracket. In some embodiments the C shaped bracket is on the field side of the rail. In other embodiments the J shaped bracket is on the field side of the rail. In additional embodiments the reverse C shaped bracket is on the gage side of the rail. In further embodiments, the reverse J shaped bracket is on the gage side of the rail.
The two brackets are joined by a hinge in a single plane to form the U shaped bracket. The hinge may be any type of hinge that allows the reverse C shaped bracket (or C shaped) and the J shaped (or reverse J shaped) bracket to rotate and/or pivot independently of each other. Each bracket may rotate and/or pivot the same or different amounts from about 0° to about 360°, preferably about 20° to about 180°, from about 30° to about 90°, from about 0° to about 75°, from about 35° to about 75° from about 35° to about 45°, from about 45° to about 90°, from about 90° to about 135° from about 90° to about 125°. In some embodiments, the hinge may allow the reverse C shaped bracket (or C shaped bracket) and the J shaped bracket (or reverse J shaped bracket) to rotate forwards and/or backwards. In other embodiments, the reverse C shaped bracket (or C shaped bracket) and/or the J shaped bracket (or reverse J shaped bracket) may rotate different amounts forward or backwards. In further embodiments, rotating the bracket a particular amount may lock it into place. Each of the reverse C shaped (or C shaped) and J shaped (or reverse J shaped) brackets additionally has a free end that may be used to lock a rail seal into place against a rail.
In another embodiment, the rail clip may be formed by joining two curved brackets with an elongated arm. The brackets may be curved the same or different amounts. The field side bracket is attached to the elongated arm on a first end with a first hinge and the gage side bracket is attached to a second end of the elongated arm with a second hinge. The hinges may be any type of hinge that allows the two curved brackets to rotate and/or pivot independently of each other in relation to the elongated arm and may be the same or different types of hinges. Each bracket may rotate and/or pivot the same or different amounts from about 0° to about 360°, preferably about 20° to about 180°, from about 30° to about 90°, from about 0° to about 75°, from about 35° to about 75°, from about 35° to about 45°, from about 45° to about 90°, about 90° to about 135°, about 90° to about 125°. In some embodiments, the hinges may allow the brackets to move forwards and backwards. In additional embodiments, the hinges may allow the brackets to move different degrees forwards or backwards. In further embodiments, the hinges may allow the brackets to move the same amounts forwards and backwards. In other embodiments, the hinges may lock into place when rotated or pivoted a particular amount. Each curved bracket additionally has a free end that may be used to lock a rail seal into place against a rail.
Generally, when rails are installed, the crossties are set in ballast such as gravel. The ballast is usually set just below the level of the crosstie creating a gap between the undersurface of the foot of the rail and the ballast. To install the rail clips as described herein, the bracket is placed flat against the ground and the elongated arm is manipulated under the foot of the rail in the gap between the foot of the rail and the ballast. In single hinged embodiments, the C or reverse C shaped bracket is rotated so that it is approximately perpendicular to the reverse J or J shaped side of the bracket. In some embodiments, the C or reverse C shaped bracket is rotated prior to manipulating the elongated arm under the foot of the rail. The entire clip is then rotated upright so that the free end of the J shaped or reverse J shaped bracket presses against the rail seal on the appropriate side, holding it in place. The C or reverse C shaped bracket is then rotated past the plane of the reverse J shaped or J shaped bracket to lock in place and clamp the rail seal against the rail. For example, in an instance in which the reverse C shaped bracket is on the gage side of the rail, the bracket is placed flat against the ground. The reverse C shaped bracket is rotated so that it is approximately perpendicular to the J shaped bracket. The elongated back of the J shaped bracket is then manipulated under the foot of the rail. The entire clip is then rotated upright so that the free end of the J shaped bracket on the field side of the rail presses against the field side rail seal. The reverse C shaped bracket is then rotated past the plane of the field side of the bracket to lock into place and clamp the gage side rail seal against the gage side of the rail.
In multi-hinged embodiments, either or both of the curved arms may be rotated approximately perpendicularly to the elongated arm prior to or after manipulation under the foot of the rail. The entire clip is then rotated upright and the rotated arms are rotated back past the plane of the elongated arm to lock in place and clamp the rail seals against the respective sides of the rail. The rail clips as described herein can be installed with minimum labor and disruption of ballast and do not require any special tools.
Other objects, features and advantages of the present invention will be apparent from the following specification and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross section view of a rail and rail seals secured by means of an embodiment of the invention.
FIG. 2 is a side view of an embodiment of the invention.
FIG. 3 is a side view of an embodiment of the invention.
FIGS. 4 A-B are top views A and side views B of the hinge portion of an embodiment of the invention.
FIG. 5 is a view of a rail seal clip of an embodiment of the invention.
FIG. 6 is a view of a rail seal clip of an embodiment of the invention.
FIG. 7 is a view of a rail seal clip of an embodiment of the invention.
FIG. 8 is a top view of an embodiment of the invention placed under a rail.
FIG. 9 is a side view of an embodiment of the invention rotated into an upright position.
FIG. 10 is a cross-sectional view of a rail and a pair of rail seals secured by an embodiment of the invention.
DETAILED DESCRIPTION
Referring now to the drawings, FIG. 1 depicts one rail 120 of a pair of rails (second rail not shown) conventionally mounted on a chair mounted on a cross-tie and held in place with railway spikes. A first rail seal 110 is held against the field side of the web 124 of a rail 120 and a second rail seal 130 is held against a second side of the web 124 on the gage side of the rail 120 by means of an exemplary rail clip 140 . The second rail seal 130 includes a recess 135 to accommodate the flanges of passing railway wheels (flangeway gap). The rail clip 140 passes underneath the foot 126 of the rail 120 . The other rail in a set of rails would be the mirror image of FIG. 1 with the second rail seal 130 on the gage side and the first rail seal 110 on the field side of the rail 120 . In a typical crossing or road level rail bed, multiple rail clips 140 would be used to ensure that the rail seals were held in place along the length of the rail in the crossing or road.
For ease of description, the rail clip is described in terms of the field side of the rail being on the left as one looks down the length of the rail and the gage side of the rail being on the right as shown in FIG. 1 . This configuration would be reversed in the second rail of a pair of rails with the field side being on the right as one looks down the length of the rail and the gage side being on the right (not shown).
The rail clip 140 comprises a J shaped bracket 150 (field side) and a reverse C shaped bracket 160 (gage side) which are connected by a hinge 170 . The hinge 170 may be any type of hinge generally used to connect brackets such that it allows the brackets to rotate or pivot independently of one another. In alternate embodiments, the rail clip 140 is the reverse, with a C shaped bracket on the field side and a reverse J shaped bracket on the gage side connected by a hinge 170 ′.
In some embodiments, each bracket may rotate up to about 360° or any fraction thereof as seen in a universal joint, universal coupling, U joint, Cardan joint, Hardy-Spicer joint, or Hooke's joint in relation to the other end. Exemplary hinges additionally include a gate hinge which may pivot from about 90° to about 180°. In other embodiments, the rotation may be about 45° to about 180°, about 45° to about 95°, about 45° to about 90°, about 90° to about 135°, about 90° to about 125° in relation to the various axes. In some embodiments the hinge may allow the brackets or a bracket to move forward or backward. In other embodiments the hinge may allow the brackets to move more in one direction than the other. For example, the hinge may allow the bracket to move about 90° forwards, towards an installer and then back about 125°, i.e. about 35° past its uniplanar starting position to lock in place. In other embodiments, the hinge may allow the bracket to move about 90° backwards, so that the end of the bracket 180 is facing the installer and then forwards about 125°, i.e. about 35° past its uniplanar starting position to lock in place. In some embodiments, the hinge may be secured. The hinge 170 or 170 ′ may be spring loaded, secured with a locking sleeve, screw or other fastening device known to those of skill in the art. In other embodiments it may snap in place. In further embodiments, it may lock in place when a particular rotation is achieved. In some embodiments, the rotation of different parts of the device may be in one or more planes. In other embodiments, the J end and the C end of the rail clip rotate and/or pivot so that they are perpendicular to each other. In additional embodiments, each end of the hinge may rotate and/or pivot independently and in varying degrees in comparison to the other. For example, the C end of the rail clip may rotate about 135° to about 85°, about 125° to about 90°, about 95° to about 80°, preferably about 90° whereas the J end of the bracket may rotate about 45° or less, about 40° to about 35°, about 40° to about 30° from a uniplanar position or vice versa. In some embodiments, the J end of the rail clip may rotate about 35°. As shown in FIG. 1 , the respective free ends 190 and 180 of the J bracket and reverse C bracket of the rail clip 140 may be curved. In other embodiments they may be straight. In some embodiments, one or the other may independently be straight or curved. The ends 190 and 180 may be curved the same amount or different amounts as shown in FIG. 1 . Rail seals may be secured to a rail using one or more rail clips 140 along the length of the rail 120 as necessary. After the rail clips 140 are installed, the rest of the rail crossing structure may be constructed in the typical fashion.
Referring to FIG. 2 , the rail clip is described in terms of the field side of the rail being on the left as one looks down the length of the rail and the gage side of the rail being on the right for ease of description. This configuration would be reversed in the second rail of a pair of rails with the field side being on the right as one looks down the length of the rail and the gage side being on the right (not shown).
The rail clip 240 comprises a J shaped bracket 250 (field side) and a reverse C shaped bracket 260 (gage side) which are connected by a hinge 270 . In alternate embodiments, the hinge 270 may be on the left side of the image (not shown) such that the rail clip 240 comprises a C shaped bracket connected to a reverse J shaped bracket. The hinge 270 may be any type of hinge generally used to connect brackets such that it allows the brackets to rotate independently of one another. In some embodiments, each end may rotate up to about 360° or any fraction thereof as seen in a universal joint, universal coupling, U joint, Cardan joint, Hardy-Spicer joint, or Hooke's joint in relation to the other end. Exemplary hinges additionally include a gate hinge which may pivot from about 90° to about 180°. In other embodiments, the rotation may be about 45° to about 180°, about 45° to about 95°, about 45° to about 90°, about 90° to about 135°, about 90° to about 125°, in relation to the various axes. In some embodiments the hinge may allow the brackets or a bracket to move forward or backward. In other embodiments the hinge may allow the brackets to move more in one direction than the other. For example, the hinge may allow the bracket to move about 90° forwards, towards an installer, and then back about 125°, i.e. 35° past its uniplanar starting position to lock in place. In other embodiments, the hinge may allow a bracket to move about 90° backwards, away from an installer and then forward about 125°, i.e. about 35° past its uniplanar starting position to lock in place. The hinge 270 may be spring loaded, secured with a locking sleeve, screw or other fastening device known to those of skill in the art. In other embodiments it may snap in place. In further embodiments, it may lock in place when a particular rotation is achieved. In some embodiments, the rotation of different parts of the device may be in one or more planes. In other embodiments, the J end and the C end of the rail clip rotate and/or pivot so that they are perpendicular to each other. In some embodiments, the C end of the rail clip rotates about 90° from the J end of the rail clip for installation and then rotates back about 10°, about 15°, about 20°, about 25°, about 40°, about 45°, about 50°, about 60°, about 95°, about 100°, about 105°, about 110°, about 115°, about 120°, about 125°, about 130°, about 125°, about 135°, about 140°, about 145°, to lock into place, holding a rail seal against a rail. As shown in FIG. 2 , the respective free ends 290 and 280 of the J bracket and reverse C bracket of the rail clip 240 may be curved. In other embodiments they may be straight. In some embodiments, one or the other may independently be straight or curved. The ends 290 and 280 may be curved different amounts or the same amount as shown in FIG. 2 .
Referring now to FIG. 3 , a multi-hinged embodiment of a rail clip is shown in which the field side of the bracket is on the left and the gage side of the bracket is on the right. In a second rail (not shown), the configuration would be reversed with the gage side of the clip on the left and the field side of the clip on the right. For convenience, the rail clip is described as shown in FIG. 3 but the mirror image would also apply.
In this embodiment, the rail clip 340 comprises two curved brackets 350 and 360 attached by hinges 375 and 370 to an elongated arm 345 . The field side curved bracket 350 is joined by a first hinge 375 to a first end of the elongated arm and a gage side curved bracket 360 is joined by second hinge 370 to a second end of the elongated arm such that the field side curved bracket 350 and the gage side curved bracket 360 can rotate independently of one another in relation to the elongated arm.
The two curved brackets 350 and 360 have free ends 390 and 380 respectively which may be curved as shown or straight. In some embodiments, either bracket end may independently be curved or straight. The two curved arms 350 and 360 may be the same or different lengths and have the same or different degrees of curvature. Either or both of the curved arms 350 and 360 may rotate through the hinge 375 and 370 respectively. The hinges 375 and 370 may be any type of hinge generally used to connect brackets such that it allows the brackets to rotate and/or pivot independently of one another in relation to the elongated arm. In some embodiments the hinges may be the same type of hinge. In other embodiments each hinge may be a different type of hinge. In some embodiments, each curved bracket 350 and 360 may rotate up to about 360° as seen in a universal joint, universal coupling, U joint, Cardan joint, Hardy-Spicer joint, or Hooke's joint in relation to the other end. In other embodiments, the rotation may be about 30° to about 180°, 35° to about 95°, about 35° to about 90°, about 35° to about 75°, about 90° to about 135° in relation to the various axes. In some embodiments the hinge may allow the brackets or a bracket to move forward or backward. In other embodiments the hinge may allow the brackets to move more in one direction than the other. For example, the hinge may allow the bracket to move about 90° forwards, towards an installer and then back about 125°, i.e. about 35° past its uniplanar starting position to lock in place. In other embodiments, the hinge may allow the bracket to move about 90° backwards, so that the end of the bracket 380 is facing the installer and then forwards about 125°, i.e. about 35° past its uniplanar starting position to lock in place. Exemplary hinges additionally include a gate hinge which may pivot from about 90° to about 180°. The hinge 370 may be spring loaded, secured with a locking sleeve, screw or other fastening device known to those of skill in the art. In other embodiments it may snap in place. In further embodiments, it may lock in place when a particular rotation and/or pivot is achieved or any other locking mechanism that is generally used to secure a hinge.
In some embodiments, the rotation of different parts of the device may be in one or more planes. In other embodiments, one or both of the curved brackets may rotate perpendicular to the elongated arm 340 . In additional embodiments, each end of the hinge may rotate independently and in varying degrees in comparison to the other. For example, the gage side end of the rail clip may rotate from about 0° to about 360°, from about 180° to about 85°, from about 180° to about 95°, from about 180° to about 80°, preferably from about 180° to about 90°, more preferably from about 180° to about 75° whereas the field side end of the bracket may rotate about 45° or less, about 40° to about 35°, about 40° to about 30° or vice versa.
An embodiment of a hinge that may be used in embodiments of the invention is shown in FIG. 4 . The hinge comprises a pin (not shown) and two halves, a male half 410 and a female half 430 . When assembled, a pin (not shown) is inserted in a hole 440 in the female half 430 and through the hole 420 in the male half 410 , connecting the two pieces of the hinge.
Referring now to FIGS. 5 , 6 , and 7 , the rotation of the parts of an exemplary rail clip as disclosed herein is depicted. A side view of an embodiment of a rail clip 540 with the field side of the bracket on the left and the gage side of the bracket on the right as described herein is shown in FIG. 5 . For convenience, the rail clip is described as shown in FIG. 5 with the field side on the left and the gage side on the right, but the mirror image (not shown) would apply to the second rail with the gage side of the bracket on the left and the field side of the bracket on the right. The rail clip 540 shown in FIG. 5 comprises a J shaped bracket 550 connected to a reverse C shaped bracket 560 by a hinge 570 . The reverse C shaped bracket 560 is rotated forwards about 90° as shown in FIG. 6 and the rail clip 540 is maneuvered under a rail (not shown) so that the long arm of the J shaped bracket 555 is perpendicular to the rail. The end 590 of the J shaped bracket is then positioned to hold a rail seal in place. The reverse C shaped bracket 560 is then rotated more than 90°, about 95°, about 100°, about 105°, about 110°, about 115°, about 120°, about 125°, about 130°, about 135°, about 140°, about 145°, back past its starting position in FIG. 5 so that the end 580 holds a rail seal against a rail and the reverse C shaped bracket locks in place as shown in FIG. 7 .
Referring to FIGS. 8 , 9 , and 10 , a method installing a rail clip as disclosed herein is depicted. A top view of an embodiment of a rail clip 840 with the field side of the bracket on the left and the gage side of the bracket on the right is shown in FIG. 8 along with an end view of a rail. Any of the rail clips as described above may be installed using these methods. For convenience, the rail clip is described as shown in FIG. 8 but the mirror image would apply to the second rail. The rail clip 840 shown in FIG. 8 comprises a J shaped bracket 850 connected to a reverse C shaped bracket 860 by a hinge 870 . As shown in FIG. 8 , the reverse C shaped bracket 860 is rotated forwards about 90° towards an installer and the rail clip 840 is maneuvered under the foot 826 of a rail 820 so that the long arm 855 of the J shaped bracket 850 is perpendicular to a rail. The rail clip 840 is then rotated upwards so that the end 890 of the J shaped bracket may be positioned to hold a rail seal 810 in place against the web 824 of a rail 820 as shown in FIG. 9 . The reverse C shaped bracket 860 is then rotated more than 90°, about 95°, about 100°, about 105°, about 110°, about 115°, about 120°, about 125°, about 130°, about 135°, about 140°, about 145°, past its starting position to lock into place, holding a second rail seal 830 against a rail 820 as shown in FIG. 10 .
References to “one embodiment” or “an embodiment” do not necessarily refer to the same embodiment, although they may. Unless the context clearly requires otherwise, throughout the description and the claims, the words “comprise,” “comprising,” and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is to say, in the sense of “including, but not limited to.” Words using the singular or plural number also include the plural or singular number respectively. Additionally, the words “herein,” “above,” “below” and words of similar import, when used in this application, refer to this application as a whole and not to any particular portions of this application. When the claims use the word “or” in reference to a list of two or more items, that word covers all of the following interpretations of the word: any of the items in the list, all of the items in the list and any combination of the items in the list.
Those skilled in the art will recognize that it is common within the art to describe devices and/or processes in the fashion set forth herein, and thereafter use standard engineering practices to integrate such described devices and/or processes into larger systems. That is, at least a portion of the devices and/or processes described herein can be integrated into a railway via a reasonable amount of experimentation.
The foregoing described aspects depict different components contained within, or connected with, different other components. It is to be understood that such depicted architectures are merely exemplary, and that in fact many other architectures can be implemented which achieve the same functionality. In a conceptual sense, any arrangement of components to achieve the same functionality is effectively “associated” such that the desired functionality is achieved. Hence, any two components herein combined to achieve a particular functionality can be seen as “associated with” each other such that the desired functionality is achieved, irrespective of architectures or intermedial components. Likewise, any two components so associated can also be viewed as being “operably connected”, or “operably coupled”, to each other to achieve the desired functionality.
While a preferred embodiment of the present invention has been illustrated, those skilled in the art will recognize that many modifications and variations are possible in accordance with the above teachings without varying from the spirit and scope of the invention. It is to be understood that such modifications and variations are within the spirit and scope of the present invention as set forth in the following claims. | A rail clip to be used to fasten rail seals or flangeway fillers to a rail. The rail clip includes a generally U-shaped hinged clip with one or more hinges formed by two curved arms of the same or different curvatures and an elongated back. The elongated back is designed to fit between the foot of the rail and the ballast. One or more of the arms may be rotatable such that it is perpendicular to the elongated arm and the other arm, allowing the clip to be put in place. Once the clip is in place, the arm is rotated to the desired position and locked into place, holding each rail seal against the rail. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. provisional application Ser. No. 61/813,588 filed on Apr. 18, 2013, the entirety of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
The technical field of the invention pertains generally to lighting used in the production of video and film, and, more particularly, to improvements in the Fresnel luminaire commonly used in the production of video and film.
Fresnel lights utilize a lens with grooves cut to disperse and soften the edges of the projected beam of light, consequently softening the shadows cast by objects illuminated using a Fresnel light and allowing for softer transitions between other Fresnel lights being used on a production set. Fresnel lights have a unique diffusion of light due to the lens, and may be adjusted/focused from a flood or wide beam to a spot or narrow beam by moving the bulb longitudinally away from the lens. The scatter of light from the Fresnel lens is typically controlled or shaped using barn door attachments.
Prior Fresnel lights utilize a bulb configured within a cylindrical or otherwise fixed volume so as to move fore and aft longitudinally toward (fore) and away from (aft) of the focusing (eg. Fresnel type) lens in order to obtain broader or narrower (more focused) spread/dispersion of light projected forward toward the video/film subject. Fresnel lights have been used in the video and film industry, but all require substantial space when transporting them to and from and about a production set. Existing designs used in the industry typically do not allow for easy disassembly or collapsing or otherwise meaningfully reducing space requirements for storage or transport, or for that matter, simply moving equipment about a production studio/set. The large size, heavy weight, and resulting bulk of existing and conventional Fresnel light units are problems.
Conventional Fresnel lights typically use high wattage bulbs that consume large amounts of power to operate, generate high amounts of heat, have a relatively short life, and are expensive to replace. Further, the orientation of the bulb in conventional Fresnel fixtures has an impact on life of the bulb. A conventional Fresnel utilizes a single high wattage bulb set upright in a screw in bulb socket affixed to structure within a can-shaped housing, a slide bar or other knob used to move the bulb forward closer to the Fresnel lens or rearward to increase the distance from the Fresnel lens and widening the beam of projected light. A Fresnel light may be held by a film crew member, positioned using a stand, or mounted on a variety of (often overhead) stage lighting structures, and the orientation of the Fresnel with respect to its lamp/bulb may not be attended to or easily maintained. Burning the lamp upside down, for example, shortens lamp life substantially.
A major problem of conventional Fresnel lights is the heat produced by the high wattage bulb. The heat given off by conventional Fresnel lights tends to create an uncomfortable setting for the talent/subject of the film or video. Fans or other heat management devices or equipment are commonly needed to control heat projected toward the talent/subject of the film or video. Furthermore, the can- or cylindrical-shaped housing comprising all existing Fresnel light designs does not lend itself to sufficient heat management of the Fresnel light device itself because the light and heat source is enclosed within the can- or cylindrical-shaped housing. Venting the can structure introduces cost and light leakage, and may be insufficient without internal cooling fans. And internal cooling fans add cost, noise, power consumption, and product complexity/added product failure modes.
What is needed, therefore, are new designs for a Fresnel light that address shortcomings of the available existing and conventional Fresnel lights.
The foregoing and other objectives, features, and advantages of the invention will be more readily understood upon consideration of the following detailed description of the invention taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE SEVERAL DRAWINGS
For a more complete understanding of the present invention, the drawings herein illustrate examples of the invention. The drawings, however, do not limit the scope of the invention. Similar references in the drawings indicate similar elements.
FIG. 1 is a side cut view of a Fresnel light unit in a storage, or fully collapsed, position.
FIG. 2 is a perspective view of the light as in FIG. 1 .
FIG. 3 is a top plan view of a portion of the light as in FIG. 1 .
FIG. 4 is a perspective view of the light as in FIG. 3 .
FIG. 5 is a side cut view of the light as in FIG. 1 but in a partially extended first operable position.
FIG. 6 is a perspective view of the light as in FIG. 5 .
FIG. 7 is a top plan view of a portion of the light as in FIG. 5 .
FIG. 8 is a perspective view of the light as in FIG. 7 .
FIG. 9 is a side cut view of the light as in FIG. 1 but in a fully extended operable position.
FIG. 10 is a perspective view of the light as in FIG. 9 .
FIG. 11 is a top plan view of a portion of the light as in FIG. 9 .
FIG. 12 is a perspective view of the light as in FIG. 11 .
FIG. 13 is an enlarged detail of a first portion of an exploded view of the light as in FIG. 1 , this first portion including a Fresnel lens and a dual basket type design for adjusting a distance between the Fresnel lens and a light source.
FIG. 14 is an enlarged detail of a second portion of an exploded view of the light as in FIG. 1 , this second portion including a bellows and an enclosure, the bellows adjustable in length between a Fresnel lens and the enclosure affixed to a light source.
FIG. 15 is an enlarged detail of a third portion of an exploded view of the light as in FIG. 1 , this third portion including a light source, a heat sink, and a focus knob for adjusting a distance between the light source and a Fresnel lens.
FIG. 16 illustrates a frontal perspective view of a novel Fresnel light, fully assembled and mounted on a stand/mounting, according to various embodiments.
FIG. 17 illustrates a frontal perspective view of a novel Fresnel light, fully assembled and mounted on a stand/mounting, including barn door attachments, according to various embodiments.
FIG. 18 is an exemplary light output diagram for a light as disclosed, in a narrow/spot beam mode of operation, in various embodiments, with Tungsten light generated by a light engine comprising LEDs.
FIG. 19 is an exemplary light output diagram for a light as disclosed, in a wide/flood beam mode of operation, in various embodiments, with Tungsten light generated by a light engine comprising LEDs.
FIG. 20 is another exemplary light output diagram for a light as disclosed, in a narrow/spot beam mode of operation, in various embodiments, with Daylight wavelength light generated by a light engine comprising LEDs.
FIG. 21 is another exemplary light output diagram for a light as disclosed, in a wide/flood beam mode of operation, in various embodiments, with Daylight wavelength light generated by a light engine comprising LEDs.
DESCRIPTION OF PREFERRED EMBODIMENTS
In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the preferred embodiments. However, those skilled in the art will understand that the present invention may be practiced without these specific details, that the present invention is not limited to the depicted embodiments, and that the present invention may be practiced in a variety of alternate embodiments. In other instances, well known methods, procedures, components, and systems have not been described in detail.
Although preferred embodiments are presented and described in the context of a portable-sized Fresnel lighting instrument adapted for use in the production of video and film, numerous separable inventive aspects are presented that may be used in a wide variety of other lighting applications and with the use of a wide variety of other types equipment associated with various lighting applications. Further, various separable inventive aspects are disclosed that may be particularly adapted to non-lighting applications. For example, the structures and methods discovered and disclosed herein for extending one plane from another, while maintaining a substantially parallel relationship between the two, and for also maintaining the relative orientation of the first plane with the other throughout the separation of one from the other, may find particular application in other non-lighting applications.
The present inventor(s) discovered new, unique, and truly innovative methods, systems, and apparatus for improving a light for use as a Fresnel light in video and film production. Various embodiments are illustrated and described in the figures, sketches, details, descriptive materials, and pictures submitted herewith. The various embodiments include separable inventive aspects which are separately patentable. The listed inventive aspects are not exhaustive or comprehensive, and further/additional separable inventive aspects are included in the submitted materials but may not be specifically or particularly identified or described in words due to the need to capture (in many instances in detailed illustrations, pictures, or sketches) the many separable inventive aspects in this disclosure.
FIG. 1 is a side cut view of a Fresnel light unit 102 in a storage, or fully collapsed, position 100 . No other known Fresnel-type light unit includes features, methods, or structures for collapsing the light into a compact storage position. A very thin light engine 104 is used, preferably comprising a number of LEDs. The storage position as shown is where the outward subject facing lens 106 is fully retracted so as to fully collapse the flexible bellows 108 toward the rear heat sink 110 . The fully collapsed unit is preferably small enough (i.e. thin enough in the dimension shown in FIG. 1 ) so as to fit 3 collapsed units side-by-side as oriented in FIG. 1 within a standard-sized milk crate.
FIG. 2 is a perspective view of the light 102 as in FIG. 1 .
FIG. 3 is a top plan view of a portion of the light 102 as in FIG. 1 . In its storage configuration 100 the two counter rotating rings 112 and 114 , each ring affixed to four extender members (or bars) (inward bars 116 , 118 , 120 , and 122 attached to inner ring 112 ; outward bars 124 , 126 , 128 , and 130 attached to outer ring 114 ), are preferably held in place relative to one another and relative to the rear heat sink 110 upon which the light engine 104 is mounted, by an index pin (not shown) (that may be used to release the two rings so as to permit counter rotation and thereby extension of the bellows 108 and movement of the lens 106 longitudinally away from the light engine 104 and heat sink 110 ) or gear 132 (that may incorporate a detent or other mechanical feature to resist or arrest counter rotation of the inner and outer rings 112 , 114 ). In other preferred embodiments, a detent feature is incorporated into operation of a gear 134 rotatable by rotation of a motor (not shown) and/or focus knob 136 .
In still other preferred embodiments, rotation of a motor (not shown) and/or focus knob 136 rotates a gear 134 (or other engagement member) to begin counter rotation of the two rings 112 and 114 , with the storage configuration 100 comprising the first operable position of the light 102 , and in such first operable position as shown in FIG. 1 a Fresnel lens 106 is minimally separated from a light source or light engine 104 , providing a wide/flood beam of projected light from the light 102 . As will be discussed the wide/flood beam is preferably about 70 degrees and decreases to a narrow/spot beam of preferably about 16 degrees when the Fresnel lens 106 and light engine 104 are maximally separated, such maximal separation achieved by rotating a gear 136 so as to counter rotate the inner and outer rings 112 and 114 to fully extend the corresponding extender members.
The heat sink 110 to which the light engine 104 is thermally connected (mounted) is preferably (as shown) a substantial portion of the rearmost structure. Light output control electronics are preferably included on a separate circuit board that is thermally connected (mounted) to a smaller (lowermost) portion 138 of the rearmost heat sink structure. As shown, there is a smaller portion 138 of the heat sink on one (shown as lowermost) side in FIG. 3 . This smaller portion 138 of the heat sink 110 is substantially thermally separate from the larger portion, thereby providing better thermal separation between the light engine 104 and the control electronics. In preferred embodiments, thermal separation between the larger portion of the heat sink 110 where the light engine 104 is mounted and the (lowermost) smaller portion 138 where the control electronics are mounted is achieved by one or more areas of discontinuity such as the discontinuity/thermal separator 140 shown between the larger portion of the heat sink 110 and its smaller portion 138 . In other preferred embodiments, backside fins comprising heat sink 110 may be oriented so as to be substantially parallel with the discontinuity/thermal separator 140 shown in FIG. 3 and not, as shown in FIG. 4 , perpendicular, or the backside fins may themselves be discontinuous between the larger portion of the heat sink 110 and its lower portion 138 below the discontinuity/thermal separator 140 .
FIG. 4 is a perspective view of the light as in FIG. 3 .
FIG. 5 is a side cut view of the light 102 as in FIG. 1 but in a partially extended first operable position 200 . When moved from its storage position 100 to a first operable position 200 , preferably by depressing or pulling or actuating a mechanical index or release mechanism (to allow for rotation of the counter rotating rings) and subsequent rotation of a focus knob 136 (configured to rotate a gear 134 situated between the counter rotating rings 112 and 114 and to engage with teeth formed in each of the rings to move the rings in the opposite direction from one another) causes the bars (extending members) to move and thereby extend the lens 106 away from the light engine 104 . The first operable position 200 provides a distance between the lens 106 and light engine 104 for a first focusing position for the light unit. The first focusing position of a Fresnel-type light typically corresponds to a widest angle of light projected by the light unit, with increasing separation between the lens 106 and light engine 104 causing greater/narrower focus of a light spot or light beam directed from the subject facing lens.
FIG. 6 is a perspective view of the light 102 as in FIG. 5 .
FIG. 7 is a top plan view of a portion of the light 102 as in FIG. 5 . In the first operable position 200 , the extending members (bars) comprising one set (eg. of four) affixed to one of the counter rotating rings and another set (eg. of four) affixed to the other counter rotating ring move opposite one another so as to extend the lens away from the light engine/heat sink. The rings are shown in FIG. 7 as being moved out of the storage (or fully compressed) position 100 , the rings 112 and 114 now shown counter rotated with the extender members partially extended.
FIG. 8 is a perspective view of the light 102 as in FIG. 7 . Preferably, each ring 112 , 114 is connected to four extending members as shown. Different numbers of bars may be used, and they may be configured differently. And the bars need not be rigid extending members. Cable material may be used for the extending members. In preferred embodiments, however, four bars are mounted to each of the counter rotating rings 112 and 114 , and each bar of one ring is positioned so as to pair up with a bar of the other ring to simplify connection of the bars to an outward lens retaining portion of the focusing assembly (the focusing assembly comprising the counter rotating rings, extender members/bars, and Fresnel lens retainer). As shown in FIG. 8 , each of inward bars 116 , 118 , 120 , and 122 are pivotally mounted at one end to the inner ring 112 , and each of outward bars 124 , 126 , 128 , and 130 are pivotally mounted at one end to the outer ring 114 . The other end of each inward bar is pivotally mounted to an attachment member that is pivotally mounted to the other (non-ring) end of an outward bar, as shown. For example, as shown in FIG. 8 , the non-ring end of inward bar 116 is pivotally mounted to an attachment member 202 , which is in turn pivotally mounted to the non-ring end of outward bar 126 ; inward bar 118 is pivotally mounted to an attachment member 204 , which is pivotally mounted to outward bar 130 ; inward bar 122 is pivotally mounted to an attachment member 206 , which is pivotally mounted to outward bar 128 ; and inward bar 120 is pivotally mounted to an attachment member 208 , which is pivotally mounted to outward bar 124 . As the counter rotating rings 112 and 114 move opposite one another, the bars extend and do so such that the lens (retained by a Fresnel lens retainer attached to the bars via bar attachment members 202 , 204 , 206 , and 208 ) is moved longitudinally away from the light engine 104 with substantially no rotation (allowing for barn doors or other attachments to the lens portion to maintain its orientation relative to the rearmost heat sink 110 , mounting frame, etc.). That is, as the lens 106 is extended outward away from the light engine 104 , the lens 106 moves substantially only longitudinally away from the light engine 104 toward the subject being lighted, with substantially no rotation of the lens 106 relative to the light engine 104 or rearmost heat sink structure 110 .
FIG. 9 is a side cut view of the light as in FIG. 1 but in a fully extended operable position 300 . The focus knob 136 , in a preferred embodiment, is shown in the heat sink portion (as for FIGS. 1 and 5 ). In a fully extended mode (for the longest distance between Fresnel lens 106 and light engine 104 ) the extending member (bars) are fully extending so that one end of each bar is attached to the heat sink/light engine portion and the other end is attached to structure retaining the lens 106 , with a bellows 108 or other material expanded therebetween so as to contain light generated by the light engine 104 and allowing light to be projected through the subject facing lens 106 .
FIG. 10 is a perspective view of the light 102 as in FIG. 9 .
FIG. 11 is a top plan view of a portion of the light 102 as in FIG. 9 . In various embodiments, the fully extended position (as shown) includes mechanical stops such as end-of-gear teeth and/or alignment of detents in each of the counter rotating rings such that a mechanic index pin may be used to provide additional retention of the rings and bars in the fully extended position. Preferably and as shown in FIG. 11 , the portion of the focusing assembly that extends the Fresnel lens 106 away from the light source/engine 104 comprises two concentric rings 112 and 114 with at least one gear 134 therebetween engageable with teeth formed on each of the rings so as to allow counter rotation of the two rings with respect to one another when the gear 134 is rotated. Four extender members 116 , 118 , 120 , and 122 are (evenly spaced about and) pivotally mounted to the inner ring 112 , the four (inward) extender members and inner ring comprising an inward basket-type design. Four additional extender members 124 , 126 , 128 , and 130 are (evenly spaced about and) pivotally mounted to the outer ring 114 , with the four (outward) extender members and outer ring comprising an outward basket-type design. The two (inward plus outward) basket-type designs/structures are combined with at least one gear 134 interposed between the inner ring 112 and outer ring 114 so that rotation of the gear 134 causes the inner ring 112 and outer ring 114 to rotate in opposite directions (i.e. counter rotation of the two rings). Each of the extender members are further pivotally mounted to one of four attachment members 202 , 204 , 206 , and 208 such that each of the extender members pivotally mounted to the inner ring 112 is connected to an extender member pivotally mounted to the outer ring 114 via pivotal mounting to one of the attachment members 202 , 204 , 206 , and 208 . Each of the attachment members 202 , 204 , 206 , and 208 pivotally connects an extender member pivotally mounted to the inner ring 112 with an extender member pivotally mounted to the outer ring 114 , forming a connected pair of extender members. As the two rings 112 and 114 are rotated in opposite directions, the extender member ends pivotally mounted to the rings are either drawn closer together causing the attachment member connecting the opposite ends of those extender members to extend away from the plane defined by the two concentric rings 112 and 114 , or drawn apart from one another causing the attachment member (and the plane defined by the Fresnel lens retainer structure attached thereto) to compress/collapse inward toward the plane defined by the concentric rings 112 and 114 .
FIG. 12 is a perspective view of the light 102 as in FIG. 11 .
FIGS. 13, 14, and 15 comprise an exploded view of the light 102 as in FIG. 1 showing components as they may be assembled/disassembled for assembly/disassembly of the light, in various embodiments. FIG. 13 is an enlarged detail of a first portion of an exploded view of the light 102 as in FIG. 1 , this first portion including a Fresnel lens 106 and a dual basket type design/structure or focusing assembly 402 for adjusting a distance between the Fresnel lens 106 and a light source 104 . Lens retainers 404 are shown for retaining Fresnel lens 106 to an outward lens retainer portion 406 of the focusing assembly 402 , with a lens seal 408 therebetween. Ring retainers 410 and 412 are used to retain rings 112 and 114 to the heat sink portion 110 so that the rings 112 and 114 are able to slide/rotate within the plane defined by rings 112 and 114 but not move longitudinally fore and aft in the direction that the lens 106 extends from and retracts to the plane defined by rings 112 and 114 (and within which the light source/engine 104 preferably resides). The ring retainers 410 and 412 preferably oppose one another. Different ring retaining means may be used, or a different number of retainers 410 , 412 may be used. The retainers 410 , 412 preferably include guide material to maintain alignment of each of the counter rotating rings 112 and 114 .
The focusing assembly 402 preferably comprises a dual basket type design having a pair of counter rotating rings defining a first plane, a lens holding member defining a second plane, and extensible bars or extending members therebetween and affixed to the counter rotating rings and lens holding member as shown in FIG. 13 so as to provide an assembly whereby the lens holding member is extendable away from the counter rotating rings by rotating one or both of the rings. With the extending members arranged as shown, the lens holding member is extendable away from the rotating rings so that the first and second planes remain substantially the same in relation to one another when extended as when collapsed (i.e. parallel to one another). And the lens holding member (and its first plane) is extendable away from the rings (and its second plane) with substantially no rotation along the longitudinal travel between the collapsed or shorter separation and the extended or longer separation between the first and second planes. Attachments 414 , 416 , 418 , and 420 (four of them) are shown for attachment of barn doors or other attachments typically used with lighting units used in the video and film industry.
FIG. 14 is an enlarged detail of a second portion of an exploded view of the light 102 as in FIG. 1 , this second portion including a bellows 108 and an enclosure 422 , the bellows 108 adjustable in length between a Fresnel lens 106 and the enclosure 422 affixed to a heat sink portion 110 and a light source 104 affixed thereon.
FIG. 15 is an enlarged detail of a third portion of an exploded view of the light 102 as in FIG. 1 , this third portion including a light source 104 , a heat sink 110 , and a focus knob 136 for adjusting a distance between the light source 104 and a Fresnel lens 106 . As shown in FIG. 15 , the focus knob 136 is preferably connected to a focus gear 134 that protrudes through opening 424 in the heat sink assembly/portion 110 . The focus gear 134 rotates and engages with teeth formed on rings 112 and 114 to extend or retract the lens 106 from the light source/engine 104 . In one embodiment, a release pin is used in place of the idle gear 132 shown. In various embodiments, gears 132 , 432 , and 434 function as idle gears to stabilize and ensure smooth rotation of the rings 112 and 114 retained to the heat sink assembly 110 by retainers 410 and 412 . In preferred embodiments, a light source or engine 104 comprises an LED module 436 as illustrated in FIG. 15 . The LED module 436 may be mounted to the heat sink 110 with an LED thermal PSA 428 therebetween, with an LED PCB assembly 426 mounted over and surrounding the LED module 436 . A control PCB assembly 430 is preferably mounted to a lower portion 138 of the heat sink 110 .
FIG. 16 illustrates a frontal perspective view of a novel Fresnel light 102 , fully assembled and mounted on a stand/mounting 502 , according to various embodiments. FIG. 17 illustrates a frontal perspective view of a novel Fresnel light 102 , fully assembled and mounted on a stand/mounting 502 , including attachments 414 , 416 , 418 , and 420 utilized to mount barn door attachments 504 , according to various embodiments.
In one embodiment, the Fresnel light unit as described and illustrated in the figures is operated by actuating a release mechanism to allow for extending the lens away from the light engine; rotating a focus knob to extend the lens longitudinally outward away from the light engine to a first operable position; turning on the light engine to project light through the lens; and further rotating the focus knob to adjust the distance between lens and light engine (to focus the light beam projected from the lens onto a subject, as desired). Light characteristics such as the color temperature (or color) of light projected, intensity, etc. may be controlled manually using control knobs/buttons/sliders/etc. provided on the light unit, or remotely using various wired or wireless means. The light unit may be returned to a storage configuration by powering off the light engine; and rotating the focus knob to retract the lens inward longitudinally toward the light engine/heat sink to fully collapse the bellows to bring the lens fully inward toward the light engine.
The present inventor(s) designed a novel Fresnel light, in the various embodiments described herein, to represent the next generation in Fresnel lights, providing the hallmarks of a traditional Fresnel light—single shadow beam shaping through barn doors, continuous focusing and a smooth light field—and provide the additional functionality of both wireless and DMX control, the low power consumption and cool operation of an LED light source/engine, unique and innovative compact structure that operates differently than any previous Fresnel and collapses down to a fraction of the size (and weight and bulk) of existing Fresnel lights, and is designed to have a water-resistant IP54 rating and rugged construction for field reliability.
FIG. 18 is an exemplary light output diagram for a light 102 as disclosed, in a narrow/spot beam mode of operation, in various embodiments, with Tungsten (color temperature, 3200K) light generated by a light engine comprising LEDs. In this mode, the Fresnel light 102 has its bellows 108 and focusing assembly 402 in a fully extended mode of operation, to achieve a narrow/spot beam of about 16 degrees.
FIG. 19 is an exemplary light output diagram for a light as disclosed, in a wide/flood beam mode of operation, in various embodiments, with Tungsten light generated by a light engine comprising LEDs. In this mode, the Fresnel light 102 has its bellows 108 and focusing assembly 402 in a fully compressed/collapsed mode of operation, to achieve a wide/flood beam of projected light, of about 70 degrees.
FIG. 20 is another exemplary light output diagram for a light as disclosed, in a narrow/spot beam mode of operation, in various embodiments, with Daylight wavelength light (color temperature, 5600K) generated by a light engine comprising LEDs.
FIG. 21 is another exemplary light output diagram for a light as disclosed, in a wide/flood beam mode of operation, in various embodiments, with Daylight wavelength light generated by a light engine comprising LEDs.
The present inventor(s) invented a new Fresnel light, according to various embodiments, with the following advertised features and capabilities: Ultra high output LED that provides the equivalent output of a traditional 650 W light; High quality glass 8 inch round Fresnel lens; Ultra thin/compact design is only 15″×12.6″×4.6″ and just 9.5 lbs; Water resistant IP54 rating; Provides continuous focus variable from spot (16 degree beam width) to flood (70 degree beam width); Completely silent operation (no cooling fans); Fully dimmable 100 to 0 percent; Available in Tungsten (3200K) and Daylight (5600K) versions; DMX or wireless operation; Wireless operation uses 2.45 GHz and provides 9 user selectable channels; Wireless operation includes the capability to link together as many other Zylight/Zylink instruments as needed, and includes the capability to adjust the controls on all of the linked lights by adjusting the controls on any one of the instruments/lights linked in the group; Use battery (14.4 v) or worldwide AC power; Use with yolk mount, pole mount, or handles; Low power draw at only 90 W to 100 W; Very cool operation due to use of LED light engine instead of conventional high wattage bulb; LED life is 50,000 hours minimum; Tested flicker free at 5600 fps.
The terms and expressions which have been employed in the foregoing specification are used therein as terms of description and not of limitation, and there is no intention in the use of such terms and expressions of excluding equivalents of the features shown and described or portions thereof, it being recognized that the scope of the invention is defined and limited only by the claims which follow. | A Fresnel lighting instrument for use in film and video production, having a LED light engine mounted to a heat sink defining a first plane, a dual basket type focusing assembly adapted to longitudinally extend or retract a Fresnel lens away from and back to the first plane substantially without rotation along the longitudinal range of extension, to provide a fanless, cool operating, highly compact and lightweight Fresnel light suitable for studio or field use. The dual basket type design allows for transporting three Fresnel units in a standard milk crate since the unit collapses down whereas existing Fresnel lights all use a constant volume can-shaped housing within which the light source is repositioned. | 5 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Divisional of pending U.S. patent application Ser. No. 11/247,510, filed Oct. 11, 2005 and entitled “SWITCHING DEVICE FOR A PIXEL ELECTRODE AND METHODS FOR FABRICATING THE SAME,” the contents of which are incorporated by reference herein.
BACKGROUND
[0002] The invention relates to a display device, and more particularly to a switching device for a pixel electrode and methods for fabricating the same.
[0003] Bottom-gate type thin film transistors (TFTs) are widely used for thin film transistor liquid crystal displays (TFT-LCDs). FIG. 1 is a sectional view of a conventional bottom-gate type TFT structure 100 . The TFT structure 100 typically comprises a glass substrate 110 , a gate 120 , a gate-insulating layer 130 , a channel layer 140 , an ohmic contact layer 150 , a source 160 and a drain 170 .
[0004] As the size of TFT-LCD panels increases, metals having low resistance are required. For example, gate lines employ low resistance metals such as Cu and Cu alloy in order to improve operation of the TFT-LCD.
[0005] However, Cu can react with radicals to form Cu oxide in subsequent processes, thereby increasing resistance. Also, Cu diffuses easily and reacts with silicon to form CuSi x , significantly affecting reliability of the device.
[0006] JP 2000-332015, the entirety of which is hereby incorporated by reference, discloses a method of forming CuSi x . A layer of CuSi x is formed between a silicon-rich nitride layer and a Cu layer, enhancing adhesion therebetween.
SUMMARY
[0007] Thin film transistors and fabrication methods thereof are provided. Diffusion of Cu is reduced, and no extra processes such as photolithography are required.
[0008] An embodiment of a fabrication method comprises forming a gate on a substrate. A first CuSi x layer is formed on the gate by plasma treatment on the gate in a silane-containing chamber. The temperature of the chamber is substantially about 180° C. to 370° C.
[0009] To enhance the barrier properties of the first CuSi x layer, a subsequent plasma treatment is performed on the first CuSi x layer in a chamber containing N 2 and NH 3 . The temperature of the chamber is substantially about 180° C. to 370° C.
[0010] An insulating layer is formed on the first CuSi x layer. A semiconductor layer is formed on the insulating layer. A source and a drain are formed on the semiconductor layer. A pixel electrode is formed, electrically connecting to the source or the drain.
[0011] Another embodiment of a method comprises forming a second CuSi x layer between the semiconductor layer and the source/drain.
[0012] Formation of the second CuSi x layer comprises forming a Cu layer or a Cu alloy layer on the semiconductor layer and performing a plasma treatment on the Cu layer or the Cu alloy layer in a silane-containing chamber. The temperature of the chamber is substantially about 180° C. to 370° C.
[0013] To enhance the barrier properties of the second CuSi x layer, a subsequent plasma treatment is performed on the second CuSi x layer in a chamber containing N 2 and NH 3 . The temperature of the chamber is substantially about 180° C. to 370° C.
[0014] In these embodiments, the first CuSi x layer is conformally formed on the gate. The substrate comprises a glass substrate. The insulating layer comprises a silicon oxide, silicon nitride, silicon oxynitride, tantalum oxide or aluminum oxide layer. The semiconductor layer comprises silicon. The source/drain comprises Cu or Cu alloy.
[0015] Thin film transistors (TFTs) of the invention can be bottom-gate or top-gate, serving as a switching device for a pixel electrode when the source/drain are electrically in contact with a pixel electrode. In addition, the TFTs of the invention can be applied in display such as LCD.
DESCRIPTION OF THE DRAWINGS
[0016] The invention can be more fully understood by reading the subsequent detailed description in conjunction with the examples and references made to the accompanying drawings.
[0017] FIG. 1 is a sectional view of a conventional TFT structure.
[0018] FIGS. 2A to 2F are sectional views of an exemplary process for fabricating a first embodiment of a TFT structure of the present invention.
[0019] FIGS. 3A to 3H are sectional views of an exemplary process for fabricating a second embodiment of a TFT structure of the present invention.
DETAILED DESCRIPTION
First Embodiment
[0020] An exemplary process for fabricating a first embodiment of TFTs of the invention is shown in FIGS. 2A-2F .
[0021] In FIG. 2A , a Cu layer (not shown) is formed on a substrate 210 , for example, by chemical vapor deposition (CVD), electrochemical plating (ECP), or physical vapor deposition (PVD). The Cu layer is deposited, forming a gate 220 on the substrate 210 . The substrate 210 may be a glass substrate. The gate 220 may be copper with thickness substantially about 100 nm to 500 nm.
[0022] In FIGS. 2B and 2C , a first CuSi x layer 227 is conformally formed on the gate 220 by plasma treatment 225 of the gate 220 in a silane-containing chamber. The temperature of the chamber is substantially about 180□ to 370□. Silicon atoms react with the surface of the gate 220 of Cu, forming the first CuSi x layer 227 , preventing Cu from diffusing to the insulating layer 230 shown in FIG. 2E . The thickness of the first CuSi x layer 227 is substantially about 5 nm to 100 nm.
[0023] In FIG. 2D , a subsequent plasma treatment 225 a is performed on the first CuSi x layer 227 in a chamber containing N 2 and NH 3 . The temperature of the chamber is substantially about 180° C. to 370° C. Nitrogen atom reacts with the surface of the first CuSi x layer 227 to form N—Si bond, thereby enhancing the barrier properties of the first CuSi x layer.
[0024] In FIG. 2E , an insulating layer 230 is formed on the first CuSi x layer 227 . A semiconductor layer (not shown) is formed on the insulating layer 230 . The insulating layer 230 comprises silicon oxide, silicon nitride, silicon oxynitride, tantalum oxide or aluminum oxide. The semiconductor layer comprising a channel layer 240 and an ohmic contact layer 250 is defined on a portion of the gate-insulating layer 230 by deposition and patterning. The channel layer 240 can be an undoped amorphous silicon layer formed by CVD. The ohmic contact layer 250 can be an impurity-added silicon layer formed by CVD. The impurity can be n type dopant (for example, P or As) or p type dopant (for example, B).
[0025] In FIG. 2F , a Cu layer (not shown) is formed on the ohmic contact layer 250 , for example, by CVD, ECP, or PVD. The source/drain 260 / 270 , of Cu or Cu alloy, are formed on the ohmic contact layer 250 by selectively etching through the Cu layer, the ohmic contact layer 250 , exposing a portion of the surface of the channel layer 240 . A pixel electrode is formed, electrically connected to the source/drain 260 / 270 . A resultant thin film transistor 200 is obtained.
Second Embodiment
[0026] An exemplary process for fabricating a second embodiment of TFTs of the present invention is shown in FIGS. 3A-3H .
[0027] In FIG. 3A , a Cu layer (not shown) is formed on a substrate 210 , for example, by chemical vapor deposition (CVD), electrochemical plating (ECP), or physical vapor deposition (PVD). The Cu layer is etched, forming a gate 220 on the substrate 210 . The substrate 210 may be a glass substrate. The gate 220 may be copper with thickness substantially about 100 nm to 500 nm.
[0028] In FIGS. 3B and 3C , a first CuSi x layer 227 is conformally formed on the gate 220 by performing plasma treatment 225 of the gate 220 in a silane-containing chamber. The temperature of the chamber is substantially about 180° C. to 370° C. Silicon atoms react with the surface of the gate 220 of Cu, forming the first CuSi x layer 227 , preventing Cu from diffusing to the insulating layer 230 shown in FIG. 3E . The thickness of the first CuSi x layer 227 is substantially about 5 nm to 100 nm.
[0029] In FIG. 3D , a subsequent plasma treatment 225 a is performed on the first CuSi x layer 227 in a chamber containing N 2 and NH 3 . The temperature of the chamber is substantially about 180° C. to 370° C. Nitrogen atom reacts with the surface of the first CuSi x layer 227 to form N—Si bond, thereby enhancing the barrier properties of the first CuSi x layer.
[0030] In FIG. 3E , an insulating layer 230 is formed on the first CuSi x layer 227 . A semiconductor layer (not shown) is formed on the insulating layer 230 . The insulating layer 230 comprises silicon oxide, silicon nitride, silicon oxynitride, tantalum oxide or aluminum oxide. The semiconductor layer comprising a channel layer 240 and an ohmic contact layer 250 is defined on a portion of the gate-insulating layer 230 by deposition and patterning. The channel layer 240 can be an undoped amorphous silicon layer formed by CVD. The ohmic contact layer 250 can be an impurity-added silicon layer formed by CVD. The impurity can be n type dopant (for example P or As) or p type dopant (for example B).
[0031] In FIG. 3E , a Cu layer 252 is formed on the ohmic contact layer 250 , for example, by CVD, ECP, or PVD.
[0032] In FIGS. 3F and 3G , a Cu layer 252 is formed on the semiconductor layer. In other embodiments, a Cu alloy layer can be formed in place of the Cu layer. Plasma treatment is performed on the Cu layer 252 , completely forming a second CuSi x layer 252 a . The second CuSi x layer 252 a prevents diffusion of Cu from the source/drain 260 / 270 shown in FIG. 3H to the underlying substrate. The plasma treatment 254 is performed in a silane-containing chamber. The temperature of the chamber is substantially in a rang of about 180° C. to about 370° C. The thickness of the second CuSi x layer 252 a is substantially in a rang of about 5 nm to 100 nm.
[0033] In FIG. 3G , a subsequent plasma treatment 254 a is performed on the second CuSi x layer 252 a in a chamber containing N 2 and NH 3 . The temperature of the chamber is substantially about 180° C. to 370° C. Nitrogen atoms react with the surface of the second CuSi x layer 252 a to form N—Si bond, thereby enhancing the barrier properties of the second CuSi x layer.
[0034] In FIG. 3H , a Cu layer (not shown) is formed on the second CuSi x layer 252 a , for example, by CVD, ECP, or PVD. The source/drain 260 / 270 , of Cu or Cu alloy, is formed on the second CuSi x layer 252 a by selectively etching through the Cu layer, second CuSi x layer 252 a , the ohmic contact layer 250 , exposing a portion of the surface of the channel layer 240 . A pixel electrode is formed, electrically connecting to the source/drain 260 / 270 . A resultant thin film transistor 300 is obtained.
[0035] While the invention has been described by way of example and in terms of preferred embodiment, it is to be understood that the invention is not limited thereto. On the contrary, it is intended to cover various modifications and similar arrangements as would be apparent to those skilled in the art. Therefore, the scope of the appended claims should be accorded the broadest interpretation so as to encompass all such modifications and similar arrangements. | The invention discloses a switching element of a pixel electrode for a display device and methods for fabricating the same. A gate is formed on a substrate. A first copper silicide layer is formed on the gate. An insulating layer is formed on the first copper silicide layer. A semiconductor layer is formed on the insulating layer. A source and a drain are formed on the semiconductor layer. Moreover, a second copper silicide layer is sandwiched between the semiconductor layer and the source/drain. | 7 |
CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable
MICROFICHE APPENDIX
Not Applicable
BACKGROUND OF THE INVENTION
The present invention relates to electrically operated actuator mechanisms and particularly relates to such mechanisms which employ an electromagnetic operator and which are suitable for use in automotive applications such as, for example, a locking/unlocking mechanism for a fuel filler access door.
In recent times, it has been desired to provide remote electrical control of the locking and unlocking of an automotive fuel filler access door and to combine such electrical control of the filler access door with a mechanical override unlocking function to permit opening of the access door, in the event of failure of any of the electrical components.
In providing a actuator mechanism which is remotely electrically operated, and particularly suitable locking and unlocking for an automotive fuel filler access door, it has been found difficult to provide for latching or holding of the mechanism in the energized actuator or unlocked state without the need to maintain electrical power to the mechanism. For example, if an actuator mechanism is spring biased to the locked position in the electrically de-energized state and is actuated and unlocked by electrical energization, it is thus necessary to maintain power to the electrical operator in order to maintain the mechanism in the unlocked state. For low voltage applications, such as encountered in on-board automotive power supplies, the electrical power necessary to overcome the bias spring force on the actuator bolt results in a prohibitively expensive electrical actuator where power is maintained to the actuator during the time that it is energized for unlocking.
In automotive fuel filler door latch applications, the variation in sheet metal component dimensions occurring during assembly of the vehicle body requires a wide latitude of adjustment of the latching mechanism for engagement of the actuator bolt member with the striker in order to secure the fuel filler access door in the closed position. Heretofore, it has been difficult to design an electrically operated remote locking/unlocking mechanism which could be readily assembled in mass production of automotive vehicles for the fuel filler access door application and which could accommodate a wide variation in position of the parts at assembly.
Thus, it has long been desired to provide a way or means of electrically remotely locking and unlocking a mechanism in a manner which enables the mechanism to be held or retained in the actuated or unlocked state without the need for maintaining electrical power to the operator. It has further been desired to provide such a mechanism which is capable of accommodating wide variations in the assembly of the latching member with a striker or retainer so as to permit low cost manufacturing and ease of assembly in high volume mass production. It has been particularly desired to provide such a remotely controlled electrically operated locking/unlocking mechanism for an automotive fuel filler access door application.
BRIEF SUMMARY OF THE INVENTION
It is an object of the present invention to provide a relatively low cost electrically operated remotely controlled actuator mechanism spring biased to the unactuated position and maintained in the actuated position after energization and de-energization of the electrical operator.
It is a further object of the present invention to provide the aforesaid type of remotely controlled electrically operated actuator for use as a latching bolt and to provide for a wide variation in location of the striker upon installation.
The present invention provides a solution to the above-described problem of enabling remote control of an electrically operating latching/unlatching mechanism such as one suitable for moving a bolt member against a striker for remotely locking and unlocking a door. In particular, the invention provides for remote control of an electromagnetically operated latching/unlatching mechanism having a bolt member moved in contact with a striker by a bias spring and unlocked or moved away from the striker by electrical energization of a solenoid. The operator includes a permanent magnet attached to a pole piece and coil which are slidably moveable on a base or housing. Upon energization the solenoid armature moves the bolt member to the unlocked position and maintains the mechanism in the unlocked position by force of the magnetic attraction. The electrical energization of the solenoid may then be discontinued and the bolt member is retained in the unlocked position without electrical power.
The unlocking is accomplished by energizing the solenoid with electrical current flow in one direction in the coil such that the pole piece is magnetized in a manner complementing the permanent magnet to provide sufficient force to overcome the force of the bias spring and move the armature to unlock the mechanism. Upon discontinuing of the electrical energization, the permanent magnet is sufficiently strong to retain the armature mechanism in the actuated or unlocking state. Upon energization of the coil with current flow in the opposite direction, the magnetization of the pole piece members opposes the magnetic poles of the permanent magnet and neutralizes the magnetic attraction of the magnet thereby permitting the bias spring to return the bolt member to its locking position.
The slidable mounting of the coil, pole piece bolt and magnet sub-assembly on the housing permits the bolt to be adjusted for the locked position so as to provide adequate stroke of the solenoid armature and bolt member upon electrical energization in a manner which can accommodate wide variation of the components encountered in the sheet metal assembly, particularly the variation encountered in the assembly of mass produced motor vehicles.
The present invention thus provides a low cost, self-positioning electromagnetic operator for providing remote electrical locking and unlocking of a mechanism and is particularly suitable for locking and unlocking of an automotive fuel filler access door.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross-section view of the mechanism of the present invention in the de-energized condition;
FIG. 2 is a view similar to FIG. 1 showing the mechanisms in the de-energized state with the pole frame and moved to accommodate assembly/installation dimensional variations;
FIG. 3 is a view similar to FIG. 1 showing the solenoid in the unlocked condition and the open position of the door shown in dashed outline;
FIG. 4 is an axonometric view of the moveable actuator or latch bolt of the present invention;
FIG. 5 is an axonometric view of the pole frame spacer of the present invention;
FIG. 6 is an axonometric view of the moveable actuator member of the present invention; and, FIG. 7 is a view of a portion of the magnetic pole frame of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, the actuator assembly of the present invention is indicated generally at 10 and is shown as having a moveable bolt member 12 having a striker surface 14. When the bolt 12 is in the extended position, the striker surface contacts the edge of the device to be locked indicated by reference numeral 18 which may be a hinged door as, for example, an automotive fuel filler access door. The door is moved or rammed against surface 14; and, the bolt is depressed rightwardly and slides along the surface of the door until engaging slot 16 in the door whereupon the bolt is spring biased into slot 16.
The housing 20 has an end member 22 which is adapted to be mounted on a suitable supporting structure (not shown) as for example the automobile body upon which the access door 18 is hinged. Housing 20 has an electrical receptacle 24 formed in an end thereof opposite end member 22. Receptacle 24 has provided therein at least one electrical connector terminal adapted external electrical connection thereto as, for example, by a wiring harness connector.
Housing 20 has disposed therein a generally tubular bobbin member 28 with a pair of spaced annular flanges 30, 32 provided thereon about which is wound a solenoid coil 34 of electrical conductor. Bobbin flange 32 has attached thereto an extension 36 which is anchored to housing 20 adjacent the electrical receptacle 24. The bobbin 28 has a tubular extension 38 extending axially outwardly from the flange 30. Referring to FIGS. 1 and 6 extension 38 has the end thereof received in and supported by counterbore 40 provided in a bolt guide member 41.
An annular pole piece 42 is slidably received in the right hand end of the bobbin 28 and has a reduced diameter portion 44 thereof engaging an aperture 46 formed in a first pole frame member 48. Member 48 has a generally right angular configuration with a flange 49 of the member 48 biased against the end of bobbin flange 32 by a compression spring 50 having one end registered against the member 48 with the opposite end registered against housing 20.
Referring to FIGS. 1 and 7, a second pole frame member 52 extends from member 48 along the coil and over flange 30 and has a right angle flange portion 54 configured to slidably register against the surface of bobbin extension 38 via sliding surface 56 provided on the end of flange 54. It will be understood that the surface 56 is generally semicircular in shape to conform to the curved surface of extension 38.
Referring to FIGS. 1 and 5, a pole frame spacer member 58 is provided between the flange 54 of pole frame member 52 and the right hand end of the bolt guide member 41. The spacer having a pair of oppositely disposed internal notches 59 into one of which is slidably received an orientation lug 60 provided on bolt member 62, which lug is registered in a slot 64 provided in the bolt guide member 41. Spacer 58 has a pair of oppositely disposed outwardly extending lugs 66 provided thereon which are adapted for engagement by portions of the bolt guide 41 as will hereinafter be described.
Referring to FIG. 6, the groove 64 formed in the bore 40 of bolt guide member 41 is illustrated in greater detail. Referring to FIGS. 1, 4 and 6, it will be understood that a flange 70 provided on bolt 12 is sized for being slidably received in bore 40 in the bolt guide member 41.
Referring to FIG. 1 an annular armature 72 is slidably disposed in the tubular extension 38 of the bobbin; and, armature 72 has a convolution or annular rib 74 formed on the end thereof remote from pole piece 42. The tubular extension 38 is received in the bore 40 of bolt guide member 41. The armature rib 74 is engaged in a groove 76 formed in the inner periphery of the bolt 12 on a cylindrical portion 78 thereof extending from flange 70 in a direction oppositely directed from the striker surface 14.
The armature 72 is biased in a direction away from pole piece 42 by a spring 80 disposed therebetween. The engagement of the armature rib 74 in groove 76 of bolt extension 78 thus causes movement of the bolt 12 with movement of the armature 72.
An emergency actuation cable 82 is received through a bore 84 formed in the housing; and, the cable extends through pole piece 42, armature 72 and outwardly through the left end of the armature with respect to FIG. 1. The end of the cable 82 has a retainer in the form of a ferrule 86 crimped over the end thereof to prevent withdrawal of the cable. It will be understood that leftward movement of the emergency pull-cable causes ferrule 86 to register against the left end of the armature 72; and, continued movement of the cable effects movement of the armature in a rightward direction until the right hand end of the armature 72 is in contact with the left end of pole piece 42. This rightward movement of the armature by cable 82 retracts bolt 12 from door aperture 16.
A permanent magnet 88 is disposed between the end of pole frame member 48 and the end of pole frame member 52 and is secured therebetween by an annular clamping band 90, which in the presently preferred practice comprises heat shrink tubing.
Referring to FIG. 6, the bolt guide 41 has an annular outward extending flange 92 formed on one end thereof which flange has disposed on opposite sides thereof a pair of axially extending lugs 94, 96 each of which has a slot formed therein denoted respectively 98, 100 with integrally formed spring tabs 102, 104 extending therein.
In assembly, the spacer 58 is assembled over the extension 78 of the bolt and registered against the face of flange 70 with projection 60 of the spacer 58 aligned with one of the slots 59. The cable 82 is then assembled through armature 72; and, the rib 74 of the armature is engaged in groove 76 of the bolt 12. The spring 80 is received over the cable; and, the cable is fed through pole piece 42 and bore 84 in the housing to extend externally thereof for a suitable distance to provide the desired remote emergency actuation.
Referring to FIGS. 1, 4, 5, 6 and 7 the washer 58 is then assembled over portion 78 of the bolt and is registered against the face of flange 70 such that the extension 60 is aligned with a notch 59. The bolt 12 is then received in the bolt guide 41 with the projection 60 engaged in slot 64. The spring tabs 102, 104 are then engaged over suitable surfaces such as tabs 106, 108 provided on opposite sides of flange 54 of pole frame 52.
The extension 66 on the spacer 58 extend through the slots 98, 100 formed in the projections 94, 96 on the bolt guide 41.
Referring to FIG. 1, the actuator assembly is illustrated in the locked condition in solid outline which bolt 12 has engaged the slot 16 in the door 18 to be locked; and, the door is shown in dashed outline in the open position. In the condition illustrated in FIG. 1, coil 34 is de-energized and the bias force of spring 80 is sufficient to move the armature 72 and bolt 12 leftward until the flange 70 on the bolt is registered against the end of bore 40 in guide 41. In the actuator condition shown in FIG. 1, the door 18 is positioned with respect to housing 22 such that cover 52, spacer 58, pole frame member 52, magnet 88, pole frame piece 48 and pole piece 42 are moved leftward by the bias force of spring 50 to a position where the flange 92 on cover 62 has reached the leftward limit of its movement. In the position shown in FIG. 1, the flange 49 of pole frame member 48 is registered against the right hand end face of bobbin flange 32 under the urging of spring 50.
Referring to FIG. 2, the actuator assembly 10 is shown installed in a position where the door 18 is spaced slightly closer to end member 22; and, with the end of bolt guide 41 registered against door 18, the end flange 92 of guide 41 is moved further away from the right hand end of end member 22. In the position shown in FIG. 2, the flange 49 of pole frame member 48 is spaced from the end face of bobbin flange 32 by a corresponding amount as shown by the space therebetween in FIG. 2. Thus, the pole frame, magnet and bolt guide as a subassembly is slidably moveable on the tubular extension 38 of the bobbin to accommodate during assembly, variations in the location of the door 18 with respect to the end 22 of the housing assembly.
Referring to FIG. 3, the actuator assembly 10 is shown in the coil energized or unlocked and latched condition in which the magnetic force of attraction of the solenoid coil 34 has added to the magnetic force of attraction of magnet 88 and caused the armature 72 to move rightward to contact the end of pole piece 42 and register thereagainst. The armature thus has moved bolt 12 rightward and disengaged the bolt from slot 16. When the coil is subsequently de-energized, the magnetic force of attraction of magnet 88 in the pole frame members 52, 48 is sufficient to hold the armature 72 against pole piece 42 and maintain the bolt 12 latched into the unlocked position permitting the door 18 to be moved from the position shown in solid outline FIG. 3 to the position shown in dashed outline in FIG. 3 for opening the door.
Subsequently, upon energization of coil 34 such that current flows in a direction opposite to that required to move the armature 72 rightward, the force of magnet 88 is neutralized by the magnetic field of the coil 34; and, the spring 80 is operative to bias the armature leftward to return it to the position shown in FIGS. 1 or 2 thus re-engaging bolt 12 with the door slot 16.
The present invention thus provides a unique and novel electrically operated actuator assembly which is magnetically latched in the unlocked position by a permanent magnet upon coil energization by current flow in one direction. Upon re-energization with current flow in the opposite direction in the coil, the magnet is neutralized to permit the return spring to re-engage the bolt. The subassembly of the pole frame, magnet and bolt is slidably moveable on the coil bobbin to permit the bolt guide to accommodate variations in location of the bolt guide with respect to the door or article to be engaged.
Although the invention has hereinabove been described with respect to the illustrated embodiments, it will be understood that the invention is capable of modification and variation and is limited only by the following claims. | An electrically operated actuator mechanism for remote locking and unlocking of a door. The moveable bolt is coupled to a solenoid armature for movement in a guide which is registered against the door in the closed position. The solenoid coil bobbin is stationary and the pole frame including a magnet, bolt guide and bolt are slidable thereon for locating the bolt guide against the door at installation. A spring biases the bolt into engagement with the door. Upon coil energization in one direction, the magnetic flux of the coil and magnet are sufficient to move the armature and retract the bolt unlocking the door. Upon de-energization of the solenoid coil the magnet holds the armature and bolt in the unlocked position. Upon subsequent re-energization of the coil in the opposite direction, the magnet flux is neutralized and the spring returns the armature and bolt to the locked position. The actuator is particularly suitable for automotive fuel filler access door locking/unlocking applications. | 4 |
CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of an earlier filed application of the same title, Ser. No. 366,372 filed Apr. 7, 1982.
BACKGROUND AND BRIEF SUMMARY OF THE INVENTION
The invention disclosed herein is an improvement of my prior invention, U.S. Pat. No. 4,261,012, issued April, 1981. The prior art discussed in that patent is still considered to be the most relevant prior art.
This invention relates to a system of the type enabling a suject using the system to view a composite picture showing part of the subject himself (or herself) together with some separate article or object as though the subject were actually wearing such article. For instance, such a system when used in ladies bridal salon, might allow a customer to sample the effects of various wedding gowns and choose the most becoming one without actually having to try them on.
Systems of this general kind have already been proposed and have utilized various optical expedients for producing the composite picture. However, none of such prior art devices so far as known to applicant, have been entirely satisfactory.
Perhaps the simplest type of system used employes a semi-transparent mirror positioned before the subject, with means for positioning the actual articles to be displayed, at a suitable position behind the mirror, so that a subject when looking at the semi-transparent mirror will see the reflected image of his or her face or figure, together with the article, as seen by transparency through the semi-transparent mirror so that it will appear to be naturally joined with the reflected image. Systems of this kind are advantageously simply, but have the serious drawback that they require a large number of articles, samples or models to be physically present, and the system will in many instances involve a prohibited amount of storage space.
Other composite display systems have accordingly been proposed in which these difficulties are eliminated through the use of projection slides for displaying the images of the articles in the composite pictures, thereby dispensing with the need, for a physical presence of the actual articles. Slides of course are much easier to store in large numbers and more convenient to manipulate, than are the articles themselves.
Another system requires a black draped subject looking through a semi-transparent mirror, the reflection of her own face in the mirror is formed on the plane of a screen, together with the projected image of a slide formed by a projector on the screen. The slides represent headless models wearing different articles of clothing whereby the subject appears to see composite pictures of herself as though wearing the articles.
Although this system will allow a full figure composite image, it does so under conditions which are not entirely comfortable for the viewing subject, and has serious drawbacks. For the system to work, it must be used in a darkened room which many people find uncomfortable especially in the presence of strangers (salespeople/system operators). Further, the subject must sit with a black cape on her body from the neck down keeping her head fixed in a preset position so as not to misalign the composite image, additionally, there is an inherent inability to produce a composite image of dark or black skinned people. In producing the reflection of the viewer's face from the mirror, a black cape is used to black out the viewer's body below the neck, this ability of the mirror not to reflect the blacked out part of the viewer's body also makes it impossible for the mirror to reflect adequately a dark or black skinned face. Further, in order to have a common background for the composite image as seen in the mirror, the slides are photographed against a black background which will not allow a high quality (detail) reproduction in the slides of black articles of clothing. With this system, the operator attempts to correspond the body size of the projected image (model's body) to the viewer's body by means of a zoom lens on the projector. Inherently, a zoom lens will increase or decrease the size of its projected image proportionately in all directions. Therefore, with this apparatus, it is impossible to create a short fat image or a tall, thin image but rather only a short thin, tall fat or a well proportioned image in between which may or may not correspond with the viewer's own body. Another drawback of this system is the large amount of space it requires making its use impractical except in very large stores.
The prior art in this field is believed to be best represented by U.S. Pat. No. 1,133,311, wherein the subject's head and a garment are composed on a mirror; U.S. Pat. No. 2,722,600, superimposition of two separate images on a common screen; U.S. Pat. Nos. 2,730,565, and 3,576,945, composite pictures where background scenes are blended with a separate image; U.S. Pat. No. 3,398,664, directed to an automatic photoprocessor, and U.S. Pat. No. 3,849,596, directed to various techniques for using a television camera for automatic alignment of two images side-by-side.
None of the foregoing references teach a system which is compact, allows the customer to be photographed in an open area and allows the composite picture to be proportioned along at least one of two axes such that the image of the model's body can be adjusted to be proportioned to the customer's head.
My invention encompasses a composite display system which overcomes the difficulties of the prior art and which is convenient to use and operate, will enable a full figure, full sized display under comfortable conditions for the customer viewer, can be readily adjusted and operated by the system operator in order to view sequentially a series of composite full figure picture displays at a rate as fast or slow as desired.
My invention is broadly directed to a system for displaying to a customer, composite views including part of the customer together with the image of an article as though said article were actually associated with or worn by the customer, which system comprises means to record and display a portion of a body of a customer; means to store a plurality of images, which images when combined with the recorded portion of the customer will provide a full figure display; means to vary the dimensions of the stored image; means to combine and display the combined images.
The method of my invention of providing a proportioned full figure image which includes: displaying at least a portion of a customer on a medium, recording at least a portion of an article of clothing on a medium, combining the images to produce a full figure image, scaling of one of the images with respect to the other to provide a proportional full figured composite image.
The present invention as with the prior invention overcomes the prior art problems discussed therein and, further, this invention has the following advantages or improvements over my prior invention, namely, there is greater flexibility in scaling the height and width of the customer's body. That is, the whole X and/or Y and/or any portion or different portions of the X and/or Y can be scaled. The present invention, is not necessarily limited to making the subject's body taller or shorter, fatter or thinner; the model's body which originally modeled the garment can be scaled to the customer's overall measurements. Perferably, this is accomplished by stretching and/or shrinking rasters, horizontally and/or vertically, based on a calculated stretch and/or shrink factor. For example, I can scale the model which is stored in memory to the bust, hip, waist, and height measurements of the customer. A further improvement is that the skin tone of the model can be adjusted to more nearly simulate the skin tone of the customer.
In the preferred embodiment the system comprises a video camera, a frame grabber, a CPU, an image buffer, a memory, and a television monitor. The videocamera takes the image of the customer which is digitized by and stored in the frame grabber and ultimately displayed on a video screen. Pre-recorded articles of clothing to be combined with the image of the customer are stored. Through use of the central processing unit, at least one of the images, preferably that of the article of clothing are varied at least along horizontal and vertical axes to provide a proportioned full figured composite.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a block and pictorial diagram representing the preferred embodiment of my invention;
FIGS. 2a and 2b are schematics illustrating the composite on a screen.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, television camera or video camera 10, such as a JVC Model KY 1900 CH communicates with a frame grabber 12, such as a DATACUBE 150. The camera 10 records the customer 14 to provide a first image 16; see FIG. 2a.
Various articles of clothing are modeled to provide second images. The images are coded and stored in a memory 18, such as a DSD 880; via a CPU 20, such as a DEC LSI-11/23. As many recordings of various articles of clothing as desired are taken and stored in sequence in the memory 18. The second images from the memory 20 are input to an image buffer 22 such as a DATACUBE 150. The image in the image buffer is scaled and the output is displayed on a video screen 24.
The control of the computer 20 is accomplished through instructions. The instructions are written in terms of the particular mode of operation desired. The computer thus has stored in its memory the programs or routines corresponding to each mode or operation of the computer. It is well known to those skilled in the art, that the computer comprises suitable controls, storage and computational units for performing the various arithmatic and logical functions on data which it processes in digital form. Any standard computer can be used for the instructions. The routines are not described in detail, since they can be written in any desired notations, formats or sequences, depending upon the particular program being utilized, computer language, etc. For the specific computer of the preferred embodiment, the manufacturer's handbook sets forth the necessary program which includes the sequence of internal interconnections which have been added by the preparation and loading of the program into the internal memory of the computer.
It will be only a rare instance when the view of the customer's head and neck will be proportional with the previously recorded view of the article of clothing modeled from the neck down. Therefore, the vertical and horizontal adjustments are necessary, as distinguished from those adjustments which are commonly found with a zoom lens. For example, the customer may be a size 16 and the model a size 8; preferably, horizontal and/or vertical rasters are scaled so that a true proportional full figure composite will be presented to the viewer-customer.
With the above system, it is clear it is not dependent on black in either the background or as a means of eliminating any portion of the customer's body below the neck. Further, this system can be viewed under normal interior lighting conditions much the same as home television viewing thereby providing for more comfortable environment for both the customer and the salesperson. Also, once the customer's image has been recorded by the video camera, the customer is free to assume any position or location comfortable and convenient for viewing the display screen. Still further, because there is no need to record or photograph the articles of clothing against a black background the clothing can be shown against backgrounds which enhance the color of the clothing. In this regard, the system is so designed could allow the composite image to be superimposed over a background which would be a natural setting for the use of the clothing displayed, like an evening gown displayed over the background of a formal ballroom, such as employing the techniques disclosed in U.S. Pat. No. 3,576,945. Lastly, although all of the components have been shown in block diagram form, all components may be housed in a single cabinet which requires only a few square feet of floor space, will need no special areas or darkened rooms and can be placed anywhere convenient for its use in any sized department or store.
Referring to FIG. 2, in the operation of the invention, after all components are actuated a memory of articles or second images 26 is created. This is accomplished by use of the T.V. camera and the frame grabber and the images are stored in memory. The video signals from the T.V., camera are grabbed by the frame grabber 12. The image in the frame is composed of horizontal lines of information called `rasters`. There is one image for each article of clothing and each image is in color. Each image is coded and stored in memory 18 raster by raster. Also, the clothing size of the second image is identified (coded) as a standard. Further, each image stored in the memory is the same size top to bottom.
The customer 16 then is viewed by the color T.V. camera 10; see FIG. 2a. The customer's clothes size is fed to the computer 20 and if the cutomer's size does not match the standard size the computer calculates a horizontal and/or vertical stretch and/or shrink factor to be applied to the stored images so that depending upon whether the customer's size is smaller or larger, the stored image may be proportioned properly to match with the customer's size. The customer selects an image, say a particular bridal gown and the coding information for this image is input into the computer. The image of the customer is displayed on the screen 24 and that portion below the client's neck (indexed at a specific raster location) may or may not be shown as originally photographed. The horizontal and/or vertical stretch and/or shrink factor is applied to the stored image on a raster by raster bias, and the stretched or squeezed result is fed to the display device 24, overriding the image of the client up to but not over the face at the specified raster location.
More particularly, the article of clothing chosen by the customer is read into the computer memory. Starting at the specified raster of the image (near the neck area), each raster is stretched and/or shrunk horizontally and/or vertically by the stretch and/or shrink factor, and a new raster calculated.
Two alternatives may be used in this step. First, a simple re-partitioning of the raster using fractions of pixels according to the stretch and/or shrink factor; or secondly, a low pass filtering and sampling according to the pixel spacing; preferably, two dimensional filtering (incorporating the rasters above and below the current raster) should contribute less distortion to the stretch image.
Each new computer raster is loaded into the display device on top of the customer image and the next rasters are computed in sequence until the composite image is complete as shown in FIG. 2b.
Alternatively, the first image can be input in digitized form into the image buffer and not initially displayed at 24. The second image is overlayed or combined electronically with the first image and the composite image is scanned out and displayed. A separate buffer may be used to store the first image and the images from both buffers combined and displayed. | As apparatus to allow a prospective consumer of articles of clothing to try on one or more articles of clothing without actually putting the articles of clothing on his or her person. This is accomplished by means of an electronically produced full figure image which is composed of the consumer's head and a model's body, the model's body attired in articles of clothing to be presented. The composite image is viewed by the consumer on a television screen and this gives the effect of the consumer being attaired in the articles of clothing presented. | 6 |
BACKGROUND OF THE INVENTION
The present invention relates to the field of textile machines, and particularly to a draw frame with a calender system consisting usually of two calender disks facing each other (or calender roller pair) by means of which a fiber sliver is compressed. The invention relates to a guide system with guide nozzles for the introduction of the fiber sliver between the calender disks. The invention also relates to the wear or replacement parts of the guide system which are subject to greater wear in operation. The invention proposes a process making it possible to accelerate and at the same time simplify the preparation or introduction of the drafted fiber sliver between the calender disks.
According to the state of the art, it is known that the output of the drafting equipment of a draw frame (e.g. of a fiber processing machine) is constituted by a pair of delivery rollers. Immediately following the delivery rollers the fiber sliver is spread out in accordance with the roller width. The person schooled in the art designates the fiber sliver spread out at this location as a fiber fleece. The fiber fleece, i.e. the spread-out fiber sliver, is conveyed into the opening of a fleece funnel. The fiber fleece is collected in the fleece funnel and in the outlet of the fleece funnel it is again formed into a fiber sliver. The fiber sliver is conveyed through the funnel outlet of the fleece funnel to a fiber sliver channel which is of considerable length. At the end of the fiber sliver channel the fiber sliver is introduced into a fiber sliver funnel (also called a sliver funnel) which deflects the conveying direction of the fiber sliver by approximately 90° and is introduced between a pair of calender rollers (also called a pair of calender disks). After passing through the pair of calender rollers the fiber sliver, which was compressed by the calender rollers, is conveyed to the depositing device of the draw frame. Such an example is shown in the left half of FIG. 1, whereby the fiber sliver channel is given reference number 8 and the delivery rollers of the draw frame is given reference numbers 70a and 70b. A setup with a long fiber sliver channel 8 is also described in EP 593 884 A1. Another example of a long fiber sliver channel (also designated by reference number 8 therein) is U.S. Pat. No. 4,372,010. The pair of calender rollers bears references 9a, 9b therein. Another example for the common use of the long fiber sliver pipe is shown in DE-A 26 23 400. Therein the fiber sliver pipe itself is bent at an angle of approximately 90° and guides the fiber sliver without change in angle between the calender disks which are designated therein by 5, 6. An oval shape of the channel bearing reference number 14 therein is described as being advantageous (see also page 9, last paragraph therein).
Finally, DE 290 697 also shows a collection channel. In this case the fleece funnel and sliver funnel are clearly at a distance from each other. A ventilation opening (8) clearly allows the air flowing in at the beginning of the collection channel (5) to escape completely before the narrowest point of the sliver funnel.
DE-PS 36 12 133 relates to a sliver introduction channel between output rollers of the drawing equipment and downstream sliver funnel on a spinning plant preparation machine. The sliver guiding channel relates to the automatic introduction of the sliver beginning into the sliver funnel (column 1, lines 9-10). The sliver guiding channel is relatively long and is given the large diameter which is usual in the state of the art, without any change in cross-section. The sliver guiding channel imparts the necessary guidance to the fiber sliver on its way to the sliver funnel. Along this route, several injectors (air channel, compressed-air channel) are installed. The total sliver mass of the sliver beginning is pulled by means of an injector into the sliver guiding channel. The total sliver mass of the sliver beginning must then be compressed exclusively in the sliver funnel (column 1, lines 54-58).
The problem of air back-up in the sliver funnel (column 1, lines 59-62) exists. In order to eliminate this problem, the sliver funnel must have a device for rapid enlargement of its cross-section. This is a pre-condition for the automatic introduction of the fiber sliver.
It is a further disadvantage of the state of the art that the calender disks must be, in addition, opened for automatic introduction of the sliver beginning. The sliver beginning cannot be pulled into the nip of the calender disks when they are closed and when they are rotating into their nip. The state of the art mentions calender rollers or calender disks in the past. A calender disks has simply a smaller width than a calender roller. This has however no effect upon the function of the invention described herein, so that for the sake of simplification, only calender disks or a pair of calender disks shall be mentioned hereinafter.
OBJECTS AND SUMMARY OF THE INVENTION
The invention departs from the conventional configuration and has as a principal object to create an automatic transportation of the fiber sliver from the fleece funnel to the nip of the calender disks in a compact design, while at the same time simplifying fiber guidance. Additional objects and advantages of the invention will be set forth in the following description, or may be obvious from the description, or may be learned through practice of the invention.
According to the invention, the long fiber sliver channel is omitted and the fleece funnel (as a first nozzle section) and the sliver funnel (as a second nozzle section) are installed directly one after the other, while being interlocked in such a manner that they can either be tilted against each other or so that their angle position can be changed (tilted) jointly relative to another nozzle section. Tilting the axis of the first nozzle and of the second nozzle makes it possible to change the route of the fiber sliver which goes one time through the above-mentioned nozzle insert and another time not through the nozzle insert, this being the so-called pre-work or preparation position.
The fiber sliver guiding device may be made in one part or in several parts, whereby its insert is smaller and is inserted into the nozzle as a replaceable wear part. The wear parts are designated as being internal inserts. The calender guiding nozzle, which reaches over the pair of calender disks in the area of the nip, constitutes one side of the swivel bearing of the nozzle section located above, or of its internal inserts.
By omitting the fiber sliver channel, the fiber guiding system according to the invention becomes especially short and compact, and at the same time long distances, and thereby undesirable technological dead-times, can be reduced. Despite its compact construction, the fiber sliver guidance device is easy to handle and even allows for two positions of the interlocked nozzle sections, one for normal operation and one for preparation. Surprisingly, the compact fiber sliver guidance system is then particularly easy in maintenance, easy to adjust, and is more user-friendly in its adjustment effort than the long fiber sliver guidance systems known in the state of the art.
Easy and rapid replacement of the sections of fiber guidance system subjected to wear is possible with the internal inserts. Adjustment tasks in assembly, as well as for replacement work, are eliminated to a great extent due to the plug-in system of the individual sections. Work is concentrated on a narrow area between the output of the delivery rollers and the pair of calender disks and can be managed easily. To start maintenance work, only the fiber sliver channel above the calender disks need be swivelled around an axis which lies in the fiber sliver channel and is aligned at a right angle to same.
The new design also makes it possible to accelerate and simplify the introduction of the fiber fleece which has not yet been drafted and to convey with the calender guiding nozzle to behind the nip, in part with air flow (up to the nip) and in part with rotational impulse of the closed calender rollers (through the nip). If the calender disks are spread apart (open nip), the air stream alone suffices for complete introduction of the fiber sliver between the calender disks. The beaks of the guiding nozzle near the calender are provided with axially traversing (slight) widening areas extending in the radial direction which guide air past the nip. The beaks (beak halves) have a length and a width (L, W) coordinated with the widening so that practically the greater portion of the guiding air, or all of it, is introduced into the widening and is sealed off without contact in transversal (radial) direction to a considerable extent.
The beaks can be made in one part with the body of the nozzle through a cone but their distance need not be adjustable, nor their alignment relative to the body part of the sliver funnel holder.
If the width of the calender disks is changed, a suitable sliver funnel holder is selected into which the same sliver funnel can be inserted. Adjustment and adaptation tasks are eliminated through modular adaptation.
The invention's proposal of omitting the long fiber sliver channel causes the calender guiding nozzle to be moved close to the fleece funnel and constitutes the fixed part of the nozzle insert relative to which the fleece funnel axis can be tilted.
The individual nozzle sections of the fiber sliver guiding device are all placed close together. The central axis of each section constitutes the axis of the fiber sliver channel whereby each section may be one of several inserts. The design with several inserts has the advantage that despite compact construction, only those element of the overall fiber sliver guiding system need be replaced which are subject to greater wear. Thus two internal inserts are provided: One of them is an internal insert of the fleece funnel located right after the delivery rollers of the drafting equipment; the other internal insert is the one constituting the sliver funnel at which the greatest diameter change of the fiber sliver channel occurs. The replaceability is also ensured when batches are changed.
The possibility of swivelling one axial section relative to the other axial section can be realized by the internal insert having a rounded articulation surface on its forward end which is seated in a convex bearing surface provided on the other internal insert. The rounded articulation surface and the convex bearing surface together constitute a guide channel which is air tight in the radial direction when the first internal insert sits on top of the second internal insert and is swivelled into operating position. However, swivelling is possible, whereby the sealing effect is ensured in the radial direction in both swivel positions.
The essentially loss-free air transport through the two internal inserts results in good air maintenance and little loss with respect to an automated introduction of fiber sliver between the calender disks. The lateral flow openings which are provided for this and are provided in the .second internal insert are preferably non-swivelling and thus in fixed position. The injector in this embodiment is located on the sliver funnel and the fiber sliver channel above the injector can be swivelled above the rounded articulation surface. The guiding system has no additional channels for the entry of air flow above the sliver funnel.
In addition to its suction effect, the injector is able to impart a twist on the guided fiber sliver. This is achieved if two injector bores let out parallel offset relative to each other in a plane of the channel of the sliver funnel.
An alternative fiber sliver guiding system is obtained if the nozzle section constituting the sliver funnel is itself capable of being swivelled and if the injector channels provided in it swivel together with it. The position of only one guidance section remains swivelled without change relative to this guidance section in the immediate proximity of the calender disks and of the nip (calender guiding section), and the remainder of the fiber sliver channel extending to within close proximity of the delivery rollers swivels relative to this guiding section. The above-mentioned rounded articulation surface is then located at the forward end of the sliver funnel and the convex bearing surface on the fixed calender guiding section. Here too, the coupling is air-tight in radial direction in operating position, so that good air management and few losses are achieved in spite of the ability to swivel and the modular construction of the fiber sliver channel (corresponding to a guiding channel).
The low losses in air management are maintained also beyond the calender nip if the calender guiding nozzle which is a replacement and exchange part is bilaterally open in its beak section, so that the calender disks are able to enter the beaks in part from the side. The air stream guided over the articulation surface can thus be conveyed up to the nip and even beyond the nip and past the calender disks, so that the fiber sliver to be introduced can be guided up to the nip and beyond it. Guidance with the two partially round beaks of the calender guidance nozzle is obtained here independently of whether the calender disks are spread apart (so that they produce an open nip) or are pushed together (so that the nip has practically no passage opening.)
At the input of the fiber sliver guiding system, an additional deflection roller which clearly changes the direction of travel of the fiber fleece FV is provided. The clear change is in the direction of the bent nozzle axis of the fiber sliver guiding system so that the first nozzle (the fleece funnel) of the guidance system is able to receive the drafted fiber sliver and to bring it together. An angle of approximately 60° is preferred by which the deflection roller changes the path FV of the fleece. The axis of this additional deflection roller is located in the plane defined by the swivel axis V and the nip.
The first nozzle has a funnel area as well as a ramp or plateau area, so that the fiber sliver is able to achieve the rolling up, deflection and gathering of the fiber sleeve when this nozzle is in its operating position and so that when the first nozzle is tilted, the ramp area ensures that the fleece conveyed to it is deflected so that it is conveyed out of the area without blocking the area of the drafting equipment and can be removed easily by the operator.
The ramp area also ensures that no back-up of the fiber fleece can form because the first nozzle is swivelled automatically under the force of the fleece conveyed to it and the ramp area deflects the fleece which continues to be fed out of the interior of the drafting equipment until the delivery rollers are switched off. The first nozzle has at the same time assumed its preparation position, i.e. the position which it assumes when back-up occurs.
The swivelling first nozzle can be supported in the sliver funnel nozzle (the cylindrical-funnel-shaped nozzle) so as to be capable of swivelling; the first nozzle can however also be supported on the above-mentioned calender guiding section together with a nozzle section following it immediately and made in the form of a sliver funnel and be capable of swivelling.
The nearly totally loss-free movement of air from the fleece funnel to the nip of the calender disks is characteristic for the process of air-assisted introduction of the spread-out fiber sliver (fiber fleece) into the fiber sliver guiding channel of the textile machine. The nearly loss-free movement of air is subdivided into a completely loss-free segment and a second segment in which no considerable losses occur.
a) The air flow from the fleece funnel (which rolls up the drafted, spread-out fiber sliver (fiber fleece) and gathers it together) to the sliver funnel (which causes the compression before the pair of calender disks) is guided without losses. In this area no lateral opening through which air could escape is made in the guiding channel. Only lateral inflow bores exist in this area, producing and maintaining the suction air stream.
b) In the area following the sliver funnel, the air stream is screened from lateral beaks to such an extent that it is guided past the calender disks and its suction effect can be maintained for the fiber sliver up to the nip. Since the calender disks rotate in operation and since a rotation impulse is used also when the fiber sliver (or part of the fiber sliver) is introduced in order to transport the fiber sliver which is conveyed to the nip, by air suction entirely through the nip while being compressed at the same time, the insides of the beaks are separated by a small distance from the lateral surfaces of the calender disks. The calender disks are thus able to rotate without friction because the mechanical screening used for air guidance does not come into contact with them. At the same time, it is ensured that the clearance which remains between the areas of the screening directly next to the sides of the calender disks is as small as possible so that practically no air escapes. Only at the front end of the screening does this air escape. This point lies behind the (open or closed) nip (as seen from the direction of fiber sliver conveying).
Due to the mostly closed air guidance, the process for automatic introduction of the beginning of the spread-out fiber sliver (fiber fleece) is very economic from the point of view of air management. At the same time, the process is unaffected by fluctuations in the compressed air and can operate reliably with a wide range of pressures of the compressed air which becomes a suction flow formed above as it is brought in at an angle relative to the fiber sliver channel direction.
No mechanical threading of a section of fiber fleece into the fleece funnel takes place. The fiber fleece need merely be brought to a narrow width at its forward end (to width F1) and the remaining, narrower section must be shortened to a predetermined length (length H) which depends on the weight of the sliver and the length of the fiber sliver channel from the fleece funnel to the nip. Switching on controls for the feeding of compressed air in order to produce a brief compressed-air impulse causes the threading of the narrowed section up to the nip, where enabling a brief rotational impulse of the calender disk realizes the complete threading or the complete introduction of the fiber sliver between the calendar disks.
The compressed-air impulse can be coupled advantageously to a rotational impulse of the calender disks that is slightly offset in time, so that the operator requires only one push button to thread the fiber sliver.
A fiber sliver cannot be presented, introduced and placed in operating position in any simpler, more rapid and reliable manner.
The suction air stream above the location of entry of compressed air is constituted reliably if the compressed air is introduced at the point of the fiber sliver channel which has the smallest diameter. As a rule, this is the sliver funnel which is located close to the calender rollers. A stream of compressed air fed here in the direction of the calender rollers produces a reliable suction stream above the feed point and up to the fleece funnel, as no air losses occur there.
In the entire section from the fleece funnel to the sliver funnel, no openings at a right angle to the fiber sliver channel are provided which could allow air to escape. The reliable build-up of the suction air stream starting at the forward end of the conveying path and acting back to the point of entry of the fiber sliver--the fleece funnel--makes it possible to dispense with any additional inflow of air in this area, such as is usually the case in the state of the art when compressed-air inflow points are provided at the fleece funnel or shortly thereafter, while venting is provided on the sliver funnel or shortly before it.
According to this invention, the fiber sliver is thus seized at its forward end by the air stream, is pulled along the entire fiber sliver channel and is presented directly to the calender disks. The fiber sliver is not "pushed" by compressed air and vented far from the calender disks.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows the superposition of a conventional configuration of a fiber sliver guidance system with a long fiber sliver channel and an example of a compact design with interlocked nozzle inserts 30, 40, 50, 60 of which two nozzle inserts 40, 50 are able to tilt relative to the other two nozzle inserts 30, 60 which are installed on a fixed nozzle holder 20 located above the calendar disks 100a, 100b. The superimposed drawing serves to show the shortening of the conveying path.
FIG. 2 explains the fiber sliver guiding system of the state of the art--taken form EP 593 884--with a long fiber sliver channel 8, sliver funnel 9 and calender disks 100a, 100b. The fleece funnel is designated by 1 and the output rollers of the draw frame by 70a, 70b.
FIGS. 2a and 2b show the two swiveling positions α A , α B of the interlocked nozzles of the overall nozzle insert as an example of an embodiment of the invention.
FIG. 3 shows the preparation of the fiber fleece F for introduction into the fleece funnel 50.
FIGS. 3a and 3b show the two tilting positions relative to the fiber sliver introduction and in operation of the draw frame.
FIGS. 4a and 4b show the internal insert 40 of the fleece funnel 50.
FIGS. 5a, 5b and 5c and 5d show the sliver funnel 30 for insertion into a holder 60 in accordance with FIG. 6a.
FIGS. 6a, 6b and 6c show the holder 60 in form of a beak funnel, of the sliver funnel 30.
FIG. 7 shows a schematic top view of the nip 100c which is formed by the pair of calender disks 100a, 100b. The air channels 65a, 65b are delimited on the outside by the beaks 61, 61b which are installed on the sliver funnel holder 60 at the front. This view is shown in detail in FIG. 6c without calendar disks.
FIGS. 7a and 7b show a detail of the nip shown schematically in FIG. 7, once closed 100c, once open 100d, by switching off one calendar disk 100b relative to the other.
FIGS. 8a and 8b show an embodiment comparable to that of FIGS. 3a, 3b, in which the swivelling area has at the same time a bend K in the guidance axis 200a, 200b of the fiber sliver guidance. A calendar guidance section (61') remains under the axial bend K as a fixed section 61'. All the nozzle function elements--also the sliver funnel area--between delivery rollers 71, 70a, 70b and calendar disks 100a, 100b are able to swivel. The area above section 61' is made in one part as insert 40, 30 into the fleece funnel 50, surrounded by a cylindrical holder 80.
FIGS. 9a and 9b show the fleece funnel 50 with the tilting articulation 50c on the stationary holder 20 in which the sliver funnel 60, 30 is held and is detachable. The forward end 41 of the upper insert 40 is able to swivel and is supported in the lower insert 30 of the sliver funnel 60, for which two articulation surfaces 41a, 41b and 35 are used which interact radially to seal off air in operational position.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Reference will now be made in detail to the presently preferred embodiments of the invention, one or more examples of which are illustrated in the drawings. Each example is provided by way of explanation of the invention, and not meant as a limitation of the invention. For example, features illustrated or described as part of one embodiment can be used on another embodiment to yield a still further embodiment. It is intended that the present invention cover such modifications and variations.
The superposition shown in FIG. 1 clarifies the difference with the state of the art which is shown schematically in FIG. 2. The fiber sliver FV, which is not yet properly drafted as it is introduced, is introduced in the state of the art via drafting rollers 68a, 68b, 69a, 69b and delivery rollers 70a, 70b into a long guiding channel 8 which lets out into a sliver funnel 9. The funnel channel 9 deflects the fiber sliver FB by about 90° into the nip of the calender with its calendar disks 100a, 100b. The calendered fiber sliver KF emerges vertically downward from the calender and is fed into a depositing device (not shown). This fiber sliver guide is also shown in FIG. 2 with the same reference numbers.
An embodiment of the invention given as an example shortens the path of the fiber sliver and omits the fiber sliver channel 8. An additional deflection roller 71 causing a deflection of approximately 60° in the direction of fleece conveying FV, and which introduces the fiber sliver into one of several functional elements constituting the fiber sliver channel (guiding channel), is added.
The first element is the fleece funnel 50 (also called nozzle). The fleece funnel is a nozzle with an essentially rectangular opening. The fleece funnel has a ramp surface 50b and a funnel section 50a following it immediately in which the fiber sliver (fiber fleece) arrives in a wide form and is rolled, folded over and introduced into a first channel segment. The channel segment is constituted by a insert 40 which is inserted on the back of the funnel section 50a of the fleece funnel 50 and is attached with a screw. It can be adjusted.
The fleece funnel 50 (with internal insert) can be tilted by means of a handle segment 51 in such manner that the ramp surface 50b can be swivelled in the direction of travel of the fiber fleece (i.e. conveying direction) and the funnel section 50a can be swivelled next to it.
An articulation surface 41a, 41b is provided at the forward end of the insert 40 and in the angle position α B shown in FIG. 1 or FIG. 2b it seals off the guiding channel from the downstream sliver funnel 30.
The articulation surface of the forward, cylindrical segment of the internal insert 40, which is symmetrical with the central plane of the first insert 40, consists of two surface segments 41a, 41b which narrow towards the back (in axial direction) and are constantly curved. These surface segments 41a, 41b engage a corresponding bearing surface 35on the sliver funnel 30. FIGS. 4a and 4b show this articulation surface in two views at the forward end of insert 40 of the fleece funnel 50. Swivelling the fleece funnel 50 in the direction α in the other angular position α A does not open the radial air-tight closure between fleece funnel and sliver funnel. In the closed (α B ) as well as in the open (α A ) state, a radial air-tight fiber sliver conveying is achieved.
The radial tightness of the articulation surface 41a, 41b at the bearing surface 35 can be adjusted. The upper part (above the articulation surface) can be displaced for this in axial direction, in particular in radial direction, relative to the lower part. The fixed holder 20 in which the sliver funnel 30 is inserted constitutes the basis for the adjustment.
If the fleece funnel 50 is made in two parts, with an insert 40 inserted in it against the conveying direction of the fiber sliver, the previously mentioned relative adjustment can be carried out using a handle 51.
The fiber sliver is conveyed through the fleece funnel 50, the internal insert 40, and the sliver funnel 30 into the guiding channel and up to the nip 100c, and for this the fleece funnel 50 is swivelled out. The fiber fleece part F1, which was manually narrowed according to FIG. 3 and is held into the funnel outlet 50a, is sucked in via injection bores 34a, 34b, 64a, 64b on the sliver funnel. A brief suction flow lasting 500 milliseconds suffices in order to convey the narrowed fiber fleece segment F1 until it is in front of the nip 100c, since the articulation surface 35 and the bearing surfaces 41a, 41b of the internal insert 40 are radially air-tight. No mechanical means to assist insertion are needed.
In order to convey the segment F1 of the fiber fleece, and with it the full width F of the fiber fleece through the nip, a brief rotational impulse of duration T 2 is given the calendar disks. After a predetermined suction period T 1 , the brief suction flow is able to switch itself off. It can be superimposed on the duration T 2 or can be initiated separately and manually.
The form of the sliver funnel 30 is clearly shown in FIGS. 5a, 5b and 5c in which the direction and the placement of injection bores 34a, 34b, 64a, 64b in the sliver funnel are also shown in a larger scale. They let out into a cylindrical channel 31 which constitutes the forward end of the fiber sliver channel. The cylindrical section 31 widens over a conical segment 32a to reach the diameter of channel 32 which is predetermined by the internal insert 40. The bearing surface 35 is provided at the upper end of the cone 32a and follows the articulation surface 41a, 41b in its curve.
The slanted injection bores 34a, 34b can extend at an angle of approximately 45° relative to the axis 200b of the sliver funnel insert 30. They are advantageously parallel offset. This makes it possible to center the fiber sliver in the fiber sliver channel. Furthermore, the fiber sliver is given a twist therein. This imparts strength to the fiber sliver. The parallel offset injection bores 34a, 34b can be seen in FIG. 5d. They let out above a cylindrical section 33 of the insert 30 in a ring channel that is open to the outside.
A sliver funnel holder 60 according to FIGS. 6a, 6b, 6c is provided with a central, approximately cylindrical opening 62 into which the sliver funnel insert 30 is inserted in its upper, approximately cylindrical section 67. A ring channel 63 which is open towards the inside extends in the cylindrical opening and can be fed compressed air by two or more cylindrical bores 64a, 64b. Starting from the ring channel, the compressed air introduced from the outside is introduced into the previously mentioned sloped injection bores 34a, 34b when the sliver channel insert 30 is inserted, to let out into the cylindrical segment 31 of the fiber sliver channel which is close to the nip 100c.
FIGS. 6a and 6b show the cylindrical beak 61 of the sliver funnel holder 60 which follows a conical section 68 constituting the transition between the upper cylindrical end 67 and the beak 61. It possesses a length L and a diameter which is shown as width b in the cross-section of FIG. 6b. The beak 61 is fixed and has two halves as it is split on the side, as shown in FIG. 6c. As shown in the schematic drawing of FIG. 7, a segment of the rotating calender disks 100a, 100b engage either of the two above-mentioned slits. This can also be seen clearly in FIG. 1, right half of the drawing. The nip is located in the center of the beak of the sliver funnel holder 60, i.e. in the axis 200b of the fiber sliver guide, and this nip can be closed (nip 100c) or can be opened by stopping one calender disk 100b (open nip 100d) as shown in FIGS. 7a and 7b.
The integrated beak halves 61a, 61b formed by the above-mentioned slits 61c, 61d in the cylindrical beak 61 guide the conveying air past the nip 100c or 100d. This conveying air was previously introduced via the injection bores 64a, 64b into the ring channel 63 and from there via the injection bores 34a, 34b of the sliver funnel 30 which form an angle with the axis 200b into the fiber sliver channel. The beaks make it possible to prevent the conveying air from escaping before the gap 100c, 100d, and instead it is conveyed beyond the gap to behind the nip. A first narrow channel section 65a on the one side of the calendar disks or a second narrow channel section 65b on the other side of the calendar disks, said channels having a nearly semi-circular cross-section, are used to convey this air. Either channel is very narrow as compared with the thickness d or width b of the beak 61 or its inner wall, which directly adjoins the lateral surface of the calendar disk.
Due to the lateral air conveying beyond the calendar gap by means of the beak halves 61a, 61b which have a length L equal to approximately one half the diameter of the calendar disks in the embodiment shown, the width b of the beak and of the covering d of the inside of the beak half have a sealing effect relative to the calendar disk. This sealing effect is constituted without contact by definite to considerable lateral flow resistance against the axial lateral air channels 65a, 65b.
Thus, only an almost exclusively axial air movement past the calendar nip is possible.
Only if the calendar nip 100d is open as shown in FIG. 7b, is the air conveyed not only past the calendar gap but clearly also through the calendar nip. The guiding air serves to thread the fiber sliver through the calendar nip and the calendar disk 100b can then be moved in so as to reach the operating position together with the threaded fiber sliver. In this case, where the calendar nip is open, the sealing surface (part of the covering d) is also large enough in View of the air resistance of the now enlarged passage channel consisting of the channel segments 65a, 65b and the open calendar nip 100d in order to prevent radial escape of the conveying air.
In the position of the calendar disks as shown in FIG. 7a, as well as in the position shown in FIG. 7b, the fiber sliver is presented in the same manner:
The user swivels the fleece funnel (also called a nozzle) 50 by the grip 51 into preparation position which brings the ramp section 50b into the direction of fleece movement KF;
A pre-run impulse of the rollers 86a to 70b and 71 of the drafting equipment conveys a short segment of fiber fleece on the ramp section 50b and out of conveying direction FV-FK;
The user shortens the fiber fleece taken out and narrows it as per FIG. 3;
The fleece funnel 50 being swivelled out, the user holds the narrow end F1 of the fiber fleece into the funnel opening 50a of the fleece funnel 50 and an air impulse is initiated via a push button or an automatic device at the narrowest location 31 of the fiber sliver guiding channel;
The shortened and narrowed starting section is sucked into the fiber sliver channel by the almost loss-free air guidance--even if the fleece funnel 50 being swivelled out--and is taken up to the nip 100c (as per FIG. 7a) or even through the open nip 100d (FIG. 7b);
The fleece funnel 50 is swivelled back into its operating position. A rotation impulse on the calendar disks 100a, 100b, if applicable with calendar disk 100b already moved in and/or on the delivery rollers of the drafting equipment 70a, 70b, conveys the fiber sliver reliably and without mechanical insertion assistance into the fiber sliver channel (guiding channel) with axis 200a (in the upper area) and 200b (in the lower area).
Due to the air-tight conveying V in the fiber sliver channel, it is also possible to swivel the fleece funnel 50 back into the operating position shown in FIG. 1 only when the rotation impulse is terminated and the fiber fleece is already completely threaded.
The air pressure to be used may be 4 bar, adapted to a channel diameter 31 of approximately 3.8 mm in the sliver funnel 30 and approximately 8 mm in the channel 45 of the insert 40 of the fleece funnel 50. Tests have shown that a compressed-air impulse of only approximately 500 milliseconds (ms) duration suffices for reliable introduction of the forward portion F1 of the fiber fleece up to nip 100c. The length H1 of the manually narrowed fiber fleece is adapted here to the distance between the fleece funnel 50 and the nip 100c and thereby to the length of the air-tight fiber sliver channel.
The previously mentioned ring channel 63 directed inward can also be made in the form of a channel 36 directed outward on the insert 30, e.g. in form of a surrounding notch. The two channels 63, 36 can be provided so as to form a ring channel together when the funnel 30 and the holder 60 are plugged into each other.
The sliver funnel holder 60 has a truncated-cone clearance 68 between its upper cylindrical section 62 and its beak section 61. With it, and with the cylindrical section 68, it can be inserted into a support 20 which is placed close to and above the calendar disks 100a, 100b in such a manner that the beak section 61 of the holder 60 reaches over the calendar disks and the nip. Also held on the support 20 at a distance via bearing brackets 52a, 52b, is the fleece nozzle 50 which is capable of swivelling. All parts of the nozzle systems can thus be exchanged, but are nevertheless fixed precisely in their position.
The replaceability of all parts of the nozzle system opens the possibility of modular construction of the fiber sliver guiding system between the output of the delivery rollers and the depositing of the calendared fiber sliver. Adjustments or settings with adaptation to given calendar disk width or for certain fiber types or processing conditions are no longer required. If processing conditions are stipulated, modular nozzles for these are provided, and are connected to each other via their respective inserts. The inserts fit any of the modular nozzles and establish the connection between the different technological parts. The replaceability also makes it possible to operate changes following a batch change.
The insert 40 was described through FIGS. 4a, 4b. It is plugged in opposition to the direction of fiber sliver movement into the fleece funnel 50. Its forward end is the articulation surface 41a, 41b which is attached to a cylindrical channel section 41. It has a constant curve which is oriented backwards on both sides of the central plane of the insert 40 while its width decreases symmetrically on both sides. The reduction of the width is at a right angle to the axial direction of the guiding channel 200a. The greatest width of the articulation surface is on the front end.
The channel segment 41 on which the articulation surface 41a, 41b is installed is made in one piece on a conical section 43 which merges into a cylindrical area 45 which has a slightly larger diameter than the also cylindrical plug-in section 42. Thus the cylindrical section 45 is able to function as a stop when the plug-in section 42 is plugged into the fleece funnel 50 from behind (contrary to the direction of movement of the fiber sliver).
The internal insert 30 for the sliver funnel holder 60 is shown in FIGS. 5a to 5d. It has the receiving bearing surface 35 in addition to the articulation surface 41a, 41b of the previously described insert. The bearing surfaces 35 also become narrower in the direction of axis 200a of the conveying path. The smallest width of the bearing surface 35 is at the forward intake end of the insert 30.
The outside dimensions of the insert 30 are sized so that it can be inserted into the sliver funnel holder 60. The holder 60 is made in one piece and is explained in further detail through FIGS. 6a to 6c in three different views. It is visibly larger than the actual sliver funnel which is constituted by insert 30 in this embodiment.
The holder 60 is installed fixedly relative to the calendar disks, and it is fitted out with injection nozzles 64a, 64b in order to feed air into the fiber sliver guiding system in the direction of travel. The fixed installation of the holder facilitates air feeding since it need not also be swivelled. FIGS. 9a, 9b show the fixedly installed holder 20 into which the sliver funnel holder 60 is introduced in a conical plug-in section, so that it is fixed precisely across from the calendar disks.
The beak halves 61a, 61b extending over the calendar disks are semi-circular in this embodiment. They are made in one piece with a cone 68 to which they are attached, and which is also on one piece with the cylindrical section 67 of the holder 60 into which it merges.
A cylindrical opening 62 into which any desired sliver funnel insert 30 can be inserted is provided in the cylindrical section 67. The outside dimensions of each sliver funnel 30 to be used is adapted to the inside dimensions of the holder 60. Even if different technological requirements apply which prescribe the sliver funnel in a form of channel 32a, 32, 31, the same sliver funnel holder 60 can be used.
Flow-through openings 64a, 64b by means of which air can be fed in proximity of the calendar disks in proximity of the calendar disks are provided in the cylindrical section 67 of the holder 60. This air is conveyed through the semi-circular beaks 61 in such a manner that it is at least prevented from escaping before the calendar nip 100c (or 100d according to FIG. 7b). Widening areas 65a, 65b are provided for this, leading past the calendar nip 100c according to FIG. 7. Their size by comparison with the width of the calendar disks or with the width b of the semicircular beaks can clearly be seen from FIGS. 7a or 7b. They are determined by the compression effect of the cover surface d which defines the inner sealing side of the semi-circular beaks against the calendar disks by means of flow resistance, whereby a contact-less seal is achieved through markedly greater flow resistance in perpendicular direction than the low flow resistance in axial direction which is defined by the size of the widening area.
FIGS. 8a and 8b show the configuration of a guiding section made essentially in one piece and containing the fleece nozzle 50 as well as the sliver funnel 30. The sliver funnel 30 is here inserted directly into the fleece funnel 50 and its position is furthermore fixed by a pipe holder 80. The forward end of the sliver funnel 30 is supported in comparable bearing cups and rounding surfaces as described through FIGS. 4b and 5c in connection with the fleece funnel insert 40.
The radial seal is achieved thus also in FIGS. 8a and 8b, where a remaining section 61' of the guiding section is fixedly held relative to the calendar disks, e.g. on holder 20 according to FIG. 9a. The remaining guiding section 61' corresponds to the beak area L of the sliver funnel holder 60 of FIG. 6a. In this embodiment the air is introduced via slanted injection bores 34a, 34b into the combined fleece funnel/sliver funnel at its forward end, whereby a swivelling motion provokes a slight swivelling of the location of air introduction which is however minimal because of its proximity to the pivot point K.
The two swivel positions shown in FIGS. 8a and 8b are designated α A and α B , but may be of slightly different size, since the swivelling part in FIGS. 8a and 8b is larger or longer than in FIGS. 3a and 3b.
Different bores and corresponding conical transition sections in the insert 40 which is at the same time fleece funnel insert and sliver funnel 30 define the fiber sliver guiding sections. Replacement of the insert 40 represents at the same time a replacement of the sliver funnel 30. Readjustments or alignment tasks can be omitted because of the one-piece configuration.
The ring-shaped holder 80 is not entirely flush with the combined fleece funnel/sliver funnel, but leaves a ring space 81 between the inside of the funnel and the outer diameter of the mostly cylindrical combination funnel 30/40. The ring space 81 guides the compressed air used for fiber conveying, and is sealed at the forward end by flush (ring-shaped) contact against the combination nozzle, below the injection bores 34a, 34b. At a suitable height selected as a function of the application, a main air stream is conveyed outwardly and lets out in the ring space, being able to build up compressed air at that location in order to feed the injection bores 34a, 34b.
The injection bores are clearly at an angle in this example relative to the axis 200b, and stop directly in front of the radially air-tight articulation K where a radial, air-tight support is provided in the two positions of FIGS. 8 and 8b.
The angles α 1 and α 2 are slightly smaller than in the example of FIGS. 2a and 2b, but are within the same indicated range as in FIG. 2. The precise angle in this embodiment is approximately 5° for α 2 , for α 1 approximately 25° (±10%), while in FIG. 2a an angle of α A of approximately 30° and in FIG. 2b an angle of approximately 7° (±10%) have worked reliably in the experiment.
The plateau area 50b in FIGS. 8a and 8b is accordingly somewhat adapted relative to the angle of the ramp area 50b in FIGS. 2a and 7b. It is connected to the angles α in the respective final swivel positions, whereby the swivel position α 1 and α A require an angle of the ramp such that the direction of movement of the fiber fleece FV is clearly perpendicular coming out of the output area of the draw frame. Here it is advantageous if the perpendicular direction FV' contains a slight downward component, e.g. if it is slightly at a downward angle from the horizontal.
The ramp area is given a slight slope of 1° to 2° for that purpose from the funnel area, or is slightly conical.
Two different fiber sliver channel sizes are shown in the combination funnel 30/40 in FIGS. 8a and 8b, one narrow and one wide, each with a conical shoulder towards the narrowest cylindrical section of the fiber sliver channel.
FIGS. 9a and 9b show a side view and top view of the fleece funnel 50 with its ramp area 50b and its funnel area 50a according to FIG. 3. The swivel axis V is perpendicular to the guide axis 200a, 200b and extends through the air-tight articulation 41a, 41b and 35, as shown in FIGS. 4 and 5. At the same time the swivel axis V extends through bearings 50c which are constituted by lateral holding brackets 52a, 52b and journals which can be set on the forward, half open swivel seat. The fleece funnel 50 can thus be removed and tilted, while the guiding channel 200a, 200b is at the same time air-tight.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope and spirit of the invention. It is intended that the present invention cover such modifications and variations as come within the scope of the appended claims and their equivalents. | A fiber sliver guidance system for a textile machine drafting equipment is provided and includes a first nozzle section disposed relative to the delivery rollers to receive a fiber fleece therefrom and form the fiber fleece into a fiber sliver. A second nozzle section is connected to the first nozzle section to receive the fiber sliver therefrom. The second nozzle section includes an essentially cylindrical sliver channel disposed to guide the sliver to the nip of the calender rollers. The sliver channel of the second nozzle section includes a guiding section defined by spaced apart end segments which extend on opposite sides of an alongside the calender rollers past the nip. The side signals cooperate with the calender rollers to define a limited air loss channel for the fiber sliver directly to the nip. | 3 |
This is a division of application Ser. No. 845,989 filed May 21, 1986.
FIELD AND BACKGROUND OF THE INVENTION
The present invention relates in general to the field of gasification for carbon-containing fuel, and in particular to a new and useful process and device for gasifying carbon-containing fuel, in particular coal, whereby a portion of the produced synthesis gas is burned to heat a fluidized bed reactor in which the fuel is gasified.
In coal gasification, a distinction is made between "autothermal" and "allothermal" processes. In autothermal gasification, the heat needed to sustain the gas-forming reactions is produced by combustion reactions that take place in the reactor itself. Not just coal and steam, but air and/or oxygen as well, are fed into the reactor, so that incomplete or sub-stoichiometric combustion of the coal occurs as synthesis gas is produced. In practice, this means that a considerable portion, typically about 30-40% of the coal is lost in the production of heat and only the remainder is converted into available product gas. Another disadvantage is that the available gas is loaded with combustion products and, unless pure oxygen is used for processing, the gas is also loaded with a large proportion of ballast material in the form of nitrogen, which diminishes its usefulness and means that the downstream purification and desulfurizing units must be built correspondingly larger in size. Finally, the relatively high temperature produced in the reactor by the combustion reaction is also disadvantageous, because it makes it more difficult to maintain the fluidized bed and may favor the formation of nitrogen oxides (NO x ) harmful to the environment. Also known to the art are autothermal coal gasification processes wherein a portion of the gas produced is recycled to the reactor and again takes part in the reaction (e.g. German Pat. No. 32 23 702).
In allothermal gasification, heat is supplied from an outside source. Apart from the coal dust, essentially only steam is introduced into the reactor to act as a reaction medium and to sustain the fluidized bed, while the reaction heat required for gasification is essentially provided by an exchange of heat by the reactor with a hot heat exchange medium fed in from the outside. In this process, the coal can be converted essentially completely into available gas, and the produced gas is largely free of combustion residues, nitrogen ballast, etc. Furthermore, the temperature in the reactor can be kept at a lower or optimal level for the gas-forming reaction. The problem there, however, is that to heat the heat exchange medium to be fed into the reactor, an additional source of heat and hence a corresponding demand for primary energy is required. The allothermal process is most advantageous if a nuclear reactor is available to act as such an additional source of energy. In such case, a secondary helium cooling circuit heated by the primary helium cooling circuit of the nuclear reactor can serve both as a heat exchange medium for heating up the reactor and also for the production of the steam required in the reactor (see van Heek and Kirchhoff In "HdT-Vortragsveroffentlichungen" (Haus der Technik Lecture Publications), 453, 1982, p. 59).
SUMMARY OF THE INVENTION
The present invention provides a process of the kind indicated, that makes use of the advantages of allothermal gasification of the coal or fuel but requires no outside sources of heat, as well as a device with which to perform the process.
Accordingly an object of the present invention is to provide a process for gasifying a carbon-containing fuel, in particular coal, with subsequent use of a product gas therefrom, comprising supplying finely ground or atomized carbon-containing fuel to a fluidized bed reactor, gasifying the fuel in the reactor by means of an essentially allothermal gasification reaction and by feeding in steam to the reactor, heating the reactor by indirect heat exchange with a heat exchange medium, with synthesis gas being produced in the reactor from the fuel, removing dust and sulfur from the synthesis gas to form purified synthesis gas, burning at least a portion of the purified synthesis gas to form hot flue gas, and using the resulting hot flue as the heat exchange medium to heat the reactor.
A further object of the present invention is to provide a device for performing this process which includes a fluidized bed reactor with a heat exchanger therein, feed means for feeding ground coal or other carbon containing fuel to the reactor, purifying means for purifying gas produced by the reactor to remove dust and sulfur from the gas, steam producer means connected to the reactor for producing steam and for supplying steam to the reactor, and heating means for heating up a heat exchange medium to be fed to the heat exchanger, the heating means comprising a combustion chamber for receiving the purified synthesis gas to burn the gas and form the heat exchange medium.
The process of the invention makes it possible to run an allothermal gasification reactor without the aid of an additional heat source, because the requisite heat is obtained by burning a portion of the available product gas. In this process, to be sure, as is the case with the autothermal process, only part of the coal is ultimately converted into available gas, but the other disadvantages described above of the autothermal process are avoided.
The process pursuant to the invention is particularly advantageous when the flue gas obtained by burning the product synthesis gas is used for power production, and is preferably used in one or more expansion gas turbines. In such case, the product of the process as a whole is not available product gas but electrical power, and the system as a whole constitutes a power plant. Customarily, in coal-fired power plants the coal is burned and the flue gas used to run the gas turbines or produce steam is obtained directly from that. In comparison, the process pursuant to the invention whereby the coal is first degasified and the gas is then burned would seem at first glance to involve unnecessary extra expense. The process pursuant to the invention, however, does offer substantial advantages over direct coal-burning. Since the synthesis gas produced by degasification is already purified and desulfurized, the flue gases deriving from the subsequent burning of the gas do not require further purification. Since the volume of the synthesis gas is substantially smaller than that of the flue gases, the expense involved in removing dust and sulfur is correspondingly less. While with direct coal burning, flue gas with a high NO x content is produced, with coal gasification, because of the substantially lower temperatures in the gasification reactor, the formation of nitrogen oxides is largely eliminated, and even the subsequent burning of the synthesis gas can be controlled in such a way that nitrogen oxide formation is substantially lower than with coal burning.
The process pursuant to the invention thus proves to be particularly sound from an environmental standpoint. A power plant operating with such a process can thus be run in whole or in part even on fuels that contain heavy amounts of pollutants. In particular, solid household or industrial refuse, waste oil or the like, if necessary with an appropriate admixture of coal, can be fed into the reactor. The pollutants contained in them remain for the most part in the solid slag removed from the reactor. To the extent that they are transferred to the product gas, they are separated by gas purification before the burning step, so that flue gas purification is no longer necessary. Such a power plant can therefore be built in or near residential areas, which is advantageous with respect to the power-heat connection.
Accordingly a further object of the invention is to provide a process which efficiently gasifies carbon-containing fuel, and a device for performing that process which is simple in design, rugged in construction and economical to manufacture.
The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and specific object attained by its uses, reference is made to the accompanying drawings and descriptive matter in which preferred embodiments of the invention are illustrated.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a flow chart of the process pursuant to the invention where the synthesis gas is used for power production;
FIG. 2 is a similar flow chart to that of FIG. 1, but for different embodiment of the invention.
FIG. 3 is a flow chart of a different embodiment of the process with several gasification reactors connected in series; and
FIG. 4 is a flow chart for another embodiment of the process pursuant to the invention where the synthesis gas is used to produce ammonia.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the drawings in particular, the invention embodied therein comprises a process and device for the gasification of carbon-containing fuel, in particular coal.
Coal ground in a coal mill A is conveyed via an appropriate system of locks (with the aid of a propellant gas) to a fluidized bed reactor B. The coal is gasified allothermally in the reactor by means of a steam/flue gas mixture (primarily steam) produced in a combustion chamber H and conveyed to the reactor B via line 22. The required reaction heat is supplied by indirect heat exchange with flue gas, which flows through a heating coil or heat exchanger 25.
The synthesis gas leaving the reactor B via line 1 is freed of dust in a cyclone separator C and corresponding filter devices. Via line 2, the gas (at 800°-900° C.) enters a waste-heat boiler D and leaves it via line 3, in order to be cooled in a condenser E to the point that it can enter a suitable sulfur scrubber F over a line 4.
The desulfurized gas leaving the sulfur scrubber F goes via line 5 to a combustion chamber G, where it is burned sub-stoichiometrically to the point where the resulting flue gas is at a temperature of approx. 900° C. This flue gas enters the heat exchanger 25 of the reactor B.
In reactor B, the amount of heat required for the gasification reaction is taken from the flue gas (a portion of the heat supply also comes from the steam/flue gas mixture from H). The flue gas leaving the reactor via line 8 at, for instance, 750°-800° C. enters a burner heat exchanger chamber I, where it serves to reheat the flue gas proceeding via line 10 from the first step J 1 to the second step J 2 of an expansion turbine. The flue gas leaving the burner/heat exchanger chamber I via line 9 enters the first step J 1 of the expansion turbine at a pressure of, for example, 40 bar. The flue gas leaving the second step J 2 via line 11 at, for example, a final pressure of 1.2 bar and a temperature of 250° C. is first fed into a heat exchanger R to superheat the steam and then cooled in a waste-heat boiler L and fed to a boiler feed-water preheater M after a line 12 and subsequently to a chimney via line 13.
The steam produced in the waste-heat boilers L and D is collected in a steam collecting drum N and superheated in R. The steam is then expanded through a steam turbine O, which drives a generator S. The condensation heat of the expanded steam is conveyed to a cooling tower P over a line 20 and and via line 15 to a condensate treatment unit Q, as is the condensate from E via line 14. The treated condensate is then fed back into the process via line 19. The feed water conveyed via line 16 from the preheater M is used for steam production.
A portion of the steam leaving the steam collecting drum N is conveyed via line 17 to the combustion chamber H, where the steam is directly mixed, and thereby superheated, with hot flue gas that is derived from the combustion of a portion of the synthesis gas that comes from line 5, is conveyed via line 6 to the combustion chamber and is burned with combustion air from compressor K.
Combustion in H should preferably be stoichimetric, but can also be sub-stoichiometric. If the operating method is sub-stoichiometric, the free oxygen serves to provide additional heat by the combustion of C or CO in the reactor B via the coal feed line (by using air as the propellant gas).
The quantity of free oxygen that should be supplied to the reactor B with the air must be optimized in any case (e.g. the greater the quantity of oxygen that is brought into the process in the air, the greater the quantity of N 2 in the synthesis gas and hence the greater must be the design capacity of units C, D, E and F; conversely, however, the heat exchanger in B can be designed smaller).
In such cases, therefore, a certain amount of autothermal heat production takes place in the reactor B, which can also affect the composition of the gas. This amount, however, is so small in any case that the process does not lose its overall allothermal character.
A further portion of the synthesis gas from line 5 can be fed to the burner/heat exchanger chamber I via line 7, where it is burned and produces extra hot flue gas, which is mixed with the flue gas from 8, so that the temperature of the flue gas fed into the gas turnbine J 1 can be raised again to, for example, 900°-1000° C. Higher temperatures than that are generally inappropriate because of the heat stress on the turbine blades.
The expansion turbines J 1 and J 2 that admit the flue gas drive a generator T to produce electric current. In addition, the turbines may drive compressor K that compresses the combustion air that is fed to combustion chambers G and H via line 21 to, for example, 40 bar, whereby the air is simultaneously heated to a temperature of over 600° C., for example.
The flue gas produced in combustion chamber G is involved only in an indirect heat exchange with the reactor B. It is advantageous to have the combustion in the combustion chamber G carried out under heavily superstoichiometric conditions so that, first of all, the volume of the gas is greater and the energy release in the expansion turbines J 1 , J 2 is correspondingly increased and, secondly, the gas exiting the heat exchanger 25 via line 8 still carries surplus air for the combustion of the additional synthesis gas fed to the burner/heat exchange chamber I via line 7.
With the system described, which is used for power production, efficiencies (terminal output) of 42-45% can be achieved, depending on the application.
The advantages of this combined power plant in comparison with convetional coal-fired systems with the flue gas desulfurization can be summarized as follows:
(a) better efficiencies;
(b) lower cost of producing electric current;
(c) substantially lower water requirements;
(d) reduced heat losses; and
(e) possibility of locating the plant in the vicinity of environmentally-protected districts.
If gasification in the reactor B is performed at temperatures of between 700° and 800° C. and at pressures of around 40 bar, one can obtain per ton of coal about 3,200 m 3 of product gas with approximately the following composition (% by volume): 58% H 2 , 2% CO, 30% CO 2 , 10% CH 4 . The CO 2 content can be eliminated by a CO 2 scrubber, and the proportions of H 2 and CH 4 increased to 83% and 14% by volume, respectively, which means that a conversion step can be eliminated that is necessary as a rule with gas obtained by autothermal gasification. The fact that no oxygen is required for the gasification is another considerable advantage over autothermal processes. For combustion in the combustion chambers approximately 1/3rd of the quantity of gas is required, so that about 2,000 m 3 of gas per ton of coal are available for combustion in the heat exchanger chamber I or for other purposes.
In the embodiment shown in FIG. 2, which differs in some details, the process works as follows:
After milling and drying (M1), the prepared coal is blown into the gasifier (V1), where it is up to 97% gasified in a fluidized bed with the aid of steam. The steam enters the gasifier at a temperature of 850° C., after it has passed through the heat exchanger W14 in the combustion chamber BK1. The heat required for gasification is fed to the reaction chamber via the heat exchanger W17. The ashes and the residual carbon (ungasified coal) are discharged via a cellular wheel sluice and a system of locks (M2).
The raw gas leaving the gasifier V1 via a double cyclone (Z1/Z2) is cooled by passing through the raw gas cooling train W1 to W7 and in the quencher T3, whereby the water vapor is condensed out of the raw gas and the evaporation heat is thus utilized. The condensate is fed to a water treatment unit and is returned to the process via a boiler feed water treatment. The use of process water is thereby reduced to a minimum. The cooling train W1 to W6 is used to produce intermediate pressure steam at drum T1 (25 bar) or low-pressure steam at drum T2 (3.6 bar). The cooled raw gas is fed to a sulfur scrubber. This scrubber operates according to an oxidative process. The H 2 S contained in the raw gas is converted directly into S by means of air (LO-CAT process). The sulfur can be removed in solid form.
Via the heat exchangers W7 and W16, a portion of the now purified raw gas (synthesis gas) goes to the burner of the combustion chamber BK1. In this combustion chamber, the synthesis gas is burned with air coming from the compressor K1/2, in order to enter the heat exchanger W17 of the gasifier V1 at a temperature of 950° C., after raw gas (F2/K3) or steam (from T1) recirculated in the heat exchangers W15 or W16 has been heated to 850° C.
The air/flue gas mixture leaves reactor W17/V1 at a temperature of 800° C. After passing through heat exchanger W16, it enters the first step GT1 of the expansion turbine GT at 760° C. In GT1, pressure is reduced from 20 bar to 7.5 bar. The off gas from GT1 goes to a combustion chamber BK2, which is hooked up upstream of the second step, GT2 and heated with another portion of the synthesis gas, and the off gas is again heated up (reheating). In the turbine or turbine step GT2, pressure is reduced to 3 bar. In combustion chamber BK3, the rest of the synthesis gas is burned with the residual oxygen in the flue gas from GT2 (2nd reheating). In turbine GT3 pressure is dropped to 1.05 bar.
The flue gas leaving the expansion step GT3 at approximately 600° C. enters a flue gas cooler WR with heat exchangers W9 to W13. In drum and heat exchanger combination T5/W10, high-pressure steam (45 bar) is produced that is superheated in W9 to 480° C. In combination T4/W12, low-pressure steam (3.6 bar) is produced. The flue gas leaves WR after an economizer W13 at 105° C.
Both the high-pressure and the low-pressure steam from T2 or T4 are fed into a steam turbine DT1. Both steam turbine and the GT1 as well drive the compressor K/2. Both gas turbine steps GT2 and GT3 are coupled with a generator G. The condensate from the steam turbine DT1 is cooled by means of a cooling tower KTL and pumped back into the cycle.
For structural and operational reasons, the size and hence the capacity of the gasification reactor B or V1 in the embodiments pursuant to FIGS. 1 and 2 are necessarily limited, which means that the quantity of energy produced or the output of the power plant is limited as well. The process, however, can readily be expanded for greater capacity by using several gasifiers. An example of such an embodiment is shown in FIG. 3.
The mixture of air and flue gas exiting the first gas producer V1 enters the combustion chamber BK2 of the second gas producer V2 at 800° C. There the air/flue gas mixture is reheated by combustion of a portion of the synthesis gas, the flue gas and steam are heated to 880° C., and the flue gas, which still has a high oxygen content, is fed to the heat exchanger of the second gasifier V2 at 950° C. This process can be repeated with additional gasifiers V3 and V4 and burners BK3 and BK4, i.e. repeated four times, for example, using as a basis the data given in FIG. 1. The four gasifiers are thus hooked up in parallel with respect to fuel feed and synthesis gas discharge, but in series with respect to flue gas feed to the heat exchangers.
The flue gas (with an O 2 content of 6%) exiting the last heat exchanger is fed to an expansion turbine. This expansion turbine drives the air compressor. The surplus power of 12 MW can be given out (to the network). The flue gas, which still has a temperature of approximately 350° C., is used to produce steam.
The synthesis gas produced is fed into the combustion chamber of a gas turbine unit (after desulfurization). Electric power production by means of this combined power plant is similar to that shown in FIG. 2.
If the plant shown in FIGS. 1, 2 or 3 is run with less output, surplus synthesis gas can be produced which is put under pressure of, for example, 200 bar via another compressor and conveyed to a storage container (FIG. 3). If electric current production must be increased suddenly, the synthesis gas is expanded out of the storage container into the combustion chamber of the gas turbine. The gas turbine can thus be brought up very quickly. The storage capacity must be great enough that the gasifier can be brought up to full capacity within that space of time.
The invention is not limited to the embodiments described, which are used only for power production. The synthesis gas produced by the coal gasification can also be used as process gas for downstream processes to the extent that it is not burned up in heating the reactor. If the process is altered in this way, the combustion shown in FIG. 1 of the surplus synthesis gas conveyed via line 7 in the heat exchanger I would be eliminated, and instead of that the process gas line of a downstream processing step would be hooked up to line 7. One would continue, however, to use the flue gases leaving the heat exchanger coil of the reactor B via line 8 to perform work in expansion turbines J 1 , J 2 , which could also serve for power production, but at the least for driving the compressor K.
As examples of other uses for the unburned surplus of synthesis gas, we might mention:
USE AS TOWN GAS
After the CO 2 is removed by scrubbing, the product gas produced in the reactor B already meets the specifications for town as in terms of its calorific value. Conversion and methanation are not necessary.
PRODUCTION OF SPONGE IRON
After removal of the CO 2 by scrubbing, the product gas can be fed into the reducing gas circuit of a reduction reactor for sponge iron. Another hook-up with the process schema depicted in the drawing is possible and consists of having the reducing gas circuit flow through a heat exchanger coil placed in the heat exchanger chamber I and be thereby heated in an indirect exchange of heat by the flue gases exiting the reactor B.
PRODUCTION OF STEEL
Again in this instance, the product gas is fed via line 7 to a reduction reactor, which it passes through only once. The furnace gas that results in the reduction reactor can be fed to the heat exchanger chamber I and there burned, so that exta hot flue gas is obtained to be admitted into the expansion turbines J 1 , J 2 . With the current produced in generators S and T, the sponge iron can be melted together with scrap iron in an electric arc furnace. The result is a mini steel plant, which is suitable for regions with poor quality scrap and poor electric power supply and is particularly safe for the environment.
In addition, the product gas produced in the reactor B is particularly suitable to be methanized for production of SNG or to be converted directly into methanol.
Another example of the use of the synthesis gas is shown in FIG. 4. Here the synthesis gas is used to produce ammonia. In this case, two gasifiers V1, V2 are provided, which are hooked up in series in the same way as described for FIG. 3. Part of the synthesis gas discharged from each gasifier V1, V2 is recycled in order to use the water vapor contained in it as process steam. The rest of the synthesis gas is subjected to a sulfur scrubbing and then to a molecular sieve PSA process, in which the H 2 hydrogen is separated out of the synthesis gas. The remainder of the synthesis gas, consisting primarily of CO 2 is conveyed to the combustion chambers BK1 and BK2 in order to produce the flue gas for the indirect heating of the gasifiers V1, V2.
From the total flue gas discharged from the second gasifier V2, a portion is diverted and conveyed to a combustion chamber BK3, where it is after burned stoichiometrically with a portion of the synthesis gas coming from the molecular sieve PSA process, so that the resulting flue gas now contains essentially only N 2 and CO 2 . After cooling, the CO 2 is removed by a CO-scrubber. The remaining nitrogen is mixed with the hydrogen from the molecular sieve PSA process and condensed by a compressor K to 200 bar, heated and fed to an NH 3 contact reactor KO, where the reaction between hydrogen and nitrogen results in the formation of ammonia, which is then washed out by a NH 3 scrubber.
The process may be taken further by causing the produced ammonia to react with the sulfur derived from the desulfurization of the synthesis gas in order to produce ammonium sulfate. The result is an environmentally safe, artificial fertilizer plant that can also produce process steam and perhaps power as well.
While specific embodiments of the invention have been shown and described in detail to illustrate the application of the principles of the invention, it will be understood that the invention may be embodied otherwise without departing from such principles. | Part of the synthesis gas produced by coal gasification in an allothermically heated fluidized bed reactor is burned after removal of dust and sulfur and serves as a source of energy to heat the reactor by indirect heat exchange and to produce the steam required for the gasification process. The flue gas exiting from the heat exchanger of the reactor can be used to perform work in expansion turbines. The rest of the synthesis gas is available for use in downstream processes, such as iron ore reduction, or can be burned and used to perform work in turbines to produce electric current. The result is a process that is environmentally safer and operates with a better yield than direct coal burning or autothermal coal gasification, but requires no outside source of energy, such as nuclear power, as prior art allothermal coal gasification processes do. | 2 |
FIELD OF THE INVENTION
[0001] The present invention relates to a surgical tool device, kit and method thereof. More particularly, the present invention is directed at a surgical tool device having two different frequency light sources and having a stimulating electrode, a kit and a method thereof for use in performing surgical procedures at or near nerve structures.
BACKGROUND OF THE INVENTION
[0002] Nearly every surgical operation involves establishing some sort of opening or channel to gain access into and around a given surgical target site. Oftentimes, based on the anatomical location of the surgical target site, surgical tools are required to maintain this working channel within a close proximity to various nerve structures and bundles. Accordingly, the surgeon must be diligent in avoiding, or at least in minimizing, any contact with these exposed nerve structures to avoid injuring the exposed nerve structures.
[0003] Therefore, a need exists for a new and improved dual frequency LED/electrode surgical device having a low frequency LED, a high frequency LED and a stimulator electrode. In this respect, the dual frequency LED/electrode surgical device according to the present invention substantially departs from the conventional concepts and designs of the prior art, and in doing so provides an apparatus primarily developed for the purpose of providing a convenient means for making it possible to promoting healing and sanitizing a surgical wound as well as providing a means for identifying a particular nerve structure.
SUMMARY OF THE INVENTION
[0004] The present device, kit and method of using, according to the principles of the present invention, overcomes a number of the shortcomings of the prior art by providing a novel dual frequency LED/electrode surgical device, kit and method for use in promoting healing and sanitizing a surgical wound as well as providing a means for identifying a particular nerve structure. The device includes a probe having a low frequency LED, a high frequency LED and a stimulator electrode. The kit includes the un-interconnected elements of the device. The method includes the steps of adjoining, affixing, attaching, and obtaining.
[0005] The present invention provides an improved dual frequency LED/electrode surgical device, which will be described subsequently in great detail, that provides a new and improved dual frequency LED/electrode surgical device which is not anticipated, rendered obvious, suggested, or even implied by the prior art, either alone or in any combination thereof.
[0006] The present invention essentially comprises a dual frequency LED/electrode surgical device that includes a probe assembly coupled to a handle assembly. The probe assembly has a low frequency light emitting diode (LED), a high frequency LED, and a stimulator electrode. The low frequency LED is used to thought to promote healing and the high frequency LED is thought to promote a microbe free surgical area. The handle assembly has a system on a chip (SOC) electrically coupled to the low frequency LED, to the high frequency LED, and to the stimulator electrode. The kit includes the unattached components of the device and may also include an detector electrode probe along with an optional monitoring system. The method includes the steps of adjoining, affixing, attaching, and obtaining.
[0007] 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 of the art may be better appreciated.
[0008] The invention of the device may also optionally include a plurality of control switches and a power supply. The invention of the kit may also optionally include a detector electrode probe, a cable, and a monitoring system. The invention of the method may also optionally include the steps of aligning, dispensing, displaying, emitting, irradiating, inserting, making, pressing, pulling, stimulating, and withdrawing.
[0009] The present invention provides a dual frequency LED/electrode surgical device that provides in the apparatuses and methods of the prior art some of the advantages thererof, while simultaneously overcoming some of the disadvantages normally associated therewith.
[0010] Also the present invention provides a kit comprising the non connected components of the dual frequency LED/electrode surgical device.
[0011] Lastly, the present invention provides a new and improved method of using comprising the steps of adjoining, affixing, attaching, and obtaining.
[0012] Numerous other features and advantages of the present invention will be readily apparent to those of ordinary skill in the art upon reading of the following detailed description of presently preferred, but nonetheless illustrative, embodiments of the present invention when taken in conjunction with the accompany drawings. In this respect, before explaining the current embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and to the arrangements of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments and of being practiced and carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein are for the purpose of description and should not be regarded as limiting.
[0013] 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.
[0014] Further, the purpose of the foregoing abstract is to enable the U.S. Patent and Trademark Office and the public generally, and especially the scientist, engineers and practitioners in the art who are not familiar with patent or legal terms or phraseology, to determine quickly from a cursory inspection the nature and essence of the technical disclosure of the application. The abstract is neither intended to define the invention of the application, which is measured by the claims, nor is it intended to be limiting as to the scope of the invention in any way.
[0015] These and other features of the invention, along with the various features of novelty that characterize the invention, are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be had to the accompanying drawings and description matter in which there are illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The invention will be better understood will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
[0017] FIG. 1 is a perspective view of an embodiment of the surgical tool device constructed in accordance with the principles of the present invention;
[0018] FIGS. 2A , 2 B, and 2 C depict various probe assembly designs of the surgical tool device of the present invention;
[0019] FIGS. 3A , 3 B, and 3 C depict a close up partial view of some of the various engagement surfaces of the probe assembly 12 of the surgical tool device 10 ;
[0020] FIG. 4 depicts a perspective view of an assembled kit of the surgical tool device;
[0021] FIG. 5 depicts a logical communication scheme of the surgical tool device;
[0022] FIG. 6 depicts a logical communication scheme of the kit for the surgical tool device; and
[0023] FIGS. 7A , 7 B, 7 C, 7 D, 7 E, 7 F, 7 G, 7 H, and 7 I depict various electronic schemes for driving the low and high frequency LEDS of the surgical tool device.
[0024] The same reference numerals refer to the same parts throughout the various figures.
DETAILED DESCRIPTION
[0025] The following detailed embodiments presented herein are for illustrative purposes. That is, these detailed embodiments are intended to be exemplary of the present invention for the purposes of providing and aiding a person skilled in the pertinent art to readily understand how to make and use of the present invention.
[0026] Accordingly, the detailed discussion herein of one or more embodiments is not intended, nor is to be construed, to limit the metes and bounds of the patent protection afforded the present invention, in which the scope of patent protection is intended to be defined by the claims and their equivalents thereof. Therefore, embodiments not specifically addressed herein, such as adaptations, variations, modifications, and equivalent arrangements, should be and are considered to be implicitly disclosed by the illustrative embodiments and claims described herein and therefore fall within the scope of the present invention.
[0027] Further, it should be understood that, although steps of various the claimed method may be shown and described as being in a sequence or temporal order, the steps of any such method are not limited to being carried out in any particular sequence or order, absent an indication otherwise. That is, the claimed method steps are to be considered to be capable of being carried out in any sequential combination or permutation order while still falling within the scope of the present invention.
[0028] Additionally, it is important to note that each term used herein refers to that which a person skilled in the relevant art would understand such term to mean based on the contextual use of such term herein. To the extent that the meaning of a term used herein, as understood by the person skilled in the relevant art based on the contextual use of such term, differs in any way from any particular dictionary definition of such term, it is intended that the meaning of the term as understood by the person skilled in the relevant art should prevail.
[0029] Furthermore, a person skilled in the art of reading claimed inventions should understand that “a” and “an” each generally denotes “at least one,” but does not exclude a plurality unless the contextual use dictates otherwise. And that the term “or” denotes “at least one of the items,” but does not exclude a plurality of items of the list.
[0030] Unless otherwise defined, all scientific and technical terms used herein are to be construed as having the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present document, including definitions, will control. Unless otherwise indicated, materials, methods, and examples described herein are illustrative only and not intended to be limiting.
[0031] It will be understood that light will be defined herein as an electromagnetic radiation ranging from infrared, visible to ultraviolet wavelengths. Accordingly, the term light will be defined as any electromagnetic radiation ranging between about 250 nm to 1,500 nm.
[0032] It will be understood that a photosensitizer will be defined herein as a chemical compound that produces a biological effect upon photoactivation, or a biological precursor of a compound that produces a biological effect upon photoactivation. The photosensitizer must have a sufficiently low toxicity to permit administration of the photosensitizer to the patient within an acceptable level of safety. Preferably, the photosensitizer is essentially nontoxic, however due to their polycyclic aromatic nature or their multiple conjugated rings that allow for light absorption, fluorescence, phosphorescence and photoactivation, some of these photosensitizers may exhibit some toxicity.
[0033] Referring now to the drawings, and in particular FIGS. 1 to 7 thereof, one preferred embodiment of the present invention is shown and generally designated by the reference numeral 10 . The same reference numerals refer to the same parts throughout the various figures.
[0034] One preferred embodiment of a surgical tool device 10 comprises a probe assembly 12 coupled to a handle assembly 14 , in which the probe assembly 12 has a low frequency light emitting diode (LED) 16 , a high frequency LED 18 , and a stimulator electrode 20 ; and the handle assembly 14 has a system on a chip (SOC) 22 electrically coupled to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 .
[0035] The low frequency LED 16 may be any commercially available low frequency LED 16 . One embodiment is that the low frequency LED 16 is configured to emit light between red and infrared. One embodiment is that the low frequency LED 16 may be configured to emit monochromatic light within a wavelength range between about 600 nm to about 1000 nm. Another embodiment is that the low frequency LED 16 may be configured to emit a spectral band of light of at least 10 nm wide within a wavelength range between about 600 nm to about 1000 nm. Still another embodiment is that the low frequency LED 16 may be configured to emit light at about 1 μW/cm 2 to about 1 W/cm 2 .
[0036] The high frequency LED 16 may be any commercially available high frequency LED 16 . One embodiment of the high frequency LED 18 is that it is configured to emit light between green and ultraviolet. A more preferred embodiment of the high frequency LED 18 is that it is configured to emit monochromatic light within a wavelength range between about 250 nm to about 550 nm. Another embodiment of the high frequency LED 18 is that it is configured to emit a spectral band of light of at least 10 nm wide within a wavelength range between about 250 nm to about 550 nm. Still another embodiment is that the high frequency LED 18 is that it is configured to emit light at about 1 μW/cm 2 to about 1 W/cm 2 .
[0037] The probe assembly 12 of the surgical tool device 10 may be shaped and designed in any configuration suitable for surgical purposes. One preferred embodiment of the shape of the probe assembly is that it has an arcuate engagement surface 28 .
[0038] The stimulator electrode 20 may be powered by AC or DC current or voltage signals driven and coordinated by the SOC.
[0039] Another embodiment of the surgical tool device 10 comprises the probe assembly 12 having the low frequency LED 16 , the high frequency LED 18 , the stimulator electrode 20 and the SOC 22 attached to the probe assembly 12 . The SOC 22 is electrically coupled to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 . Finally, the handle assembly 14 is attached to the probe assembly 12 .
[0040] An optional plurality of control switches 24 may be added to the surgical tool device 10 . One embodiment of the optional control switches is that it is attached to the handle so that the control switches 24 are electrically coupled to the SOC 22 , to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 .
[0041] An optional power supply 26 may be added to the surgical tool device 10 . One embodiment is that the optional power supply 26 is attached to the handle so that the power supply 26 is electrically coupled to the SOC 22 , to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 . The power supply is selected from the group consisting of a battery power supply and a high capacity capacitor power supply.
[0042] One preferred embodiment of the kit for the surgical tool device 10 comprises the unattached probe assembly 12 and the handle assembly 14 of the surgical tool device 10 . The probe assembly 12 of the kit has the low frequency LED 16 , the high frequency LED 18 , and the stimulator electrode 20 attached to the probe assembly 12 . The handle assembly 14 is configured to be attached to the probe assembly 12 , in which the handle assembly 14 has an SOC 22 , a a plurality of control switches 24 , and a power supply 26 . The SOC 22 is configured to be electrically coupled to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 . The control switches 24 are attached to the handle, in which the control switches 24 are configured to be electrically coupled to the SOC 22 , to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 . The power supply 26 is attached to the handle, in which the power supply 26 electrically coupled to the SOC 22 , to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 .
[0043] An optional detector electrode probe 30 may be added to the kit for the surgical tool device 10 in which the detector electrode probe 30 is configured to be electrically coupled to the SOC 22 .
[0044] An optional cable 32 may be added to the kit for the surgical tool device 10 in which the cable 32 is configured to electrically couple together the detector electrode probe 30 to the SOC 22 , and to the stimulator electrode 20 .
[0045] An optional monitoring system 34 may be added to the kit for the surgical tool device 10 in which the monitoring system 34 is configured to be electrically coupled to the detector electrode.
[0046] One preferred embodiment of a method of using a kit for the surgical tool device 10 comprising the steps of adjoining, affixing, attaching, and obtaining. The step comprises obtaining the kit comprising: a probe assembly 12 having: a low frequency light emitting diode (LED) 16 attached to the probe assembly 12 ; a high frequency LED 18 attached to the probe assembly 12 ; and a stimulator electrode 20 attached to the probe assembly 12 ; a handle assembly 14 configured to be attached to the probe assembly 12 , the handle assembly 14 having: a system on a chip attached to the handle, the SOC 22 configured to be electrically coupled to the low frequency LED 16 , to the high frequency LED 18 , and to the stimulator electrode 20 ; a plurality of control switches 24 attached to the handle, the control switches 24 electrically coupled to the SOC 22 ; and a power supply 26 attached to the handle, the power supply 26 electrically coupled to the SOC 22 , and to the control switches 24 ; a detector electrode probe 30 configured to be electrically coupled to the SOC 22 ; a cable 32 configured to electrically couple together the detector electrode probe 30 to the SOC 22 , to the stimulator electrode 20 ; and a monitoring system 34 configured to be electrically coupled to the detector electrode. The attaching step comprises attaching operatively together the probe assembly 12 to the handle assembly 14 so that the SOC 22 is electrically coupled to the low frequency LED 16 , to the high frequency LED 18 , to the stimulator electrode 20 , to the power supply 26 , and to the control switches 24 . The adjoining step comprises adjoining operatively together the cable 32 to the handle and to the detector electrode so that the SOC 22 is electrically coupled to the detector electrode. The affixing step comprises affixing together the detector electrode to the monitoring system 34 so that the detector electrode and the stimulator electrode 20 are operatively coupled to the monitoring system 34 .
[0047] The medical procedure supported by this method may be anyone of the following surgical procedures and non-surgical procedures, such as, endoscopic procedures, fluoroscopic procedures, stent delivery procedures, aortic aneurysm repairs, cranial aneurysm repairs, delivery of drugs, delivery of biological agents, cardiac surgery with cardiopulmonary bypass circuits, cardiac surgery without cardiopulmonary bypass circuits, brain surgery, cardiograms, heart valve repair, heart valve replacement, revascularization procedures, transmyocardial revascularization, percutaneous myocardial revascularization, anstomosis procedures, beating heart surgery, vascular surgery, neurosurgery, electrophysiology procedures, dianostic procedures, therapeutic procedures, ablation procedures, ablation of arrhythmias, endovascular procedures, treatment of the liver, treatment of the spleen, treatment of the heart, treatment of the lungs, treatment of major blood vessels, noninvasive procedures, invasive procedures, imaging procedures, CAT scan procedures, MRI procedures, gene therapy procedures, cellular therapy procedures, cancer therapy procedures, radiation therapy procedures, transplantation procedures, coronary angioplast procedures, atherectomy procedures, atherosclerotic place removal procedures, birthing procedures, spinal cord procedures including intrathecal access, epidural access and transcutaneous access.
[0048] An optional set of steps may be added to the method to further comprise the steps of aligning, dispensing, displaying, emitting, irradiating, inserting, making, pressing, pulling, stimulating, and withdrawing. The making step comprises making a opening into flesh near a nerve. The dispensing step comprises dispensing an aliquot of a photosensitizer into the opening. The inserting step comprises inserting the probe assembly 12 into an opening. The aligning step comprises aligning the probe adjacent to the nerve while the probe is inserted into the opening. The pressing step comprises pressing on one control switch 24 to activate the stimulator electrodes 20 to produce electrical impulses while the probe is aligned adjacent to the nerve. The stimulating step comprises stimulating the nerve with the electrical impulses. The displaying step comprises displaying a response of the detector electrode while stimulating the nerve to identify the nerve and to verify the alignment of the probe. The irradiating step comprises irradiating low frequency light from the low frequency LED 16 onto the nerve while the probe is aligned next to the nerve. The emitting step comprises emitting high frequency light from the high frequency LED 18 onto the nerve while the probe is aligned next to the nerve. The pulling step comprises pulling the nerve aside with the probe assembly 12 . The withdrawing step comprises withdrawing the probe assembly 12 from the opening.
[0049] Any number of photosensitizers can be used in conjunction in practicing with the claimed method of the present invention. They differ in the properties of light absorption and fluorescence, biodistribution, temporal uptake, clearance, and mechanisms of photoactivatable cytotoxicity. Classes of photosensitizers include acridine dyes, bacteriochlorins, bacteriochlorophylls, chlorins, hematoporphyrins, phthalocyanines, porphyrins, purpurins, naphthalocyanines, non-tetrapyrrole photosensitizers, texaphyrins, uroporphyrins.
[0050] Referring now to FIG. 1 that depicts a perspective view of an embodiment of the surgical tool device showing the surgical tool device 10 having a probe assembly 12 coupled to a handle assembly 14 . The probe assembly 12 is shown having a low frequency LED 16 , a high frequency LED 18 , and a stimulator electrode 20 . The handle assembly 14 is shown having a system on a chip (SOC) 22 and having plurality of control switches 24 . The SOC 22 of the handle assembly is electrically coupled to the low frequency LED 16 , to the high frequency LED 18 , to the stimulator electrode 20 and to the control switches 24 .
[0051] Referring now to FIG. 2A , 2 B, and 2 C that depict various probe assembly 12 designs of the surgical tool device 10 . The probe assembly 12 is shown having any number of designs, including a curved nerve hook design as in FIGS. 2B and 2C as well as a straight needle design as shown in FIG. 2A . Also shown in FIGS. 2A-2C are the low frequency LED 16 , the high frequency LED 18 , and a stimulator electrode 20 attached to the probe assembly 12 .
[0052] Referring now to FIG. 3A , 3 B, and 3 C that depict a close up partial view of some of the various engagement surfaces 28 of the probe assembly 12 of the surgical tool device 10 . Also shown in FIG. 3A-3C are the low frequency LEDs 16 , the high frequency LEDs 18 , and a stimulator electrodes 20 attached to the probe assembly 12 .
[0053] Referring now to FIG. 4 that depicts a perspective view of an assembled kit of the surgical tool device 10 . The kit is shown to include the surgical tool device 10 having the probe assembly 12 coupled to a handle assembly 14 . The probe assembly 12 is shown having a low frequency LED 16 , a high frequency LED 18 , and a stimulator electrode 20 . The handle assembly 14 is shown attached to the probe assembly 12 and having a plurality of control switches 24 . A cable 32 is shown attached to the handle assembly 14 , to the monitoring system 34 and to the detector electrode probe 30 .
[0054] Referring now to FIG. 5 that depicts a logical communication scheme of the surgical tool device 10 . The SOC 22 is shown to be in operative communication (i.e., electrically coupled to the power supply 26 , to the low frequency LED 16 , to the high frequency LED 18 , to the stimulator electrode 20 and to the control switches 24 .
[0055] Referring now to FIG. 6 that depicts a logical communication scheme of the kit for the surgical tool device. The SOC 22 is shown to be in operative communication (i.e., electrically coupled) to the power supply 26 , to the low frequency LED 16 , to the high frequency LED 18 , to the stimulator electrode 20 , to the control switches 24 . The SOC 22 is also shown to be in operative communications, via the cable 32 , with the detector electrode probe 30 and with the monitoring system 34 .
[0056] Referring now to FIGS. 7A , 7 B, 7 C, 7 D, 7 E, 7 F, 7 G, 7 H, and 7 I that depict various electronic schemes for driving the low and high frequency LEDS of the surgical tool device. The power supply 26 is shown to be in operative communication (i.e., electrically coupled) with the low frequency LEDs 16 and the high frequency LEDs 18 .
[0057] As to the manner of usage and operation of the present invention, the same should be apparent from the above description. Accordingly, no further discussion relating to the manner of usage and operation will be provided.
[0058] While a preferred embodiment of the dual frequency LED/electrode surgical device has been described in detail, it should be apparent that modifications and variations thereto are possible, all of which fall within the true spirit and scope of the invention. With respect to the above description then, it is to be realized that the optimum dimensional relationships for the parts of the invention, to include variations in size, materials, shape, form, function and manner of operation, assembly and use, are deemed readily apparent and obvious to one skilled in the art, and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention.
[0059] Throughout this specification, unless the context requires otherwise, the word “comprise” or variations such as “comprises” or comprising or the term “includes” or variations, thereof, or the term “having” or variations, thereof will be understood to imply the inclusion of a stated element or integer or group of elements or integers but not the exclusion of any other element or integer or group of elements or integers. In this regard, in construing the claim scope, an embodiment where one or more features is added to any of the claims is to be regarded as within the scope of the invention given that the essential features of the invention as claimed are included in such an embodiment.
[0060] Those skilled in the art will appreciate that the invention described herein is susceptible to variations and modifications other than those specifically described. It is to be understood that the invention includes all such variations and modification which fall within its spirit and scope. The invention also includes all of the steps, features, compositions and compounds referred to or indicated in this specification, individually or collectively, and any and all combinations of any two or more of said steps or features.
[0061] Therefore, the foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention. | A surgical tool device, a kit and a method are described which provide a novel dual frequency LED/electrode scheme for use in manipulating nerve and innervated structures. The surgical tool device includes a probe assembly coupled to a handle assembly. The probe assembly has a low frequency light emitting diode (LED), a high frequency LED, and a stimulator electrode. The low frequency LED is used to promote healing and the high frequency LED is to aid in promoting a microbe free surgical area. The handle assembly has a system on a chip (SOC) electrically coupled to the low frequency LED, to the high frequency LED, and to the stimulator electrode. The kit includes the unattached components of the device and may also include an detector electrode probe along with an optional monitoring system. The method includes the steps of adjoining, affixing, attaching, and obtaining. | 0 |
[0001] The present invention relates generally to the field of subsea pipelines and manifolds, and in particular, to the field of subsea fluid connections having check valves. Even more particularly, the present invention relates to subsea connections having integral surplussing check valves with variable cracking pressure.
INTRODUCTION
[0002] Often, hydrocarbons, such as oil and gas, are deposited in rock formation located beneath the seabed. Thus, in order to explore and produce the hydrocarbons, wellbores, associated ancillary equipment and pipelines have to be installed subsea. The wellbore- and ancillary equipment, such as seabed pipelines and pigging equipment (Pipeline Inspection Gauge), generally require the use of high-pressure lines/hoses, couplings and valves, in order to manage fluid flow (e.g. hydrocarbons, drilling fluids etc.) between the reservoir and/or subsea production facilities. The extreme deep-sea pressures the equipment may be exposed to during deep-water operations, can pose considerable challenges to developers and engineers alike.
[0003] FIG. 1 shows a simplified example of a typical offshore setup for servicing pipelines or other subsea equipment using a surface vessel 10 and a hose 12 . In this particular example, pigging operations may be conducted on pipelines 14 that have been laid on the seabed 16 and which have an internal pressure at atmospheric pressure. Here, the labels P h-1 , P h-2 , P h-3 , P h-4 illustrate the hydrostatic pressure at various depths subsea. Understandably, the hydrostatic pressure P h-4 is considerably higher than the hydrostatic pressure P h-1 . Given that the inner pressure of the pipeline 14 is at atmospheric pressure, there may be a significant pressure differential between the pipeline interior and P h-4 . Consequently, before it is possible to inspect, clean or flush the pipeline 14 , it would need to be flooded in order to equalise the internal pressure (at atmospheric pressure) with the external deep-water pressure P h-4 . Flooding of the pipeline is usually achieved by a hose 12 that is extended from the surface vessel 10 and through which filtered seawater and/or cleaning chemicals are supplied into the pipeline 14 . The extended hose 12 is under an internal pressure that is suitable to withstand the external deep-water pressure (P h-1 to P h-4 ) and therefore prevent hose collapse. When the hose 12 is opened to the pipeline 14 , the considerable pressure differential causes the fluid to rush into the pipeline 14 . The extreme fluid flow and instant loss of internal hose pressure, as well as the considerable external hydrostatic pressure P h-1 , P h-2 , P h-3 , P h-4 may cause the hose 12 to collapse. The hose collapse may be prevented by using a hose 12 that is strong enough to withstand the external hydrostatic pressure, but such hoses are likely to be significantly more expensive than an ordinary hose. Also, the depths at which pipelines 14 are laid today are exceeding the capacity of even the best anti-collapse hoses currently available, so that using stronger hoses is neither viable nor cost-effective.
[0004] Therefore, in order to prevent or at least minimise the risk of hose collapse during pipeline flooding, check valves 20 , such as the Moffat Surplussing Valve™ are used. Typical embodiments of such a check- or surplussing valve are shown in FIGS. 2 ( a ), ( b ) and ( c ). The surplussing valve 20 is bubble tight in its reverse fluid flow direction, allowing the hose 12 to be deployed with an internal hose pressure applied to balance the respective external hydrostatic pressures P h-1 , P h-2 , P h-3 , P h-4 . As shown in the schematic cross section of FIG. 2 ( a ), the check valve 20 is specifically designed to only allow fluid flow in the forward direction at a predetermined fluid pressure, also known as “cracking pressure”. In particular, the cracking pressure is predetermined by the spring 22 , and the valve member 24 is moved downstream when the fluid pressure exceeds the cracking pressure, therefore, opening a fluid flow path through the check valve 20 . The internal hose pressure required to prevent hose collapse is directly proportional to the external hydrostatic pressure. Therefore, the cracking pressure of the check valve 20 (i.e. a predetermined spring force provided by spring 22 ) has to be set to a pressure that is suitable at that specific subsea depth.
[0005] For example, the Moffat Surplussing Valve® is manufactured in sizes ranging 1 inch, 2 inch, 3 inch, 4 inch, 6 inch and 8 inch (Nominal Bore), wherein the design pressure of the Moffat Surplussing Valve™ has three main tiers: 414 bar (6,000 psi), 690 bar (10,000 psi) and 1035 bar (15,000 psi), in accordance with typical subsea equipment used in the industry (i.e. flanges, valves, hotstabs etc. are typically pressure rated at 6,000 psi, 10,000 psi or 15,000 psi). Typical “cracking pressures” can be anywhere from 0 to 100 bar (1,450 psi), depending on the subsea depths where the check valve is applied.
[0006] During operation, once the hose 12 is connected to the pipeline 14 via the check valve 20 , the internal hose pressure is raised beyond the predetermined cracking pressure causing the check valve 20 to open and allow fluid flow into the pipeline 14 . However, if the internal hose pressure drops below the cracking pressure, the check valve 20 closes and therefore prevents the hose 12 from collapsing.
[0007] It is understandable that check valves 20 used on pipelines 14 laid at different subsea depths require different “cracking pressures” in order to maintain operability of the check valve 20 , i.e. open and close the valve 20 to flood the pipeline 14 and prevent hose collapse. Consequently, different check valves have to be either made for different hydrostatic pressures, or existing check valves have to be modified to provide a new cracking pressure suitable for the new hydrostatic pressure.
[0008] However, modifying existing check valves or purchasing new check valves suitable for specific hydrostatic pressure ranges can be very time consuming and/or costly. Therefore, it would be desirable to have a check valve that is suitably operable at any hydrostatic pressure.
[0009] Accordingly, it is an object of the present invention to provide a check valve with a self-regulating cracking pressure. It is a further object of the present invention to provide a stab connector incorporating a check valve mechanism with a self-regulating cracking pressure.
SUMMARY OF THE INVENTION
[0010] Preferred embodiments of the invention seek to overcome one or more of the disadvantages of the prior art.
[0011] According to a first aspect of the present invention, there is provided a check valve assembly for subsea applications, comprising:
a housing, having an inlet port and an outlet port forming an internal fluid passageway through said housing; a valve member, moveable within said internal fluid passageway between a first position, where fluid flow through said internal fluid passageway is prevented, and a second position, where fluid flow through said internal fluid passageway is permitted; a biasing member, adapted to urge said valve member into said first position at a predetermined cracking force, and a pressure interface, operatively linking said valve member and an external fluid of a region exterior of the check valve assembly so as to provide a supplemental force, proportional to the ambient pressure of said external fluid, adapted to urge said valve member towards said first position.
[0016] This provides the advantage that the ambient pressure of the external fluid surrounding the check valve actively adjusts the cracking pressure making it suitably operably at any subsea depth. Therefore, where the prior art had to use various different check valves at different subsea depths, a single check valve can now be suitably used for any subsea depth without having to replace, adjust or retrofit the now inoperable existing check valves. In particular, the constant biasing force provided by the biasing member is set to a force that is suitable at the lowest feasible hydrostatic pressure (i.e. operable with pipelines laid at the lowest possible subsea depths), and the “subsea-depth dependent” variable external hydrostatic pressure actively supplements the constant biasing force of the biasing member so as to provide a check valve cracking pressure operably suitable at that specific subsea-depth. Hence, the check valve can be used at any subsea-depth and automatically adjusts its cracking pressure accordingly.
[0017] Advantageously, the check valve assembly may comprise a valve seat surface formed within said internal passageway coaxially about said inlet port. Furthermore, the valve member may comprise a first surface, adapted to sealingly engage said valve seat surface when in said first position, and a second surface, operatively linked to said pressure interface. Preferably, the first surface may be located on the upstream side of said valve member, and the second surface may be located at an opposing side to said first surface.
[0018] This provides the advantage of a particularly simplistic mechanism that is hard wearing and inexpensive to manufacture.
[0019] The pressure interface may comprise at least one external fluid passageway adapted to provide fluid communication between said external fluid and at least part of said second surface. Preferably, the external fluid may be in direct fluid communication with said at least part of said second surface. Advantageously, the at least one external fluid passageway may be fluidly sealed from said internal fluid passageway.
[0020] This provides the advantage of minimizing the required parts required to provide the pressure interface between the valve member and the external fluid, subsequently minimizing cost of manufacture.
[0021] Alternatively, the pressure interface may comprise an actuator operatively coupled to said valve member and adapted to transfer the force provided by said ambient pressure of said external fluid to said valve member, so as to supplement said predetermined cracking force provided by said biasing member.
[0022] Advantageously, the valve member may further comprise a seal portion at the downstream side and at least one flow portion at the upstream side of said valve member, the seal portion being engageable with said housing to prevent fluid flow past said seal portion, and wherein said flow portion is adapted to provide a fluid path between said inlet port and said outlet port. The seal portion may sealingly close said internal fluid path when said valve member is in said first position, and wherein said flow portion provides a flow path through said internal fluid passageway when said valve member is in said second position.
[0023] This provides the advantage to maximise stability of the valve member during operation. In particular, either the flow portion or the seal portion are in engagement with the interior walls of the housing at the first position and second position, providing more stability during the movement of the valve member. Preferably, the biasing member may be a spring.
[0024] The check valve assembly may further comprise a snap-action mechanism adapted to independently move said valve member into said first position and/or said second position at a predetermined condition. Advantageously, the predetermined condition may be a predetermined distance between the valve member and said first position and/or said second position. Even more advantageously, the snap-action mechanism may comprise at least one magnetic element adapted to provide a force acting on said valve member so as to urge said valve member towards said first position and/or said second position.
[0025] This provides the advantage of minimizing potential ‘chatter’ of the valve member at low pressure differentials, i.e. low subsea depths.
[0026] According to a second aspect of the present invention, there is provided a stab connector for providing a fluid flow path between a first fluid reservoir and a second fluid reservoir, comprising:
a stab body coupleable to a receptacle in fluid communication with the second fluid reservoir, and a check valve assembly according to the first aspect of the present invention, operatively arranged within said stab body and adapted to control fluid flow between the first fluid reservoir and the second fluid reservoir.
[0029] This provides the advantage that hoses fitted with the stab connector of the second aspect of the present invention are automatically protected from potential collapse in the event of an excessive pressure loss from the hose when connecting to a pipe that has an interior pressure set at approximately atmospheric pressure. Advantageously, the pressure interface of said check valve assembly may be arranged within the distal end portion of said stab body. Even more advantageously, the pressure interface may be fluidly sealed from the first and second fluid reservoir.
BRIEF DESCRIPTION OF THE DRAWINGS
[0030] A preferred embodiment of the present invention will now be described, by way of example only and not in any limitative sense, with reference to the accompanying drawings, in which:
[0031] FIG. 1 shows an example of a typical offshore setup when servicing a pipeline, either for installation, repair or pigging utilizing a flexible hose that is extended from a surface vessel;
[0032] FIG. 2 shows (a) a cross section of a known Surplussing Valve™ (Moffat 2000 Ltd) as currently used to prevent subsea hose collapse, and (b) a typical embodiment of the Surplussing Valve™, as well as, (c) the embodiment complete with Female FIG. 1502 Hammer-Lug Union on the inlet and a Male FIG. 1502+Nut on the outlet;
[0033] FIG. 3 shows a cross section of a preferred embodiment of the check valve assembly of the present invention;
[0034] FIG. 4 shows a functional diagram of the check valve assembly of FIG. 3 when (a) in its closed state, and (b) in its open state;
[0035] FIG. 5 shows a cross section of an alternative embodiment of the check valve assembly of the present invention;
[0036] FIG. 6 shows a functional diagram of the check valve assembly of FIG. 5 when (a) in its closed state, and (b) in its open state;
[0037] FIG. 7 shows a cross section of an exemplary stab connector incorporating the check valve assembly of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0038] In accordance with the preferred first embodiment of the present invention, FIG. 3 depicts a check valve assembly 100 having a housing 102 , an inlet port 106 , an outlet port 108 , a biasing member 110 in form of a compression spring, a valve member 112 and corresponding valve seat surface 114 , as well as a pressure interface 116 linking the pressure provided by the external fluid with a contact surface of the valve member 112 . Sealing members 118 are arranged in the housing 102 and valve member 112 so as to fluidly seal the fluid flow path between inlet port 106 and outlet port 108 when the valve member 112 is in its closed position, and to fluidly seal the fluid flow path between the inlet port 106 and the outlet port 108 from the pressure interface linking the valve member 112 with the pressure provided by the external fluid, independent of the position of the valve member 112 .
[0039] FIG. 4 ( a ) shows the check valve assembly 100 in situ (connecting hose and pipeline not shown) with the hose fluid 120 pressing against an upstream surface of the valve member 112 with an internal hose pressure P 1 provided by a pump (not shown) that is connected to the hose (not shown). A constant biasing force, such as a spring force F s provided by the compression spring 110 , urges the valve member 112 towards the valve seat surface 114 , so as to seal the fluid flow path between the inlet port 106 and the outlet port 108 . In this particular example, the compression spring 110 is operatively arranged between a downstream surface 122 of the valve member 112 and an interior wall 124 of the housing 102 . The pressure interface 116 , linking the external fluid (not shown) with the valve member 112 , is in form of an open external fluid path between the external fluid (not shown) and the downstream surface 122 of the valve member 112 . In accordance with Pascal's law, the hydrostatic pressure P h-x at the subsea depth X is applied directly to the downstream surface 122 of the valve member, so as to supplement the constant spring force F s provided by the compression spring 110 . Therefore, the cracking pressure P c (x) the hose fluid 120 has to overcome at the subsea depth X to open the fluid flow path of the check valve assembly 100 is determined by the force F h (x) provided by the hydrostatic pressure P h-x at subsea depth X acting on the downstream surface 122 of the valve member 112 , the spring force F s (constant) provided by the compression spring 110 and the internal pressure of the pipeline P 1 (assumed constant) acting on the downstream surface 122 .
[0000] P c ( x )= F h ( x )+ F s +P 1 [1]
[0040] In order to prevent hose collapse, the hose is pressurized at an internal hose pressure P 1 that is directly proportional to the hydrostatic pressure P h-x . Hence, the cracking pressure Pc(x) is proportional to the internal hose pressure P 1 at subsea depth X, therefore, automatically providing the appropriate cracking pressure P c suitable for the internal hose pressure P 1 at subsea depth X. Any significant pressure drop in the hose (not shown) that reduces P 1 to below P c (x), causes the valve member 112 to move back into its closed position, therefore preventing the hose to collapse.
[0041] In accordance with an alternative second embodiment, FIG. 5 depicts a check valve assembly 200 comprising a housing 202 , an inlet port 206 , an outlet port 208 , a biasing member 210 in form of a compression spring, a valve member 212 , a valve seat surface 214 , a pressure interface 216 , sealing members 218 and a downstream surface 222 . In this particular embodiment, the inlet port 206 and outlet port 208 of the check valve assembly 200 are arranged perpendicular to each other. The pressure interface 216 is arranged in line with the inlet port 206 so that the valve member 212 can move between a closed position, where the fluid flow between inlet port 206 and outlet port 208 is prevented, and an open position, where fluid flow between inlet port 206 and outlet port 208 is permitted. FIG. 6 shows the alternative check valve assembly 200 in situ (without hose and pipeline attachments) (a) in its closed position, where the internal hose pressure P 1 is less than the cracking pressure Pc(x) provided at subsea depth X, and (b) in its open position, where the internal hose pressure P 1 exceeds the cracking pressure P c (x) at subsea depth X.
[0042] During operation, the internal hose fluid 220 provides a pressure P 1 against the valve member 212 . As soon as P 1 exceeds a cracking pressure P c (x), which is determined by a force F h (X) provided by the hydrostatic pressure P h-x at subsea depth X acting on the downstream surface 222 of the valve member 212 and the spring force F s provided by the compression spring 210 , the valve member 212 is moved into its open position so as to provide a fluid flow path between the inlet port 206 and the outlet port 208 . The cracking pressure P c (x) does not include the internal pipeline pressure P 1 , because the outlet port 208 is perpendicular to the inlet port 206 and pressure interface 216 . Any significant pressure drop in the hose reducing P 1 to below P c (x), causes the valve member 212 to move back into its closed position, therefore preventing the hose to collapse.
[0000] P c ( x )= F h ( X )+ F s [2]
[0043] Alternatively, the pressure interface 116 , 216 may comprise an actuator (not shown) that is adapted to transfer a force proportional to the hydrostatic pressure P h-x provided by the external fluid (not shown) to act on the valve member 112 , 212 supplementing the biasing force provided by the biasing member 110 , 210 (e.g. spring force provided by a compression spring). The actuator may simply be a plunger arranged within the housing 102 , 202 so as to transfer the hydrostatic pressure P h-x of the external fluid onto the downstream surface 122 , 222 of the valve member 112 , 212 .
[0044] In yet another alternative arrangement, the actuator (not shown) may be an indirect actuator (not shown) which may comprise an external sensor, adapted to measure the hydrostatic pressure of the external fluid and provide a signal to an actuator mechanism that is capable of providing an actuator force F a acting on the downstream surface 122 , 222 of the valve member 112 , 212 to supplement the biasing force of the biasing member 110 , 210 . The actuator force F a generated by the actuator mechanism (not shown) may be proportional to the hydrostatic pressure P h-x of the external fluid.
[0045] In yet another alternative arrangement, the check valve assembly 100 , 200 may comprise a snap-action mechanism (not shown) that is adapted to independently move the valve member 112 , 212 into the open and/or closed position at a predetermined condition. The predetermined condition may be a distant threshold between the valve member 112 , 212 and the final position of the valve member 112 , 212 when in the open position and/or closed position. For example, magnetic elements may be used to provide a pulling force acting on the valve member 112 , 212 towards the open and/or closed portion at a predetermined threshold distance.
[0046] It is understood by the skilled person in the art that the predetermined constant spring force F s provided by the biasing member (e.g. compression spring) 110 , 210 is made suitable to be operable at any subsea depth, so that the check valve assembly 100 , 200 may be reliably used at any subsea depth. It is further understood by the skilled person in the art that the biasing force that is suitable to urge the valve member 112 , 212 toward the valve seat surface 114 , 214 may be provided by any suitable biasing member 110 , 210 .
[0047] FIG. 7 shows an alternative aspect of the present invention in the form of a stab connector 300 that may comprise a check valve assembly in accordance with any one of the first and second embodiment of the present invention.
[0048] In this particular example, the stab connector 300 incorporates a variation of the second embodiment of the check valve assembly 200 within its housing 302 . During operation, the stab connector 300 is coupled to a hose (not shown) and extended to a subsea location, where a diver or Remotely Operated Vehicle (ROV) inserts the stab connector 300 to a female coupling so as to form a fluid path between the hose and the interior of the pipeline. A pressure interface 316 is provided at the distal end of the stab connector 300 such that it is in fluid communication with the external fluid when the stab connector 300 is locked in the female coupling. When the internal hose pressure P 1 exceeds the cracking pressure P c (x) provided by the spring force F s and the hydrostatic pressure P h-x at subsea depth X, the valve member 312 moves into its open position, therefore creating a flow path between the inlet port 306 and the outlet port 308 of the stab connector 300 .
[0049] It will be appreciated by persons skilled in the art that the above embodiments have been described by way of example only and not in any limitative sense, and that various alterations and modifications are possible without departing from the scope of the invention as defined by the appended claims. | A check valve assembly ( 100, 200 ) is provided for subsea applications. The check valve assembly comprises a housing ( 102, 202 ), having an inlet port ( 106, 206 ) and an outlet port ( 108, 208 ) forming an internal fluid passageway through the housing; a valve member ( 112, 212 ), moveable within the internal fluid passageway between a first position, where fluid flow through the internal fluid passageway is prevented, and a second position, where fluid flow through the internal fluid passageway is permitted; a biasing member ( 110, 210 ), adapted to urge the valve member into the first position at a predetermined cracking force, and a pressure interface ( 116, 216 ). The pressure interface operatively links the valve member and an external fluid of a region exterior of the check valve assembly so as to provide a supplemental force, proportional to the ambient pressure of the external fluid, adapted to urge the valve member towards the first position. | 4 |
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0001] The United States Government has rights in this invention pursuant to contract No. DE-AC05-96OR22464 between the United States Department of Energy and Lockheed Martin Energy Research Corporation.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to carbon foam, and more particularly to a process and apparatus for extruding a thermally conductive carbon foam.
[0003] The extraordinary mechanical properties of commercial carbon fibers are due to the unique graphitic morphology of the extruded filaments. See Edie, D. D., “Pitch and Mesophase Fibers,” in Carbon Fibers, Filaments and Composites, Figueiredo (editor), Kluwer Academic Publishers, Boston, pp. 43-72 (1990). Contemporary advanced structural composites exploit these properties by creating a disconnected network of graphitic filaments held together by an appropriate matrix. Carbon foam derived from a pitch precursor can be considered to be an interconnected network of ligaments or struts. As such interconnected networks, they would represent a potential alternative as a reinforcement in structural composite materials.
[0004] Recent developments of fiber-reinforced composites has been driven by requirements for improved strength, stiffness, creep resistance, and toughness in structural engineering materials. Carbon fibers have led to significant advancements in these properties in composites of various polymeric, metal, and ceramic matrices.
[0005] However, current applications of carbon fibers has evolved from structural reinforcement to thermal management in application ranging from high density electronic modules to communication satellites. This has stimulated research into novel reinforcements and composite processing methods. High thermal conductivity, low weight, and low coefficient of thermal expansion are the primary concerns in thermal management applications. See Shih, Wei, “Development of Carbon-Carbon Composites for Electronic Thermal Management Applications,” IDA Workshop, May 3-5, 1994, supported by AF Wright Laboratory under Contract Number F33615-93-C-2363 and AR Phillips Laboratory Contract Number F29601-93-C-0165 and Engle, G. B., “High Thermal Conductivity C/C Composites for Thermal Management,” IDA Workshop, May 3-5, 1994, supported by A F Wright Laboratory under Contract F33615-93-C-2363 and A R Phillips Laboratory Contract Number F29601-93-C-0165. Such applications are striving towards a sandwich type approach in which a low density structural material (i.e. honeycomb or foam) is sandwiched between a high thermal conductivity facesheet.
[0006] Structural cores are limited to low density materials to ensure that the weight limits are not exceeded. Unfortunately, carbon foams and carbon honeycomb materials are the only available materials for use in high temperature applications (>1600° C.). High thermal conductivity carbon honeycomb materials are extremely expensive to manufacture compared to low conductivity honeycombs, therefore, a performance penalty is paid for low cost materials
[0007] Typical foaming processes utilize a “blowing” technique to produce a foam of the pitch precursor. The pitch is melted and pressurized, and then the pressure is reduced. Thermodynamically, this produces a “Flash,” thereby causing the low molecular weight compounds in the pitch to vaporize (the pitch boils), resulting in a pitch foam. See Hagar, Joseph W. and Max L. Lake, “Novel Hybrid Composites Based on Carbon Foams,” Mat. Res. Soc. Symp., Materials Research Society, 270:29-34 (1992), Hagar, Joseph W. and Max L. Lake, “Formulation of a Mathematical Process Model Process Model for the Foaming of a Mesophase Carbon Precursor,” Mat. Res. Soc. Symp., Materials Research Society, 270:35-40 (1992), Gibson, L. J. and M. F. Ashby, Cellular Solids: Structures & Properties, Pergamon Press, New York (1988), Gibson, L. J., Mat. Sci. and Eng A110, 1 Knippenberg and B. Lersmacher, Phillips Tech. Rev., 36( 4 ), (1976), and Bonzom, A., P. Crepaux and E. J. Moutard, U.S. Pat. No. 4,276,246, (1981). Additives can be added to promote, or catalyze, the foaming, such as dissolved gases (like carbon dioxide, or nitrogen), talc powder, freons, or other standard blowing agents used in making polymer foams.
[0008] Then, unlike polymer foams, the pitch foam must be oxidatively stabilized by heating in air (or oxygen) for many hours, thereby, cross-linking the structure and “setting” the pitch so it does not melt, and deform the structure, during carbonization. See Hagar, Joseph W. and Max L. Lake, “Formulation of a Mathematical Process Model Process Model for the Foaming of a Mesophase Carbon Precursor, Mat. Res. Soc. Symp., Materials Research Society, 270:35-40 (1992) and White, J. L., and P. M. Shaeffer, Carbon, 27:697 (1989). This is a time consuming step and can be an expensive step depending on the part size and equipment required.
[0009] Next, the “set” or oxidized pitch foam is then carbonized in an inert atmosphere to temperatures as high as 1100° C. Then, a final heat treatment can be performed at temperatures as high as 3000° C. to fully convert the structure to carbon and produce a carbon foam suitable for structural reinforcement. However, these foams as just described exhibit low thermal conductivities.
[0010] Other techniques may utilize a polymeric precursor, such as phenolic, urethane, or blends of these with pitch. See Hagar, Joseph W. and Max L. Lake, “Idealized Strut Geometries for Open-Celled Foams,” Mat. Res. Soc. Symp., Materials Research Society, 270:41-46 (1992), Aubert, J. W., (MRS Symposium Proceedings, 207:117-127 (1990), Cowlard, F. C. and J. C. Lewis, J. of Mat Scid., 2:507-512 (1967) and Noda, T., Inagaki and S. Yamada, J. of Non - Crystalline Solids, 1:285-302, (1969). However, these precursors produce a “glassy” or vitreous carbon which does not exhibit graphitic structure and, thus, has a very low thermal conductivity and low stiffness as well. See Hagar, Joseph W. and Max L. Lake, “Idealized Strut Geometries for Open-Celled Foams,” Mat. Res. Soc. Symp., Materials Research Society, 270:41-46 (1992).
[0011] One technique developed by the inventor of the present invention, and is fully disclosed in commonly assigned U.S. patent application Ser. No. 08/921,875. It overcomes these limitations, by not requiring a “blowing” or “pressure release” technique to produce the foam. Furthermore, an oxidation stabilization step is not required, as in other methods used to produce pitch-based carbon. This process is less time consuming, and therefore, will be lower in cost and easier to fabricate than the prior art above. More importantly, this process is unique in that it produces carbon foams with high thermal conductivities, greater than greater greater 58 W/m·K. However, the method described in U.S. patent application Ser. No. 08/921,875 is a batch process. This prevents large scale production at reasonable costs. Therefore, it is desirable to provide a continuous process that will produce carbon foam, so as to reduce costs and increase throughput.
SUMMARY OF THE INVENTION
[0012] The present invention provides a method of extruding a pitch or mesophase (herein after called pitch) based foam. The method includes the steps of: forming a viscous pitch foam; passing the viscous pitch foam through an extrusion tube; and subjecting the viscous pitch foam in the extrusion tube to a temperature gradient which varies along the length of the extrusion tube to form an extruded pitch derived foam, carbon foam, or graphitic foam, depending on the maximum temperature during the extrusion cycle.
[0013] A general objective of the present invention is to provide an extrusion method which can be continuous. This objective is accomplished by passing a viscous pitch foam through an extrusion tube and coking (solidifying) the viscous pitch foam as it passes through the tube.
[0014] Another objective of the present invention is to extrude carbon foam having specific properties. This objective is accomplished by heat treating the pitch derived foam in the extrusion tube to form carbon foam having specific properties, such as a carbonized or graphitized carbon foam.
[0015] Another aspect of the present invention provides an apparatus for extruding carbon foam. The apparatus includes a melting chamber for melting pitch, a foaming chamber communicatively connected to the melting chamber for foaming the melted pitch to form a viscous pitch foam, and a heated extrusion tube having a passageway communicatively connected to the foaming chamber, wherein the viscous pitch foam formed in the foaming chamber passes through said extrusion tube passageway to form an extruded pitch based foam of virtually any extrudable shape.
[0016] These and other objectives are accomplished by a method of extruding a pitch based foam which includes the steps of: forming a viscous pitch foam in a container; transferring the precursor from the container into an extrusion tube; and hardening the extruded pitch based foam.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] [0017]FIG. 1 is a batch apparatus for extruding carbon foam which incorporates the present invention;
[0018] [0018]FIG. 2 is a graph showing an optimum foaming temperature range for ARA24 mesophase pitch;
[0019] [0019]FIG. 3 is a temperature gradient suitable for use with the apparatus of FIG. 1; and
[0020] [0020]FIG. 4 is a continuous carbon foam extruding apparatus incorporating the present invention; and
[0021] [0021]FIG. 5, is another embodiment of a continuous carbon foam extruding apparatus incorporating the present invention
DETAILED DESCRIPTION OF THE INVENTION
[0022] A pitch based foam, such as fully disclosed in U.S. patent application Ser. Nos. 08/921,875, and 08/923,877 which are commonly owned by the assignee of the present application, and which teachings are fully incorporated herein by reference, is formed by first extruding a viscous pitch foam, such as derived from a mesophase or isotropic pitch, through an extrusion tube. The viscous pitch foam can be heat treated in the tube to form an extruded carbon foam having desirable properties. The extrusion process can be continuous to provide continuous production of the carbon foam or a batch process. If the extrusion is only a pitch derived foam, then it can be heat treated in a separate furnace to produce a carbon or graphitic foam.
[0023] Whether the foam is pitch derived, carbon, or graphitic depends upon the heat treatment of the foam. If the maximum temperature of the extrusion is less than 800° C. then the molecular structure of the material still contains non-carbon atoms, and therefore is considered a pitch derived foam. If the maximum temperature of the extrusion is between 800° C. and about 2000° C., then the molecular structure of the material contains only carbon atoms, and therefore is considered a pitch derived carbon foam. If the maximum temperature is greater than 2000° C., then the material is beginning to show signs of graphitic structure (depending on original pitch precursor) and therefore is considered a pitch derived graphitic foam. The foam, whether viscous, pitch derived, carbon, or graphitic is generically referred to in this application as pitch based.
[0024] As shown in FIG. 1, an apparatus 10 for extruding carbon foam in a batch process includes a melting/foaming chamber 12 for melting pitch materials 14 , and foaming the melted pitch materials 14 to form a viscous pitch foam 16 . The melting/foaming chamber 12 is a heatable container, such as a crucible, which can withstand internal pressures exerted on container walls by the expanding viscous pitch foam 16 . The viscous pitch foam 16 expands in the chamber 12 and forces its way into an extrusion tube 18 communicatively connected to the chamber 12 . The extrusion tube 18 heats the extruded foamed pitch precursor 16 in accordance with a predetermined temperature gradient along the tube length to coke the viscous pitch foam 16 , and heat treat the hardened foam 20 . As discussed above, the properties of the extruded foam will depend on the maximum temperature of the heat treatment in the extrusion tube 18 .
[0025] The melting/foaming chamber 12 is a crucible 22 with a lid 24 . Pitch 14 is placed in the crucible 22 , and the lid 24 is secured to the crucible top 26 . Grafoil gasket material 28 is clamped between the lid 24 and crucible 22 using graphite clamps 30 to provide a tight seal.
[0026] The heated extrusion tube 18 extends from the lid 24 , and has a shaped inner passageway 32 through which the extruded materials pass. The passageway 32 is shaped to form a desired extruded material cross section shape. Alternatively, the viscous pitch foam can pass through an orifice disposed in the passageway 32 to form the desired extruded material cross section.
[0027] The extrusion tube 18 is heated to provide a predetermined temperature gradient along the tube length. The temperature gradient along the length of the tube determines the characteristics of the extruded carbon foam 20 . The tube 18 is heated using conventional heating methods known in the art, such as by using radiant energy, in the form of IR lamps, microwave energy, induction heating, band heaters, and the like.
[0028] When the viscous pitch foam 16 expands, it forces its way out of the chamber 12 through the extrusion tube 22 . A throttle valve 31 disposed in the extrusion tube throttles the flow of extruded material to maintain the desired pressure in the foaming chamber 12 , and control the flow of extruded material.
[0029] Once the extruded carbon foam 20 passes through the extrusion tube 18 , a sectioning device 33 disposed downstream of the tube 18 cuts the extruded foam 20 to desired section lengths. The sectioning device 33 can be any suitable cutting devices, such a saw, shear, and the like.
[0030] In use, the pitch 14 , in the form of pitch powder, granules, pellets, or the like, are placed in the chamber 12 . The pitch 14 can be solvated if desired. The pitch 14 is heated in a substantially oxygen-free environment to avoid oxidation of the pitch materials 14 during heating. Preferably, the pitch 14 is heated by placing band heaters around the chamber 12 to a temperature approximately 50 to 100° C. above its softening point. For example, where Mitsubishi ARA24 mesophase pitch is used, a temperature of 300° C. is sufficient. The chamber is pressurized initially with a nitrogen purge (or other inert gas) to the desired pressure of foaming and the throttle valve is used to regulate the pressure during foaming
[0031] Preferably, the pressure inside the chamber 12 is then increased up to 1000 psi. The temperature of the pitch 14 is then raised to cause the evolution of pyrolysis gases in the pitch 14 . The pyrolysis gases foams the melted pitch 14 to form the viscous pitch foam 16 which expands into the extrusion tube 18 . Preferably, the temperature of the pitch 14 is increased to an optimum foaming temperature range for the particular molten pitch in the melting/foaming chamber 12 . An optimum foaming temperature is a temperature in which the foam yield is maximized. For example, as shown in FIG. 2, a preferred foaming temperature range for ARA24 mesophase pitch is between 420 C and 520 C. Most preferably, the foaming temperature range is between 420 C and 450 C.
[0032] The expanding viscous pitch foam 16 passes through the throttle valve and into the extrusion tube 18 which shapes and heat treats the extruded material to form the carbon foam. The extrusion tube 18 is heated in order to subject the extruded material to a temperature gradient, such as disclosed in FIG. 3, which forms carbonized and graphitized carbon foam 20 .
[0033] As shown in FIG. 3, the extruded viscous pitch foam 16 is heated in a first zone to coke (harden) the extruded viscous pitch and form the pitch derived foam 20 . For example, the temperature of a viscous pitch foam derived from ARA mesophase pitch is preferably increased along the length of the tube to about 500 C-1000 C
[0034] The pitch derived foam 20 can be exposed to additional temperature gradients in the extrusion tube 18 to produce carbon foam or graphitized foam. For example, prior to cooling the pitch derived foam 20 , the temperature of the foam 20 can be further increased to carbonize or graphitize the foam. As shown in FIG. 3, the pitch derived foam 20 is further heated in a second zone to further increase the foam temperature to carbonize the foam 20 . Following carbonizing, the extruded material is heated in a third zone to approximately 2800 C to further increase the carbon foam temperature causing it to graphitize, depending on the pitch precursor. Preferably, the graphitizing zone includes a period of constant peak temperature to ensure the carbon foam is substantially isothermal.
[0035] Finally, the graphitized carbon foam 20 is cooled in a fourth zone below includes 200 C in order to allow-handling of the extruded material, such as conveying or sectioning the extruded carbon foam 20 . Preferably, the temperature along the length of the tube 18 in the fourth zone is gradually decreased to a temperature at which the carbon foam does not oxidize.
[0036] It will thus be seen that the present invention provides for the production of an extruded pitch-based foam. The process involves the fabrication of a foam from a mesophase or isotropic pitch which can be synthetic, petroleum, or coal-tar based. A blend of these pitches can also be employed. The foam is formed by melting the pitch in a melting chamber, and then foaming the melted pitch in a foaming chamber (which may be the same as the melting chamber) to form a viscous pitch foam The viscous pitch foam is extruded through an extrusion tube which heat treats the precursor to provide a pitch derived foam or pitch derived carbon foam, depending on maximum temperature.
[0037] Preferably, the foam can have a relatively uniform distribution of pore sizes (average between 50 and 500 microns), very little closed porosity, and a density ranging from approximately 0.20 g/cm 3 to 0.7 g/cm 3 . However, deviations from this preferable properties are possible by changing the operating conditions and the pitch precursor. When a mesophase pitch is used, the domains are stretched along the struts (or cell walls) of the foam structure and thereby produces a highly aligned graphitic structure parallel to the cell walls (or struts). When graphitized, these struts will exhibit thermal conductivities similar to the very expensive high performance carbon fibers (such as P-120 and K1100). Thus, the foam will exhibit high thermal conductivity at a very low density (≈0.5 g/cc). By utilizing an isotropic pitch, the resulting foam can be easily activated to produce a high surface area activated carbon. Also, isotropic pitches will typically results in stronger materials, especially if derived from coals.
[0038] The carbon foam can also be continuously extruded using an apparatus incorporating the present invention. This is very similar to the previously described apparatus with the addition of a separate melting chamber and device to continuously add molten pitch to the foaming chamber. As shown in FIG. 4, an apparatus 40 for continuously extruding carbon foam 42 includes a melting chamber 44 for melting pitch materials 46 , and a foaming chamber 48 . The foaming chamber 48 is communicatively connected to the melting chamber 44 by a passageway 50 for foaming the melted pitch materials 47 to form a viscous pitch foam 52 . A pump, not shown, between the melting chamber and the foaming chamber will regulate the flow of molten pitch into the pressurized foaming chamber. The viscous pitch foam 52 produced in the foaming chamber expands into an extrusion tube 54 communicatively connected to the foaming chamber 48 . The extrusion tube 54 heats viscous pitch foam 52 in accordance with a predetermined temperature gradient along the tube length to coke the viscous pitch foam 52 , and shape the foam 42 . Preferably, the extrusion tube 54 also heat treats the carbon foam 42 to provide a carbon or graphitic foam with specific properties.
[0039] The melting chamber 44 is a heatable container having a feed tube 58 which feeds solid pitch 46 into the chamber 44 . The feed tube 58 continuously feeds pitch powder, granules, pellets, or the like into the melting chamber 44 which is heated to transform the solid pitch 46 into molten pitch 47 . The pitch 46 is heated in the melting chamber 44 in an oxygen free environment, such as nitrogen, and exits the chamber 44 through an outlet 60 formed in a melting chamber wall into the passageway 50 . Preferably, the pitch is heated to about 100 C above the pitch softening point to provide a flowable molten pitch 47 . For example, an ARA24 mesophase pitch is preferably heated to about 350 C.
[0040] Preferably, an agitating mechanism 64 agitates the molten pitch 47 in the melting chamber 44 to ensure uniform pitch temperature and homogeneity. The agitating mechanism 64 includes a rotatable mixing shaft 66 having a mixing end 68 disposed in the molten pitch 47 . The mixing end 68 rotates to agitate the molten pitch 47 . Although a rotating mixing shaft 46 is disclosed, other methods known in the art can be used to agitate the molten pitch 47 , such as rotating the melting chamber, vibrating paddles in the molten pitch, and the like.
[0041] The molten pitch 47 passes through the passageway 50 to the foaming chamber 48 . The passageway 50 has an inlet 70 which receives the molten pitch 47 from the melting chamber 44 , and an outlet 72 through which the molten pitch 47 enters the bottom 74 of the foaming chamber 48 . In one embodiment, the melting chamber 44 is disposed above the foaming chamber 48 to gravity feed the molten pitch 47 into the foaming chamber 48 . A valve 76 or meter pump disposed in the passageway 50 can regulate the flow of molten pitch into the foaming chamber 48 to maintain a pressure therein.
[0042] The foaming chamber 48 is a pressurized heatable container which heats the molten pitch 47 under pressure to cause the evolution of pyrolysis gases to form the foam precursor 52 . As in the melting chamber 44 , the molten pitch is heated in an oxygen free environment to avoid oxidation of the molten pitch 47 .
[0043] The molten pitch 47 enters the foaming chamber 48 through the passageway outlet 72 , and is heated in the foaming chamber to a temperature sufficient to cause the molten pitch 47 to foam at the foaming chamber pressure to form the foam precursor 52 . For example, at a pressure of approximately 68 atm (1000 psi), ARA24 mesophase pitch will foam at a temperature between approximately 420 C and 480 C. Preferably, the temperature in the foaming chamber is maintained at approximately 450 C. under a pressure between approximately 27 atm and 68 atm (400 psi and 1000 psi) when foaming molten ARA24 mesophase pitch.
[0044] The viscous pitch foam 52 expands in the foaming chamber 48 , forcing its way through the extrusion tube 54 . As in the first embodiment, a throttle valve (not shown) disposed in the extrusion tube 54 throttles the flow of extruded materials to maintain the desired pressure in the foaming chamber 48 , and control the flow of extruded materials.
[0045] The expanding viscous pitch foam 52 passes through the extrusion tube 54 which shapes and heat treats the extruded material to form the pitch derived foam 42 . The extrusion tube 54 subjects the extruded material to a temperature gradient, such as disclosed in FIG. 3, which forms carbonized and graphitized carbon foam 42 .
[0046] As in the first embodiment, the extrusion tube 54 is heated to provide a predetermined temperature gradient along the tube length such as disclosed above in FIG. 3. The temperature gradient along the length of the tube 54 determines the characteristics of the extruded foam 42 . The tube 54 is heated using conventional heating methods known in the art, such as by using radiant energy, in the form of IR lamps, microwave energy, induction heating, and the like.
[0047] In another embodiment of the present invention, shown in FIG. 5, molten pitch is continuously fed into a foaming chamber 80 by a metering pump 82 interposed between the foaming chamber 80 and a melting chamber B 4 . Pitch is continuously supplied to the melting chamber 84 by a hopper 86 mounted proximal to a feed end 88 of the cylindrical melting chamber 84 . The heated melting chamber 84 melts the pitch and, and a feed screw 90 disposed in the melting chamber urges the melted pitch toward the metering pump 82 disposed at the melting chamber pump end 92 . Advantageously, the feed screw 90 mixes the pitch to ensure uniform temperature and homogeneity of the melted pitch. Exposure of the pitch to oxygen is minimized to avoid oxidation by methods known in the art, such as by evacuating the melting chamber 84 , maintaining an inert gas blanket in the melting chamber 84 , and the like.
[0048] The metering pump 82 disposed at the melting chamber pump end 92 pumps the molten pitch into the pressurized foaming chamber 80 . The foaming chamber 80 foams the molten pitch to form a viscous pitch foam by heating the molten pitch under pressure to cause the formation of pyrolysis gases. The pitch is foamed in an oxygen free environment, such as in the presence of an inert gas, to avoid oxidation. The expanding viscous pitch foam forces its way through an opening 94 in the foaming chamber 80 , and into an extrusion tube 96 . A modified standard screw feed melt extruder would be suitable for this task.
[0049] As disclosed in the first embodiment, the extrusion 96 tube subjects the extruded viscous pitch foam, and resulting carbon foam to a predetermined temperature gradient. The predetermined temperature gradient cokes and heat treats the extruded material to form carbon foam having particular qualities, such as disclosed in the first embodiment. Although not shown, valves controlling the extrusion process, and a cutting mechanism can be provided as in the first embodiment.
[0050] While there has been shown and described a preferred embodiment of the invention, it will be obvious to those skilled in the art that various changes and modifications can be made therein without departing from the scope of the invention defined by the appended claims. | A method and apparatus for extruding pitch based foam is disclosed. The method includes the steps of: forming a viscous pitch foam; passing the precursor through an extrusion tube; and subjecting the precursor in said extrusion tube to a temperature gradient which varies along the length of the extrusion tube to form an extruded carbon foam. The apparatus includes an extrusion tube having a passageway communicatively connected to a chamber in which a viscous pitch foam formed in the chamber passes through the extrusion tube, and a heating mechanism in thermal communication with the tube for heating the viscous pitch foam along the length of the tube in accordance with a predetermined temperature gradient. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable
REFERENCE TO A MICROFICHE APPENDIX
Not Applicable
BACKGROUND OF THE INVENTION
This invention relates to a method for the novel preparation of some N-substituted-1-adamantanecarboxamides and some 1-adamantaneacetamides by treating 1-adamantanecarboxylic acid or 1-adamantaneacetic acid with N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine, followed by the addition of aqueous ammonia or amines.
The amide linkage is present in peptides and proteins. Moreover, the amide functional group is present in many medicinal compounds. Thus, reactions that lead to the formation of the amide linkage and/or the amide functional group are useful in pharmaceutical research as well as the development of drugs.
N-Substituted-1-adamantanecarboxamides are useful as potential antiviral agents as well as intermediates in the synthesis of antiviral agents. Therefore, this invention has potential commercial application as a convenient and rapid method for the preparation of adamantanecarboxamides, other carboxamides, more complex compounds containing the amide functional group, and compounds containing the amide linkage.
Traditionally, carboxamides in general, and adamantanecarboxamides in particular (Novakov, et al., Khim - Farm. Zh ., 1987, 21(4), 454-8; Danilenko, et. al., Khim .- Farm. Zh ., 1976, 10(5), 49-52) have been prepared from the corresponding acids via the acid chlorides. In general,this method is long and tedious.
According to most methods, preparation of acid chlorides requires refluxing the acids in excess thionyl chloride from thirty minutes to as long as several hours, followed by distillation to remove unreacted thionyl chloride. According to one method 1,3-adamantane(bis)acetic acid was refluxed in excess thionyl chloride for twenty-four hours to prepare the corresponding acid chloride (Aigami, et. al., J. Med. Chem ., 1975, 18(7), 713-21). Another method for the preparation of some adamantanecarboxamides involved refluxing the corresponding acid in thionyl chloride and benzene for eight hours, followed by distillation to remove the benzene and excess thionyl chloride (Krasutskii, et al., Khim .- Farm. Zh ., 1985, 19(7), 825-29). Still another method involved refluxing the adamantanecarboxylic acids in thionyl chloride containing a catalytic amount of N,N-dimethylformide (Fridman, et. al., Khim .- Farm. Zh ., 1974, 8(7), 6-8). Also, adamantanecarboxamides have been prepared by heating the corresponding acids with phosphorus pentachloride in carbon tetrachloride for one hour (Danilenko, et. al., Khim .- Farm. Zh ., 1976, 10(6), 37-41). Usually, after the acid chloride has been isolated from excess co-reactant, solvent, and/or by products, it is dissolved in a solvent such as anhydrous tetrahydrofuran or anhydrous dioxane, aqueous ammonia or the amine is added, and the mixture is allowed to stand for about twelve hours.
There are several disadvantages to using the methods described above. These methods require: 1) reflux and distillation apparatus; 2) traps for the hydrogen chloride and sulfur dioxide evolved in the thionyl chloride reaction; 3) heating apparatus; and 4) isolation of the acid chloride. Thus, unlike the method described in this invention, the above methods are long and tedious.
Additionally, adamantanecarboxamides have been prepared in our laboratories using DATE [1-(N,N-diethylamino)-1,1,2-trifluoro-2-chloroethane] (Anderson, et. al., Synthetic Comm ., 1988, 18(16 & 17), 1967-1974; Anderson, et. al., The Chemist , January/February 2000, 7-10). The reagent DATE was prepared from diethylamine and chlorotrifluoroethylene, according to a modified procedure of Yarovenko and Raksha (Yarovenko and Raksha, J. Gen. Chem. USSR , 1959,29,2125-28). Chlorotrifluoroethylene gas was bubbled slowly into diethylamine contained in a gas drying tube cooled by an ice water bath. This was continued for at least twelve hours, and the product was collected by vacuum distillation. There are several disadvantages to using this reagent. First, the procedure for preparation of the reagent required about twenty four hours. Second, the reagent is not very stable at room temperature and decomposes within a few days even when stored in the refrigerator. Third, preparation of the reagent requires somewhat sophisticated equipment. The reagent used in this invention is commercially available from Lancaster Synthesis in Windham, N.H. Further, the reagent is stable over a long period of time. Thus, unlike the method described in this invention, the procedure using DATE is long and tedious.
BRIEF SUMMARY OF THE INVENTION
The invention described herein provides a method for preparing adamantanecarboxamides and adamantaneacetamides in high yields (80-100%) by treating the 1-adamantanecarboxylic acid or 1-adamantaneacetic acid with N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine, followed by addition of aqueous ammonia or the appropriate amine. The procedure is convenient and rapid, requiring no more than one or two hours. Several reactions can be carried out simultaneously.
DETAILED DESCRIPTION OF THE INVENTION
The carboxamides are prepared by a procedure that is carried out in a wide mouth polyethylene bottle on a magnetic stirrer at ambient temperature. Isolation of the amide is completed by filtering and washing with water, followed by a small amount of ethyl ether. The entire reaction, including isolation of the product, can be completed within one or two hours. The method works equally as well for the preparation of 3-substituted-1-adamantanecarboxamides and 3-substituted-1-adamantaneacetamides. In the case of 3-hydroxy-1-adamantanecarboxylic acid and 3-hydroxy-1-adamantaneacetic acid, the hydroxy group must be protected otherwise it is converted to a fluoro group. Thus, 3-hydroxy-1-adamantanecarboxylic acid yields 3-fluoro-1-adamantanecarboxamide.
The procedure consists of adding the 1-adamantanecarboxylic acid to N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine contained in a wide mouth polyethylene bottle during which time the acid fluoride forms immediately through an exothermic reaction. The rate of addition of the acid may be adjusted to control the temperature and prevent the evolution of hydrogen fluoride or the reaction bottle may be cooled in an ice water bath briefly. The intermediate acid fluoride is not isolated. After the reaction mixture cools to room temperature by allowing it to stand at room temperature or by cooling it in an ice water bath, cold aqueous ammonia or the desired amine is added and the amide precipitates immediately. An excess of an inexpensive amine is added to convert the hydrogen fluoride to the amine salt. For more expensive amines, aqueous base is added to convert the hydrogen fluoride to the salt prior to the addition of the amine. The amide is collected by filtration and washed copiously with water followed by a minimum amount of ethyl ether. For large scale preparations the oily amide by product, N,N-diethyl-2,3,3,3-tetrafluoropropionamide, can be collected from the filtrate by separation from the water phase using a separatory funnel. Similarly, for large scale preparations, the hydrogen fluoride salt of ammonia or the amine can be recovered by evaporation of the water. Several reactions can be carried out simultaneously.
Some examples of the preparation of compounds, presented as illustrations and not intended to be limiting, are as follows.
EXAMPLE 1
Preparation of 1-Adamantanecarboxamide
1-Adamantanecarboxylic acid (10.8 g, 0.06 mole) was added to N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine (13.4 g, 0.06 mole) contained in a wide mouth polyethylene bottle with magnetic stirring. The acid dissolved immediately during which time a highly exothermic reaction occurred. The reaction mixture was allowed to cool to room temperature and cold aqueous ammonia (250 ml) was added slowly. A heavy precipitate of the amide appeared almost immediately. After the addition was complete, the reaction mixture was stirred for about fifteen minutes. The 1-adamantanecarboxamide was collected and washed copiously with water followed by ethyl ether and dried. Yield: 10.7 g, 100%; mp 189.4-190.2° C. (Lit. mp 189° C., Stetter, et. al., Chem. Ber ., 1960, 226-230). The analytical sample was recrystallized from cyclohexane and sublimed. Anal. Calcd. for C 11 H 17 NO: C, 73.76; H, 9.49; N, 7.82. Found: C, 73.67; H. 9.60; N, 7.78.
EXAMPLE 2
Preparation of 1-Adamantaneacetamide
1-Adamantaneacetic acid (11.7 g, 0.06 mole) was dissolved in N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine (13.4 g, 0.06 mole) during which time a highly exothermic reaction occurred. The reaction mixture was allowed to cool to room temperature and cold aqueous ammonia (250 ml) was added slowly. The 1-adamantaneacetamide was isolated as described in example 1 to yield 10.5 g, 90.6 %; mp 173.6-174.0° C. The analytical sample was recrystallized from cyclohexane and sublimed. Anal. Calcd. for C 12 H 19 NO: C, 74.63; H, 9.89; N, 7.25. Found: C, 74.36; H, 9.84; N, 7.15.
EXAMPLE 3
Preparation of N-Cyclohexyl-1-Adamantanecarboxamide
1-Adamantanecarboxylic acid (10.8 g, 0.06 mole) was dissolved in N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine (13.4 g, 0.06 mole) as described in example 1. After the reaction mixture cooled to room temperature, cyclohexylamine (14.88 g, 17.2 ml, 0.15 mole) was added slowly and a heavy precipitate of the amide appeared almost immediately. The N-cyclohexyl-1-adamantanecarboxamide was isolated as described in example 1 to give 14.8 g, 94.4%; mp 199.3-200.4° C. The analytical sample was recrystallized from cyclohexane and sublimed. Anal. Calcd. for C 17 H 27 NO: C, 78.18; H. 10.34; N, 5.36. Found: C, 77.97; H, 10.46; N, 5.32.
EXAMPLE 4
Preparation of N-p-Methoxyphenyl-1-Adamantanecarboxamide
1-Adamantanecarboxylic acid (10.8 g, 0.06 mole) was dissolved in N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine (13.4 g, 0.06 mole) as described in example 1. After the reaction mixture cooled to room temperature, a solution of p-anisidine (18.5 g, 0. 15 mole) in ethyl ether (minimum amount) was added and the reaction mixture was stirred for about an hour. The ethyl ether was removed at the rotary evaporator and the N-p-methoxyphenyl-1-adamantanecarboxamide was isolated as described in example 1 to give 15.8 g, 92%; mp 186-187° C. The analytical sample was recrystallized from cyclohexane and sublimed. Anal. Calcd. for C 18 H 23 NO 2 : C, 75.80; H, 8.07; N, 4.91. Found: C, 75.69; H, 8.17; N, 4.92.
Further examples of some of the compounds prepared according to these procedures are given in Table 1. The N-substituted-1-adamantanecarboxamides shown in Table 1 are: Example 5, N-isopropyl-1-adamantanecarboxamide; Example 6, N-tert-butyl-1-adamantanecarboxamide; Example 7, N-sec-butyl-1-adamantanecarboxamide; Example 8, N-α-methylbenzyl-1-adamantanecarboxamide; Example 9, N-p-methylphenyl-1-adamantanecarboxamide; Example 10, N-2-(1-methoxypropyl)-1-adamantanecarboxamide; Example 11, N-3,4-dinethoxyphenyl-1-adamantanecarboxamide; Example 12, N-phenyl-1-adamantanecarboxamide; Example 13, N-p-n-butylphenyl-1-adamantanecarboxamide; Example 14, N-m-bromophenyl-1-adamantanecarboxamide; Example 15, N-methyl-1-adamantanecarboxamide; and Example 16, N-ethyl-1-adamantanecarboxamide.
TABLE 1
Some N-Substituted-1-Adamantanecarboxamides Prepared According To This Method
Example
Calculated
Found
Number
N-Substituent
% Yield
MP ° C.
Anal Calcd For
C
H
N
C
H
N
5
(CH 3 ) 2 CH—
89.3
179.6-180.0
C 14 H 23 NO
76.03
10.40
06.33
76.08
10.50
06.37
6
(CH 3 ) 3 C—
84.5
182.7-184.0
C 15 H 25 NO
76.61
10.63
05.95
76.65
10.75
05.99
7
CH 3 —CH 2 —CH(CH 3 )—
93.5
166.0-167.0
C 15 H 25 NO
76.61
10.63
05.95
76.35
10.76
05.89
8
C 6 H 4 —CH(CH 3 )—
95.1
170.6-170.7
C 19 H 25 NO
80.58
08.83
04.94
80.75
08.90
04.94
9
P—CH 3 —C 6 H 4 —
94.6
192.1-192.5
C 18 H 23 NO
80.31
08.54
05.20
80.28
08.66
05.14
10
CH 3 O—CH 2 —CH(CH 3 )—
91.1
114.2-114.6
C 15 H 25 NO 2
71.73
09.95
05.57
71.77
09.98
05.61
11
3,4-(CH 3 O—) 2 —C 6 H 3 —
95.1
226.1-227.6
C 19 H 23 NO 3
72.40
07.93
04.44
72.45
07.99
04.41
12
C 6 H 5 —
91.4
200.2-202.3
C 17 H 21 NO
80.01
08.23
05.49
80.04
08.29
05.55
13
p-CH 3 —(CH 2 —) 3 —C 6 H 4 —
87.8
134.5-134.9
C 21 H 29 NO
81.04
09.32
04.50
81.07
09.42
04.53
14
m-Br—C 6 H 4 —
96.3
191.0-191.5
C 17 H 20 NOBr
61.12
05.99
04.19
61.24
06.06
04.17
15
CH 3 —
81.6
144.4-145.1
C 12 H 19 NO
74.63
09.84
07.25
74.68
09.93
07.28
16
CH 3 —CH 2 —
81.3
128.1-128.5
C 13 H 21 NO
75.38
10.14
06.76
75.34
10.16
06.82
REFERENCE CITED
1. Novakov, I. A., Kulev, I. A., Radchenko, S. S., Birznieks, K. A., Boreko, E. I., Vladyko, G. V., and Korobehenko, L. V., “Synthesis and Antiviral Activity of the Hydrochlorides of AlicyclicMono- and Diamines,” Khim .- Farm. Zh ., 1987,21(4), 454-8. (English Translation)
2. Danilenko, G. I., Votyakov, V. I., Andreeva, O. T., Timofeeva, M. M., Shashikhina, M. N., Denisova, L. V., Boreko, E. I., Bruskova, I. V., Dikolenko, E. I., and Smirnova, N. A., “Synthesis and Biological Activity of Adamantane Derivatives.III. Virus Inhibiting Effect of 1-(4-Aminophenyl)adamantane Derivatives,” Khim .- Farm. Zh ., 1976,10(5), 49-52. (English Translation)
3. Aigami, K, Inamoto, Y., Takaishi N., and Hattori, K, “Biologically Active Polycycloalkanes. 1. Antiviral Adamantane Derivatives,” J. Med. Chem ., 1975, 18(7), 713-21.
4. Krasutskii, P. A., Semenova, I. G., Novikova, M. I., Yurchenko, A. G., Leont'eva, N. A., and Veselovskaya, T. V., “Amino Acids of the Adamantane Series I. Synthesis and Antiviral Activity of Alpha Amino Acids of the Adamantane Series and their Derivatives,” Khim .- Farm. Zh ., 1985, 19(7), 825-29. (English Translation)
5. Fridman, A. L., Zalesov, V. S., Moiseev, I. K, Kolobov, N. A., and Dobrilkin, K. V., “Synthesis and Physiological Activity of Some Adamantanecarboxylic Acids and Their Derivatives,” Khim . - Farm. Zh ., 1974, 8(7), 6-8. (English Translation)
6. Danilenko, G. I., Votyakov, V. I., Andreeva, O. T., Boreko, E. I., Denisova, L. V., Shashikhina, M. N., Timofeeva, M. N., Dilolenlo, E. I., and Utocbka, T. N., “Synthesis and Biological Activity of Adamantane Derivatives. IV. Virus Inhibiting Effect of Some Adamantylamines,” Khim . - Farm. Zh ., 1976, 10(6), 37-41. (English Translation)
7. Stetter, H., Mayer, J., Schwarz, M., and Wulaf, K., “Uber Verbindmigen mit Urotropin-Struktur. XVI. Beitrage zur Chemie der Adamantyl-(1)-Derivative,” Chem. Ber ., 1960,93, 226-30. (German)
8. Anderson, G. L., Burks, W. A., and Harruna, I. I., “Novel Synthesis of 3-Fluoro-1-Amino-Adamantane And Some Of Its Derivatives,” Synthetic Communications 1988, 18(16 & 17), 1967-1974
9. Anderson, G. L. and Kaimari, T., “Novel Synthesis Of Some 3-Halo-1-Aminoadamantanes,” The Chemist , January/February 2000, 7-10
10. Yarovenko, N. N. and Raksha, M. A., “Fluorination By Means of Alpha Fluorinated Amines,” J. Gen. Chem USSR , 1959, 29, 2125-28 (English Translation) | This invention relates to a method for the novel preparation of 1-adamantanecarboxamides and 1-adamantaneacetamides. Adamantanecarboxamides and adamantaneacetamides are prepared in high yields (80-100%) by treating adamantanecarboxylic acid and adamantaneacetic acid with N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine, followed by addition of aqueous ammonia or the appropriate amine. The procedure, carried out at ambient temperature using common laboratory equipment, is both convenient and rapid, requiring no more than one or two hours. Several reactions can be carried out simultaneously. | 2 |
This is a continuation of application Ser. No. 653,983, filed Feb. 11, 1991, now U.S. Pat. No. 5,245,808, which is a file wrapper continuation of Ser. No. 444,666, filed Dec. 1, 1989, now abandoned.
TECHNICAL FIELD
The present invention generally relates to an adhesively glazed curtainwall system and more particularly relates to a butt-glazed curtainwall system including mechanical retention members which retain vertical edges of glass panels while providing minimal sight lines, thus permitting glazing and weathersealing to be accomplished from the interior side of the curtainwall.
BACKGROUND OF THE INVENTION
In building structures, it is often aesthetically desirable to cover large portions of the outside of the structures with as much glass and as little outside framing elements as possible, thereby providing the structures with a smooth and unbroken outside surface appearance. Therefore, it is known in the art to provide a structural adhesive bond between the building structure and the inside surfaces of glass panels to attach the panels to the building structure, thus reducing or eliminating the need for permanent outside retention members. Such bonding configurations are commonly known as "Structural Silicone Glazing" or "SSG" systems.
Typical SSG systems fall into two major classes: two-sided and four-sided. Four-sided SSG systems typically include a plurality of vertical structural mullions in combination with a plurality of horizontal structural mullions, which combine to form a mullion framework having a plurality of panel-shaped openings which are slightly smaller than the glass panels to be supported. The mullion framework is fixed about the exterior of a building structure. Each glass panel is positioned adjacent to the exterior surface of the mullion framework and over a corresponding panel-shaped opening by a plurality of temporary retaining clips, such that the edges of the panel slightly overlap the panel-shaped opening and a small gap exists between the inside surfaces of the glass panel and the framework. Structural adhesive, typically structural silicone, is then applied into the gap. After the silicone adhesive cures, it provides a structural bond between the mullion framework and the glass panel which can completely support the glass panel without any aid from the temporary retaining clips or other outside retention means. For weatherproofing purposes, additional silicone adhesive is then applied from the outside of the building into gaps created by the abutting edges of the adjacent glass panels. Disadvantageously, this "weatherbead" must be applied from the exterior of the building.
Two-sided SSG systems differ in that a structural adhesive bond as described above is provided along two (usually vertical) opposing edges of the glass panels. In two-sided SSG systems, the two edges not being structurally bonded to the mullion framework are retained by other means. This is normally done by conventional window glazing means which enclose the entire edge of the glass panels, thus not providing the smooth continuous appearance of four-sided SSG systems. As in the four-sided SSG systems, additional silicone adhesive must be applied from the outside of the building into the gap created by the abutting edges of the glass panels.
Although such SSG systems are in demand, the cost for such systems is high. As discussed above, in four-sided SSG systems, temporary mechanical retentioners for the glass panels must be installed to allow the structural silicone adhesive to cure, and then must be removed after the curing process. Sealant must then be added to cover holes left behind by the temporary fasteners. As such installation and removal processes must be performed from the exterior of the building structure, these processes are typically labor- and cost-intensive, as scaffolding must be installed to provide access to the exterior of the building. In both two- and four-sided systems, the weatherproofing joint must be installed from the building exterior, and the quality of the weatherproofing joint is highly dependent upon the skill of the field laborer installing the glass and applying the sealant.
Safety is also a concern associated with SSG systems, as high reliance is placed upon structural bonding. The structural adhesive is subject to rupture under certain loading conditions, such as high negative pressure on the lee side of the building during periods of strong winds. Such a rupture can cause a glass panel to fall from a building and crash to the ground, possibly causing catastrophic personal injury and property damage.
Various approaches to overcome the above deficiencies have been proposed, such as that disclosed in U.S. Pat. No. 4,650,702, wherein each pane of glass of the curtainwall system has a prebonded structural interface adhered along at least two of its edges. The structural interface is clipped onto the face of the mullion framework during installation to fasten the pane to the mullion framework. Also disclosed is a non-structural weatherseal between adjacent panels which is installed from the interior side of the curtainwall system.
U.S. Pat. No. 4,562,680 discloses a butt glazing system including a specially configured frame member with a front wall forming an angle of at least 135 degrees. A semicircular channel open along its forward portion is formed at the apex of the angled front wall. A special elongate mullion has a gasket formed along its front edge. The rear edge of the mullion insert has a T-shaped connector portion formed thereon. The "head" of the T-shaped connector portion is wider than the opening of the front of the semicircular channel, such that the head of the connector can be inserted into the channel only by introducing it at an angle and rotating it into place. When so installed, the mullion insert is held within the semicircular channel as long as it is not permitted to rotate relative to the channel. To install a curtainwall according to this system, a first glazing panel is positioned against the end mullion and the adjacent interior mullion from inside the building. A mullion insert as described is then fastened to a chevron-shaped mullion as described, and pivoted such that the gasket portion of the insert abuts the edge of the first panel. A second panel is then positioned against the opposite side of the mullion insert and against the next adjacent mullion. The glazing procedure is then repeated progressively.
Although such systems include advantages, none have proven so successful as to attain industry acceptance. Therefore, efforts continue to solve this problem.
Thus, there is a recognized need to provide a system for structural silicone glazing wherein glazing and weatherproofing may be accomplished from the interior side of the building.
There is also a need to provide such a system which is easy to install, tolerates non-regular or non-plumb installation of glass, and provides improved safety characteristics.
SUMMARY OF THE INVENTION
As will be seen, the present invention solves the above needs associated with prior art butt-glazed curtainwall systems. Stated generally, the present invention comprises a retainer for accepting edges of glass panels and retaining the edges relative to a framing member, comprising an elongate retainer profile having a generally H-shaped transverse cross section, thereby forming a pair of elongate U-shaped retaining channels, the first of the retaining channels configured to accept an edge of a first of the glass panels, and the second of the retaining channels configured to accept an edge of a second of the glass panels, panel securing means for securing the first and second panel edges within the first and second channels, respectively, and profile securing means for securing the profile coextensively along the framing member, such that one side of the pair of retaining channels is urged against the framing member.
The elongate retaining channels provide means for retaining glass panels in place during the application of structural adhesive, and also serve as means for retaining the edges of glass panel in the event that structural adhesive should fail. Weathersealing is also provided by the existence of strategically placed pads intended for contact with the smooth glass surface.
Therefore it is an object of this invention to provide a retainer and weatherseal between adjacent glass panels in a curtainwall framing system having structurally bonded glazing.
It is another object to provide such a retainer which permits structurally bonded glazing to be installed on curtainwall framing entirely from the interior of a building and which eliminates any need to weather seal the glass panels working from the building exterior.
It is another object to provide such a retainer which retains adjacent glass panels while their structural adhesive bonding cures, thereby eliminating necessity for temporary retainers.
It is another object to provide such a retainer which aesthetically does not detract from the smooth, unbroken appearance of structurally bonded glazing.
It is another object to provide such a retainer which enhances the structural integrity of the adhesively bound glass panels without detracting from the smooth, unbroken appearance of the glass panels.
It is another object to provide such a retainer which tolerates non-plumb installation of glass panels.
Other objects, features and advantages of the invention will become apparent upon reading the following detailed description in conjunction with the drawings and the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a pictorial view of a representative portion of the curtainwall framing system as viewed from the exterior.
FIG. 2 is a horizontal cross-sectional view through a curtainwall framing system according to a first preferred embodiment of the present invention, including a vertical framing member, a first preferred embodiment retainer, and two glass panels. However, spacers and structural adhesive according to the present invention are not yet in place.
FIG. 3 is similar in view to FIG. 2, except that the spacers and structural adhesive are shown in place.
FIG. 4 is an isolated cross-sectional view of a first preferred embodiment of the retainer of the present invention.
FIG. 5 is a partial close up view of that shown in FIG. 4.
FIG. 6 is an isolated cross-sectional view of a second preferred embodiment of the retainer of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring more particularly to the drawings, in which like numerals represent like parts throughout the separate views, FIG. 1 shows a representative portion of a "two-sided" SSG curtainwall framing system including vertical framing members 10, horizontal framing members 13, horizontal exterior retention members 15, a glass panel or panels 19, and vertical retainers 28.
Vertical framing members 10 may be linked together by means known in the art to horizontal framing members 13 to form a substantially rigid framework to which the plurality of glass panels 19 may be attached.
The weight of each of the glass panels 19 is supported by shelves attached to or an integral part of the horizontal frame members 13, as known in the art. As this is a two-sided SSG system, two edges of each glass panel, in this case the horizontal edges, are retained by horizontal exterior retention members 15, such as is known in the art. The other, in this case, vertical edges of the glass panels are captured and-retained by retainers 28, as discussed in further detail later in this application. FIG. 3 shows a transverse cross section through a vertical framing member 10, an elongate profile extruded of architectural aluminum. Adjacent glass panels 12 and 14 are secured to the outward face 11 of the framing member 10 by structural adhesive beads 16 and .18, respectively. In the preferred embodiment, the structural adhesive is structural silicone adhesive. Each glass panel has dual panes, specifically, interior and exterior panes 20, 22, respectively, separated and linked as known in the art by a glass spacer 24 along the edges of the panel so as to form an air space 26 between the panes 20 and 22 for thermal insulation purposes. The silicone beads 16, 18 extend along the height of the glass panels 12, 14, to sufficiently bond the panels to the vertical framing member 10.
A retainer 28 provides mechanical retention of the adjacent glass panels 12, 14 to the framing member 10 to facilitate installation of the silicone beads 16, 18, as discussed in further detail below, and also to provide a safety feature should the silicone adhesive fail. The retainer 28 is elongate and extends lengthwise along the framing member 10. The elongate retainer 28 has a generally I-shaped transverse cross section (not including its "T"-shaped securing head 52) which forms a pair of opposing elongate channels 58, 60 (see FIG. 4), each configured to accept the edge of a corresponding glass panel 12, 14 and also to accept a corresponding spacer 40, 42.
The retainer 28 includes a generally planar base element 30 which, when installed, is urged against the outward face 11 of the vertical framing member 10. The retainer 28 also includes a generally planar foot element 32 which, when installed, contacts the exterior vertical edges 34 and 36 of the adjacent glass panels 12 and 14. The base element 30 and foot element 32 are spaced apart by a generally planar spine element 38 by a distance roughly equal to the combined thickness of the glass panel 12 and the spacer 40. It should be understood that in the preferred embodiment of the retainer in its unloaded configuration as shown in FIG. 4, the primary planar surfaces of the spine 38 are substantially perpendicular to the primary planar surfaces of the base element 30 and the foot element 32.
Referring to FIG. 4, a first preferred embodiment of the retainer according to the present invention is shown as 28.
Referring now to FIG. 3, elongate resilient spacers 40 and 42, when installed, are wedged between the base element 30 of the retainer and the interior edges 44 and 46 of the glass panels, and are positioned within the channels 58, 60 defined by the retainer. Each spacer 40, 42 in transverse cross section has a leading wedge-shaped nose to facilitate its insertion and has an interior compression void 48, 50, respectively, provided to enhance deformability. The spacers 40, 42, are elongate and coextensive with the silicone bead and the framing member, and, when in position, provide opposing forces sufficient to urge its associated glass panel outwardly and securely against the foot element 32 of the retainer. When the spacers 40, 42 are in place, they also urge the outside edges of the glass panels 12, 14, respectively, against the foot 32 of the retainer 28.
As previously discussed, the retainer 28 includes a securing head 52 extending from the center of the retainer base element 30 opposite the foot element 32. The securing head 52 has a T-shaped transverse cross section and extends lengthwise along the retainer 28. The securing head 52 is configured for engagement with a reciprocal T-shaped channel 54 defined by framing member 10. As will be discussed in further detail later in this application, T-shaped securing head 52 may slide freely within securing channel 54 when the spacers 40, 42 are not in position, such as shown in FIG. 2. However, when the spacers 40, 42 are in position as shown in FIG. 3, the securing head 52 is urged against the framing member 10 such that the frictional force between the elements 52, 10 effectively "locks" the elements together.
Installation of the overall assembly proceeds as follows. First, referring to FIG. 2, the securing head 52 of the elongate retainer 28 is slipped inside the securing channel 54 of the vertical framing member 10 and slidably positioned along the vertical framing member as desired. Then, the glass panels 12 and 14 are inserted into the U-shaped glazing channels 58 and 60 of the retainer 28, respectively, proceeding left to fight, for example. Next, now referring to FIG. 3, the spacers 40 and 42 are wedged into place between the flanges of the base 30 of the retainer 28, and the glass panels 12, 14, respectively, thereby snugging the fit of the glass panels 12 and 14 inside the glazing channels 58 and 60 (see only FIG. 4) of the retainer.
It should be understood that when the spacers are wedged into place, the glass panels are urged outwardly against the foot 32 of the retainer 28. As the foot is urged outwardly, it will exert an outward force upon the spine 38 of the retainer, therefore tending to pull outwardly on the center of the base 30. However, the spacers are likewise providing an inward force against the outer edges of the base 30. Therefore, as shown in FIG. 3, the center of the base will tend to deflect downwardly somewhat relative to the outer edges of the base, which will remain in contact with the outer surface 11 of the frame member 10. Due to the geometry of the retainer 28, spacers 40, 42 and the securing channel 54, this deflection causes the T-shaped head 52 of the retainer to come into frictional contact with the securing channel 54, thus providing frictional securement between the retainer and the frame member 10.
Finally, the structural silicone beads 16 and 18 are gunned and tooled, as known in the art, into the space behind the wedge shaped spacers 40 and 42, thereby contacting the framing member 10 and the inside vertical edges 44 and 46 of the glass panels 12 and 14. Installation across the framing system continues left to fight in a similar manner.
After the structural silicone cures, a strong structural adhesive bond is formed which provides primary support of the glass panels. However, should the silicone rupture, the retainer provides temporary support until the ruptured silicone bead can be repaired.
Referring to FIG. 6, preferably, the second preferred retainer profile 128 includes cushion pads 56, 57, preferably coextruded as an integral part of retainer 28. The cushion pads 57, hereinafter referred to as "spine" cushion pads 57, protrude from the spine 38 of the retainer 128, and serve the purpose of cushioning contact between the retainer 128 and either of the glass panels 12 and 14 beyond that afforded by the resiliency of the retainer itself. This cushioning is especially effective when one of the glass panels 12, 14, is in contact with the retainer 128, and the other of the glass panels 12, 14 is brought into contact with the retainer. Cushioning pads 56, hereinafter referred to as foot cushioning pads 56, extend from the inside of the foot 32 of the retainer 128, and contact the outside surfaces of the glass panels when installed, providing a cushioning and weatherproofing function.
Retainers 28 or 128 are each preferably coextruded profiles composed of different materials, with most of the retainer (the securing head, spine, head, and base) composed of a substantially rigid but deflectable and resilient compound polyvinyl chloride known in the art as CPVC, such as that sold under the brand name "Temprite 88997". The pads 56, 57, if used, are preferably composed of dense elastomeric material, deformable but resilient, such as that known as "ALCRYN", manufactured by Dupont. The outside surface of the foot 32 (see FIG. 5) may be provided with a coextruded layer 33 of semirigid polyvinyl chloride, treated as known in the art to be "UV resistant" (capable of resisting deterioration due to ultraviolet light exposure).
The spacers 40, 42 are preferably extruded from an elastomeric rubber material (compatible with structural silicone) being deformable but resilient.
Therefore it may be seen that the present invention provides a simple, cost-efficient, and reliable retainer assembly for effective retention and weathersealing of glass panels in structural silicone adhesive systems. The retainer assembly may be installed from the inside of the building, thus obviating the need for exterior scaffolding. The retainer assembly maintains glass panels in place during the application of structural adhesive, and also acts as a safety means should the adhesive fail. The portion of the retainer assembly viewable from the exterior of the building is unobtrusive, thus providing a desirable smooth outside appearance.
While the invention has been described in detail with particular reference to the disclosed embodiments, it is to be understood that variations and modifications may be utilized without departing from the principles and scope of the invention as defined by the following claims. | A retainer and weatherseal for structurally bonded glazing, which includes an elongate retainer profile having a generally H-shaped transverse cross section, thereby forming a pair of elongate U-shaped retaining channels; and securing device for securing the profile coextensively along a curtainwall framing member, such that one side of the pair of retaining channels is urged against the framing member. The retainer may be in combination with a curtainwall framing member, which includes a framing member having securing device longitudinally along the outward face of the framing member, for receiving the securing device and which are reciprocally configured, the retainer being secured to the framing member with the securing device interlocked in the securing device. The retainer and framing member combination are utilized in a curtainwall framing system having structurally bonded glazing wherein each of the intermediate vertical framing members of the system include the retainer and framing member. | 4 |
TECHNICAL FIELD
[0001] This invention relates to wafer bonded vertical cavity surface emitting laser (VCSEL) systems and methods of making the same.
BACKGROUND
[0002] A VCSEL is a laser device formed from an optically active semiconductor layer (e.g., AlInGaAs or InGaAsP) that is sandwiched between a pair of highly reflective mirror stacks, which may be formed from layers of metallic material, dielectric material or epitaxially-grown semiconductor material. Typically, one of the mirror stacks is made less reflective than the other so that a portion of the coherent light that builds in a resonating cavity formed in the optically active semiconductor layer between the mirror stacks may be emitted from the device. Typically, a VCSEL emits laser light from the top or bottom surface of the resonating cavity with a relatively small beam divergence. VCSELs may be arranged in singlets, one-dimensional or two-dimensional arrays, tested on wafer, and incorporated easily into an optical transceiver module that may be coupled to a fiber optic cable.
[0003] In general, a wafer bonding technique may be characterized as a direct wafer bonding technique or a metallic wafer bonding technique. In direct wafer bonding, two wafers are fused together by mass transport at a bonding interface. Direct wafer bonding may be performed between any combination of semiconductor, oxide, and dielectric materials. Direct wafer bonding typically is performed at high temperature and under uniaxial pressure. In metallic wafer bonding, two substrates are bonded together by a metallic layer that is melted and re-solidified at a bonding interface.
[0004] Wafer bonding techniques have been used in the fabrication of optoelectronic devices. For example, U.S. Pat. No. 6,320,206 has proposed a scheme for forming optical devices having aluminum gallium indium nitride active layers and high quality mirror stacks that are wafer bonded on one or both sides of the active layers. U.S. Pat. No. 5,837,561 describes a vertical cavity surface emitting laser that is wafer bonded to a transparent substrate. A top circular metal contact is disposed on the transparent substrate and a second metal contact is disposed over the bottom mirror of the vertical cavity surface emitting laser. The transparent substrate serves as an escape medium for laser emission through the top circular metal contact. This configuration allows the heat producing active layer of the vertical cavity surface emitting laser to be mounted near a heat sink, thereby improving the performance of the device.
SUMMARY
[0005] The invention features vertical cavity surface emitting laser systems and methods of making the same. In particular, the invention features a vertical cavity surface emitting laser system having a bottom side that may be flip-chip mounted to a driver substrate and a top side configured to transmit light through an optically transparent substrate. By this configuration, the invention enables vertical cavity surface emitting laser systems to be packed together with a greater density and operated at greater speeds relative to, for example, wire bonded vertical cavity surface emitting laser systems. In addition, such systems may be flexibly tailored to produce light over a wide range of wavelengths. Such systems also may be efficiently packaged on a wafer scale.
[0006] In one aspect, the invention features a vertical cavity surface emitting laser (VCSEL) system, comprising a substrate, a vertical stack structure, and a pair of contacts. The substrate is optically transparent to light in a selected wavelength range. The vertical stack structure has a substantially planar top side, which is wafer bonded to the optically transparent substrate, and a bottom side. The vertical stack structure includes a top mirror, a bottom mirror, and a cavity region that is disposed between the top mirror and the bottom mirror and includes an active light generation region that is operable to generate light in the selected wavelength range. The vertical stack structure is constructed and arranged to direct light generated in the cavity region to the optically transparent substrate.
[0007] First and second contacts are disposed over the bottom side of the vertical stack structure and are electrically connected for driving the cavity region.
[0008] Embodiments in accordance with this aspect of the invention may include one or more of the following features.
[0009] In some embodiments, the optically transparent substrate comprises glass (e.g., borosilicate glass). In other embodiments, the optically transparent substrate comprises gallium phosphide.
[0010] The VCSEL system may further comprise a lens that is disposed on the glass substrate in alignment with the active light generation region.
[0011] In some embodiments, at least one of the top mirror and the bottom mirror has a layer with a peripheral region that is oxidized into an electrical insulator as a result of exposure to an oxidizing agent. In these embodiments, the VCSEL system may further comprise two or more etched holes each extending from a substantially planar surface of the bottom mirror to the oxidized peripheral region.
[0012] The top mirror and the bottom mirror preferably each comprises a system of alternating layers of different refractive index materials. For example, the top mirror and the bottom mirror each may comprise a system of alternating layers of relatively high aluminum content AlGaAs and relatively low aluminum content AlGaAs.
[0013] In some embodiments, the VCSEL system further comprises an integrated circuit that is bonded to the pair of contacts and is operable to drive the cavity region.
[0014] In another aspect, the invention features a method of fabricating the above described VCSEL system. In accordance with this inventive method, a sacrificial substrate is provided. A vertical stack structure having a substantially planar top side and a bottom side is formed over the vertical stack structure. The vertical stack structure includes a top mirror, a bottom mirror, and a cavity region that is disposed between the top mirror and the bottom mirror and includes an active light generation region operable to generate light in a selected wavelength range. The vertical stack structure is constructed and arranged to direct light generated in the cavity region away from the sacrificial substrate. The substantially planar top side of the vertical stack structure is wafer bonded to a substrate that is optically transparent to light in the selected wavelength range. The sacrificial substrate is removed after the optically transparent substrate has been wafer bonded to the substantially planar top side of the vertical stack structure. First and second contacts that are electrically connected for driving the cavity region are formed over the bottom side of the vertical stack structure.
[0015] Other features and advantages of the invention will become apparent from the following description, including the drawings and the claims.
DESCRIPTION OF DRAWINGS
[0016] [0016]FIG. 1 is a diagrammatic cross-sectional side view of a vertical cavity surface emitting laser system that is flip chip mounted to a driver substrate and an optical fiber positioned on an opposite side of a package window to receive light generated by the vertical cavity surface emitting laser system.
[0017] [0017]FIG. 2 is a flow diagram of a method of making the vertical cavity surface emitting laser system of FIG. 1.
[0018] [0018]FIG. 3A is a diagrammatic cross-sectional side view of a bottom mirror formed over a sacrificial substrate.
[0019] [0019]FIG. 3B is a diagrammatic cross-sectional side view of a cavity region formed over the bottom mirror of FIG. 3A.
[0020] [0020]FIG. 3C is a diagrammatic cross-sectional side view of a top mirror formed over the cavity region of FIG. 3B and oxidation holes formed in the resulting vertical stack structure.
[0021] [0021]FIG. 3D is a diagrammatic cross-sectional side view of an optically transparent substrate wafer bonded to the top mirror of FIG. 3C.
[0022] [0022]FIG. 3E is a diagrammatic cross-sectional side view of the vertical cavity surface emitting laser system of FIG. 3D after the sacrificial substrate has been removed.
[0023] [0023]FIG. 3F is a diagrammatic cross-sectional side view of the vertical cavity surface emitting laser system of FIG. 3E after the bottom surface has been patterned and a pair of contacts has been formed over a bottom side of the vertical stack structure.
DETAILED DESCRIPTION
[0024] In the following description, like reference numbers are used to identify like elements. Furthermore, the drawings are intended to illustrate major features of exemplary embodiments in a diagrammatic manner. The drawings are not intended to depict every feature of actual embodiments nor relative dimensions of the depicted elements, and are not drawn to scale.
[0025] Referring to FIG. 1, in one embodiment, a vertical cavity surface emitting laser system 10 includes an optically transparent substrate 12 , a vertical stack structure 14 , and a pair of contacts 16 , 18 that are flip chip bonded to a driver substrate 20 . In operation, a driving circuit disposed on driver substrate 20 applies a current between contacts 16 , 18 that drives vertical stack structure 14 to generate light 22 in a selected wavelength range. Light 22 passes through optically transparent substrate 12 and is collimated by a first lens 24 that is disposed on optically transparent substrate 12 . A second lens 26 , which is disposed on an optically transparent package window 28 , focuses the collimated light 22 received from first lens 24 into an optical fiber 30 .
[0026] Referring to FIGS. 2 and 3A- 3 F, and initially to FIGS. 2 and 3A, vertical cavity surface emitting laser system 10 may be fabricated as follows. Initially, a bottom mirror stack 32 is formed on a sacrificial substrate 34 (step 36 ; FIG. 2). Bottom mirror stack 32 includes a system of alternating layers of different refractive index materials that forms a distributed Bragg reflector (DBR) that is designed for a desired operating laser wavelength (e.g., a wavelength in the range of 650 nm to 1650 nm). For example, bottom mirror stack 32 may be formed of alternating layers of high aluminum content AlGaAs and low aluminum content AlGaAs. The layers of bottom mirror stack 32 preferably have an effective optical thickness (i.e., the layer thickness multiplied by the refractive index of the layer) that is about one-quarter of the operating laser wavelength. Sacrificial substrate 34 preferably is formed from a material that is lattice-matched to the layers of bottom mirror stack 32 . For example, sacrificial substrate 34 may be formed from GaAs, InP, sapphire (Al 2 O 3 ), or InGaAs and may be undoped, doped n-type (e.g., with Si) or doped p-type (e.g., with Zn). A buffer layer (not shown) may be grown on sacrificial substrate 34 before bottom mirror stack 32 is formed. As shown in FIG. 3B, a cavity region 38 is formed over bottom mirror stack 32 (step 40 ; FIG. 2). Cavity region 38 includes one or more active layers 42 , 44 (e.g., a quantum well or one or more quantum dots). In some embodiments, active layers 42 , 44 may be sandwiched between a pair of spacer layers (not shown). In other embodiments, active layers 42 , 44 may be located above or below a single spacer layer. Active layers 42 , 44 may be formed from AlInGaAs (i.e., AlInGaAs, GaAs, AlGaAs and InGaAs), InGaAsP (i.e., InGaAsP, GaAs, InGaAs, GaAsP, and GaP), GaAsSb (i.e., GaAsSb, GaAs, and GaSb), InGaAsN (i.e., InGaAsN, GaAs, InGaAs, GaAsN, and GaN), or AlInGaAsP (i.e., AlInGaAsP, AlInGaAs, AlGaAs, InGaAs, InGaAsP, GaAs, InGaAs, GaAsP, and GaP). Other quantum well layer compositions also may be used. The first and second spacer layers (if present) may be formed from materials chosen based upon the material composition of the active layers.
[0027] Referring to FIG. 3C, a top mirror stack 46 is formed over cavity region 38 (step 48 ; FIG. 2). Top mirror stack 46 preferably is formed from the same material system as bottom mirror stack 32 . In the illustrated embodiment, bottom and top mirror stacks 32 , 46 are cooperatively designed so that laser light 22 is emitted from a substantially planar top surface 50 of vertical stack structure 14 and through optically transparent substrate 12 (see FIG. 1).
[0028] The layers of vertical stack structure 14 may be formed by conventional epitaxial growth processes, such as metal-organic chemical vapor deposition (MOCVD) and molecular beam epitaxy (MBE). As shown, in the illustrated embodiment, vertical stack structure 14 has a planar structure that includes a number of holes 52 , 54 that expose a number of respective side regions of the bottom and top mirror stacks 32 , 46 to be oxidized. At least a portion of each of bottom mirror stack 32 and top mirror stack 46 is oxidized from the exposed side regions inwardly toward a centrally located aperture region 56 . In this embodiment, four holes (two of which are not shown in the drawings) are opened at locations that are equidistant from the center of aperture region 56 . The holes 52 , 54 extend from a bottom surface of bottom mirror stack 32 to the layer (or layers) corresponding to the portion of vertical stack structure 14 to be oxidized. When the vertical stack structure 14 is exposed to heated water vapor, the heated water vapor enters the holes and oxidizes one or more layers of vertical stack structure 14 in a radial direction away from the holes. The oxidation process continues until an oxidation front from each hole merges to form the un-oxidized aperture region 56 . Other vertical stack structure embodiments may include more or fewer exposure holes or exposed regions with other shapes, such as divided arcs or rings.
[0029] As shown in FIG. 3D, optically transparent substrate 12 is wafer bonded to the substantially planar top surface 50 of vertical stack structure 14 (step 58 ; FIG. 52). The optically transparent substrate 12 preferably is substantially transparent to light in a selected wavelength range. In general, the selected wavelength range encompasses the wavelength of light generated by vertical stack structure 14 . For example, in some embodiments the optically transparent substrate 12 is substantially transparent to light having a wavelength in the range of 650 nm to 1650 nm. In some embodiments, optically transparent substrate 12 is formed from glass (e.g., borosilicate glass). The use of borosilicate glass in gallium arsenide based embodiments is particularly advantageous because the thermal expansion properties of borosilicate glass and gallium arsenide are closely matched. Borosilicate glass also is advantageous because it allows low temperature processing and is transparent to visible and near-IR wavelengths of light. In other embodiments, optically transparent substrate 12 is formed from gallium phosphide. In other embodiments, optically transparent substrate 12 may be formed from other materials. In general, optically transparent substrate 12 may be attached to surface 50 by a conventional direct wafer bonding process or a conventional metallic bonding process that is tailored to the selected material systems of optically transparent substrate 12 and vertical stack structure 14 .
[0030] As shown in FIG. 3E, after the optically transparent substrate 12 has been wafer bonding to vertical stack structure 14 (step 58 ; FIG. 2), sacrificial substrate 34 is removed (step 60 ; FIG. 2). In general, sacrificial substrate 34 may be removed by any one of a wide variety of conventional substrate removal processes. For example, in one embodiment, sacrificial substrate 34 may be removed by a selective wet chemical etching process. In this embodiment, an etch stop layer 62 (see FIG. 3D) preferably is formed between the sacrificial substrate 34 and bottom mirror stack 32 . In another embodiment, sacrificial substrate 34 may be removed by laser melting. In some embodiments, etch stop layer 62 also may be removed.
[0031] Referring to FIG. 3F, after sacrificial substrate 34 has been removed (step 60 ; FIG. 2), vertical stack structure is patterned and etched, and contacts 16 , 18 are formed over the bottom side of the patterned vertical stack structure (step 64 ; FIG. 2). The vertical stack structure may be formed by a conventional photolithographic patterning and etching process.
[0032] Referring back to FIG. 1, in the illustrated embodiment, lens 24 is formed on the opposite surface of optically transparent substrate 12 as the vertical stack structure 14 . Lens 24 (and the corresponding lens 26 of package window 28 ) may be a replicated epoxy lens or a diffractive optical element (DOE).
[0033] In the illustrated embodiment, contacts 16 , 18 may be bonded to corresponding contacts of a suitable driving circuit disposed on driver substrate 20 using a flip-chip solder bonding process. In this embodiment, solder bumps 66 , 68 are disposed between contacts 16 , 18 and the corresponding metallization pattern of the driving circuit. The Z-axis dimensions of solder bumps 66 , 68 are selected to separate the bottom side of vertical stack structure 14 from the driving circuit by an appropriate distance. During manufacture, solder bumps 66 , 68 originally may be disposed on the metallization pattern of the driving circuit. Vertical cavity surface emitting laser system 10 is aligned with the driving circuit to within an accuracy required for solder bumps 66 , 68 to contact the corresponding driving circuit metallization pattern. The assembly then is raised to a temperature at or above the melting point of solder bumps 66 , 68 . Solder bumps 66 , 68 wet the solderable contacts 66 , 68 and surface tension forces pull vertical cavity surface emitting laser system 10 and driver substrate 20 into very precise alignment (e.g., to within +4 μm). The assembly is cooled to form a solidly bonded, accurately aligned structure.
[0034] Electrical contacts 16 , 18 enable vertical cavity surface emitting laser system 10 to be driven by the driving circuit that is disposed on driver substrate 20 . In operation, an operating voltage is applied across electrical contacts 16 , 18 to produce a current flow in vertical stack structure 14 . In general, current flows through a central region of the vertical stack structure 14 and lasing occurs in a central portion of cavity region 38 (hereinafter the “active region”). The oxidized portions of bottom and top mirror stacks 32 , 36 form an oxide confinement region that laterally confines carriers and photons. Carrier confinement results from the relatively high electrical resistivity of the confinement region, which causes electrical current preferentially to flow through a centrally located region of vertical stack structure 14 . Optical confinement results from a substantial reduction of the refractive index of the confinement region that creates a lateral refractive index profile that guides the photons that are generated in cavity region 38 . The carrier and optical lateral confinement increases the density of carriers and photons within the active region and, consequently, increases the efficiency with which light is generated within the active region.
[0035] Other embodiments are within the scope of the claims. | Vertical cavity surface emitting laser systems and methods of making the same are described. In one aspect, a vertical cavity surface emitting laser system has a bottom side that may be flip-chip mounted to a driver substrate and a top side that is configured to transmit light through an optically transparent substrate. By this configuration, vertical cavity surface emitting laser systems may be packed together with a greater density and operated at greater speeds relative to, for example, wire bonded vertical cavity surface emitting laser systems. In addition, such systems may be flexibly tailored to produce light over a wide range of wavelengths. Such systems also may be efficiently packaged on a wafer scale. | 7 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to an attachment apparatus for a walker caddy and, more particularly, to an attachment apparatus that is adjustable to accommodate a variety of walker designs.
2. Description of the Related Art
Many medical patients, elderly people, and the like need aid in moving about. Walkers are widely known aids for the aged, handicapped, injured or other individuals who require some stabilization while walking. When using a walker, both hands of the individual are needed in order to move the walker itself with each step taken. Therefore, it can be extremely difficult for walker users to carry other items with them.
Numerous attempts have been made to correct for the foregoing problems. For instance, U.S. Pat. No. Des. 340,012, issued in the name of Azzarelli, which is hereby incorporated herein by reference in its entirety, discloses the ornamental design for a walker caddy container. The inventor of this reference is the same inventor of the present invention herein. Additionally, U.S. Pat. No. Des. 324,504, issued in the name of Olsen, discloses the ornamental design for a carrier for use with a walker. Further, U.S. Pat. No. 4,974,760, issued in the name of Miller, discloses an article carrier attachable to a front brace of a walker and composed of a flexible material whereby the article carrier is foldable with the walker as the walker is collapsed for storage or transport.
However, the above references do not address the problem of attaching the walker caddy container to a variety of walker designs. As is well-known in the art, some walkers have a straight bar design, while other walkers have a V-bar design. This variety of walker designs prevents some walker caddy containers from being attached to some walker designs. Consequently, a need has been felt for providing an attachment apparatus for a walker caddy container that is adjustable to accommodate a variety of walker designs for efficient universal attachment thereto.
SUMMARY OF THE INVENTION
It is therefore an object of the present invention to provide an improved attachment apparatus for a walker caddy container that is adjustable to accommodate a variety of walker designs for efficient universal attachment thereto.
It is a feature of the present invention to provide an improved attachment apparatus that is adjustable by pivoting a support arm about a rotating disc.
It is a further feature of the present invention to provide an improved attachment apparatus that has a mounting bracket that receives a hanger arm in a one of a plurality of positions.
It is a further feature of the present invention to provide an improved attachment apparatus that provides a hanger arm that is vertically adjustable.
Briefly described according to one embodiment of the present invention, an improved apparatus for attaching a walker caddy container to a conventional walker is provided, wherein the apparatus is easily adjustable, without additional adapters, to accommodate attachment to a variety of walker designs. The apparatus comprises a pair of hanger arms which are adjustable and which provide vertical support by hanging from a horizontal connecting member of the walker, while a pair of support arms provide horizontal support by pressing against one each of a pair of forward leg members of the walker. The support arms are attached to a rotatable disc positioned beneath the walker caddy container, thereby to provide extendable adjustability to the support arms in order to accommodate horizontal support against a variety of walker designs. The support arms are slidably mounted to the walker caddy container and are lockable into a desired position.
Another preferred embodiment of the present invention provides an apparatus for attaching a container to a walker, which walker includes a first pair of legs having upper end portions and a first hand grip means connecting the upper end portions, a second pair of legs having upper end portions and a second hand grip means connecting the upper end portions of the second pair of legs, the first pair of legs spaced a predetermined distance from the second pair of legs, and a structural member connecting the upper end portion of one of the first pair of legs with the upper end portion of one of the second pair of legs to define a space within the walker bounded by the first and second pairs of legs, the apparatus for attaching the container comprising: hanger means for hanging the container from the structural member; support means for supporting the container against one of the first pair of legs and one of the second pair of legs; mounting means for mounting the hanger means and the support means to the container.
An advantage of the present invention is easy attachment to and detachment from a walker.
Another advantage of the present invention is adjustability to accommodate different walkers having a variety of different structural designs.
BRIEF DESCRIPTION OF THE DRAWINGS
The advantages and features of the present invention will become better understood with reference to the following more detailed description and claims taken in conjunction with the accompanying drawings, in which like elements are identified with like symbols, and in which:
FIG. 1 is a perspective view of walker caddy container which has been removably attached to a walker with an attachment apparatus according to a preferred embodiment of the present invention;
FIG. 2 is a bottom plan view of the walker caddy container showing the attachment apparatus according to a preferred embodiment of the present invention;
FIG. 3 is an exploded perspective view of the molded support arm and associated disc according to a preferred embodiment of the present invention;
FIG. 4 is an exploded perspective view of the mounting bracket and hanger arm with associated hardware, according to a preferred embodiment of the present invention; and
FIG. 5 is a partial cross-section of the mounting bracket of FIG. 4.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
1. Detailed Description of the Figures
Referring now to FIG. 1, there is shown generally a walker caddy container 10 which is removably attached to a conventional foldable walker 12. A preferred embodiment of the walker caddy container 10 defines therewithin a cylinder-shaped drink cup area 10a, a storage area 10b, and cylinder-shaped pencil areas 10c and 10d.
The walker 12 includes a first pair of generally vertical leg members comprising a forward leg member 14 and an aft leg member 16. The upper ends of the leg members 14 and 16 are joined by a generally horizontal connecting member 17 which may be a separate member connected thereto or, as shown, integral with the upper portions of the legs. The connecting member 17 may include a suitable hand grip 15 intermediate thereof. As used herein, the terms "vertical" and "horizontal" are meant to be relative to the upright position of the walker 12 and caddy container 10, as shown in FIG. 1, for ordinary use. The walker 12 also includes a second pair of leg members comprising a forward leg member 18 and an aft leg member 20 which are similar to leg members 14 and 16 and the upper ends of which are suitably connected by a connecting member 22 which is similar to connecting member 17 and which may also include a suitable hand grip 15. A pair of members 24 may be suitably connected between and intermediate the ends of the first pair of leg members 14 and 16 for structurally stabilizing, i.e. bracing, thereof. Similar bracing members 26 may be suitably attached between and intermediate the ends of the second pair of leg members 18 and 20. Each of the leg members may be provided with suitable rubber feet 28 for contacting the floor.
A sleeve 30 circumferentially surroundingly engages the upper portion of forward leg member 14 and is circumferentially slidable thereabout. A similar sleeve 32 similarly engages the forward leg 18. A brace member 34 extends between and is suitably and rigidly attached to the upper portions of the sleeves 30 and 32. Suitable means (not shown), which are conventionally known in the art, are provided to lock the positions of the forward leg members 14 and 18 circumferentially relative to the respective sleeves 30 and 32 to the open position of the walker 12 for use as shown in FIG. 1, the locking means being releasable to allow circumferentially slidable movement of the forward legs 14 and 18 within the respective sleeves 30 and 32 for collapsing or folding the walker for storage or transportation thereof such as in the trunk of an automobile or the like. The walker 12 which has been described may be of any suitable shape and size, and such walker are conventionally known to those of ordinary skill in the art to which this invention pertains. For example, to accommodate most adults, each of the legs 14, 16, 18, and 20 may have a height of perhaps 30 to 38 inches, the distance between each forward leg member and the respective aft leg member at the upper portions thereof may be perhaps 11 inches, and the length of the brace member 34 may be perhaps 16 inches, whereby the first pair of leg members 14 and 16 is spaced from the second pair of leg members 18 and 20, when the walker 12 is open and ready for use, a distance 36, which is equal to perhaps 16 inches (equal substantially to the length of the brace 34). Thus, a space 38, of perhaps 11 inches by 16 inches in a horizontal plane is provided between the pairs of leg members and rearwardly of the brace member 34 in which space 38 a user may position his or her body while standing. It is to be understood that the composition and sizing of the walker 12 may be different from that shown in FIG. 1. For instance, the brace member 34 may form a "V-bar" between the forward leg members 14 and 18. Further, the forward leg members 14 and 18 may be parallel to the aft leg members 16 and 20, respectively. Moreover, the forward leg members 14 and 18 may be sloped relative to the aft leg members 16 and 20, respectively.
Referring to FIG. 1, a pair of mounting brackets 100 is affixed to the walker caddy container 10. The mounting brackets 100 accept a pair of hanger arms 102 in a plurality of orifices 104 and 106, respectively. The pair of hanger arms 102 have a square shape 103 at a top portion thereof, thereby to be slidingly engaged within one of the plurality of orifices 104 and 106, which are also square-shaped, thereby to prevent rotatable movement of the hanger arm 102 therewithin. A molded support arm 108 and 110 (see FIG. 2) extends outwardly from beneath each of the pair of mounting brackets 100.
Referring to FIGS. 2 and 3, a bottom plan view of the pair of mounting brackets 100, as affixed to the walker caddy container 10 is shown in FIG. 2. An exploded perspective view of the mounting bracket 100 affixed to a partial walker caddy container 10 is shown in FIG. 3. The pair of hanger arms 102 are not shown. The molded support arms 108 and 110 are rotatably affixed with a bolt 202 and 204, respectively, through an orifice (not shown) and an orifice 205 respectively, proximal to an outer radius of a disc 206 and 208 respectively, which discs 206 and 208 are rotatably affixed to the walker caddy container 10 about an axle bolt 210 and 212, respectively. The bolt 204 is threaded into a nut 213, and the bolt 202 is similarly threaded into a nut (not shown). The axle bolt 212 is threaded through an orifice 215 and into a nut 217. The axle bolt 210 is similarly threaded into a nut (not shown). Additionally, the molded support arms 108 and 110 are slidably mounted upon a bolt 214 and 216 respectively, each of which is threaded through the cylinder-shaped pencil area 10c and 10d respectively (see FIG. 3) and affixed with a nut 218 and 220 respectively, thereby to adjustably extend and retract the support arm 108 and 110 from the pair of mounting brackets 100 by permitting slidable movement of the support arms within a defined slot 222 and 224 respectively, wherein the nut 218 and 220 may be tightened against the support arm 108 and 110 in order to restrict the slidable movement thereof.
In FIG. 4, an exploded perspective view of the mounting bracket 100 and hanger arm 102 with associated hardware is shown, according to a preferred embodiment of the present invention. The mounting bracket 100 houses a pair of spacers 402, one each of which is positioned beneath the plurality of orifices 104, 106, thereby to receive a cylindrical shaft 404 which extends from the square shape 103 of the top portion of the hanger arm 102 when the cylindrical shaft 404 is inserted into one of the plurality of orifices 104, 106. A stamped steel plate 406, which is positioned beneath the spacers 402, is held into place within the mounting bracket 100 by threading a machine screw 407 into a machine screw orifice 408, through the mounting bracket 100, and into a threaded orifice 409 within the stamped steel plate 406. The cylindrical shaft 404 has sufficient length to extend through either one of the spacers 402 and through the stamped steel plate 406, thereby to extend a threaded end 410 through the stamped steel plate 406. The threaded end 410 receives one of a pair of nylon washers 412 prior to receiving a nut 414 threaded thereon. The hanger arm 102 is vertically adjustable by moving the nylon shoulder washer 412 along the threaded end 410 and subsequently tightening the nut 414 thereagainst the nylon shoulder washer 412.
FIG. 5 shows a partial cross-section of the mounting bracket 100, taken along the line V--V of FIG. 4, wherein the mounting bracket 100 is affixed to a partial perspective view of the walker caddy container 10, and the hanger arm 102 is shown in full perspective view seated properly within the cross-sectional view of the mounting bracket 100.
2. Operation of the Preferred Embodiment
In operation, the support arms 108 and 110 are adjusted accordingly to extend outwardly from the walker caddy container 10, thereby to press against the forward leg member 114 and 118, respectively, in order to horizontally support the walker caddy container 10 against the conventional walker 12. The adjustment is made by rotating the respective disc 206 and 208 in order to urge the support arm 108 and 110 along slidable movement within the respective slots 222 and 224, thereby to alternately extend and retract the support arm 108 and 110 from beneath the walker caddy container 10. Upon proper adjustment to fit the conventional walker 10, the nut 218 and 220 is tightened against the support arm 108 and 110, respectively, in order to restrict the slidable movement thereof within the respective defined slots 222 and 224.
Subsequently, the pair of hanger arms 102 is fitted within the plurality of orifices 104 and 106, depending upon the width of the connecting member 17, thereby to be adjustable to a variety of widths of connecting member 17. The hanger arms 102 are passed through the spacers 402 positioned within the mounting brackets 100, and are affixed to the mounting brackets 100 by threading the nut 414 thereupon beneath the mounting bracket 100. The walker caddy container 10 is attached to the conventional walker 12 by being vertically supported by hanging from the connecting member 17 with the hanger arm 102 while the support arms 108 and 110 horizontally support the walker caddy container 10 by pressing against the forward leg member 14 and 18, respectively. In this position, the present invention is easily removable from the conventional walker 12 and easily adjustable to accommodate a variety of walker designs, such as those with a straight bar design and those with a V-bar design.
The foregoing description of the preferred embodiment of the present invention has been presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the present invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teachings.
The preferred embodiment was chosen and described in order to best explain the principles of the present invention and its practical application to those persons skilled in the art, and thereby to enable those persons skilled in the art to best utilize the present invention in various embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the present invention be broadly defined by the claims which follow. | An improved apparatus for attaching a walker caddy container to a conventional walker is provided, wherein the apparatus is easily adjustable, without additional adapters, to accommodate attachment to a variety of walker designs. The apparatus comprises a pair of hanger arms which are adjustable and which provide vertical support by hanging from a horizontal connecting member of the walker, while a pair of support arms provide horizontal support by pressing against one each of a pair of forward leg members of the walker. The support arms are attached to a rotatable disc positioned beneath the walker caddy container, thereby to provide extendable adjustability to the support arms in order to accommodate horizontal support against a variety of walker designs. The support arms are slidably mounted to the walker caddy container and are lockable into a desired position. | 0 |
BACKGROUND
This invention relates generally to bonding systems and more particularly concerns a method in which two components are bonded together using gold without other intermediate bonding materials.
Acousto-optic Bragg cells are manufactured by bonding a piezo electric substrate to an optical substrate. Cold welding systems have been used but the cold welding process is limited both in types of metals that may be used for bonding and in possible yields of working parts. For instance, indium is suited to the cold welding process, but when using indium the cold welding process must be carried out in a vacuum. In the cold welding process, the parts being cold welded together may delaminate if the parts are not sufficiently planarized with respect to each other.
Other processes which use ultrasonic welding have also been described. Ultrasonic welding allows a greater variety of metals to be used and welding pressures to be reduced by introducing heat and ultrasonic energy to the welding process. A description of ultrasonic welding apparatus and techniques is contained in Ultrasonically Welded Piezoelectric Transducers by John D. Larson, III and D. K. Winslow published in IEEE Transactions on Sonics and Ultrasonics, volume su-18, number 3, July 1971. The process, as described by Larson et. al., is to first coat the substrates with a flash of chromium or titanium to insure good adhesion of subsequent metals. Then the substrates are coated with the bonding metal and placed, with bonding surfaces in contact with each other, inside a heater. Once the heater has obtained the desired temperature, a static pressure and acoustic waves are applied to the substrates until bonding is completed.
While this system is an improvement upon traditional cold welding systems, excessive substrate heating and inadequate planarization of the substrates can cause improper bonding and breakage of parts.
Other attempts to achieve gold to gold bonds have been unsuccesful because the pressures to achieve bonding cause breakage of parts. Reduction of bonding pressure causes improper bonding and lack of adhesion.
The present process provides an alternative to both traditional cold welding process and traditional ultrasonic welding processes. This process uses a combination of interferometric planarization feedback, thermal agitation and profile heating to optimize the bonding process. This process produces better bonding characteristics with higher yields then previously known processes.
Further advantages of the invention will become apparent as the following description proceeds.
SUMMARY OF THE INVENTION
Briefly stated and in accordance with the present invention, there is provided a bonding system for bonding two substrates together where a chuck is used for holding two substrates, a heater is used for heating the two substrates, and a press is used for pressing the substrates together. The press is attached to the chuck and the press includes a window for receiving one of the substrates against it during pressing. A light source is arranged to shed light on the two substrates. The light source is chosen to pass through the window of the press while being reflected by the two substrates. A light collector is arranged to collect light from the light source after reflection from the two substrates and is attached to a display to display the light collected by the collector. An adjuster is also attached to the press for optimizing the planarity of the two substrates with each other.
The bonding system can be used in a bonding process to bond the two substrates by first viewing two surfaces of the two substrates under an initial pressure by looking at display means, then optimizing the planarity of the two surfaces according to the display on the display means by adjusting the adjuster and then finally increasing the initial pressure to a bonding pressure.
The bonding system and bonding process can be used to produce two substrates bonded together with a single bonding material between them.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front view of a bonding system including a user interface/control module, a planarizing and bonding module, a chuck and agitation module, an interferometric vision system, and a CRT display.
FIG. 2 is a front, internal view of the chuck and agitation module in the bonding system in FIG. 1.
FIG. 3 is a top view of the chuck and agitation module in FIG. 2.
FIG. 4 is an optical schematic of the interferometric vision system and the CRT display of the bonding system in FIG. 1.
FIG. 5 is a front, internal view of the chuck and agitation module with planarizing and bonding module of the bonding system in FIG. 1.
FIG. 6 is the displayed output on the CRT display from the interferometric vision system when planarization is inadequate for bonding.
FIG. 7 is the displayed output on the CRT display from the interferometric vision system when planarization is adequate for bonding.
While the present invention will be described in connection with a preferred embodiment and method of use, it will be understood that it is not intended to limit the invention to that embodiment/procedure. On the contrary, it is intended to cover all alternatives, modifications and equivalents as may be included within the spirit and scope of the invention as defined by the appended claims.
______________________________________Alpha-Numeric List of Elements______________________________________10 bonding system12 user interface/control module14 planarizing and bonding module16 line20 line22 chuck and agitation module24 line26 interferometric vision system28 CRT display30 upper substrate32 lower substrate33 planarization plate34 chuck35 upper surface36 insulating bellows37 lower surface38 heated air nozzles39 upper surface40 bonding interface42 wedged viewing window43 upper surface44 insulated chamber46 heated air tube47 heated air nozzle48 laser50 beam52 neutral density filter54 polarizer56 beam steering optic58 beam steering optic60 spatial filter62 collimator64 beam68 beamsplitter70 beamsplitter76 polarizer78 camera assembly80 main actuator82 fine actuator84 central plate86 interference pattern lines______________________________________
DETAILED DESCRIPTION OF THE INVENTION
Turning now to FIG. 1 a block diagram of the bonding system 10 is shown. Operator control of the bonding system 10 is through a user interface/control module 12. The user interface/control module 12 controls operation of a planarizing and bonding module 14 through line 16, and a chuck and agitation module 22 through two lines 20, 24. Additionally, an interferometric vision system 26 provides visual data of the bonding process to a CRT display 28. Based on the visual data displayed on the CRT display 28, an operator may make infinitesimal adjustments to the bonding system 10 through the user interface/control module 12.
FIG. 2 represents a frontal view of the chuck and agitation module 22. Upper substrate 30 and lower substrate 32 are mated at the lower surface 37 of the upper substrate 30 and the upper surface 39 of the lower substrate 32, and inserted into a chuck 34. Both the lower surface 37 and the upper surface 39 are coated with bonding materials such as gold, and when mated, the bonding materials form a bonding interface 40.
The chuck 34 is located on planarization plate 33. The planarization plate 33 mates with insulating bellows 36 containing heated air nozzles 38. When the planarization plate 33 is mated with the insulating bellows 36, an insulated chamber 44 is formed. The heated air nozzles 38 are aimed inside the insulated chamber 44 at the mated substrates 30, 32. The upper substrate 30 has its upper surface 35 pressed up against a wedged viewing window 42. Heated air tube 46 is also attached to the insulating bellows 36 with a heated air nozzle 47 directed at the upper surface 43 of a wedged viewing window 42. Between the mated substrates 30,32 is a bonding interface 40.
FIG. 3 shows a top view of the mated upper substrate 30 and the lower substrate 32 as viewed from section line 3--3 in FIG. 2. On opposing sides of the mated upper substrate 30 and lower substrate 32 are the heated air nozzles 38.
FIG. 4 shows a schematic of the interferometric vision system 26 operating with the wedged viewing window 42 and the planarizing and bonding module 14. A light source 48 sends a beam 50 through a neutral density filter 52, a polarizer 54, two beam steerers 56, 58 and spatial filter 60 before hitting a collimator 62. When the beam 50 emerges from the collimator 62 it passes through a beamsplitter 68. Beam 50 then travels through a right angle prism 86 and is directed through the wedged viewing window 42. After passing through the wedged viewing window 42, beam 50 is bounced back from the lower surface 37 and the upper surface 3 of the upper substrate 30 which is inside the planarizing and bonding module 14 as beam 64. Beam 64 is then returned to the right angle prism 86 and then is steered by two beamsplitters 68, 70. Beam 64 then travels through a polarizer 76 and camera assembly 78 before being displayed on a CRT display 28.
In operation the interferometric vision system 26 uses the interference of two reflected portions, from the lower surface 37 of upper substrate 30 and the upper surface 35 of upper substrate 30, of a coherent light. When the two reflected portions are recombined they produce interference fringes which describe the separation between the two surfaces. To work correctly, the beam 50 must be chosen to have the correct coherent length. The coherent length is the distance the beam 50 travels while remaining in phase. If the distance between the two reflecting surfaces is two inches apart, the beam 50 must have a coherent length of at least two inches. Most monochromatic light sources such as a mercury lamp, neon lamp or a laser light source would satisfy this requirement. If the distance is very small, then the coherent length of the beam 50 may be very short, however if the beam 50 has a long coherent length compared to the distance between the reflecting surfaces, then interference from other reflecting surfaces in the path will show up in the results. Therefore, it is important that the coherent length of the beam 50 be longer then the distance between the reflecting surfaces but not unduly so. For example, fluorescent light would be appropriate for looking at two surfaces very close together because the short coherent length would not introduce interference from other surfaces.
FIG. 5 shows a diagram of the chuck and agitation module 22 with the planarizing and bonding module 14. The chuck and agitation module 22 includes the upper substrate 30 and lower substrate 32 mounted on the chuck 34. The insulated chamber 44 is formed by the insulating bellows 36, wedged viewing window 42, and planarization plate 33. Heating takes place through the heated air nozzles 38 in the insulating bellows 36. The upper substrate 30 is pressed against the wedged viewing window 42 by the planarizing and bonding module 14.
The planarizing and bonding module 14 includes both a main actuator 80 and fine actuators 82. The main actuator 80 and the fine actuators 82 can use a motorized drive or a piezo actuator or an electro-pneumatic mechanism. A central plate 84 rides on the main actuator. The fine actuators 82 are mounted on the central plate 84 and utilize a three point configuration in floating contact with the chuck and agitation module 22. Each of the fine actuators 82 are individually adjustable by the operator through the user interface/control module 12 and line 16 which controls the planarizing and bonding module 14.
The bonding process works as follows. An upper substrate 30 whose lower surface 37 has been coated with a bonding material and a lower substrate 32 whose upper surface 39 has been coated with a bonding material are mated and placed into the chuck 34. In this example, the bonding material is gold. The upper substrate 30 is coated with a thin film of a clear liquid on the surface to be pressed against the wedged viewing window 42. This is done to prevent the upper substrate 30 from adhering to the wedged viewing window 42 during the bonding process. Any clear, thin film that can withstand the temperatures in the chuck and agitation module 22 such as vegetable or baby oil can be used. The operator then initiates the bonding process with the user interface/control module 12. The user interface/control module 12 causes the main actuator 80 to preload the chuck 34 by pressing the upper substrate 30 against the wedged viewing window 42 with a pressure of approximately 25 psi to 200 psi depending upon the substrates used.
At this point, the interferometric vision system 26 is turned on using a light with a relatively long coherent length to check the planarization and cleanliness at the bonding interface 40 of the parts. FIG. 6 illustrates a typical interference pattern for the bonding interface 40 when it is poorly planarized. FIG. 6 shows many interference pattern lines 86 which are not parallel with each other indicating poor planarization. FIG. 7 illustrates a typical interference pattern for the bonding interface 40 after planarization has been achieved. The interference pattern lines 86 have been minimized and are all parallel with each other. The operator looks at the pattern displayed on the CRT display 28 and makes adjustments to the fine actuators 82 by entering input into the user interface/control module 12. The operator continues to make planarization adjustments with the fine actuators 82 until the interference pattern lines have been minimized in number and become parallel as illustrated in FIG. 7.
The planarization procedure is verified with a light of a very short coherent length to check the planarization of the upper substrate 30 with respect to the wedged viewing window 42.
Bonding will occur at a pressure of approximately 50 psi to 1000 psi, depending upon the parts used. As the pressure is raised, the interferometric vision system 26 is used to insure that the bonding interface 40 retains good planarization characteristics. When both the final pressure is correct and planarization is complete the position of the main actuator 80 and the fine actuators 82 are locked.
After locking the main actuator 80 and the fine actuators 82 into place the chuck and agitation module 22 is activated to provide warm air through the heated air nozzles 38 to the insulated chamber 44. The warm air is directed by the heated air nozzles 38 towards the upper substrate 30 and the lower substrate 32 to provide uniform heating of the upper substrate 30 and the lower substrate 32. The upper substrate 30 and the lower substrate 32 are heated through the diffusion of heat from the heated air nozzles 38. Non-uniform heating of the upper substrate 30 and the lower substrate 32 results in deformation of the bonding interface 40 as different areas of the upper substrate 30 or lower substrate 32 expand at different rates. To further control uniformity of heating expansion, the heated air nozzle 47 directs warm air to the wedged viewing window 42 which the upper substrate 30 is pressed up against. The heated air flowing to the heated air nozzles 38 and the heated air nozzle 47 should preferably be at a temperature of approximately between one hundred degrees centigrade and three hundred degrees centigrade and the insulated chamber 44 should also reach a temperature of approximately between one hundred degrees centigrade and three hundred degrees centigrade depending upon the bonding media used. To avoid cracking of the upper substrate 30 and the lower substrate 32 or deformation of the bonding interface 40 due to too rapid heating the heating rate in the insulated chamber 44 should remain below 0.2 degrees per second.
Once the bonding temperature and pressure have been obtained, the pressure and temperature in the insulated chamber 44 must be maintained for at least two minutes to insure that bonding occurs. After the bonding time has elapsed, the temperature of the insulated chamber 44 is lowered by lowering the temperature of air coming from the heated air nozzles 38, with pressure still applied to the upper substrate 30 and the lower substrate 32. Again, to avoid weakening of the bond or cracking of the upper substrate 30 and the lower substrate 32 due to cooling contraction of the upper substrate 30 or the lower substrate 32, the cooling rate of the insulated chamber 44 should not exceed 0.2 degrees per second.
Once the insulated chamber 44 has reached the cool down temperature of 60 percent of the bond temperature, the pressure on the upper substrate 30 and the lower substrate 32 is released by lowering the main actuator 80. The upper substrate 30 and the lower substrate 32 remain in the insulated chamber 44 until cooldown is finished and the insulated chamber 44 has reached a temperature of twenty-one degrees centigrade. At this time the bonding process is completed and the bonded upper substrate 30 and lower substrate 32 may be removed from the bonding system 10.
The use of the interferometric vision system 26 to display the planarity of the bonding interface 40 allows submicron adjustments to be made and insures the good planarity of the bonding interface 40. Good planarity is critical to the bonding process because it allows much greater pressures to be obtained in the bonding process without breakage of the fragile upper substrate 30 or lower substrate 32. The combination of heat and higher pressures facilitates direct gold to gold bonding without the need for intermediate, softer metals such as indium, with no vacuum. | A bonding system with interferometric inspection for real time planarity feedback and control is used to bond two substrates at atmospheric pressure. The interferometric vision system includes a crt monitor display to display the relative planarity between two objects to be bonded. If the planarity is not sufficient, the operator, based on the information displayed, may make infitesimal adjustments to the bonding system to improve the planarity. After the desirable planarity is achieved, a heat system is activated to further facilitate bonding. | 1 |
FEDERAL SPONSORSHIP
[0001] None
FIELD OF THE INVENTION
[0002] The present invention is directed to a class of polyesters that are lightly crosslinked polyesters made by reacting alkoxyglyceryl units, and dimer acid. As will become clear, lightly crosslinked as used herein relates to reactions in which there is an excess of hydroxyl groups on a molar basis to carboxylic groups on the dimer acid. The polymers and a contribute softness, lubricity and antistatic properties when applied to hair, skin, textile fiber and paper. The presence of the specific dimer fatty group, and water-soluble alkoxyglyceryl group provides unique and heretofore unobtainable properties on a variety of substrates.
BACKGROUND OF THE INVENTION
[0003] Surfactants are a well known materials that possess an oil soluble and a water soluble group. The literature is full of surface active agents that have a fatty hydrophobe and a water soluble hydrophilic portion. Polysorbates are one class.
[0004] Wikiopedia defines polysorbate as an oily liquid. It is a class of emulsifiers used in some pharmaceuticals and food preparation. It is often used in cosmetics to solubilise essential oils into water based products. Polysorbates are derived from PEG-ylated sorbitan (a derivative of sorbitol) esterified with fatty acids. Surfactants that are esters of plain (non-PEG-ylated) sorbitan with fatty acids are usually referred to by the name Span.
[0005] U.S. Pat. No. 4,297,290 to Stockberger issued Oct. 27, 1981 teaches that sorbitan fatty acid esters can be prepared by forming anhydro sorbitol (a mixture of sorbitans, isosorbide, and unreacted sorbitol) by acid-catalyzed anhydrization, then reacting the resulting anhydro sorbitol with a fatty acid in the presence of a base at a temperature not exceeding about 215° C. Use of temperatures not over 215° C. results in products having substantially less color than those obtained at higher temperatures.
[0006] Polysorbates are emulsifiers, but are sticky on the hair and skin and do not provide appreciable softness, conditioning or antistatic properties.
[0007] U.S. Pat. No. 6,800,275 issued to O'Lenick, issued Oct. 5, 2007, incorporated herein by reference discloses “a series of polyester compounds made from the reaction of (a) a difunctional hydroxy compound, specifically polyoxyalkylene glycols, (b) a difunctional carboxylic acid, specifically dimer acid and hydrogenated dimer acid, and (c) a capping carboxylic acid, which only contains one acid group.” The patent teaches, “another critical component is the mono-functional carboxylic group, which caps the polymer and provides terminal oil soluble portion to the molecule. This lowers the critical micelle concentration and provides improved skin deposition”.
[0008] We have surprisingly found that the reaction of a alkoxyglyceryl, with dimer acid without the required capping fatty acid offers improved lubricity and skin feel.
THE INVENTION
Object oe the Invention
[0009] It is the object of the invention to provide materials, which provide outstanding softness, antistatic properties and conditioning properties to a variety of substrates including hair, skin, textile fiber and paper.
[0010] Another object of this invention is to provide a process for treating hair, skin and textile fiber with the polyesters of the present invention.
SUMMARY OF THE INVENTION
[0011] The present invention is directed to unique polyester made by reaction of dimer acid with alkoxyglyceryl.
[0012] Polyesters of this type are complicated mixtures of oligomers. We anticipate that the various hydroxyl groups on the alkoxyglyceryl offer little regiospecificity, that is react about equally as well as each other. Since the analytical techniques do not yet exist to differentiate the reaction on one or another hydroxyl groups, product by process claims are the optimum way to claim the present reaction product. The product has the repeating groups linked through an ester linkage with dimer acid.
[0013] These polyesters because of their structure are outstanding lubricants and skin feel modifiers. While not wanting to be bound by any one theory of operation, we believe that the polyester's lowest free energy from aqueous solution is one in which the fatty group on the polysorbate is orientated toward the substrate, the water soluble polysorbate polyoxyalkylene groups are orientated away from the substrate. This repeating pattern results in a “sewing together” of groups that are captured on the surface of the substrate. The result is a molecule that is “entangled” in the substrate, having the water soluble groups pointing out of the substrate. This results in enhanced durability and hydrophilic surface treatments. A self wetting, conditioner, providing durable softness results. These properties are highly prized in personal care applications including shampoos, body wash, and baby products. The improved hydrophilic properties makes substrates so treated water loving, a requirement for absorbent applications, and a rarity in products that have a lot of fatty content in the molecule.
DETAILED DESCRIPTION OF THE INVENTION
[0014] One aspect of the present invention is directed toward a polyester of the present invention made by the reaction of:
[0015] (a) a alkoxyglyceryl conforming to the following structure:
[0000]
[0016] e is an integer ranging from 0 to 30;
[0017] f is an integer ranging from 0 to 30;
[0000] with dimer acid conforming to the following structure:
[0000]
[0018] or hydrogenated dimer acid conforming to the following structure:
[0000]
[0019] or mixtures thereof;
[0000] at a temperature of between 150 and 200° C., said the mole ratio of said carboxyl groups in the dimer acid to hydroxyl group in the polysorbate range from 1:2 to 1:3. This partial crosslinking provides increased molecular weight and improved skin lubricity.
[0020] Another aspect of the present invention is directed toward a process for conditioning hair, skin and paper which comprises contacting the hair skin or paper with an effective conditioning concentration of a polyester made by the reaction of:
[0021] (a) an alkoxyglyceryl compound conforming to the following structure:
[0000]
[0022] e is an integer ranging from 0 to 30;
[0023] f is an integer ranging from 0 to 30.
[0000] with dimer acid conforming to the following structure:
[0000]
[0024] or hydrogenated dimer acid conforming to the following structure:
[0000]
[0025] or mixtures thereof,
[0000] at a temperature of between 150 and 200° C., said the mole ratio of said carboxyl groups in the dimer acid to hydroxyl group in the alkoxyglyceryl group range from 1:2 to 1:3.
[0026] In a preferred embodiment the process is carried out using an effective conditioning concentration ranges from 0.1 to 15% by weight.
Preferred Embodiments
[0027] The presence of polyoxyethylene groups —CH 2 CH 2 —O) x H on the alkoxyglyceryl and affects water solubility. In a preferred embodiment where the products are water-soluble the percent polyoxyethylene groups in the molecule ranges from between 40 and 65 percent of the total molecular weight of the polymer.
[0028] In a preferred embodiment the dimer acid is hydrogenated dimer acid conforming to the following structure:
[0000]
[0029] In another preferred embodiment the dimer acid is dimer acid conforming to the following structure:
[0000]
[0030] In a preferred embodiment the fiber is hair.
[0031] In a preferred embodiment the fiber is hair textile fiber.
[0032] In a preferred embodiment the fiber is hair fiber is paper.
[0033] In a preferred embodiment the effective concentration ranges from 0.1 to 15% by weight.
[0034] In a preferred embodiment e+f+g is an integer ranging from 15 to 30.
EXAMPLE
Raw Materials
Example 1
Dimer Acid
[0035] Dimer acid is an item of commerce and is available from a variety of sources including Cognis Chemical Cincinnati Ohio. It conforms to the following structure:
[0000]
Example 2
Hydrogenated Dimer
[0036] Hydrogenated dimer acid is an item of commerce and is available from a variety of sources including Cognis Chemical Cincinnati Ohio. It conforms to the following structure:
[0000]
[0037] Alkoxyglyceryl Compounds
[0038] Alkoxyglyceryl are compounds of commerce, available from a variety of sources including Croda. They conform to the following structure:
[0000]
[0039] e is an integer ranging from 0 to 30;
[0040] f is an integer ranging from 0 to 30.
[0000]
Example
e
f
3
3
3
4
7
7
5
7
8
6
7
0
7
10
10
8
30
20
9
17
16
[0041] General Procedure
[0042] Preparation of Polyester.
[0043] To the specified number of grams of the specified alkoxy glyceryl compound (Examples 3-9) is added 300 grams of dimer acid (Example 1 or 2). The reaction mass is heated to 180° C. The reaction proceeds as water is distilled off and the acid value becomes vanishingly small. The reaction is cooled and used as is in reaction sequence 2.
[0044] Dimer Acid Products
[0045] The 300 grams of dimer acid added are dimer acid Example 1.
[0000]
Alkoxyglyceryl
Example
Example
Grams
Carboxy:hydroxyl
10
3
132
1:2
11
4
948
1:3
12
5
289
1:2
13
6
132
1:3
14
7
373
1:2
15
8
1058
1:3
16
9
870
1:3
[0046] Hydrogenated Dimer Acid Products
[0047] The 300 grams of dimer acid added are dimer acid Example 2.
[0000]
Alkoxyglrceryl
Example
Example
Grams
Carboxy:hydroxyl
17
3
132
1:2
18
4
540
1:3
19
5
289
1:2
20
6
132
1:3
21
7
373
1:2
22
8
1058
1:3
23
9
870
1:3
Application Examples
[0048] As can easily be seen the technology used to prepare the compounds of the present invention provide outstanding latitude to make products that have many desirable properties. This flexibility is highly desirable in a variety of applications. The amount of water soluble group (alkylene oxide), or fatty group (dimer acid) determines the water or oil solubility, which in turn determines the type of cosmetic formulation in which the products can be used.
[0049] While the illustrative embodiments of the invention have been described with particularity, it will be understood that various other modifications will be apparent to and can be readily made by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is not intended that the scope of the claims appended hereto be limited to the examples and descriptions set forth hereinabove but rather that the claims be construed as encompassing all the features of patentable novelty which reside in the present invention, including all features which would be treated as equivalents thereof by those skilled in the art to which the invention pertains. | The present invention is directed to a class of polyesters that are lightly crosslinked polyesters made by reacting alkoxyglyceryl units (linked by the reaction of their hydroxyl groups) to the carboxyl group of dimer acid. The polymers and a contribute softness, lubricity and antistatic properties when applied to hair, skin, textile fiber and paper. | 3 |
FIELD OF THE INVENTION
The present invention is related to a cleaning device applicable to an electrostatic recording system, such as for instance a copying or a printing system, in order to remove residual developer from the surface of an image-forming member.
BACKGROUND OF THE INVENTION
In a typical printing or copying process, a charged latent image is formed on an image-forming member by image-wise exposure. The image-forming member can be an endless member such as a drum or a belt. Typical graphical processes include amongst others magnetography, ionography and electrography, particularly electrophotography. In the latter process for instance, the charged latent image is formed on a pre-charged photosensitive member by image-wise exposure to light. The latent image is subsequently made visible on the image-forming member with developer at a development zone, the developer comprising, or consisting of, charged toner. After the development of the latent image, the developed image is transferred to a recording medium, directly or via one or more intermediate image-carrying members, where it may be permanently fixed. Examples of intermediate image-carrying members are endless belts. In practice the transfer from an image-delivering member being either an image-forming member or an intermediate image-carrying member to an image-receiving member being either an intermediate image-carrying member or a recording medium may be incomplete. Multiple subsequent transfers are possible. In normal operating conditions, typical transfer efficiencies range from 95% to 100%. The residual image on the image-delivering member has to be removed because otherwise the image quality of subsequently formed or transferred images can be seriously disturbed.
This residual image has to be removed before re-entering into the development zone. Otherwise this could lead to serious image defects because of mixing up of the new developed or transferred image with the residual image.
This cleaning action is executed by a cleaning station positioned downstream from the transfer zone. The cleaning station comprises at least a revolving brush which can be engaged against the image-delivering member for removing residual developer therefrom, a high voltage collecting roller in rolling contact with the brush roller for brush de-toning and a scraper blade contacting the high voltage roller for scraping developer therefrom.
The cleaning of the high voltage roller is a problem. This roller is a rigid roller in rolling contact with the cleaning brush. In the contact zone, developer is transferred to the high voltage roller by biasing the high voltage roller such that an attractive electrical field is created. A cleaning blade is positioned downstream of the contact zone to scrape off the developer from the high voltage roller. Usually to maximize force, the cleaning blade is positioned at an obtuse contact angle. The contact angle is defined with respect to a line tangent to the point of contact of the cleaning blade with the rotating high voltage roller and is the angle between this tangent line, at the uncleaned section of the roller, and the cleaning blade. This obtuse contact angle is typically between 160 and 170 degrees. The cleaning blades used as such are usually very stiff and rigid amongst others to prevent flip over of the cleaning blade as for instance when there is no developer on the roller. As a consequence, more elastic cleaning blades are unsuited because such flip over is detrimental both with respect to the lifetime of the blade and the cleaning efficiency. A cleaning blade mounted at an obtuse contact angle is typically made of an incompressible rigid material such as stainless steel.
In U.S. Pat. No. 4870466 (lida, assigned to Ricoh) a cleaning blade is disclosed which is mounted at an acute contact angle, i.e. a trailing cleaning blade, with respect to the high voltage roller. However, the contact angle disclosed seems to be clearly smaller than 45 degrees. As a result, the contact area between the cleaning blade and the high voltage roller is rather large. It is found that cleaning at such small angles is inefficient. Moreover, the cleaning blade is mounted such that the waste toner which is removed from the high voltage roller can not fall down freely to be further removed, but instead, at least to some extent, will build up between the roller and the cleaning blade and as such may even push the cleaning blade away from the high voltage roller.
OBJECTS OF THE INVENTION
It is an object of the present invention to provide a cleaning blade to scrape off developer and debris from the surface of a collecting roller, being used as a brush de-toning device in a cleaning unit.
It is a preferred object of the invention to mount the cleaning blade such that the cleaning blade has a good cleaning ability for an extended period of time and that the waste developer which is scraped off the high voltage roller is allowed to freely fall down to be further removed by a revolving auger and/or an air flow.
It is a further preferred object of the invention to provide a compressible cleaning blade, which is not damaged when exposed to carrier particles and other debris, which may be present on the surface of the high voltage roller.
It is still a further preferred object of the invention to provide a wear-resistant cleaning blade and an associated mounting position which allows for an efficient cleaning of a collecting roller having a fairly rough surface, i.e. with Ra ranging from 0.05 to 0.15.
SUMMARY OF THE INVENTION
According to a first aspect of the invention there is provided a cleaning device being part of a copying or printing system for removing residual developer from the surface of an image-delivering member comprising:
a cleaning brush in rolling contact with said surface of said image-delivering member for removing residual developer therefrom, said cleaning brush being rotatable in a first predetermined direction;
a collecting roller in rolling contact with said revolving brush, said collecting roller being rotatable in a second predetermined direction;
means for biasing said collecting roller to generate an electrical field which attracts the residual developer from the cleaning brush and collects it onto its surface; and
a cleaning blade having a forward end portion in frictional contact with the collecting roller wherein, in an operative orientation of the device, said cleaning blade is in contact with said collecting roller at a contact position where the collecting roller is moving in an upward direction, said cleaning blade being mounted such that the contact angle (as hereinbefore defined) is less than 90 degrees.
In an embodiment of the invention, the cleaning device is retractable. The cleaning device is a part of a copying or printing system and is intended for removing residual developer from the surface of an image-delivering member such as for instance an image-forming member or an image-carrying member. Examples of image-forming members are drums or belts with a photoreceptive or a magneto-sensitive outer layer. Examples of image carrying members are seamed or seamless intermediate transfer belts. Such an intermediate transfer belt may be composed of an electrically semi-insulating or insulating material with a low surface energy, or comprises at least a top coating of such a material. Examples of such a material are polyesters such as e.g. Hytrel 7246, polyimides, polycarbonates or dissipative polymer blends.
The collecting roller in rolling contact with said revolving brush is electrically biased such that an electrical field is generated which attracts the residual developer from the cleaning brush and collects it onto its surface.
The cleaning blade is preferably composed of an elastic material with a hardness ranging from 50 to 80 Shore A.
We are aware that cleaning blades are widely used, particularly for cleaning the image-forming member. In electrophotography the image-forming member is usually a drum or a belt covered with an organic photo-conductive layer. The cleaning of this smooth sensitive layer can however in no way be compared with the cleaning of the high voltage roller, which is usually an incompressible rigid roller. Irrespective of the positioning of the cleaning blade, the force required to completely remove the residual developer from the image-forming layer is such that the image-forming layer is damaged. In practice, the cleaning blade is usually mounted such that the image-forming member is not damaged which by consequence results in an incomplete cleaning. Therefore, extra cleaning means are provided, e.g. in the form of a revolving cleaning brush in rolling contact with the image-forming members, to improve cleaning results.
The developer used in the recording system with which the cleaning device according to the invention is associated can be a mono-component or a two-component developer. A common development technique uses a two-component developer material of toner particles adhering tribo-electrically to larger carrier beads. When the developer material, contained in a developer unit, is placed in an appropriate magnetic field, the carrier beads with the toner thereon form a magnetic brush. As the carrier beads and the toner particles are oppositely charged, in the development zone the toner particles are attracted from the carrier beads to develop the latent image on the image-forming member. In case of a two-component developer it is clear that both the developed image and the residual image are primarily composed of toner particles. However, due to failures, as e.g. wrong sign carrier beads, very small numbers of carrier beads may be transferred to the image-forming member in the development zone and subsequently picked up by the cleaning brush and thereafter collected on the collecting roller. Contrary to e.g. a metal cleaning blade mounted at an obtuse contact angle, the cleaning blade of the present invention easily removes such hard carrier beads without causing damage to the blade.
The cleaning brush rotates in a first predetermined direction, which is preferably opposite to the propagation direction of the image-delivering member. The collecting roller contacts the cleaning brush and rotates in a second predetermined direction, preferably opposite to said first predetermined direction. The collecting roller may be a freely rotating roller or may be driven. The cleaning brush and the collecting roller may be independently driven and their rotation speed may be independently controlled. The collecting roller is incompressible and electrically conductive and bias means are provided to apply a voltage to the collecting roller in order to create an electrical field which is attractive for the developer gathered on the cleaning brush.
The cleaning blade according to the present invention is preferably an elastic cleaning blade with a hardness in the range from 50 to 85 Shore A. The rebound resilience is typically in the range from 20 to 40%. Preferably a polyurethane cleaning blade is used. The cleaning blade is mounted at an acute contact angle. The thickness of the cleaning blade is typically between 1.5 mm and 4 mm. The cleaning blade is partly attached to a support such that the free portion of the cleaning blade has a length typically in the range from 4 to 11 mm. The free portion of the blade is the portion which is not attached to the support. The blade material is compressible and the thickness and free length of the blade are chosen such that at least the forward end portion of the blade is allowed to bend slightly while in contact with the collecting roller, i.e. while exerting pressure on the blade. Particularly the blade is positioned such that the pressure exerted by the blade on the collecting roller would correspond to an impression of the blade in the incompressible collecting roller ranging from 0.25 mm to 1 mm. The cleaning blade is mounted such that it contacts the collecting roller at a position where the collecting roller moves in an upward direction. This enables waste developer being scraped off the collecting roller to freely fall down and inhibits potential build up of waste material between the blade and the collecting roller.
In an embodiment of the invention, the cleaning blade is mounted such that the acute contact angle of the cleaning blade with respect to the collecting roller is in the range from 60 to 80 degrees. It has been observed that smaller contact angles result in inefficient cleaning, more particularly, a contact angle below 60 degrees causes developer filming on the collecting roller which results in a decreased de-toning ability of the collecting roller and consequently in a less efficient cleaning of the image-delivering member. Moreover, a blade mounted at such a small contact angle is not able to remove carrier beads from the surface of the collecting roller. In an embodiment of the invention, the collecting roller is composed of a metal. Particularly, aluminum or steel can be used. In such case, the surface of the collecting roller may be hard anodized to increase at least the hardness of the roller. Alternatively, a ceramic coating may be provided as a surface layer. Particularly the surface can have an average roughness, Ra, in the range from 0.05 to 0.15.
In an embodiment of the invention, the cleaning device further comprises an auger, being positioned below the collecting roller to remove the waste developer, which is scraped off the collecting roller by the cleaning blade. An air flow may be provided to assist in the removal of the waste developer. Alternatively, instead of an auger, only an air flow may be provided to remove the waste.
According to another aspect of the invention, there is provided a method for cleaning a surface of an image-delivering member, which is a part of a copying or printing system, the method comprising the steps of:
contacting the outer surface of said image-delivering member with a cleaning brush to remove residual developer therefrom, said cleaning brush rotating in a first predetermined direction;
establishing a rolling contact between said revolving brush and a collecting roller rotating in a second predetermined direction,
biasing said collecting roller such that an electrical field is generated which attracts said residual developer from said cleaning brush and collects it onto its surface; and
scraping off said collected residual developer from said surface of said collecting roller with a cleaning blade, said cleaning blade having a forward end portion in frictional contact with the collecting roller at a contact position where the collecting roller is moving in an upward direction, said cleaning blade being mounted such that the contact angle (as hereinbefore defined) is less than 90 degrees.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be further described, purely by way of example, with reference to the accompanying drawings, in which:
FIG. 1 depicts a schematic representation of a cleaning device according to an embodiment of the invention.
FIG. 2A depicts a schematic prior art representation of the positioning of a cleaning blade with respect to a moving image-delivering member. The cleaning blade is mounted at an obtuse contact angle with respect to the image-delivering member.
FIG. 2B depicts, according to an embodiment of the present invention, a schematic representation of the positioning of a cleaning blade with respect to a moving image-delivering member. The cleaning blade is mounted at an acute contact angle with respect to the image-delivering member.
FIG. 3 depicts a printing system incorporating a cleaning unit according to an embodiment of the invention.
FIG. 4 depicts a printing system incorporating a cleaning unit according to an embodiment of the invention.
FIG. 5 depicts an image-forming station according to an embodiment of the invention.
FIG. 6 depicts a printing system incorporating a cleaning unit according to an embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
In relation to the appended drawings the present invention is described in detail as follows. It is apparent however that a person skilled in the art can imagine several other equivalent embodiments or other ways of executing the present invention, the spirit and scope of the present invention being limited only by the terms of the appended claims.
According to a preferred embodiment of the invention, FIG. 1 depicts a schematic representation of a retractable cleaning device 1 , which is engaged into contact with the surface of an image-delivering member 5 . Particularly, a rotating cleaning brush 2 having bristles 3 extending therefrom contacts the surface. The bristles remove the residual image from the surface of the image-delivering member. Particularly as a two-component developer is used, the residual image is primarily composed of charged toner particles. More particularly, negatively charged toner particles are used. It should however be clear that the present invention is in no way limited to the removal of negatively charged toner particles. The cleaning device of the present invention can easily cope with positively charged toner particles or other types of developer. Preferably the direction of movement of the cleaning brush is opposite to the direction of movement of the image-delivering member. A rotating collecting roller 4 is placed adjacent said rotating cleaning brush such that portions of said rotating cleaning brush selectively contact said collecting roller in a contact zone as said cleaning brush rotates. Particularly, the collecting roller is a steel roller with an average surface roughness, Ra, of 0.09. Bias means generally indicated by reference 13 are provided to apply a voltage to the collecting roller to establish an attractive electrical field in the contact zone between the cleaning brush and the collecting roller. The voltage applied to the collecting roller is typically in the range from 300 V to 1000 V. A polyurethane cleaning blade 7 contacts the collecting roller at a position where the collecting roller moves in an upward direction. The cleaning blade is partly attached to a support 6 . The attachment is executed by means of an adhesive. The free portion of the cleaning blade has a length of 7 mm. The cleaning blade has a thickness of 2 mm, a hardness of 70 Shore A and a rebound resilience of 31%. The rebound resilience is determined prior to the mounting by attaching both ends of the blade to two fixed points and measuring the rebound of a reference weight which is dropped on the blade. The cleaning blade is mounted at an acute contact angle 8 with respect to the collecting roller.
As schematically depicted in FIG. 2B, the contact angle, defined as the angle 8 between the portion of the line 9 , tangent to the collecting roller 4 at said contact position and extending towards the uncleaned portion of the collecting roller, and said cleaning blade 7 , is 69 degrees. This is in contrast to the prior-art embodiment shown in FIG. 2A, where, to maximize force, the cleaning blade is usually positioned at an obtuse contact angle. The contact angle 8 is defined with respect to a line 9 tangent to the point of contact of the cleaning blade 7 with the rotating collecting roller or high voltage roller 4 and is the angle between this tangent line, at the uncleaned section of the roller, and the cleaning blade.
In the device according to the invention, the cleaning blade is mounted as such efficiently scrapes off the developer collected on the collecting roller. The cleaning blade also efficiently removes debris and carrier beads from the collecting roller without being damaged. The waste which is removed from the collecting roller can freely fall down and is further removed by a revolving auger 10 .
In a first example, see FIG. 3, a schematic representation of an electrophotographic duplex color printer is depicted, incorporating the cleaning unit according to the present invention. The printer comprises a light-tight housing 11 , which has at its inside a stack 12 of sheets to be printed. At its output the printer has a platform 14 onto which the printed sheets are received. A sheet to be printed is removed from stack 12 and is fed through an alignment station 16 . As the sheet leaves the alignment station, it follows a straight horizontal path 17 up to output section 18 of the printer. The speed of the sheet, upon entering said path, is determined by driven pressure roller pair 47 . A number of processing stations are located along the path 17 . A first image-forming unit 20 indicated in a dash-and-dot line is provided for applying a multi-color image to the obverse side of the sheet and is followed by a second station 21 for applying a multi-color image to the reverse sheet side. A buffer station 23 then follows, with an endless transport belt 24 for transporting the sheet to a fuser station 25 . As both image forming units are similar to each other, only unit 20 will be described in more detail hereinafter.
An endless photoconductor belt 26 is guided over a plurality of rollers 27 to follow a path in the direction of arrow 22 to advance successive portions of the photoconductive surface sequentially through the various processing stations disposed along the path of movement thereof. The photoconductive belt may comprise a base layer of polyethylene terephthalate of 100 μm thickness covered with a thin layer of aluminum as a back electrode (less than 0.5 μm thickness). The organic photoconductor (OPC) layer is on top of the aluminum layer and is from 15 μm in thickness. The belt is arranged such that the photoconductive layer is positioned on the outside of the belt loop.
Initially, a portion of the photoconductive belt 26 passes through charging station 28 . At the charging station, a charge-generating device electrostatically charges the belt to a relatively high, substantially uniform potential, i.e. the dark potential. Next, the belt passes to an exposure station 29 . Exposure station 29 exposes the photoconductive belt to successively record four latent color separation images by image-wise discharging the belt. Thereafter, the belt advances these images to the development unit. This unit includes four individual developer stations 35 , 36 , 37 and 38 with for example cyan, yellow, magenta and black developer. During development of each electrostatic latent image only one developer station is in the operative position (developer station 35 in FIG. 3 ). The developer used is two-component developer consisting of non-permanently magnetised magnetic carrier beads having toner particles adhering triboelectrically thereto. A magnetic brush of developer particles is formed in the operative developer station adjacent the photoconductive belt. The negatively charged toner particles are attracted by an electrical field from the magnetic brush to thereby develop the corresponding latent image on the photoconductive belt. Each latent image is developed subsequently using the developer station of the corresponding color to thereby form four spaced-apart subsequently developed images on the photoconductive belt.
After their development, the toner images are moved to toner image transfer stations 40 , 41 , 42 and 43 where they are transferred on a sheet of support material, such as plain paper or transparent film. At the transfer stations, the sheet follows the rectilinear path 17 into contact with photoconductive belt 26 . The sheet is advanced in synchronism with the movement of the belt such that at each transfer station an image is transferred to the paper in perfect register one onto the other to thereby form a registered multi-color image on the sheet. After transfer of the four images, the belt, which acts both as an image-delivering and an image-forming member, is directed towards a cleaning unit 45 , which is positioned downstream from the transfer stations. In the cleaning unit a rotating fibrous-like brush contacts the photoconductive belt 26 to remove residual developer particles remaining after the transfer operation. Cleaning unit 45 is identical to the cleaning unit 10 (FIG. 1) as described above. Thereafter, lamp 46 illuminates the belt to remove any residual charge remaining thereon prior to the start of a next cycle.
In a second example, see FIG. 4, a schematic representation of another electrophotographic color printer is depicted incorporating cleaning units according to the present invention. This printer has a supply station 113 in which a roll 114 of web material 112 is housed. The web 112 is conveyed into a tower-like printer housing 144 in which a support column 146 is provided housing at least four printing stations A-D, e.g. black, yellow, magenta and cyan. (In the fig. an extra printing station E is provided, allowing to optionally add an additional color.) As shown in figure 5, each printing station comprises a cylindrical drum 124 having a photoconductive outer surface 126 . The drum acts both as an image-delivering member and as an image-forming member. Circumferentially arranged around the drum 124 there is a main charge generating device 128 capable of charging the drum surface to a high potential of about −600 V, i.e. the dark potential, an exposure device 130 will image-wise discharge (e.g. to a potential of about −250 V) the surface 126 to thereby form a latent image. This latent image is developed on the drum by the developer station 132 by contacting the drum with a magnet brush of a two-component developer of non-permanently magnetised magnetic carrier beads having toner particles adhering triboelectrically thereto formed on the surface of a magnet roller 133 . Negatively charged toner particles are attracted to the exposed (discharged) areas of the photoconductive surface. After development, the toner image on the drum surface is transferred to the moving web 112 by a transfer corona device 134 which generates an attractive electrical field for the negatively charged toner particles. This transfer corona together with the guiding rollers 136 establishes also a strong adherent contact between the web and the drum over an angle of about 15 degrees which causes the latter to be rotated in synchronism with the movement of the web 112 and urges the toner particles into firm contact with the surface of the web 112 . A web discharge corona 138 is provided to establish a controlled release of the web. Thereafter the drum surface is pre-charged by a charge generating device 140 to a potential between 0 and −600 V both for facilitating the charging by the main charge generating device and to facilitate the removal of residual images on the drum surface by a cleaning unit 142 . Cleaning unit 142 is similar to the cleaning unit 10 (FIG. 1) as described above. The cleaning unit includes an adjustably mounted fibrous-like cleaning brush 143 , the position of which can be adjusted towards or away from the drum surface to ensure optimum cleaning. The cleaning brush 143 is grounded or subject to such a potential with respect to the drum as to attract the residual developer particles away from the drum surface. The rest of cleaning unit 142 is similar to the cleaning unit 10 (FIG. 1) as described above. The rotatable cleaning brush 143 which is driven to rotate in a sense the same as to that of the drum 124 and at a peripheral speed of, for example twice the peripheral speed of the drum surface. The developer station 132 includes a magnetic roller with a brush formed thereon 133 which rotates in a sense opposite to that of the drum 124 . The resultant torque applied to the drum by the rotating developing brush 133 and the counter-rotating cleaning brush 143 is adjusted to be close to zero, thereby ensuring that the only torque applied to the drum is derived from the adherent force between the drum and the web.
After a first image of a first color is formed and transferred to the web in a first print station, the web passes successively the other print stations where images of other colors are formed and transferred in register to thereby form a registered multi-color image on the web. After leaving the final print station E, the image on the web is fixed by means of the image fixing station 116 and fed to a cutting station 120 and a stacker 152 if desired.
In a third example, see FIG. 6, a schematic representation of an electrophotographic color printer is depicted incorporating cleaning units according to the present invention. The printer comprises a primary transfer belt 212 formed of polyethylene terephthalate (PET) having a thickness of 100 m and having spaced along one run thereof a plurality of toner image-forming stations A, B, C, D. Each of these stations is similar as described in FIG. 5 and example 2. Charge generating devices 219 , 221 , 223 , 225 are provided to subsequently electrostatically transfer a toner image of a particular color from each image-forming station to the PET belt 212 while the belt is advanced over a number of guide rollers 217 along the stations to thereby form a registered multi-color toner image. The primary transfer belt 212 acts as an image-delivering member.
At the intermediate transfer nip, the multi-color toner image is transferred to an intermediate transfer belt 250 . The intermediate transfer nip 216 is formed between the guide roller 213 and an opposing guide roller 252 pressed towards each other to cause tangential contact between said primary transfer belt 212 and the heated intermediate transfer belt 250 . The guide roller 213 comprises an electrically conductive core carrying a semi-insulating covering. A supply of electrical potential is provided for electrically biasing at least the first guide roller 213 to create an electrical field at the intermediate transfer nip 216 to assist in transferring the image from the primary belt 212 to the intermediate transfer belt 250 .
The primary transfer belt 212 , with the residual image thereon passes thereafter through a cooling station 268 , where the belt is forcibly cooled by directing cooled air onto the primary transfer belt 212 . Alternatively, instead of blowing cooled air a cooling liquid such as water may be directed through roller 215 to cool the primary transfer belt. The primary transfer belt 212 is thereby cooled to a temperature of about 35 C. This cooling assists in establishing the required temperature gradient at the intermediate transfer nip 216 . The residual toner image on the primary transfer belt 212 is removed by cleaning unit 246 before the deposition of further developed toner images thereon. The cleaning unit 246 is similar to the cleaning unit 10 (FIG. 1) as described above.
The intermediate transfer belt 250 with the transferred multi-color image is advanced over a heated roller 266 to a final transfer station 226 . The final transfer station 226 comprises a nip formed between a guide roller 254 of the intermediate transfer belt 250 and a counter roller 270 , through which nip the intermediate transfer belt 250 and a substrate in the form of a paper web 258 pass in intimate contact with each other. Drive rollers 262 , driven by a motor 230 , drive the web 258 in the direction of the arrow X from a supply roll 260 continuously through the final transfer station 226 where it is pressed against the intermediate transfer belt 250 by the counter roller 270 . At this final transfer zone, the multi-color image is transferred from the intermediate transfer belt to the paper web.
Downstream of the final transfer station 226 , the intermediate transfer belt 250 passes through a cleaning station comprising a tacky cleaning roller 229 opposed to a counter roller 227 , and thereafter over a steering and tensioning roller 232 , before returning to the intermediate transfer nip 216 . | A cleaning device, being part of a copying or printing system, for removing residual developer from the surface of an image-delivering member is described. The device includes a cleaning brush in rolling contact with the surface of the image-delivering member for removing residual developer therefrom. A biased collecting roller is in rolling contact with the revolving brush. The collecting roller is biased such as to attract the residual developer from the cleaning brush and to collect it onto its surface. A trailing cleaning blade has a forward end portion in frictional contact with the collecting roller. The trailing cleaning blade is in contact with the cleaning roller at a contact position where the collecting roller is moving in an upward direction. Also disclosed is a method for removing developer from a surface of an image-delivering member. | 6 |
[0001] The present invention concerns a unit for separating a pre-cut substrate into a plurality of separate sub-substrates. The separator unit is usable notably when positioned downstream of a cutting unit in a packaging production machine.
[0002] A packaging production machine is designed for the fabrication of boxes that form packaging after folding and gluing. In this machine, an initial continuous plane substrate, such as a plane web of cardboard, is unwound and is printed by a print unit, itself constituted of sub-units in the form of printing units. The web is then transferred into a cutting unit. After cutting, the substrates or blanks obtained have waste areas that are eliminated in a waste stripping unit.
[0003] A substrate or blank is composed of a plurality of sub-substrates or boxes. Depending on the type of cutting unit used, for example with a diecutting platen, the boxes are attached to each other by nicks. The nicks join two edges of a cutting line between two boxes and constitute bridges of the same material as the boxes and the blanks. With rotary die-cutting the boxes are juxtaposed.
[0004] The substrates or blanks are then separated in a separator unit or separator to obtain individual sub-substrates or boxes. This unit is designed to move the boxes transversely away from each other and/or if necessary to break the nicks, by conveying each of the boxes along a divergent trajectory. This trajectory is obtained by a fan-shaped orientation, i.e. one with divergent directions, of the conveyor ramps designed to convey the blanks from the outlet of the cutting unit to the outlet of the separator unit.
[0005] Because of this, the precut blanks leaving the cutting unit along a longitudinal series of adjacent parallel lines are reoriented by means of the conveyor ramps along a series of laterally spaced parallel lines so that two laterally adjacent boxes are no longer joined together. The individual boxes are then routed to a stacking unit for subsequent folding and gluing.
[0006] The ramps must be disposed on either side of a median longitudinal line of the blank. The number of ramps, the angle and the distance between the ramps in a plane corresponding to that of the blanks are chosen to enable optimum separation as a function of the layout, i.e. the disposition, of the boxes on the blank. The operator must quickly and simply modify the orientation and the position of the conveyor ramps for each new job. The operator must intervene in the centre of the machine to adjust the ramps, which is not very ergonomic.
PRIOR ART
[0007] The document U.S. Pat. No. 3,860,232 describes a separator in which the orientation of the conveyor ramps is adjusted manually.
[0008] This operation is laborious and time-consuming, however. The downtime of the separator and thus of the whole of the machine used during manual adjustment of each of the ramps is reflected in the end in a serious loss of production. Moreover, in the above document, it is not possible to move the conveyor ramps laterally relative to each other.
[0009] There is also known from the document EP-1.195.335 a separator in which the orientation and the position of the conveyor ramps are adjusted automatically as a function of the job to be performed. Two towing assemblies each having a carriage are provided. Each of the carriages has engagement means designed to be engaged in a pin disposed on each of the conveyor ramps so that the carriage drives the conveyor ramp in its movement.
[0010] Optical identification of the positions of the engagement pins of the ramp to be moved accurately positions the two carriages in an initial engagement position. Computerized control coordinates the simultaneous movement of the two carriages toward the final position of the ramp. A common locking system is also provided to retain the ramps in position. The locking means are activated when the engagement means are disengaged from the corresponding pins.
[0011] By reason of the disposition of the carriage and the engagement means, the ramps must be arranged in a precise order, starting with the outermost ramp. Any new adjustment, in the event of a new job or in the event of an operator error, implies lateral stowage of all the ramps and then restarting of the two towing assemblies. Moreover, it is impossible to move a plurality of ramps at the same time, because the optical system is not able to identify a plurality of pin positions at the same time.
[0012] During movement of one of the conveyor ramps, the other conveyor ramps are no longer locked because of the common locking-unlocking. This is another drawback, because accidental movement of a correctly positioned conveyor ramp could occur during adjustment of the other conveyor ramps, leading to incorrect positioning of the boxes within the separator unit.
STATEMENT OF THE INVENTION
[0013] A main objective of the present invention consists in developing a unit designed to separate a pre-cut substrate into a plurality of separate sub-substrates positioned downstream of a cutting unit for a packaging production machine. A second objective is to optimize the accuracy of the separation of the pre-cut substrates into separate individual sub-substrates. A third objective is to produce a separator unit enabling rapid adaptation to any new job. A fourth objective is to provide a separator unit provided with means for fast and easy adjustment of the number, angle and position of the ramps. A further fifth objective is that of obtaining a separator unit enabling the drawbacks of the prior art to be avoided. A further object is that of providing a packaging production machine with a cutting unit, a waste stripping unit and a separator unit.
[0014] The invention provides a unit designed to separate a pre-cut substrate into a plurality of separate sub-substrates, comprising:
upstream transverse guide means and downstream transverse guide means, conveyor ramps adapted to convey the pre-cut substrate and the separate sub-substrates and mounted to slide and pivot on the upstream guide means and on the downstream guide means, means for moving and positioning the conveyor ramps along the upstream guide means and the downstream transverse guide means, and upstream locking means and downstream locking means able to maintain each of these conveyor ramps in a locked positioned relative to these upstream transverse guide means and said downstream transverse guide means.
[0019] According to one aspect of the present invention, the unit is characterized in that the moving and positioning means comprise a mobile element moving between said upstream transverse guide means and said downstream transverse guide means and carrying
upstream unlocking means and downstream unlocking means able to cooperate with the upstream locking means and the downstream locking means to enable release of these conveyor ramps, and upstream and downstream grasping means adapted to grasp these conveyor ramps,
so as to drive these conveyor ramps along these upstream transverse guide means and said downstream transverse guide means and to dispose them in a fan configuration.
[0022] In other words, the separator unit enables facilitated adjustment of the position and the orientation of the conveyor ramps thanks to a single mobile element. The separator unit also enables adjustment of the position and the orientation of one or more conveyor ramps with the other ramps remaining in their locked state. Because of the arrangement of the mobile element, it is possible to adjust the position of a single ramp without taking into account the position of the other ramps. The transverse movement and the angle of divergence of the ramps are thus effected ramp by ramp.
[0023] In another aspect of the invention, a packaging production machine is characterized in that it comprises the unit having one or more of the technical features described hereinafter and claimed, positioned downstream of a cutting unit and a waste stripping unit.
[0024] The upstream and downstream directions are defined with reference to the direction of movement of the substrate along the longitudinal direction in the separator unit and in the packaging production machine as a whole. The longitudinal direction is defined with reference to the direction of movement of the substrate in the separator unit and in the machine, along its longitudinal median axis. The transverse direction is defined as being the direction perpendicular to the direction of movement of the substrate.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Other advantages and features of the present invention will be better understood on reading nonlimiting embodiments of the invention and with reference to the drawings, in which:
[0026] FIG. 1 is a perspective view of a separator unit of the invention;
[0027] FIGS. 2 to 9 are partial views in perspective of a conveyor ramp and moving and positioning means, showing the various steps of moving and positioning the ramp;
[0028] FIG. 10 is a sectional view of the locking means in the locked position of a ramp; and
[0029] FIG. 11 is a lateral view of the locking means and the unlocking means in the unlocked position of a ramp.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0030] A separator unit 10 is positioned downstream of a cutting unit and a waste stripping unit in a packaging production machine (not shown). As FIG. 1 shows, the unit 10 enables separation of substrates, i.e. pre-cut blanks in this case, into sub-substrates, i.e. individual boxes 20 in this case. These blanks and thus these boxes 20 are made of cardboard, for example.
[0031] The unit 10 is designed to receive a stream of rows of adjacent boxes 20 . In this embodiment, the boxes 20 leave the cutting unit still joined to each other by small bridges of material. The boxes 20 leave the separator unit 10 separated from each other.
[0032] The production machine may then include an alignment module (not shown) positioned downstream of the unit 10 to straighten the boxes 20 and place them along a plurality of longitudinal parallel lines. The boxes 20 are then shingled in a stream unit (not shown) positioned downstream of the unit 10 .
[0033] The blanks initially all move in the longitudinal direction from a delivery upstream end of the unit 10 . The unit 10 then moves these blanks to a supply downstream end by means of a plurality of conveyor ramps 3 disposed in front of each of the rows of boxes 20 . These conveyor ramps 3 are adapted to convey the pre-cut substrate and the separated sub-substrates.
[0034] These ramps 3 have divergent orientations in a fan arrangement so as to separate the rows of boxes 20 from each other. To adjust the oblique orientation of the ramps 3 , the unit 10 includes upstream linear guide means 2 (see FIGS. 1 to 9 ) and downstream linear guide means 2 a (see FIGS. 2 to 9 ). The ramps 3 are mounted so as to slide and to pivot on the upstream guide means 2 and the downstream guide means 2 a . These guide means 2 and 2 a are attached at their two ends to a chassis 1 of the unit 10 . The guide means 2 and 2 a are substantially transverse and parallel to each other.
[0035] In order to move the boxes 20 from the delivery end to the supply end, each of the ramps 3 includes at least one drive belt 7 mounted on a plurality of guide rollers 11 (see FIG. 2 ). The belt 7 is driven by a main drive pulley 9 . Only the lower ramps 3 have been represented in FIG. 1 . To each of the lower ramps 3 there corresponds an upper ramp, the boxes being held in a pinch area between the belt 7 of a lower ramp 3 and a belt of an upper ramp.
[0036] The assembly formed by the belt 7 , the pulley 9 and the rollers 11 is supported by a support frame 13 . The upstream end 5 and the downstream end 5 a of the support frame 13 are mounted so as to slide and to pivot on the upstream guide means 2 and the downstream guide means 2 a , respectively.
[0037] The belt 7 has a flat contact surface so as to facilitate movement of the boxes 20 . The pulley 9 is plugged into a transverse drive shaft 15 . The pulley 9 is driven in rotation by the transverse drive shaft 15 , which is common to all the ramps 3 . The shaft 15 is mechanically connected to a drive motor. The pulley 9 is mobile transversely in translation along this shaft 15 . Thus the ramps 3 remain mobile in translation along this shaft 15 .
[0038] The unit 10 then comprises means for moving and positioning the ramps 3 in a fan configuration along the upstream guide means 2 and the downstream guide means 2 a . These moving and positioning means take the form of a mobile element or carriage 4 .
[0039] According to the invention, the carriage 4 moves along a central transverse rail 6 disposed between and parallel to the upstream guide means 2 and the downstream guide means 2 a . The rail 6 may be disposed equidistantly between the upstream guide means 2 and the downstream guide means 2 a . In a preferred embodiment of the invention, the carriage 4 is actuated by a toothed belt disposed inside the rail 6 and a drive motor.
[0040] According to the invention, the carriage 4 carries the unlocking means. These unlocking means comprise an upstream cylinder 8 directed longitudinally toward the delivery end, i.e. in the upstream direction, and a downstream cylinder 8 a directed longitudinally toward the supply end, i.e. toward the downstream end. The upstream cylinder 8 and the downstream cylinder 8 a each include and actuate an upstream mobile piston rod 12 and a downstream mobile piston rod 12 a , respectively. An upstream bearing member 14 and a downstream bearing member 14 a are attached to the free end of the upstream piston rod 12 and the downstream piston rod 12 a , respectively.
[0041] The ramps 3 comprises upstream locking means 17 and downstream locking means 17 a able to maintain the ramps 3 in a particular position enabling immobilization at will of these ramps 3 on the upstream guide means 2 and the downstream guide means 2 a , respectively. The locking means 17 and 17 a are disposed at the ends 5 and 5 a , respectively, of the support frame 13 of the ramps 30 . The locking means 17 and 17 a are designed to prevent movement of these ends 5 and 5 a along the guide means 2 and 2 a.
[0042] The upstream and downstream unlocking means are able to cooperate with the upstream locking means 17 and the downstream locking means 17 a to enable releasing of the ramps 3 so as to drive them along said upstream guide means 2 and said downstream guide means 2 a and to dispose them in a fan configuration. The cylinders 8 and 8 a with their piston rods 12 and 12 a and their bearing members 14 and 14 a are used to unlock the locking means 17 and 17 a.
[0043] Referring to FIGS. 2 to 9 , there are represented the successive steps of moving one of the conveyor ramps 3 . The ramp 3 goes from an initial position aligned with the longitudinal direction to a final position shifted laterally and diverging at an angle to the longitudinal direction. The unit 10 may include a parking area or volume 18 for one or more unused ramps, situated in the vicinity of the chassis 1 .
[0044] In a first position (see FIG. 2 ), the ramp 3 is stowed in the parking area 18 of the unit 10 . One or more ramps not used for the current job remain waiting during the time to adjust the position of the ramp 3 and/or during the job time for separation.
[0045] In this first position, the ramp 3 is aligned with the longitudinal direction. The ramp 3 is locked in position by the upstream guide means 2 and the downstream guide means 2 a by its upstream end 5 and its downstream end 5 a . For its part, the carriage 4 is initially positioned at the end of the rail 6 . The piston rods 12 and 12 a are fully retracted into the cylinders 8 and 8 a . The ramp 3 is then moved toward its operating position.
[0046] In a second position (see FIG. 3 ), the carriage 4 is moved (arrow C 1 in FIG. 2 ) along the rail 6 so as to position the bearing members 14 and 14 a in front of the ends 5 and 5 a.
[0047] In a third position (see FIG. 4 ), the cylinders 8 and 8 a are actuated (arrows F and Fa in FIG. 3 ) to deploy the piston rods 12 and 12 a in the direction of the ends 5 and 5 a . In this new position of the piston rods 12 and 12 a , each of the ends 5 and 5 a is unlocked by means of the bearing members 14 and 14 a . Moreover, engagement elements integrated to the bearing members 14 and 14 a are arranged so as to grasp these ends 5 and 5 a . Because of this, in this upstream and downstream unlocked position, the ramp 3 remains joined to, being hooked to the carriage 4 during its lateral movements.
[0048] In a fourth position (see FIG. 5 ), the carriage 4 is moved laterally (arrow C 2 in FIG. 4 ) along the rail 6 . The carriage 4 drives transversely in its movement the ramp 3 that has remained in its upstream and downstream unlocked position because of the action of the cylinders 8 and 8 a . In this new transverse position, the ramp 3 remains aligned with the longitudinal direction.
[0049] In a fifth position (see FIG. 6 ), the cylinder 8 is actuated so as to retract the upstream piston rod 12 in the direction of the rail 6 (arrow R in FIGS. 5 and 10 ). In this transverse position, the upstream end 5 is locked again.
[0050] In a sixth position (see FIG. 7 ), the carriage 4 is moved laterally along the rail 6 (arrow C 3 in FIG. 6 ). As it moves the carriage 4 drives only the downstream end 5 a , because of its unlocked position, but not the upstream end 5 , because of its locked position. In this transverse position, the ramp 3 is inclined relative to the longitudinal direction. This position corresponds to the final position of the ramp 3 .
[0051] In a seventh position (see FIG. 8 ), the cylinder 8 a is actuated to retract the piston rod 8 a in the direction of the rail 6 (arrow Ra in FIG. 7 ). In this transverse position the downstream end 5 a is locked again. Because of the distance between the downstream end 5 and the upstream end 5 a , the ramp 3 is locked in an oblique divergent position.
[0052] In an eighth position (see FIG. 9 ), the carriage 4 is moved laterally along the rail 6 (arrow C 4 in FIG. 8 ), so as to return to its initial position at the end of the rail 6 .
[0053] In this way, one and the same carriage 4 moves and positions adequately, one after the other, all of the ramps 3 to be used for the envisaged separation job. This movement procedure may be adapted to other initial or final positions of the ramp 3 or the carriage 4 .
[0054] The steps referred to above may be carried out in the reverse order so as to move the ramp 3 from its final position to its initial position. Using a similar principle to move the ramp 3 from one oblique position to another oblique position may also be envisaged. This principle consists notably in first moving the ramp 3 into a position aligned with the longitudinal direction, before moving the ramp 3 laterally, and then again orienting this ramp 3 in an oblique direction.
[0055] As may be seen in FIGS. 1 to 11 , the upstream locking means 17 and the downstream locking means 17 a are formed on the one hand by a slide taking the form of upstream downstream transverse rigid blade 19 and downstream transverse rigid blade 19 a , attached to the chassis 1 . The blades 19 and 19 a are substantially parallel to the upstream guide means 2 and the downstream guide means 2 a and to the rail 6 . These blades 19 and 19 a each have an oblong central opening 21 (visible in FIG. 11 ).
[0056] The interior is defined as being the area between the two guide means 2 and 2 a . The exterior is defined as being the upstream and downstream areas outside the guide means 2 and 2 a.
[0057] The locking means 17 and 17 a are formed on the other hand with exterior fixing means 22 and interior fixing means (see FIGS. 10 and 11 ), joined to the ramps 3 . The exterior fixing means 22 and the interior fixing means 23 cooperate with the corresponding blade 19 . The opening 21 enables the fixing means 22 and 23 to be passed on each side of the blades 19 and 19 a.
[0058] The ends 5 and 5 a of the support frame 13 of the ramp 3 each comprise upstream and downstream extensions 35 joined to the ramp 3 . The extensions 35 are situated at the point of pivoting and sliding on the upstream guide means 2 and the downstream guide means 2 a . The fixing means 22 and 23 are positioned on either side of the blade 19 and on either side of the extension 35 . This extension 35 includes a groove forming a rectangular profile sliding housing 36 inside which the exterior fixing means 22 and the blade 19 are positioned.
[0059] In the locked position of the upstream end 5 , the blade 19 is strongly clamped between the exterior fixing means 22 and a lower face of the wall of the housing 36 . This extension 35 is provided with an orifice 27 inside which the fixing means 23 slide.
[0060] The exterior fixing means 22 are formed of a mobile axis 24 passing through the oblong opening 21 of the blade 19 . The axis 24 is extended at an exterior end by a flat mobile head 26 . The head 26 is positioned on an exterior side of the blade 19 and clamps this blade 19 against the interior face of the wall of the housing 36 for locking purposes. The axis 24 and the head 26 are operated by the interior fixing means 23 disposed on the other side of this blade 19 .
[0061] The interior fixing means 23 are formed of a mobile actuator element or pusher 25 throughout the length of which extends a central hole receiving an interior end of the axis 24 . The pusher 25 has a tubular first part 25 a sliding inside the cavity 27 . This first part 25 a is pushed back toward the interior and out of this cavity 27 by means of a compression spring 29 disposed at the bottom of the cavity 27 .
[0062] The pusher 25 has a second tubular part or button 25 b having a bearing rim 28 configured to abut against the extension 35 in the unlocked position. This button 25 b has an interior recess 30 at its free end in which is positioned a nut 31 screwed onto the interior end of the axis 24 .
[0063] The upstream fixing means 22 and the downstream fixing means 23 are symmetrical to each other and enable locking and unlocking at will of the upstream end 5 and the downstream end 5 a to the upstream blade 19 and the downstream blade 19 a , respectively.
[0064] In the unlocked position (see FIG. 10 ), by virtue of the action of the piston rod 12 of the cylinder 8 , the bearing member 14 pushes back the pusher 25 by bearing on the button 25 b . The button 25 b is thus pushed back against the extension 35 . The button 25 b drives the first part 25 a against the compression spring 29 . The first part 25 a slides and enters the cavity 27 . The first part 25 a drives the axis outward through the oblong opening 21 of the blade 19 . Consequently, the head 26 of the axis 24 therefore no longer bears on the blade 19 .
[0065] To drive the extension 35 , and consequently the ends 5 and 5 a of the ramp 3 in their lateral movement along said upstream guide means 2 and downstream guide means 2 a and to dispose them in a fan configuration, the carriage 4 comprises in accordance with the invention upstream and downstream grasping means. These grasping means are formed of a plurality of lugs 33 disposed in the vicinity of the bearing members 14 and 14 a . The bearing member 14 is provided on its lateral edges with fixing lugs 33 . These lugs are configured to be positioned around the pusher 25 on either side of the extension 35 when the bearing member 14 moves toward and then pushes the pusher 25 .
[0066] The separator unit 10 as described above may be operated manually by an operator or may function automatically.
[0067] This movement may be effected either under the manual control of an operator or automatically. In the latter case, it is preferable to integrate detection means on the carriage 4 being able to detect the presence of marker means on the conveyor ramps 3 . These detector means are inductive detectors, for example, able to detect the presence of a metal part disposed at a short distance. The detection means are used to align the unlocking means of the carriage 4 with the locking means 17 and 17 a of the ramps 3 by accurately controlling the driving of the carriage 4 .
[0068] Computerized control means are provided for controlling automatically the movement of the carriage 4 and the cylinders 8 and 8 a . This automatic control may be effected as a function of data stored beforehand in the computer, namely the dimensions of the boxes 20 , the number of ramps 3 , the initial position of the ramps 3 relative to the boxes 20 or the lateral spacing between the boxes 20 at the supply end. Such automatic control is effected as a function of information received from the detector means detecting the position of the ramps 3 and the carriage 4 .
[0069] The present invention is not limited to the embodiments described and shown. Numerous modifications may be made without departing from the framework defined by the scope of the claims. | A unit for separating a pre-cut-out substrate into a plurality of separate sub-substrates ( 20 ). The unit includes upstream ( 2 ) and downstream ( 2 a ) transverse guides; conveyor ramps, which convey the pre-cut-out substrate and the separate sub-substrates ( 20 ), the ramps are slidably and pivotably mounted on the guides ( 4 ). Upstream and downstream locks holds each ramp ( 3 ) in a locked position. A movable element supports upstream and downstream unlocking devices for engaging the upstream and downstream locking devices to release the ramps ( 3 ). Upstream and downstream grasping devices grasp and drive the ramps ( 3 ) along the upstream ( 2 ) and downstream ( 2 a ) guides to arrange the ramps in a fan-like configuration. | 8 |
FIELD OF THE INVENTION
The present invention relates to a residential building with staggered dwellings according to the preamble of Patent Claim 1 .
BACKGROUND OF THE INVENTION
Many people dream of having their own house or flat. The accommodation available for the middle classes is made up of houses that are at a relatively large distance from urban agglomeration, of terraced housing closer to urban agglomeration or of rented and bought flats in the town or city or in suburbs. Flats which are available today in town and city centres are not only expensive but also, in many cases, are not attractive to those who are not keen on typically urban buildings.
Living space had to be created quickly in the years following the Second World War. In today's terms, bland residential buildings with dwellings were constructed. Architecture which was popular at the end of the nineteenth century and at the beginning of the twentieth century, and in which the facade of a house reflected the use of the latter, was lost. The facades were featureless and uniform. The facade was the same from the ground floor to the top floor and, if this is possible, the blandness was even emphasized by a flat roof. Even if the uniformity was combated at a later date with specific facade designs, a block with dwellings can only be rendered interesting to the observer by additional outlay and associated extra costs.
Maisonettes do indeed provide living-space alternatives, but do little to influence the facade design. Residential buildings with flats or maisonettes make good use of the urban areas available. The living quality, however, automatically suffers if construction is dominated by bland and monotonous blocks of flats.
SUMMARY OF THE INVENTION
It is the aim with all known types of accommodation such as “maisonettes”, “split-level dwellings” or Corbusier's “Unité d'habitation” to increase the amount of space available. In these types of dwelling, however, the various storeys are always rendered accessible via internal staircases. This restricts the opportunity for adaptation to individual living-style requirements.
Since individualism and affluence permit it, it is also the case nowadays that people seek to realize their personal individuality in their living space. This results in the population moving to the suburbs or even to the country, where freely designable living space is still available and affordable. This inevitably results in the countryside being overdeveloped, with less dense building on the space available. The overdevelopment of the countryside also leads to the countryside becoming “clogged up”. The traffic infrastructures for private vehicles likewise have to be constantly expanded.
It is frequently the case that very poor use is made of living space in old buildings or old factories in towns and cities. In towns and cities, for example, disused factories, warehouses and workshops are converted into living areas. This conversion preserves the structural substance of the available buildings, but does not make optimum use of the land available. Many people have become aware of such possibilities in recent years. On account of poor use being made of the space, however, the need can only be satisfied for an affluent minority of the population. In order to provide the necessary living space to meet these requirements, the relatively large areas of the former industrial spaces are divided up and converted into dwellings. The interesting and attractive feature of this living space is provided by the large rooms and the high ceilings, which let in a large amount of light and give a good sense of space. It is not uncommon for these, in “normal conditions”, to be from 3.5 m to 4 m for print shops and workshops and from 4 m to 6 m for former factories.
For dwellings and residential buildings which are to be newly constructed, for financial reasons, there is no question of building dwellings with such ceiling heights. Other possibilities are therefore sought, and found, albeit with the disadvantage that most models are two-storey living areas, two single-storey living areas being rendered accessible by staircases in the region of the living areas. Many of the known types of accommodation do not give the feeling of freedom and the possibilities for the individual utilization of an open system allowing flexible design of space.
Industrial buildings, with their need for a large continuous surface area, have always been constructed with an outer shell and a roof, the roof being borne by supports. The supports interrupt the useful floor space at certain points. It is possible, in principle, for the surface area available to be divided up, in an absolutely flexible manner, by easily removable partition walls or to be utilized as a whole.
The demographic make-up of the population is characterized by increasing numbers of elderly people. Households can be divided up into a third for those living on their own, a further third for couples and a third for families or house shares with three or more people. At the same time, in Central Europe, the amount of living area required over the last 50 years has increased by 1 m 2 per person every two years. Older generations avoid old people's homes and usually only move after having reached the age of 80, and even then usually for medical reasons, often into care homes.
The need which arises from this is an alternative, denser type of construction in urban areas with a large amount of individual design freedom. The residents' need for their own private space should not be forgotten.
The new Röntgenareal building, by Isa Stürm and Urs Wolf, by Zurich's main railway station is an example of an attempt to provide attractive residential buildings with dwellings with single-storey living areas. Nine seven-storey residential buildings have been set up on an area at the edge of the track of Zurich's station which, until developed, was used as a storage area. The individual buildings are offset in relation to one another. The space between them is affected by the noise of the railway. The dwellings occupy the four corners and are thus directed towards two sides.
The ground floor of these urban residential buildings is occupied by dwellings and front gardens. The status of the free space is thus ambiguous. On the one hand, it belongs to everybody, and is therefore public, and on the other hand it also belongs to the tenants of these ground-floor dwellings. This combination of functions reduces the value of the areas between the residential buildings which are intended for the public. The tenants of the ground-floor dwellings try to achieve a bit of private space with hedges and small walls. The same goes on the balconies. The direct view in means that the tenants are always on public view as they go about living in the dwellings and moving on the balconies and in front of the ground-floor flats.
The uniformity of the facades and of the dwellings, the constant lack of total privacy and the associated lack of clear expression restricts the living quality in such urban residential buildings, even though public space will be provided. There is an absence of individual design possibilities and of availability of a variety of different living spaces in the same residential building, which could be achieved with a corresponding type of accommodation. The same applies to the outdoor area (terrace). It is only when the latter affords a certain amount of protection from prying eyes and is noise-proofed that the outdoor area can be defined as “private” and utilized and, in particular, regarded as such by the residents.
The object of the present invention, then, is to use an open system to provide a living area of the type mentioned in the introduction such that, in each unit, a two-storey dwelling part and outdoor area (terrace) are available, a relatively large amount of space is available specifically in the third dimension (room height), the advantages of dense construction are maintained and it is possible to realize variations in all sizes of living space, levels of comfort and the individual design of dwellings.
This object is achieved by a residential building with staggered dwellings having the features of Patent Claim 1 . Further features according to the invention can be gathered from the dependent claims, and the advantages thereof are explained in the following description.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawing:
FIG. 1 shows a dwelling with an illustration of the surface areas.
FIG. 2 shows two dwellings with the single-storey living areas overlapping.
FIG. 3 shows two dwellings with the single-storey living areas overlapping.
FIG. 4 shows two dwellings with a large single-storey living area.
FIG. 5 shows a residential building with staggered dwellings.
FIG. 6 shows a residential building with staggered dwellings.
FIG. 7 a facade of a residential building with staggered dwellings.
FIG. 8 shows a section through a residential building with a shop area, an office area and staggered dwellings.
FIG. 9 shows a plan view of a ground-floor shop area.
FIG. 10 shows a plan view of an office level.
FIG. 11 shows a plan view of a storey with staggered dwellings.
FIG. 12 shows the incidence of light in a dwelling with a single-storey living area.
FIG. 13 shows the incidence of light in the two-storey dwelling part of a staggered dwelling.
FIG. 14 shows the incidence of light in the two-storey dwelling part of a staggered dwelling.
The figures illustrate preferred exemplary embodiments which will be explained by way of the following description.
DETAILED DESCRIPTION OF THE INVENTION
In the residential building with staggered dwellings on which the invention is based, each dwelling 1 has a two-storey dwelling part 11 and a single-storey dwelling part 10 . The way in which the surface area 100 of the single-storey dwelling part 10 is divided up may be largely adapted to requirements. The two-storey dwelling part 11 is divided up and has a two-storey living area 13 and a two-storey outdoor area 12 . Each dwelling 1 thus gains extra space in comparison with conventional residential buildings.
The two high, two-storey areas, the living area 13 and outdoor area 12 , are located one beside the other or one behind the other and thus allow extensive plan development.
The incidence of light into the inner zones allows a variety of different uses in the generously dimensioned single-storey dwelling part 10 . By virtue of the outer appearance of the residential building which arises from the play between the single-storey dwelling part 10 and the two-storey dwelling part 11 , an absolutely new sense of individuality, namely the individuality of the residential building with staggered dwellings ( FIGS. 5 and 6 ), is expressed in the facade. This individuality is system-specific and is not dependent on expensive facade designs.
A dwelling 1 , which forms the basis of the system of a residential building with staggered dwellings, is shown in FIG. 1 . The dwelling 1 in FIG. 1 , illustrated as a standard module, comprises two dwelling parts, a single-storey dwelling part 10 and a two-storey dwelling part 11 . The surface area 100 of the single-storey dwelling part 10 is at least equal to, but usually greater than, the surface area 110 , indicated by F, of the two-storey dwelling part 11 . The two-storey dwelling part 11 is approximately double the height of the single-storey dwelling part 10 and is divided up into an outdoor area 12 and an indoor area 13 . The outdoor area 12 is always directed towards a facade side of the residential building. The surface area of the single-storey dwelling part 10 will be greater, for practical reasons, than that of the two-storey dwelling part 11 . However, all the single-storey dwelling parts 10 on one level of a residential building with staggered dwellings will have the same total surface area 100 . The way in which the region of the single-storey dwelling parts 10 is divided up can be freely selected and can thus be adapted, with a high level of flexibility, to the respective requirements.
If the plans are based, for example, on two 4-room dwellings, it is possible, with most types, for at least one room to be optionally assigned to the neighbouring dwelling. The accommodation available is thus made up of three-room, four-room and 5-room dwellings. Like the size of dwelling, it is also possible for the standard of comfort to be adapted to the specific requirements in each case. Examples of this are as follows: direct lift access into the dwellings, increasing the size of the outdoor area 12 to the detriment of the two-storey living area 13 , the availability of a cooling system, the installation of a fireplace and chimney etc., the open construction system in the basic state allows individual completion work by the tenant. The way in which rooms are divided up, the type of kitchen and sanitary zones, and the design of floors, walls, ceilings and installations may thus be freely selected.
The surface area of the two-storey dwelling part 11 is the same for all dwellings 1 in a residential building with staggered dwellings. Different residential buildings with staggered dwellings, however, may have two-storey dwelling parts 11 with different surface areas 110 . The two-storey dwelling parts 11 always rise above a level. They are arranged alternately, which is evident from the drawings.
FIG. 2 shows how, in the case of the construction system according to the invention, a second dwelling 1 ′ with a single-storey dwelling part 10 ′ and a two-storey dwelling 11 ′ ends up located over the surface area 110 / 100 / 110 ′, with a offset in relation to the dwelling 1 . Both dwellings 1 and 1 ′ are located over the surface area 100 . While the lower dwelling 1 ′ rests on the surface areas 100 and 110 ′, the dwelling 1 has the surface area 100 located above the dwelling 1 ′. Beneath the two-storey dwelling part 11 , the surface area 110 is free by the height of the single-storey dwelling part 10 ′. The size of the single-storey dwelling part 10 ′ may be increased such that it fills the surface area 110 beneath the two-storey dwelling part 11 . In the lowermost-storey, this area may also be utilized as a storage or service area. Examples of how the surface area of the single-storey dwelling part 10 can be extended are shown in FIGS. 3 and 4 .
Residential buildings with staggered dwellings are based on a completely new urban concept. In a densely populated environment, the desire for living space goes hand in hand with the demand for commercial areas such as local shops and offices. The residents of such areas naturally want a calm and natural environment of individual design. This demand is ideally met by the system of the residential building with staggered dwellings according to the invention. Nature may be brought into the dwelling to a certain extent; indeed, the ceiling height in the two-storey dwelling part is such that it is possible to keep even relatively large plants. In respect of rail and road traffic, the concept of designing a self-contained building makes it possible to protect the living areas against noise.
Access to all the storeys of a building according to the invention is ensured via the staircase and lift installations 40 ( FIG. 9 ). The drawings each depict a lift, the number of lifts and also the number of necessary staircases depending on the overall concept of the building. This type of design makes it possible to provide the upper dwellings with direct lift access without any additional outlay.
FIG. 8 illustrates a cross section of a residential building with a shop area 52 , an office area 51 and staggered dwellings 50 . The lowermost storeys, illustrated in FIG. 8 by the ground-floor storey, are constructed with a greater ceiling height, are on one level and, as is shown in FIG. 9 , extend over the entire surface area of the building. These storeys are ideally suited for use as a shop area 52 . Artificial light is preferred for shop areas, with the result that the relatively poor incidence of light for a storey with a very large surface area does not matter. If the upper storeys of the building are designed with a facade recess 54 , the shop area 52 in this region may be provided with natural light through skylights 55 . On the ground floor, the shop area 52 may be supplemented by a covered exterior passageway 53 for the sale of promotional items, fresh vegetables or other articles which are to be made as accessible to the customer as possible.
The storeys directly above the shop areas 52 ( FIGS. 8 and 10 ) are likewise on a single level with freely designable partitioning for office areas 51 . The plan differs from that of the first storey in so far as the surface area of the facade is increased by the provision, for example, of a facade recess 54 . This makes it possible to achieve more office area 51 with direct incidence of natural light.
Above this, use is then made of the concept and system of the residential building with staggered dwellings according to the invention ( FIG. 11 ). It is also the case in this region that use is made of the large surface area of the facade in order to provide a lot of direct natural light. The two-storey living area 14 of the dwelling beneath projects into the storey plan 50 .
In this type of concept ( FIGS. 8 , 9 , 10 and 11 ), by way of example, it is possible to arrange four dwellings 1 on each storey without giving the effect of a “tower block”. Each dwelling has a two-storey living area and thus an outdoor area 12 . In this system, it is possible to construct “towers” with good accommodation availability which enrich the urban landscape and provide the residents with homely, interesting and individually designable living areas.
The incidence of light is a central advantage for the concept of the staggered dwellings according to the invention. FIGS. 12 , 13 and 14 illustrate in section how the system presented admits light right into the actual living space as a result of the height of the two-storey dwelling part 11 . The volume 30 which is not exposed to direct light ( FIGS. 12 , 13 and 14 ) is greater. The double height of the outdoor area 12 arranged on the facade side ensures more light according to the invention. | The invention presents the concept of a residential building which is constructed on the principle of staggered dwellings. The staggered dwellings each have a single-storey dwelling part ( 10, 23 ) and a two-storey dwelling part ( 11 ) with outdoor area. The living area ( 10 and 11 ) of the dwelling is open and allows individual living requirements to be realized with a variability which has not been known up until now. The division of space is not fixed by the static system. The type of accommodation presented can be realized in all types of urban construction such as blocks of flats, block-edge developments or high-rise buildings from two storeys upwards. The sizes of dwellings may be determined in accordance with the location and the target group. Combining the accommodation with service-related and commercial use is made possible in a completely new way using this principle. | 4 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The invention relates to a method for applying a scale to a carrier, in particular to an optical element of an objective as carrier, more particular to a lens.
[0003] The invention also relates to an objective for semiconductor lithography, a scale with a measuring graduation being applied to a lens or an inner holder.
[0004] When carrying out changes in position of an optical element in an objective, e.g. on the lens which is mounted in an inner holder and which is connected to an outer holder via corresponding intermediate elements, it is advantageous to determine the position of the change in position of the optical element when this experiences a corresponding offset, e.g. through the use of manipulators.
[0005] 2. Description of the Related Art
[0006] It is known to arrange on one of the two holder parts, preferably the inner holder, a separate glass carrier which is provided with a scale with an etched-in measuring graduation. In this case, the glass carrier is connected to the underlying holder, which is generally composed of steel, via fixing elements. Besides the disadvantage of an additional component and an associated higher fixing outlay, a further disadvantage of the known measuring method resides in different thermal expansions between the glass carrier with the scale and the holder on which the glass carrier with the scale is arranged. As a result of the different thermal expansions between the two parts, there is the risk of the measurement result becoming more inaccurate.
SUMMARY OF THE INVENTION
[0007] Therefore, the present invention is based on the object of providing a method for applying a scale to a carrier and an apparatus therefore which can be used to carry out measurements with simple means, with the possibility, in particular, of effecting measurement with higher accuracy and with relatively simple means, in the case of an offset of an optical element.
[0008] According to the invention, this object is achieved by means of a method for applying a scale to a carrier, a material layer being applied to said carrier in such a way that changes in length of the material layer on account of temperature changes correspond at least approximately to changes in length of said carrier on account of temperature changes, and said scale being introduced into or applied to said material layer with a measuring graduation.
[0009] More specifically, this object is achieved by means of a method for applying a scale to an optical element of an objective for semiconductor lithography, a material layer being applied to an optical element in such a way that changes in length of said material layer on account of temperature changes correspond at least approximately to changes in length of said optical element on account of temperature changes, and said scale being introduced into or applied to said material layer with a measuring graduation.
[0010] This object is also achieved in an objective for semiconductor lithography, wherein a scale being provided on an inner holder or on a lens.
[0011] By virtue of the fact that a material layer is applied directly to the carrier, e.g. to an optical element of an objective, such as e.g. an objective for semiconductor lithography, the thermal expansion profile of the carrier being forced on the thermal expansion profile of said material layer, on the one hand separate fixing elements for the scale are avoided and on the other hand problems with a varying thermal expansion coefficient no longer arise. This means that the position and changes in position of the carrier, e.g. a lens, can be ascertained with significantly higher accuracy.
[0012] In a highly advantageous improvement of the invention, it may be provided that the scale is introduced directly into the carrier, e.g. the holder of a lens, or else is introduced into or applied to the lens itself in an optically inactive region, i.e. into a region which is not required for the exposure.
[0013] In a further embodiment of the invention, it may be provided that the material layer for the scale has at least approximately the same thermal expansion coefficient as the carrier. If e.g. a lens is provided as the carrier, then the material layer for the scale may be composed of the same material as the lens. Identical thermal expansion coefficients are thus present in this case. The same material layer also results automatically when the scale is introduced directly into the lens itself, e.g. through corresponding etching-in or scribing-in.
[0014] In a highly advantageous further improvement of the invention, it may be provided that glass is used as the material layer, the measuring graduation of the scale being applied to the glass layer. In this case, the measuring graduation of the scale may be vapor-deposited onto the glass layer.
[0015] The application of the material layer to the carrier, e.g. a lens or the holder of a lens, may be effected by sputtering or vapor deposition.
[0016] If the scale is arranged on the lens or on the inner holder of the lens, then corresponding measuring elements for measurement, e.g. a sensor, which measures the position and the displacement distances of the lens by means of the measuring graduation of the scale will be provided on the associated outer holder or in a corresponding region of the objective.
[0017] A possible sensor is e.g. an incremental capacitive or incremental inductive sensor, an interferometric transmitter or else another sensor which operates with the desired high measurement accuracy, which should lie in the nanometers range.
[0018] Advantageous developments and improvements emerge from the rest of the subclaims and from the exemplary embodiments, whose principles are described below with reference to the drawing.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] [0019]FIG. 1 shows a plan view of a lens which is connected to an outer holder via an inner holder and elastic connecting elements, and
[0020] [0020]FIGS. 2 a to 2 c show enlarged illustrations of a scale introduced or applied to the lens.
DETAILED DESCRIPTION
[0021] The invention is described below by way of example for an objective which is provided for semiconductor lithography. It goes without saying that the method according to the invention is also suitable for other objectives. Furthermore, use is also possible in other technical fields in which it is important to perform measurements with a very high accuracy.
[0022] A lens 1 , which in this case functions as a carrier, is mounted in a known manner in an inner holder 2 . The inner holder 2 is connected to an outer holder 4 , which forms a fixed part of an objective 5 , via one or more connecting elements 3 arranged in a distributed manner over the periphery. The inner holder 2 and outer holder 4 may be designed in one piece together with the connecting elements 3 .
[0023] By means of actuators 6 not illustrated in greater detail (only one actuator is illustrated by broken lines for example in FIG. 1), it is possible to carry out displacements of the inner holder 2 and thus also of the lens 1 in the x/y direction, i.e. right-angled to the optical axis and in the plane of the lens, in accordance with the direction of the arrow or else in the direction of the optical axis, which is perpendicular to the lens plane. These displacements may be in the nanometers range.
[0024] In order, then, to determine these displacements or the offset of the inner holder 2 relative to the outer holder 4 , a plurality of scales 7 arranged in a distributed manner over the periphery are provided, which are arranged on the lens 1 as carrier. In a different configuration, the scales 7 are arranged on the inner holder as carrier. In the exemplary embodiment illustrated in FIG. 1, three scales 7 arranged in a manner distributed uniformly over the periphery are provided, which are fitted on flattened portions 8 in the peripheral wall of the lens 1 . In principle, two scales 7 arranged at a right angle to one another on the periphery of the lens 1 suffice for detecting displacements in the x/y direction. If three scales 7 with corresponding measurements are provided, then it is also possible for displacements of the center of the lens 1 or the off-centering thereof to be determined exactly. The respective measuring directions are specified by arrows 9 in FIG. 1.
[0025] If the intention is to measure displacements of the lens 1 in the z-direction of the captical axis, the scales 7 are to be correspondingly arranged axially (in the direction of the optical axis) along the peripheral wall of the lens 1 . In the exemplary embodiment illustrated, this means that the scales 7 are perpendicular to the plane of the drawing.
[0026] The position of a scale 7 ′ is also additionally illustrated by broken lines in FIG. 1, which scale is arranged on a corresponding flattened portion on the outer peripheral wall of the inner holder 2 . If the inner holder 2 is fixedly connected to the lens 1 , displacements of the lens 1 relative to the outer holder 4 can also be ascertained in the case of an arrangement of scales 7 ′ on the inner holder 2 .
[0027] Sensors 10 are provided for the purpose of measuring the displacement of the lens 1 , which sensors are arranged on the outer holder 4 or another part of the objective 5 and are directed at the scales 7 or evaluate the latter.
[0028] Since such sensors 10 are known in principle, they are only indicated to a basic extent in FIG. 1. What are suitable for this purpose are e.g. capacitive or inductive sensors or else interferometric transmitters such as e.g. grating interferometers, as described e.g. in the journal “Feinwerktechnik & Meβtechnik 98 (1990) 10”, page 406 in the article “Längen in der Ultra-präzisionsmeβtechnik messen” [“Measuring lengths in ultraprecision measurement technology”].
[0029] [0029]FIGS. 2 a, 2 b and 2 c specify for example three possibilities for applying the scale 7 to the lens 1 or the inner holder 2 .
[0030] In accordance with FIG. 2 a a material layer 11 is applied to the flattened portion 8 on the peripheral wall of the lens 1 , said material layer having the same thermal expansion behavior as the lens 1 itself. Preferably, the same material which is also used for the lens 1 is taken for this, if possible. E.g. glass can be used as the material layer 11 which is correspondingly applied to the lens 1 , in which case the thickness of the glass may between 2 and 7μ.
[0031] In accordance with FIG. 2 a, the scale 7 with the measuring graduation 7 a is then applied to the material layer 11 . This can be effected e.g. by vapor deposition. For the scale 7 it is likewise possible to use glass or also another material such as e.g. a metal, in particular chromium, aluminum or silver.
[0032] Instead of vapor deposition of the measuring graduation 7 a, the latter can also be etched into the material layer 11 , as is illustrated in FIG. 2 b.
[0033] During the application of the material layer for the scale to the carrier, it is merely necessary to ensure that this is applied, for the case where different materials are present, only with such a small thickness that the thermal expansion profile of the carrier is forced on the material layer.
[0034] If identical or similar thermal expansion coefficients are present for the carrier and the material layer, then the thickness of the material layer has no influence on any varying thermal expansion profile. This is case e.g. when both carrier and material layer are composed of the same material.
[0035] [0035]FIG. 2 c shows a configuration of a scale 7 , the measuring graduation 7 a being etched directly into the lens 1 , into a corresponding flattened portion 8 of the lens 1 .
[0036] Instead of application of the scale 7 to the carrier, in the exemplary embodiment the lens 1 or the inner holder 2 , by sputtering of the material layer 11 , it is also possible, if appropriate, for a scale 7 with the measuring graduation 7 a to be applied by wringing onto the flattened portion 8 of the lens 1 . | In a method for applying a scale ( 7 ) to a carrier ( 1,2 ), a material layer ( 11 ) is applied to the carrier in such a way that the change in length on account of temperature change of the material layer ( 11 ) corresponds at least approximately to changes in length of the carrier ( 1,2 ) on account of temperature change. The scale ( 7 ) is introduced into or applied to the material layer ( 11 ) with a measuring graduation ( 7 a ). The carrier may be an optical element, e.g. a lens ( 1 ) of an objective ( 5 ) for semiconductor lithography. | 6 |
PRIORITY CLAIM
[0001] This invention claims the benefit of U.S. provisional patent application Ser. No. 61/615,845 filed Mar. 26, 2012 (our ref. GARR-1-1001) and U.S. provisional patent application Ser. No. 61/671,045 filed Jul. 12, 2012 (our ref. GARR-1-1002). The foregoing applications are incorporated by reference in their entirety as if fully set forth herein.
FIELD OF THE INVENTION
[0002] This invention relates generally to analytics, and more specifically, to systems and methods for real-time and discrete analytics for web-mediated content and events.
SUMMARY
[0003] This invention relates generally to analytics, and more specifically, to systems and methods for real-time and discrete analytics for web-mediated content and events. In some embodiments, a method for real-time and discrete analytics for web-mediated content and events may be provided for the benefit of a presenter. In some embodiments, the presenter may be delivering a speech to a room full of audience members. In other embodiments, the presenter may be delivering a web-based media content over the Internet to audience members, the audience members being geographically dispersed but consuming the web-based media content being delivered by the presenter simultaneously. In some embodiments, the web-based media content may be delivered to the audience members via client software on a terminal, the terminal being any of a plurality of devices, which may include a laptop, a tablet, a smartphone, or any other device operably connected via a network connection to the one or more servers.
[0004] In some embodiments, a method for real-time and discrete analytics for web-mediated content and events may facilitate the emitting of questions to the audience members. In some embodiments, the emitting of questions may be controlled by the presenter. In other embodiments, the emitting of questions may be delivered by the one or more servers in synchronization with the presenter. In some embodiments, emitting a question results in the question being displayed on the plurality of client terminals, inviting the plurality of audience members to provide an answer, the answer being received via the network connection by the one or more servers.
[0005] In some embodiments, answers are stored as data by the one or more servers, and the data is aggregated. The aggregated data may be viewed by the presenter using a computing device. The presenter may formulate or select additional questions based upon the aggregated data being viewed on the computing device. In some embodiments, the computing device is also used to deliver a presentation to the audience members, such as a PowerPoint presentation. In other embodiments, the computing device may be used to control the timing and content of questions for the audience members.
[0006] In some embodiments, a system for real-time and discrete analytics for web-mediated content and events may include an authentication component, comprising the means for users of client devices to connect with the system; a storage component, comprising various data stores for authentication information, presentation information, question information, response information, aggregated data sets, analytics, or other data stored in conjunction with the system; an emitter component, comprising a means for a presenter or other operator of the system to emit a question which will be received by the client devices; and an analytics component, comprising a private dashboard which is displayed on a display. In some embodiments, the system may have a project component, comprising a means for users of the system to create a project file including a presentation and a plurality of questions to be emitted at certain times during the presentation.
BRIEF DESCRIPTION OF THE DRAWINGS
[0007] Embodiments of the present invention are described in detail below with reference to the following drawings:
[0008] FIG. 1 is a block diagram of an exemplary environment in which a method for real-time and discrete analytics for web-mediated content and events may be implemented, in accordance with an embodiment of the invention;
[0009] FIG. 2 is a flow diagram depicting a method for real-time and discrete analytics for web-mediated content and events, in accordance with an embodiment of the invention;
[0010] FIGS. 3-6 are a flow diagram depicting alternative embodiments of a method for real-time and discrete analytics for web-mediated content and events; and
[0011] FIG. 7 is a block diagram of a system for real-time and discrete analytics for web-mediated content and events, in accordance with an embodiment of the invention.
DETAILED DESCRIPTION
[0012] This invention relates generally to analytics, and more specifically, to systems and methods for real-time and discrete analytics for web-mediated content and events. Specific details of certain embodiments of the invention are set forth in the following description and FIGS. 1-7 to provide a thorough understanding of such embodiments. The present invention may have additional embodiments, may be practiced without one or more of the details described for any particular described embodiment, or may have any detail described for one particular embodiment practiced with any other detail described for another embodiment.
[0013] FIG. 1 is a block diagram of an exemplary environment in which a method for real-time and discrete analytics for web-mediated content and events may be implemented, in accordance with an embodiment of the invention. In some embodiments, a method for real-time and discrete analytics for web-mediated content and events may be facilitated by one or more servers 102 . The one or more servers 102 may include one or more of a web front-end, a project site, a feedback engine, a real-time viewing engine, a reporting engine, a federation engine, and/or a database tier, the database tier having one or more of account information, billing information, and/or project information. The one or more servers are operatively coupled with a network connection 104 . The network connection 104 provides connections between the servers, and also provides network connections to system clients.
[0014] In some embodiments, a method for real-time and discrete analytics for web-mediated content and events may be provided for the benefit of a presenter 130 . In some embodiments, the presenter 130 may be delivering a speech to a room full of audience members 110 . In other embodiments, the presenter 130 may be delivering a web-based media content over the Internet to audience members 110 , the audience members 110 being geographically dispersed but consuming the web-based media content being delivered by the presenter 130 simultaneously. In some embodiments, the web-based media content may be delivered to the audience members 110 via client software on a terminal, the terminal being depicted as a plurality of devices 120 , which may include a laptop 122 , a tablet 124 , a smartphone 12 N, or any other device operably connected via a network connection to the one or more servers 102 .
[0015] In some embodiments, a method for real-time and discrete analytics for web-mediated content and events may facilitate the emitting of questions to the audience members 110 . In some embodiments, the emitting of questions may be controlled by the presenter 130 . In other embodiments, the emitting of questions may be delivered by the one or more servers 102 in synchronization with the presenter 130 . In some embodiments, emitting a question results in the question being displayed on the plurality of client terminals 120 , inviting the plurality of audience members 110 to provide an answer, the answer being received via the network connection 104 by the one or more servers 102 .
[0016] In some embodiments, answers are stored as data by the one or more servers 102 , and the data is aggregated. The aggregated data may be viewed by the presenter 130 using a computing device 132 . The presenter 130 may formulate or select additional questions based upon the aggregated data being viewed on the computing device 132 . In some embodiments, the computing device 132 is also used to deliver a presentation to the audience members 110 , such as a PowerPoint presentation. In other embodiments, the computing device 132 may be used to control the timing and content of questions for the audience members 110 .
[0017] FIG. 2 is a flow diagram depicting a method for real-time and discrete analytics for web-mediated content and events, in accordance with an embodiment of the invention. In some embodiments, a method for real-time and discrete analytics for web-mediated content and events includes providing a plurality of audience members with a client platform at 202 , establishing a connection between the client platform and at least a first server at 204 , emitting a first question from the at least a first server over the connection to the plurality of audience members, the first question being received by the client platform at 206 , receiving at least one response over the connection, the response responsive to the emitting a first question at 208 , aggregating at least the at least one response into aggregated data at 210 , and displaying at least a first view comprised of at least the aggregated data at 212 . In some embodiments, the method may optionally include emitting a second question responsive to at least the aggregated data displayed by the analytics view at 214 .
[0018] In some embodiments, providing a plurality of audience members with a client platform at 202 may include the audience members connecting to a network host using a computing device. The computing device may load a web front-end as a web page, or the computing device may download client software configured for communicating with the network host. The computing device may include a smartphone, a tablet PC, a laptop computer, a desktop computer, a video game console, or any other device facilitating a connection to a network host. The network connection may be wired or wireless. The network connection may include the Internet. In some embodiments, the network hosts to which the computing devices connect are reachable without communicating via the Internet.
[0019] In some embodiments, the client platform may receive a presentation. In different embodiments, the client platform may be configured only for receiving questions and submitting answers. In some embodiments, the client platform is an application, widget, web-page, or other similar component.
[0020] In some embodiments, the establishing a connection between the client platform and at least a first server at 204 may include the client platform operably connecting with a server, perhaps including logging in and authentication with user credentials. In some embodiments, a user may create an account pursuant to establishing a connection. In different embodiments, a user may use an existing account. In yet a different embodiment, a user may not be required to log into the server but be able to receive questions and submit answers.
[0021] In some embodiments, the emitting a first question from the at least a first server over the connection to the plurality of audience members, the first question being received by the client platform at 206 includes transmitting a question over the network to the plurality of client platforms. A user may be presented with a question in the application, widget or web-page with which the user is connected to the server. The question may be accompanied by a plurality of answers from which the user may choose one or more of the answers.
[0022] In some embodiments, the receiving at least one response over the connection, the response responsive to the emitting a first question at 208 comprises the server receiving over the network the answer choice selected or entered by the user of the client platform. In some embodiments, the data is stored, potentially with information about the users who submitted the answers (including, but not limited to, the source IP address).
[0023] In some embodiments, the aggregating at least the at least one response into aggregated data at 210 comprises creating analytics directed to the question having been emitted. In some embodiments, the aggregated data can be sorted by source IP, or by geography based upon a source IP lookup.
[0024] In some embodiments, the displaying at least a first view comprised of at least the aggregated data at 212 includes providing a private dashboard for the presenter. The private dashboard may permit the presenter to pivot the data, breaking the answers down by category.
[0025] In some embodiments, the emitting a second question responsive to at least the aggregated data displayed by the analytics view at 214 comprises the presenter formulating new content or questions based upon the aggregated data displayed at 212 . Method 200 may be repeated as desired for as many questions as the presenter wishes to pose, or emit, to the audience. Each question and its responses provide another axis for analyzing or pivoting the aggregated data that is aggregated at 210 . A presenter may decide to alter the presentation, or to ask a question that elaborates on a past question.
[0026] FIG. 3 is a flow diagram depicting alternative embodiments of a method for real-time and discrete analytics for web-mediated content and events. In some embodiments, operation 202 has an optional step 216 , comprising receiving a client login from a plurality of audience members, each client login comprising at least demographic data associated with each audience member. In some embodiments, operation 210 has an optional step 218 , comprising aggregating at least the at least one response and the demographic data associated with the audience member sending the at least one response into aggregated data.
[0027] In some embodiments, receiving a client login from a plurality of audience members, each client login comprising at least demographic data associated with each audience member at 216 includes receiving geographic data from the audience member. In other embodiments, receiving a client login from a plurality of audience members, each client login comprising at least demographic data associated with each audience member at 216 includes receiving gender data from the audience member. In other embodiments, receiving a client login from a plurality of audience members, each client login comprising at least demographic data associated with each audience member at 216 includes receiving income data from the audience member. In other embodiments, receiving a client login from a plurality of audience members, each client login comprising at least demographic data associated with each audience member at 216 includes receiving ethnic origin data from the audience member. In other embodiments, receiving a client login from a plurality of audience members, each client login comprising at least demographic data associated with each audience member at 216 includes any type of demographic data from the audience member.
[0028] In some embodiments, aggregating at least the at least one response and the demographic data associated with the audience member sending the at least one response into aggregated data at 218 includes aggregating the demographic data for each response received, separating each demographic category. In some embodiments, when the resultant view of the aggregated data is displayed at 212 , the data may be pivoted, filtered, summarized, or otherwise analyzed by demographic category.
[0029] FIG. 4 is a flow diagram depicting alternative embodiments of a method for real-time and discrete analytics for web-mediated content and events. In some embodiments, operation 206 has optional embodiments including a step 2061 of emitting a first question is synchronized with a content-delivery, a step 2062 of emitting a first question is synchronized according to a particular content portion, and a step 2063 of emitting a first question is synchronized according to a length of time since the beginning of a particular content portion.
[0030] In some embodiments, a presenter who plans to present content may create one or more questions to be emitted during the presentation of the content. In some embodiments, such as emitting a first question is synchronized with a content-delivery at 2061 , the questions are synchronized in advance with the content so that they are emitted at certain points during the content. In other embodiments, such as emitting a first question is synchronized according to a particular content portion at 2062 , a question may be tagged to be emitted during a particular slide of a PowerPoint presentation, or when a video stream is switched from a studio location to an exterior location. In other embodiments, such as emitting a first question is synchronized according to a length of time since the beginning of a particular content portion at 2063 , a question may be tagged to be emitted at a particular time during the presentation, the particular time measured as the length of time since a portion of the presentation began. A duration could also be specified, such that the question is only available for a certain length of time. As can be seen in FIG. 5 , in some embodiments, such as emitting a first question is an on-demand event at 2064 , a question may be emitted when the presenter feels would be the best time to push a particular pre-determined question to the audience. As can be seen in FIG. 5 , in some embodiments, such as emitting a first question is an ad-hoc event at 2065 , a question may be emitted if a presenter wants to create a new question on-the-fly during the presentation in response to how the delivery is going.
[0031] In some embodiments, the emitting of the questions is managed by the presenter. In different embodiments, the emitting of the questions is managed by an assistant or other third-party, who may or may not be affiliated with the presenter.
[0032] FIG. 5 is a flow diagram depicting alternative embodiments of a method for real-time and discrete analytics for web-mediated content and events. In some embodiments, operation 206 has optional embodiments including a step 2064 of emitting a first question is an on-demand event, and a step 2065 of emitting a first question is an ad-hoc event. In some embodiments, operation 212 is followed by an optional step 220 of receiving at least on tweet, and an optional step of aggregating the at least one tweet with the at least a first view.
[0033] In some embodiments, the method further includes receiving at least one tweet at 220 . In addition to emitting questions which may be acted upon by audience members, those members who also have Twitter accounts may also choose to send feedback via Twitter. Such freeform text responses may be received by the servers and stored along with the responses to the questions. At operation 222 of aggregating the at least one tweet with the at least a first view, the incoming Twitter stream may be displayed on the presenter's private dashboard.
[0034] FIG. 6 is a flow diagram depicting alternative embodiments of a method for real-time and discrete analytics for web-mediated content and events. In some embodiments, operation 206 may have an optional step 224 of emitting a first question having a plurality of pre-selected responses. In some embodiments, operation 224 may have an optional step 226 of the plurality of pre-selected responses includes one or more of yes-or-no responses, likert responses, or ordinal responses.
[0035] FIG. 7 is a block diagram of a system for real-time and discrete analytics for web-mediated content and events, in accordance with an embodiment of the invention. In some embodiments, a system 300 for real-time and discrete analytics for web-mediated content and events may include an authentication component 302 , a storage component 304 , an emitter component 306 , an analytics component 308 , and a display 312 . In some embodiments, the system may have an optional project component 310 .
[0036] In some embodiments, the authentication component 302 may comprise the means for users of client devices to connect with the system 300 . The connections may in fact be unauthenticated, where a plurality of audience members make connections with the system to answer questions without providing their identities. Or, the connections may be authenticated, where audience members use a client device to create a new account (providing demographic data desired and/or required by the presenter or operator of the system 300 ), or log into an existing account.
[0037] In some embodiments, the storage component 304 may comprise various data stores for authentication information, presentation information, question information, response information, aggregated data sets, analytics, or other data stored in conjunction with the system 300 .
[0038] In some embodiments, the emitter component 306 may comprise a means for a presenter or other operator of the system 300 to emit a question which will be received by the client devices. The emitter component 306 may also receive and validate answers from the client devices, and provide the answers to the storage component.
[0039] In some embodiments, the analytics component 308 may provide a private dashboard which is displayed on the display 312 . In some embodiments, the analytics component provides a means for the presenter or other operator of the system 300 to analyze, sort, filter, correlate, pivot, or otherwise manipulate the answers, demographic data, Tweets, or other data maintained by the storage component. The presenter may use information from the analytics component to modify or create subsequent content and/or questions.
[0040] In some embodiments, the project component at 310 provides a means for users of the system 300 to create a project file including a presentation and a plurality of questions to be emitted at certain times during the presentation. The project component may include a separate authentication component which may be used to authenticate users of the project component, which may be distinct from the users of the client devices who view the presentations.
[0041] While preferred and alternative embodiments of the invention have been illustrated and described, as noted above, many changes can be made without departing from the spirit and scope of the invention. Accordingly, the scope of the invention is not limited by the disclosure of these preferred and alternate embodiments. Instead, the invention should be determined entirely by reference to the claims that follow. | During a presentation, a question is emitted over a network connection to a plurality of audience members, who utilize a computing device to respond. Client software for the audience members' heterogeneous computing devices may receive questions and upload answers. Answers from the audience are collected and aggregated, including optionally aggregating demographic information associated with each respondent and the answer of the respondent. Real-time analytics are provided to the presenter, which facilitates formulation or selection of further content and/or further questions. The timing of the questions can be synchronized with a content by linking the question to particular portions of the content, by tying the question to a particular slide or frame, by setting a length of time after which the question should be emitted, by offering a question on-demand, or some other method. A website maintains content, questions, user credentials of audience members, responses, and aggregated data, among other aspects. | 6 |
FIELD OF THE INVENTION
[0001] The present invention relates to the field of inkjet printing and in particular, inkjet printers with pagewidth printheads.
CO-PENDING APPLICATIONS
[0002] The following applications have been filed by the Applicant simultaneously with the present application:
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[0003] The disclosures of these co-pending applications are incorporated herein by reference. The above applications have been identified by their filing docket number, which will be substituted with the corresponding application number, once assigned.
CROSS REFERENCES
[0004] The following patents or patent applications filed by the applicant or assignee of the present invention are hereby incorporated by cross-reference.
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BACKGROUND OF THE INVENTION
[0005] The Applicant has developed a wide range of printers that employ pagewidth printheads instead of traditional reciprocating printhead designs. Pagewidth designs increase print speeds as the printhead does not traverse back and forth across the page to deposit a line of an image. The pagewidth printhead simply deposits the ink on the media as it moves past at high speeds. Such printheads have made it possible to perform full colour 1600 dpi printing at speeds in the vicinity of 60 pages per minute; speeds previously unattainable with conventional inkjet printers.
[0006] Printing at these speeds consumes ink quickly and this gives rise to problems with supplying the printhead with enough ink. Not only are the flow rates higher but distributing the ink along the entire length of a pagewidth printhead is more complex than feeding ink to a relatively small reciprocating printhead.
[0007] The high print speeds require a large ink supply flow rate. However, the ink flow needs to be filtered to protect the micron-scale nozzles from any ink borne contaminants. Ideally the filter pore size is relatively small to remove smaller, and therefore more particulate contaminants from the ink. Unfortunately, the smaller the filter pore size, the more it constricts the flow of ink. The area of the filter membrane can be increased so that the filter is not as much of a constriction to the flow. However, large filter membranes are generally counter to compact design.
SUMMARY OF THE INVENTION
[0008] Accordingly, the present invention provides a filter assembly for an inkjet printhead, the filter assembly comprising:
[0009] an inlet for connection to an ink supply;
[0010] an outlet for connection to an inkjet printhead;
[0011] a filter membrane for filtering ink flowing from the inlet to the outlet; and,
[0012] a chamber to house the filter membrane such that the filter membrane divides the chamber into an upstream portion for holding a quantity of the unfiltered ink, and a down stream portion for holding a quantity of the filtered ink; wherein,
[0013] the upstream portion tapers towards the outlet and the downstream portion tapers towards the inlet.
[0014] The invention recognizes that the flow rate of ink through the filter membrane is greatest at the points proximate the inlet and remote from the outlet. Therefore the high flow rate areas of the membrane need to be adjacent larger volumes of supply ink. Conversely, the areas of low flowrate do not need to be adjacent large volumes of supply ink. By tapering the upstream portion of the chamber towards the outlet, no-flow or low-flow zones are minimized. If the low-flow areas of the membrane are adjacent large volumes of ink, this is essentially a dead volume of nearly stagnant ink. Therefore, the invention maintains the filter area while reducing the chamber volume for more compact design.
[0015] Preferably, the chamber is elongate with the inlet adjacent one end of the chamber and the outlet adjacent the other end of the chamber such that the filter membrane extends diagonally across chamber. In another preferred form, the filter membrane extends in two intersecting planes within the housing. This configuration allows more membrane surface area within the same chamber volume. Preferably, the downstream portion of the chamber is between the two intersecting planes. In a further preferred form, the two intersecting planes meet at a line positioned centrally within the chamber adjacent one end. Preferably the outlet is positioned centrally within the chamber adjacent the other end. In particular embodiments, the membrane is mounted to a frame that defines the outlet to form a wedge-shaped cassette for insertion into the chamber wherein the membrane defines the sides tapering to the apex of the wedge. In a particularly preferred form, the outlet is at the base of the wedge shape.
[0016] In a particularly preferred form, the filter membrane is heat sealed to outer surfaces of the frame such that particulate contaminants generated by the heat sealing process remain on in the upstream or ‘dirty’ portion of the chamber.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Preferred embodiments of the invention will now be described by way of example only, with reference to the accompanying drawings, in which:
[0018] FIG. 1 is a schematic section view of a filter assembly according to the invention;
[0019] FIG. 2 is a schematic section view of a second embodiment of a stacked filter assembly according to the invention;
[0020] FIG. 3A shows the printhead cartridge of the present invention installed the print engine of a printer;
[0021] FIG. 3B shows the print engine without the printhead cartridge installed to expose the inlet and outlet ink couplings;
[0022] FIG. 4 is schematic representation of the print engine and printhead cartridge combination;
[0023] FIG. 5 is a perspective of the complete printhead cartridge according to the present invention;
[0024] FIG. 6 shows the printhead cartridge of FIG. 5 with the protective cover removed;
[0025] FIG. 8 is an exploded is a partial perspective of the printhead assembly within the printhead cartridge of FIG. 5 ;
[0026] FIG. 9 is partial exploded perspective of the inlet manifold and filter assembly;
[0027] FIG. 10 is an elevation of the filter assembly mounted to the inlet manifold with the sealing film removed to reveal the filter cassettes; and,
[0028] FIG. 11 is and exploded perspective of the inlet manifold.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0029] FIG. 1 is a sketch of a filter assembly 80 according to the invention is its basic form. The elongate chamber 86 houses an ink inlet 82 and an ink outlet 84 at either end. A filter membrane 88 extends diagonally across the chamber 86 to define an upstream portion 90 and a downstream portion 92 . The ink flow through the membrane is schematically depicted by the arrows 94 . The flow nearer the inlet 82 and remote from the outlet 84 is greatest, and conversely the flow remote from the inlet and near the outlet is less. Because of this, the upstream portion 90 of the chamber 86 is tapered towards the outlet 84 . The areas of the membrane 88 that have the highest flow are supplied by a greater volume of ink in the relatively thick section of the upstream portion 90 . The low flow areas of the membrane 88 are supplied with less ink from the thinner section of the upstream portion 90 . In this way, the overall volume of the chamber can be minimized for a membrane of a particular area by removing dead zones of relatively stagnant ink.
[0030] FIG. 2 is a sketch of another embodiment. Two filter assemblies 80 are shown stacked side by side. The skilled worker will understand that color printers supply the printhead with a number of differently colored inks. Hence the inlet manifold requires a filter for each color and stacking these in the most space efficient manner is necessary for compact design. In this embodiment, the filter membrane 88 for each filter assembly 80 forms a wedge shape extending centrally within the chamber 86 . The highest ink flow through the membrane occurs at the apex of the wedge. The apex is adjacent the greatest volume of upstream ink in the chamber. The lowest ink flow through the membrane occurs through the base of the wedge and this is adjacent the least volume of upstream ink. This embodiment may require the chamber to be extended to accommodate the inlet but the area of the filter membrane if effectively doubled.
[0031] The invention will now be described with reference to the Applicant's printhead cartridge and print engine shown in FIGS. 3A and 3B . A printhead cartridge recognizes that individual ink ejection nozzles may fail over time and eventually there are enough dead nozzles to cause artifacts in the printed image. Allowing the user to replace the printhead maintains the print quality without requiring the entire printer to be replaced. The print engine 3 is the mechanical heart of a printer which can have many different external casing shapes, ink tank locations and capacities, as well as different media feed and collection trays.
[0032] FIG. 3A shows a printhead cartridge 2 installed in a print engine 3 . The printhead cartridge 2 is inserted and removed by the user lifting and lowering the latch 126 . The print engine 3 forms an electrical connection with contacts on the printhead cartridge 2 and fluid couplings 120 are formed at the inlet and outlet manifolds, 48 and 50 respectively.
[0033] FIG. 3B shows the print engine 3 with the printhead cartridge removed to reveal the apertures 122 in the fluid couplings 120 . The apertures 122 engage spouts on the inlet and outlet manifolds ( 48 and 50 of FIG. 3A ). The fluid couplings 120 connect the inlet manifold to an ink tank, and the outlet manifold to a sump. These elements are described below with reference to FIG. 4 . As discussed above, the ink tanks, media feed and collection trays have an arbitrary position and configuration relative to the print engine 3 depending on the design of the printer's outer casing.
[0034] FIG. 4 is a schematic representation of the fluidics system in an inkjet printer suitable for the present invention. The printhead cartridge 2 is shown as a printhead assembly 2 supplied with ink from an ink tank 4 via an upstream ink line 8 and waste ink is drained to a sump 18 via a downstream ink line 16 . A single ink line is shown for simplicity. In reality, the printhead has multiple ink lines for full colour printing. The upstream ink line 8 has a shut off valve 10 immediately upstream of the inlet manifold 48 . The shut off valve 10 selectively isolates the printhead assembly 2 from the pump 12 and or the ink tank 4 . The pump 12 is used to actively prime or flood the printhead assembly 2 . The pump 12 is also used to establish a negative pressure in the ink tank 4 . During printing, the negative pressure is maintained by the bubble point regulator 6 .
[0035] The printhead assembly 2 has an LCP (liquid crystal polymer) molding 20 supporting a series of printhead ICs 30 secured with an adhesive die attach film (not shown). The printhead ICs 30 have an array of ink ejection nozzles for ejecting drops of ink onto the passing media substrate 22 . The nozzles are MEMS (micro electro-mechanical) structures printing at true 1600 dpi resolution (that is, a nozzle pitch of 1600 npi), or greater. The fabrication and structure of suitable printhead IC's 30 are described in detail in U.S. Ser. No. 11/246,687 (our docket no. MNN001US) the contents of which are incorporated by reference. The LCP molding 20 has a main channel 24 extending between the inlet 36 and the outlet 38 . The main channel 24 feeds a series of fine channels 28 extending to the underside of the LCP molding 20 . The fine channels 28 supply ink to the printhead ICs 30 through laser ablated holes in the die attach film.
[0036] Above the main channel 24 is a series of non-priming air cavities 26 . These cavities 26 are designed to trap a pocket of air during printhead priming. The air pockets give the system some compliance to absorb and damp pressure spikes or hydraulic shocks in the ink. The printers are high speed pagewidth printers with a large number of nozzles firing rapidly. This consumes ink at a fast rate and suddenly ending a print job, or even just the end of a page, means that a column of ink moving towards (and through) the printhead assembly 2 must be brought to rest almost instantaneously. Without the compliance provided by the air cavities 26 , the momentum of the ink would flood the nozzles in the printhead ICs 30 . Furthermore, the subsequent ‘reflected wave’ can generate a negative pressure strong enough to deprime the nozzles.
[0037] The outlet manifold 50 has a fluidic damper that resonates at a frequency selected to attenuate potentially problematic standing waves at any of the resonant frequencies of the main channel 24 . The operation of the fluidic damper is explained in detail in the Applicant's co-pending US patent application, our docket no. RRE013US, the contents of which are incorporated herein by reference.
[0038] FIG. 5 shows the printhead cartridge 2 in isolation prior to insertion in the print engine 3 (see FIG. 3B ). The printhead cartridge 2 has a top molding 44 and a removable protective cover 42 . The top molding 44 has a central web for structural stiffness and to provide textured grip surfaces 58 for manipulating the cartridge during insertion and removal. The base portion of the protective cover 42 protects the printhead ICs (not shown) and line of contacts (not shown) prior to installation in the printer. Caps 56 are integrally formed with the base portion and cover the ink inlets and outlets (see 54 and 52 of FIG. 7 ).
[0039] FIG. 6 shows the printhead assembly 2 with its protective cover 42 removed to expose the printhead ICs on the bottom surface and the line of contacts 33 on the side surface. The protective cover is discarded to the recycling waste or fitted to the printhead cartridge being replaced to contain leakage from residual ink. FIG. 7 is a partially exploded perspective of the printhead assembly 2 . The top cover 44 has been removed reveal the inlet manifold 48 and the outlet manifold 50 . The inlet and outlet shrouds 46 and 47 have been removed to better expose the five inlet and outlet conduits, 52 and 54 respectively. The inlet and outlet manifolds 48 and 50 form a fluid connection between each of the individual inlets and outlets and the corresponding main channel in the LCP molding 20 . As discussed above, the main channels extend beneath the line of non-priming air cavities 26 .
[0040] FIG. 8 is an exploded perspective of the printhead assembly without the inlet or outlet manifolds or the top cover molding. The main channels 24 for each ink color and their associated air cavities 26 are formed in the channel molding 68 and the cavity molding 72 . Adhered to the bottom of the channel molding 68 is a die attach film 66 . As discussed above in relation to FIG. 4 , the die attach film 66 mounts the printhead ICs 30 to the channel molding such that the fine channels on the underside of the are in fluid communication with the printhead ICs 30 via small laser ablated holes through the film.
[0041] Flex PCB 70 is adhered to the side of the air cavity molding 72 and wraps around to the underside of the channel molding 68 . The printer controller on the print engine connects to the line of contacts 33 . At the other side of the flex PCB 70 is a line of wire bonds 64 to electrically connect the conductors in the flex 70 to each of the printhead ICs 31 . The wire bonds 64 are covered in encapsulant 62 which is profiled to have a predominantly flat outer surface. On the other side of the air cavity molding 72 is a paper guide 74 to direct sheets of media substrate past the printhead ICs at a predetermined spacing.
[0042] FIGS. 9 , 10 and 11 show the inlet manifold 48 in detail. The manifold has an interface plate 76 with the five spouts 52 for connection to the ink tank 4 (see FIG. 4 ). Behind the interface plate 76 is a filter stack 90 . The spouts 52 feed directly into the filter inlets 82 . The inlets 82 flood their corresponding chambers 86 with ink. A filter cassette 98 is inserted into each of the chambers 86 . The cassettes are wedge-shaped with a filter membrane 88 on both of the opposing wedge surfaces. The filter outlets 84 are positioned at the base of the wedge. The filter membranes 88 are ultra sonically welded to the outside of the cassette frame to keep any particles caused by the welding process are kept on the upstream or dirty side of the filter. The portion of the chamber 86 surrounding the cassette 98 is the upstream portion 90 and the interior of the cassette 98 is the downstream portion 92 .
[0043] As seen in FIG. 11 , the cassettes 98 are sealed into their respective chambers 86 , and the chambers are sealed from each other with a polymer film 100 . The film is heat sealed to the perimeter of every chamber 86 to withstand an internal pressure of 100 kPa. The five outlets 84 feed into conduits 104 formed into the side of the inlet manifold 48 . The conduits 104 are also heat sealed with a polymer film 102 to an internal pressure of 100 kPa. During operation, the filtered ink flows down the conduits 104 to the coupling 60 . The coupling 60 forms a sealed connection to the LCP molding 20 to supply each of the main channels 24 (see FIG. 8 ).
[0044] The stack of wedge-shaped filter cassettes 98 in the inlet manifold 48 give a large filter membrane area within a small volume. This helps to keep the printhead cartridge compact and prolongs the operational life of the nozzles.
[0045] The above embodiments are purely illustrative and not restrictive or limiting on the scope of the invention. The skilled worker will readily recognize many variations and modifications which do not depart from the spirit and scope of the broad inventive concept. | A filter assembly for an inkjet printhead, that has an inlet for connection to an ink supply, an outlet for connection to an inkjet printhead, a filter membrane for filtering ink flowing from the inlet to the outlet, and a chamber to house the filter membrane. The filter membrane divides the chamber into an upstream portion for holding a quantity of the unfiltered ink, and a downstream portion for holding a quantity of the filtered ink. The upstream portion tapers towards the outlet and the downstream portion tapers towards the inlet. | 1 |
FIELD OF THE INVENTION
The present invention relates to an electronic cash register and more particularly to an electronic cash register which is adaptable to varying output formats according to different models of output devices (printer, display, etc.) connected thereto.
BACKGROUND OF THE INVENTION
The electronic cash register (hereinafter referred to briefly as ECR) is generally connected to a printer and a display as standard output devices which respectively print out and display output data.
Meanwhile, for a change in specification or an improvement in function of an ECR, it is sometimes practiced to replace the existing printer and display devices with other models of such devices or connect other additional devices. In such cases, on the part of the ECR, it is common practice to additionally mount a software enabling the ECR to adapt itself to the output format of the newly connected output device and execute the output processing operation according to the new software. When it is impossible to mount such a new software for reasons of the limited memory capacity of the ECR, the existing software is dismounted and the new software Is mounted instead.
However, the practice of replacing the existing software with a new one for adapting the ECR to the new output device has the drawback that much time and cost are incurred for the preparation of the new software. This problem is particularly serious when the change of output devices is frequent or when the same change is made for a plurality of ECRs and this means an inevitable increase in the price of the ECR (inclusive of the software). Thus, the above practice is not an effective approach to the problem.
It is, therefore, an object of the present invention to provide an electronic cash register capable of adapting itself to changes in output format due to change of associated output devices (printer and display devices) without requiring change of the software.
Other objects and advantages of the invention will become apparent from the following description and accompanying drawings.
SUMMARY OF THE INVENTION
The ECR according to the present invention is an electronic cash register which can adjust itself to change of associated output devices and, more particularly, is an electronic cash register comprising a memory means for storing information relating to output formats corresponding to different models of output devices, a model designating means which specifies the model of associated output device, a search-reader means for searching said memory means and reading out information on the corresponding output format, and an output data editing means responsive to a demand for output and adapted to edit data for output according to said output format information read by said search-reader means and a predetermined editing rule.
The electronic cash register of the invention, which has the above general architecture, does not require change of the mounted software but permits editing of data with flexibility by adapting itself to a change in output format due to change in the model of associated output device (printer or display).
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic processing flow diagram showing the output operation of an ECR embodying the principle of the invention;
FIG. 2 is a schematic diagram illustrating output devices that can be connected to an ECR embodying the invention;
FIG. 3 is a schematic diagram showing the internal configuration of the ECR shown in FIG. 2;
FIG. 4 is a schematic diagram illustrating the hardware and software interfaces of the ECR shown in FIG. 2;
FIG. 5 is a schematic diagram showing the storage area for storage of printing digit data dependent on printer models in the ROM of the ECR shown in FIG. 3;
FIG. 6(a) through (f) are schematic diagrams showing the printing rule embodying the principle of the invention;
FIG. 7 is a schematic diagram explaining the display rule embodying the principle of the invention; and
FIG. 8 is a schematic diagram showing the configuration of designated print/display data embodying the principle of the invention;
FIG. 9(a) through (d) are schematic diagrams showing the prints obtained by editing the designated print/display data of FIG. 8 according to the printing rule shown in FIG. 6(a) through (f).
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
One preferred embodiment of the present invention is described in detail below with reference to the accompanying drawings.
In the following description of the ECR, it is assumed that a printer and a display unit are connected thereto as output devices.
It is further assumed that the ECR is connected to one unit each of such printer and display but it is possible to connect the ECR to a plurality of output devices of each kind.
FIG. 1 is a generalized processing flow diagram showing an ECR 100 outputting data through the associated output devices in one embodiment of the invention.
FIG. 2 is a schematic view explaining the output devices which can be connected to the ECR 100 in one embodiment of the invention.
FIG. 3 is a schematic diagram showing the internal functional configuration of the ECR 100 shown in FIG. 2.
As shown in FIG. 2, the ECR 100 accepts any one or more of printers 200a through 200d which are dissimilar in the number of printing digits per line and any one or more of displays 300a through 300g which are dissimilar in the number of display digits per line.
For example, the number of printing digits of the printer 200a is 20, that of the printer 200b is 25, that of the printer 200c is 30, and that of the printer 200d is 35. The displays 300a through 300c are customer displays, the displays 300d through 300f are operator displays, and the display 300g is a cathode-ray tube (CRT) display.
The displays 300a through 300f are connected to the ECR 100 through a display board 400.
As shown in FIG. 2, the output data from the ECR 100 are fed to printers 200a through 200d for printing and to displays 300a through 300g for display.
The internal functional configuration of the ECR 100 shown in FIG. 2 is now explained with reference to FIG. 3.
Referring to FIG. 3, the ECR 100 includes a central processing unit (CPU) 110 which controls and monitors the operation of the ECR 100, a read-only memory (ROM) 120 and a random access memory (RAM) 130 for storing data (inclusive of programs) necessary for the operation of the ECR 100, a printing buffer 140, a display buffer 150 and a printing section 160 and a display section 170.
The printing section 160 includes one or more of the printers 200a through 200d which are shown in FIG. 2 and the display section 170 similarly includes one or More of the displays 300a through 300g shown in FIG. 2. The data to be fed to these output devices are temporarily stored in the printing buffer 140 and display buffer 150, respectively, for respective outputs in the forms of hard copy and visual display through said printing section 160 and display section 170.
In the functional configuration of the ECR100 presented in FIG. 2, the data input function is not shown, nor is described herein.
The interfaces for the hardware and software to be mounted on the ECR 100 are described below.
FIG. 4 is a schematic diagram showing the hardware and software interfaces of the ECR 100.
As illustrated, the hardware and software of the ECR 100 form a laminar interface, with a hardware layer 500 forming a substratum and a software layer 600 being superimposed thereon.
The hardware layer 500 comprises the complete hardware function 500a encompassing the peripheral devices of the ECR 100.
The software layer 600 comprises a software layer for control over the operation of said hardware function 500a (hereinafter referred to as the control software layer), an application software layer 600c which includes an application software prepared by the user, and a software layer 600b providing a variety of utility processing and other services necessary for said application software layer 600c (hereinafter referred to as the basic software layer).
The processing flow shown in FIG. 1 is included as a program in said basic software layer 600b, and the programs contained in said control software layer 600a and basic software layer 600b are written, as resident programs, into the ROM 120.
Thus, the application program prepared by the user is subject to the control software layer 600a and basic software layer 600b, so that various output devices of the ECR100 can be utilized via the hardware function 500a.
FIG. 5 is a schematic diagram showing the configuration of a storage area 120a for storing printer model-dependent printing digit data in the ROM 120 illustrated in FIG. 3.
As shown, this storage area 120a constituting a part of the ROM 120 is previously supplied with the numbers of printing digits which are dependent solely on printer models which can be connected to the ECR100.
More particularly, the numbers of printing digits corresponding to the respective printers 200a through 200d shown in FIG. 2, namely 20, 23, 30 and 35, are stored in the order mentioned.
Similarly for the displays 300a through 300g which can be connected to the ECR 100, the numbers of display digits corresponding to the respective displays are previously stored, although these are neither illustrated nor described in further detail.
The ECR 100 is previously provided with a printing rule and a display rule, both of which are designed for universal application regardless of models of output devices. Thus, the ECR 100 upon specification of a given model of output device edits and outputs data in an output format corresponding to the specified model in accordance with said printing or display rule.
The printing rule and display rule mentioned above are described in detail below.
FIG. 6(a) through (f) are schematic views explaining the printing rule employed in one preferred embodiment of the invention.
Here it is assumed that the number of printing digits per line is W digits and that each line consists of a right part R and a left part L.
As shown in FIG. 6(a), generally when the number of characters L1 available in the left part L and the number of characters R1 available in the right part R satisfy the relation (W>L1+R1), printing in the left part L is left-justified and that in the right part R is right-justified.
On the other hand, if the relation (W≦L1+R1) holds true, printing is done in two lines with the left part L being left-justified and the right part R arranged below said L and right-justified as shown in FIG. 6 (b).
The above is a general printing rule. The printing rule applicable to the left part L is now described.
Referring to FIG. 6(c) showing the printing rule applicable to the left part L, this left part L is further divided into [L.1], [L.2], . . . , [L.n]. The number of characters in the part [L.i] is assumed to be Li (hereinafter, i=1, 2, 3, . . . , n). Now, if the relation L 1 +L 2 +. . . L n ≦W holds true, printing is carried out in one line with the left part L being left-justified.
On the other hand, if the relation is L 1 +L 2 +. . . +L n >W, printing is done in two lines with the left part L being left-justified, as shown in FIG. 6(d).
The printing rule applicable to the right part R is now explained.
Referring to FIG. 6(e) which shows the printing rule applicable to the right part R, the right part R is subdivided into [R.1], [R.2], . . . , [R.n] and the number of characters per [R.n] is assumed to be Rn. Then, if the relation R 1 +R 2 . . . +R n ≦W holds true, printing is performed in one line with the right part R being right-justified.
On the other hand, if R 1 +R 2 +. . . +R n >W, printing is done in two lines with the right part R being right-justified as shown in FIG. 6(f).
The above is an explanation of the printing rule applicable to printers 200a through 200d which can be connected to the ECR100. The display rule applicable to displays 300a through 300g is now described.
FIG. 7 is a schematic diagram illustrating the display rule employed in one embodiment of the invention.
Let it be assumed that the number of display digits per line is w and the display per line consists of a left part l and a right part r. Referring to FIG. 7, if there holds the relation (w≧l1+r1+1) where l1 is the number of display characters in the left part l and r1 is that in the right part r, both parts of data are displayed concurrently in one line with the left part l being left-justified and the right part r right-justified.
On the other hand, if the relation (w<l1+r1+1) holds true, it is impossible to display the left part l and right part r concurrently in a single line. Therefore, the left part l is first displayed and, then, the display of the right part r begins to take place. However, if either the left part l or the right part r is to be displayed beyond the right-hand frame of the display, the continued display takes place from the left-hand end. That is to say, the right part r is displayed over the left part l, for instance.
Thus, the ECR 100 is provided with the above printing and display rules. Now, how the data according to the user's application program (hereinafter referred to as designated print/display-data PD) is printed according to said printing rule is explained below. The mode of display according to said display rule is not described.
FIG. 8 is a schematic diagram showing the configuration of designated print/display data PD in one embodiment of the invention.
As shown, the designated print/display data PD has a predetermined data length PDl and all the data are registered as left-justified.
The designated print/display data PD shown in a data set including variable length records R1 through R5 and said respective records R1 through R5 contain three data items.
With regard to the first data items of said three items, the output data D3 to be registered in this record (which is described later) is registered in the left part, or the output part designating code data D1 which specifies the data to be displayed and printed is registered in the right part. In the second data item, an output data length D2 indicating the length (number of bytes) of output data D3 to be recorded in the record is registered. In the third data item, the output data D3 to be recorded in the record is registered.
Therefore, the output data D3 of the first record R1 in the designated print/display data PD shown in FIG. 8, for instance, is as long as 9 bytes and the data to be printed or displayed is in the left part L.
While the designated print/display data PD shown in FIG. 8 contains records R1 through R5, the number of records that can be registered is not limited unless the data length PDl is exceeded.
FIG. 9(a) through (d) are schematic diagrams showing the prints obtained by editing the designated print/display data PD of FIG. 8 in accordance with the printing rule shown in FIGS. 6(a) through (f).
FIG. 9(a) is a schematic diagram of the print obtained by editing the designated print/display data PD according to the printing rule with the printer 200a with a number of printing digits per line of W=20 digits.
FIG. 9(b) is a schematic diagram showing the print obtained by editing the designated print/display data PD according to the printing rule with the printer 200b having a number of printing digits per line of W=25.
FIG. 9(c) is a schematic diagram showing the print obtained by editing the designated print/display data PD according to the printing rule with the printer 200c having a number of printing digits per line of W=30.
FIG. 9(d) is a schematic diagram showing the print obtained by editing the designated print/display data PD according to the printing rule with the printer 200d having a number of printing digits per line of W=35.
As illustrated in FIG. 9(a) through (d), it is clear that even if the number of printing digits is varied, that is to say irrespective of printer model, the use of said printing rule permits the editing and printing of the same designated print/display data PD in a format corresponding to the particular number of printing digits W, that is to say the particular printer model.
The details of the printing and display operations of the ECR100 are now described with reference to FIGS. 1 thorough 9.
The ECR 100 is assumed to be connected to one of said printers 200a through 200d and to one of said displays 300a through 300d.
Stored in the storage area 120a of the ROM120 are printing digit data W corresponding to printers 200a through 200d which can be connected (FIG. 5). Similarly display digit date w corresponding to connectable displays 300a through 300g are stored in another storage area of the ROM 120 (pig. 5).
While the ECR 100 gives outputs (print and display) during the routine transaction, this action is initiated as the designated print/display data PD is generated from the user's application program and a demand for output is made.
As the ECR 100 is initialized by switching its power supply on, the CPU 110 enquires about the models of the printer and display connected at step S100 as shown in FIG. 1. The model of the output device is ascertained from the state of a signal input from the terminal for connection of the printer or the terminal for connection of the display.
In response to this specification of printer and display models connected, the CPU110 proceeds to the next step S200.
At S200, using the device model code specified at S 100 as the key, the corresponding storage area is searched to read the printing digit data W and display digit data w corresponding to the respective device models. Thus, the storage area 120a of the ROM120 shown in FIG. 5 is searched using the specified device model code as the key in the normal order to read out the corresponding printing digits data W. Similarly, the display digit data w is read out.
In this manner, as the ECR 100 is initialized (this occurs whenever a peripheral device is exchanged), the models of the printer and display connected are specified and the printing digit data w and display digit data w are determined. The printing digit data W and display digit data w are temporarily stored in predetermined storage areas of the RAM130 until the next initialization.
At the next step S300, the CPU 110 enquires whether it is receiving a printing or display output demand signal according to the user's application program.
As the output demand signal is received at S300, the sequence proceeds to the next step S400. However, until reception of said demand signal, the CPU110 repeats the enquiry at S300.
As the sequence proceeds to S400, the printing and display processings are carried out. More particularly, the output demand signal is followed by said designated print/display data PD from the user's application program and therefore, the CPU110 edits the designated print/display data PD in accordance with the aforesaid printing rule and printing digit data W. The printing data thus edited is temporarily stored in a printing buffer 140 and fed to a printer connected to a printing section 160. In parallel with the above operation, display data edited according to the display digit data w and said display rule is similarly stored temporarily in a display buffer 150 and fed to a display connected to a display section 170.
Then, the sequence returns to S300 and the output processing in response to the output demand signal from the application program is carried out in the same manner as above.
The processing routine illustrated in FIG. 1 unconditionally ends upon completion of all the transactions of the ECR100 or upon termination of power supply from the power source.
Thus, even if a change is made in the model of the printer or display connected to the ECR 100, the model is specified and the display digit information w and printing digit information W are specified. Then, the designated print/display data PD are edited in accordance with the printing rule and display rule registered in the basic software layer 600b.
Therefore, even if the printer or display is exchanged, it is no longer necessary to modify or make an addition to the existing software. Thus, as shown in FIG. 4, the upper application software layer 600c need not care about the output devices to be connected to the ECR 100 and the application program functions as a universal program for output devices. In addition to the above-mentioned advantage that the software need not be modified, the invention offers the advantage of savings in the time and cost of software maintenance that might be required due to change of output devices.
The above description and the accompanying drawings are merely illustrative of a few modes of application of the principles of the present invention and are not limiting. Numerous other arrangements which embody the principles of the invention and which fall within its spirit and scope may be readily devised by those skilled in the art. Accordingly, the invention is not limited by the foregoing description, but is only limited by the scope of the appended claims. | An electronic cash register (ECR) which may be connected to different output devices having different output formats such as different characters per line comprises: a memory for storing information on respective output formats corresponding to the possible output device(s) connected to the ECR, a search-reader for searching through the memory for specified output device(s) and for reading information on an output format for the specified output device(s), and an output data editor for editing output data according to the information read by the search-reader in response to: (a) an output demand for the ECR and (b) a predetermined editing rule which uses the read information. | 6 |
[0001] The instant invention relates to aqueous sizing compositions comprising derivatives of diaminostilbene optical brightener, shading dyes, binders and optionally divalent metal salts which can be used for the optical brightening of substrates, including substrates suitable for high quality ink jet printing.
BACKGROUND OF THE INVENTION
[0002] High levels of whiteness and brightness are important parameters for the end-user of paper products. The most important raw materials of the papermaking industry are cellulose, pulp and lignin which naturally absorb blue light and therefore are yellowish in color and impart a dull appearance to the paper.
[0003] The distinction between whiteness and brightness is well-known to those skilled in the art and is discussed, for example, in WO 0 218 705 A1.
[0004] Optical brighteners are used in the papermaking industry to compensate for the absorption of blue light by absorbing UV-light with a maximum wavelength of 350-360 nm and converting it into visible blue light with a maximum wavelength of 440 nm.
[0005] It is well established that, in addition to optical brighteners, certain shading dyes or pigments can be added to the paper in order to achieve a higher level of whiteness and to control the shade of the white paper.
[0006] WO 0 218 705 A1 however teaches that the use of shading dyes or pigments, while having a positive effect on whiteness, has a negative effect on brightness. The solution to this problem is to add additional optical brightener, the advantage claimed in WO 0 218 705 A1 being characterized by the use of a mixture comprising at least one direct dye (exemplified by CI Direct Violet 35) or pigment and at least one optical brightener.
[0007] Surprisingly, we have now discovered a sizing composition comprising an optical brightener and a shading dye which enables the papermaker to reach a high level of whiteness without significant loss in brightness.
[0008] Therefore, the goal of the present invention is to provide aqueous sizing compositions containing derivatives of diaminostilbene optical brightener, shading dyes, binders and optionally divalent metal salts affording enhanced high whiteness levels while avoiding the loss of brightness characterized by the use of shading dyes or pigments when applied to the paper at the size press.
[0009] The present invention further provides a process for optical brightening and tinting paper substrates characterized in that an aqueous sizing composition containing at least one optical brightener, at least one shading dye, at least one binder and optionally at least one divalent metal salt is used.
DESCRIPTION OF THE INVENTION
[0010] The present invention therefore provides aqueous sizing compositions for optical brightening of substrates, preferably paper, comprising
[0000] (a) at least one optical brightener of formula (I)
[0000]
[0000] in which
the anionic charge on the brightener is balanced by a cationic charge composed of one or more identical or different cations selected from the group consisting of hydrogen, an alkali metal cation, alkaline earth metal, ammonium, ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched alkyl radical, ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched hydroxyalkyl radical, or mixtures of said compounds,
R 1 and R 1 ′ may be the same or different, and each is hydrogen, C 1 -C 4 linear or branched alkyl, C 2 -C 4 linear or branched hydroxyalkyl, CH 2 CO 2 − , CH 2 CH 2 CONH 2 or CH 2 CH 2 CN,
R 2 and R 2 ′ may be the same or different, and each is C 1 -C 4 linear or branched alkyl, C 2 -C 4 linear or branched hydroxyalkyl, CH 2 CO 2 − , CH(CO 2 − )CH 2 CO 2 − , CH(CO 2 − )CH 2 CH 2 CO 2 − , CH 2 CH 2 SO 3 − , CH 2 CH 2 CO 2 − , CH 2 CH(CH 3 )CO 2 − , benzyl, or
R 1 and R 2 and/or R 1 ′ and R 2 ′, together with the neighboring nitrogen atom signify a morpholine ring and
p is 0, 1 or 2,
(b) at least one dye of formula (II)
[0000]
[0000] in which
R 3 signifies H, methyl or ethyl, R 4 signifies paramethoxyphenyl, methyl or ethyl, M signifies a cation selected from the group consisting of hydrogen, an alkali metal cation, alkaline earth metal, ammonium, ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched alkyl radical, ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched hydroxyalkyl radical, or mixtures of said compounds,
(c) at least one binder,
(d) optionally one or more divalent metal salts and
(e) water.
[0014] In compounds of formula (I) for which p is 1, the SO 3 − group is preferably in the 4-position of the phenyl group.
[0015] In compounds of formula (I) for which p is 2, the SO 3 − groups are preferably in the 2,5-positions of the phenyl group.
[0016] Preferred compounds of formula (I) are those in which
[0000] the anionic charge on the brightener is balanced by a cationic charge composed of one or more identical or different cations selected from the group consisting of hydrogen, an alkali metal cation, alkaline earth metal, ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched hydroxyalkyl radical, or mixtures of said compounds,
R 1 and R 1 ′ may be the same or different, and each is hydrogen, C 1 -C 4 linear or branched alkyl, C 2 -C 4 linear or branched hydroxyalkyl, CH 2 CO 2 − , CH 2 CH 2 CONH 2 or CH 2 CH 2 CN,
R 2 and R 2 ′ may be the same or different, and each is C 1 -C 4 linear or branched alkyl, C 2 -C 4 linear or branched hydroxyalkyl, CH 2 CO 2 − , CH(CO 2 − )CH 2 CO 2 − or CH 2 CH 2 SO 3 − and
p is 0, 1 or 2.
[0017] More preferred compounds of formula (I) are those in which
[0000] the anionic charge on the brightener is balanced by a cationic charge composed of one or more identical or different cations selected from the group consisting of Li + , Na + , K + , Ca 2+ , Mg 2+ , ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched hydroxyalkyl radical, or mixtures of said compounds,
R 1 and R 1 ′ may be the same or different, and each is hydrogen, methyl, ethyl, propyl, α-methylpropyl, β-methylpropyl, β-hydroxyethyl, β-hydroxypropyl, CH 2 CO 2 − , CH 2 CH 2 CONH 2 or CH 2 CH 2 CN,
R 2 and R 2 ′ may be the same or different, and each is methyl, ethyl, propyl, α-methylpropyl, β-methylpropyl, β-hydroxyethyl, β-hydroxypropyl, CH 2 CO 2 − , CH(CO 2 − )CH 2 CO 2 − or CH 2 CH 2 SO 3 − and
p is 0, 1 or 2.
[0018] Especially preferred compounds of formula (I) are those in which
[0000] the anionic charge on the brightener is balanced by a cationic charge composed of one or more identical or different cations selected from the group consisting of
Na + , K + and triethanolammonium or mixtures of said compounds,
R 1 and R 1 ′ may be the same or different, and each is hydrogen, ethyl, propyl, β-hydroxyethyl, β-hydroxypropyl, CH 2 CO 2 − , or CH 2 CH 2 CN,
R 2 and R 2 ′ may be the same or different, and each is ethyl, propyl, β-hydroxyethyl, β-hydroxypropyl, CH 2 CO 2 − , CH(CO 2 − )CH 2 CO 2 − or CH 2 CH 2 SO 3 − and
p is 1 or 2.
[0019] The concentration of compounds of formula (I) in the sizing composition may be between 0.2 and 30 g/l, preferably between 1 and 25 g/l, most preferably between 2 and 20 g/l.
[0020] Preferred compounds of formula (II) are those in which
R 3 signifies H, methyl or ethyl, R 4 signifies paramethoxyphenyl, methyl or ethyl, M signifies a cation selected from the group consisting of hydrogen, an alkali metal cation, alkaline earth metal, ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched hydroxyalkyl radical, or mixtures of said compounds.
[0024] More preferred compounds of formula (II) are those in which
R 3 signifies methyl or ethyl, R 4 signifies methyl or ethyl, M signifies a cation selected from the group consisting of Li + , Na + , K + , ½ Ca 2+ , ½ Mg 2+ , ammonium which is mono-, di-, tri- or tetrasubstituted by a C 1 -C 4 linear or branched hydroxyalkyl radical, or mixtures of said compounds.
[0028] Especially preferred compounds of formula (II) are those in which
R 3 signifies methyl, R 4 signifies methyl, M signifies a cation selected from the group consisting of Na + , K + and triethanolammonium or mixtures of said compounds.
[0032] The concentration of compounds of formula (II) in the sizing composition may be between 0.01 and 20 mg/l, preferably between 0.05 and 10 mg/l, most preferably between 0.1 and 5 mg/l.
[0033] The binder is typically an enzymatically or chemically modified starch, e.g. oxidized starch, hydroxyethylated starch or acetylated starch. The starch may also be native starch, anionic starch, a cationic starch, or an amphoteric starch depending on the particular embodiment being practiced. While the starch source may be any, examples of starch sources include corn, wheat, potato, rice, tapioca, and sago. One or more secondary binders e.g. polyvinyl alcohol may also be used.
[0034] The concentration of binders in the sizing composition may be between 1 and 30% by weight, preferably between 2 and 20% by weight, most preferably between 5 and 15% by weight, % by weight based on the total weight of the sizing composition.
[0035] Preferred divalent metal salts are selected from the group consisting of calcium chloride, magnesium chloride, calcium bromide, magnesium bromide, calcium iodide, magnesium iodide, calcium nitrate, magnesium nitrate, calcium formate, magnesium formate, calcium acetate, magnesium acetate, calcium citrate, magnesium citrate, calcium gluconate, magnesium gluconate, calcium ascorbate, magnesium ascorbate, calcium sulphite, magnesium sulphite, calcium bisulphite, magnesium bisulphite, calcium dithionite, magnesium dithionite, calcium sulphate, magnesium sulphate, calcium thiosulphate, magnesium thiosulphate or mixtures of said compounds.
[0036] More preferred divalent metal salts are selected from the group consisting of calcium chloride, magnesium chloride, calcium bromide, magnesium bromide, calcium sulphate, magnesium sulphate, calcium thiosulphate or magnesium thiosulphate or mixtures of said compounds.
[0037] Especially preferred divalent metal salts are selected from the group consisting of calcium chloride, magnesium chloride, calcium sulphate or magnesium sulphate or mixtures of said compounds.
[0038] When the sizing composition contains divalent metal salts, the concentration of divalent metal salts in the sizing composition may be between 0.1 and 100 g/l, preferably between 0.5 and 75 g/l, most preferably between 1 and 50 WI.
[0039] When the divalent metal salt is a mixture of one or more calcium salts and one or more magnesium salts, the amount of calcium salts may be in the range of 0.1 to 99.9% by weight, % by weight based on the total weight of divalent metal salts.
[0040] The pH value of the sizing composition is typically in the range of from 5 to 13, preferably of from 6 to 11. Where it is necessary to adjust the pH of the sizing composition, acids or bases may be employed. Examples of acids which may be employed include but are not restricted to hydrochloric acid, sulphuric acid, formic acid and acetic acid. Examples of bases which may be employed include but are not restricted to alkali metal and alkaline earth metal hydroxide or carbonates.
[0041] In addition to one or more compounds of formula (I), one or more compounds of formula (II), one or more binders, optionally one or more divalent metal salts and water, the sizing composition may contain by-products formed during the preparation of compounds of formula (I) and compounds of formula (II) as well as other conventional paper additives. Examples of such additives are carriers, defoamers, wax emulsions, dyes, inorganic salts, solubilizing aids, preservatives, complexing agents, biocides, surface sizing agents, cross-linkers, pigments, special resins etc.
[0042] Optionally, the sizing composition can contain polyethyleneglycol. When the sizing composition contains polyethyleneglycol, the ratio in parts of polyethyleneglycol per part of compounds of formula (I) may be of from 0.05/1 to 2/1, preferably of from 0.1/1 and 1.5/1, more preferably of from 0.15/1 to 1/1 to function as a so-called carrier in order to boost the performances of compounds of formula (I) or compounds of formula (II). The polyethylene glycol which may be employed as carrier may have an average molecular weight in the range of 100 to 8000, preferably in the range of 200 to 6000, most preferably in the range of 300 to 4500.
[0043] Optionally, the sizing composition can contain polyvinyl alcohol. When the sizing composition contains polyvinyl alcohol, the ratio in parts of polyvinyl alcohol per part of compounds of formula (I) may be of from 0.005/1 to 1/1, preferably of from 0.025/1 to 0.5/1, more preferably of from 0.05/1 to 0.3/1 to function as a so-called carrier in order to boost the performances of compounds of formula (I) or compounds of formula (II). The polyvinyl alcohol which may be employed as carrier has a degree of hydrolysis greater than or equal to 60% and a Brookfield viscosity of between 1 and 60 mPa·s for a 4% aqueous solution at 20° C. Preferably the degree of hydrolysis is between 70% and 95%, and the Brookfield viscosity is between 1 and 50 mPa·s (4% aqueous solution at 20° C.). Most preferably, the degree of hydrolysis is between 70% and 90%, and the Brookfield viscosity is between 1 and 40 mPa·s (4% aqueous solution at 20° C.).
[0044] The sizing composition may be prepared by adding one or more compounds of formula (I), one or more compounds of formula (II), optionally one or more divalent metal salts and water to a preformed aqueous solution of the binder at a temperature between 20° C. and 90° C.
[0045] Compounds of formula (I), compounds of formula (II), and optionally the divalent metal salts can be added in any order, or at the same time to the preformed aqueous solution containing the binder at a temperature between 20° C. and 90° C.
[0046] Compounds of formula (I), compounds of formula (II), and optionally the divalent metal salts can be added as powders or as preformed aqueous solutions to the preformed aqueous solution containing the binder at a temperature between 20° C. and 90° C.
[0047] When used as a preformed aqueous solution, the concentration of compound of formula (I) in water is preferably of from 1 to 50% by weight, more preferably of from 2 to 40% by weight, even more preferably from 10 to 30% by weight, the % by weight being based on the total weight of the preformed aqueous solution containing the compound of formula (I).
[0048] When used as a preformed aqueous solution, the concentration of compound of formula (II) in water is preferably of from 0.1 to 25% by weight, more preferably of from 0.5 to 20% by weight, even more preferably from 1 to 10% by weight, the % by weight being based on the total weight of the preformed aqueous solution containing the compound of formula (II).
[0049] When used as a preformed aqueous solution, the concentration of divalent metal salt in water is preferably of from 1 to 80% by weight, more preferably of from 2 to 70% by weight, even more preferably from 3 to 60% by weight, the % by weight being based on the total weight of the preformed aqueous solution containing the divalent metal salt.
[0050] A further subject of the invention therefore is the use of the sizing compositions as defined above, also in all their preferred embodiments, preferably for optical brightening of cellulosic substrates, e.g. textiles, non-wovens or more preferably paper.
[0051] The sizing composition may be applied to the surface of a paper substrate by any surface treatment method known in the art. Examples of application methods include size-press applications, calendar size application, tub sizing, coating applications and spraying applications. (See, for example, pages 283-286 in Handbook for Pulp & Paper Technologists by G. A. Smook, 2 nd Edition Angus Wilde Publications, 1992 and US 2007/0277950). The preferred method of application is at the size-press such as puddle size press. A preformed sheet of paper is passed through a two-roll nip which is flooded with the sizing composition. The paper absorbs some of the composition, the remainder being removed in the nip.
[0052] The paper substrate contains a web of cellulose fibres which may be sourced from any fibrous plant. Preferably the cellulose fibres are sourced from hardwood and/or softwood. The fibres may be either virgin fibres or recycled fibres, or any combination of virgin and recycled fibres.
[0053] The cellulose fibres contained in the paper substrate may be modified by physical and/or chemical methods as described, for example, in Chapters 13 and 15 respectively in Handbook for Pulp & Paper Technologists by G. A. Smook, Edition Angus Wilde Publications, 1992. One example of a chemical modification of the cellulose fibre is the addition of an optical brightener as described, for example, in EP 0 884 312, EP 0 899 373, WO 02/055646, WO 2006/061399 and WO 2007/017336.
[0054] The following examples shall demonstrate the instant invention in more details. In the present application, if not indicated otherwise, “parts” means “parts by weight” and “%” means “% by weight”.
EXAMPLES
[0055] Preparative Example 1
[0056] An aqueous shading solution (S1) containing compound of formula (1) is prepared by slowly adding 40 parts of compound of formula (1) to 460 parts of water at room temperature with efficient stirring. The obtained solution is stirred for 1 hour and filtered to remove insoluble particles. The resulting shading solution (S1) has a pH in the range of from 6.0 to 7.0 and contains 8% by weight of compound of formula (1), the % by weight being based on the total weight of the final aqueous shading solution (S1).
[0000]
Application Example 1
[0057] Aqueous sizing compositions are prepared by adding aqueous shading solution (S1) containing compound of formula (1) prepared according to Preparative Example 1 at a range of concentrations of from 0 to 30 mg/l (from 0 to 2.4 mg/l of compound of formula (1) based on dry solid) to a stirred, aqueous solution containing calcium chloride (35 g/l), compound of formula (2) (7.5 g/l) and an anionic starch (50 g/l) (Penford Starch 260) at 60° C. The sizing solution is allowed to cool, then poured between the moving rollers of a laboratory size-press and applied to a commercial 75 g/m 2 AKD (alkyl ketene dimer) sized, bleached paper base sheet. The treated paper is dried for 5 minutes at 70° C. in a flat bed drier. The dried paper is allowed to condition, and then measured for CIE whiteness and brightness on a calibrated Auto Elrepho spectrophotometer. The results are shown in Table 1 and Table 2 respectively and clearly show that the instant invention provides a high level of whiteness without significant loss of brightness.
[0000]
Comparative Application Example 1
[0058] Aqueous sizing compositions are prepared by adding aqueous solution of CI Direct Violet 35 (approx. 11% by weight of dry CI Direct Violet 35, the % by weight being based on the total weight of the CI Direct Violet 35 aqueous solution) at a range of concentrations of from 0 to 30 mg/l (from 0 to 3.3 mg/l based on dry CI Direct Violet 35 compound) to a stirred, aqueous solution containing calcium chloride (35 g/l), compound of formula (2) (7.5 g/l) and an anionic starch (50 g/l) (Penford Starch 260) at 60° C. The sizing solution is allowed to cool, then poured between the moving rollers of a laboratory size-press and applied to a commercial 75 g/m 2 AKD (alkyl ketene dimer) sized, bleached paper base sheet. The treated paper is dried for 5 minutes at 70° C. in a flat bed drier.
[0059] The dried paper is allowed to condition, and then measured for CIE whiteness and brightness on a calibrated Auto Elrepho spectrophotometer. The results are shown in Table 1 and Table 2 respectively and clearly show that CI Direct Violet 35, a shading dye representative of the state-of-the-art, has a less positive effect on whiteness than the shading dye of the instant invention while having a very negative effect on brightness.
[0000]
TABLE 1
CIE Whiteness
Added shading solution
Application
Comparative Application
[mg/l]
Example 1
Example 1
0
132.4
132.4
2.5
133.1
132.5
5
134.2
132.9
10
136.3
133.4
20
138.0
135.9
30
139.7
136.6
[0000]
TABLE 2
Brightness
Added shading solution
Application
Comparative Application
[mg/l]
Example 1
Example 1
0
105.2
105.2
2.5
105.4
104.0
5
105.3
103.8
10
105.3
103.6
20
104.8
102.7
30
104.5
101.6
Application Example 2
[0060] Aqueous sizing compositions are prepared by adding preformed aqueous solution containing compound of formula (2) (18.2% by weight of compound of formula (2), the % by weight being based on the total weight of the aqueous solution containing compound of formula (2)) at a range of concentrations of from 0 to 60 WI (of from 0 to approx. 11 g/l based on dry compound of formula (2)) to a stirred, aqueous solution containing compound of formula (1) (4.0 mg/l) and an anionic potato starch (75 g/l) (Perfectamyl A4692 from AVEBE B.A.) at 60° C. The sizing solution is allowed to cool, then poured between the moving rollers of a laboratory size-press and applied to a commercial 75 g/m 2 AKD (alkyl ketene dimer) sized, bleached paper base sheet. The treated paper is dried for 5 minutes at 70° C. in a flat bed drier.
[0061] The dried paper is allowed to condition, and then measured for CIE whiteness and brightness on a calibrated Auto Elrepho spectrophotometer. The results are shown in Table 3 and Table 4 respectively and clearly show that the instant invention provides excellent build-ups of both whiteness and brightness.
Comparative Application Example 2
[0062] Aqueous sizing compositions are prepared by adding preformed aqueous solution containing compound of formula (2) (18.2% by weight of compound of formula (2), the % by weight being based on the total weight of the aqueous solution containing compound of formula (2)) at a range of concentrations of from 0 to 60 g/l (of from 0 to approx. 11 g/l based on dry compound of formula (2)) to a stirred, aqueous solution containing an anionic potato starch (75 g/l) (Perfectamyl A4692 from AVEBE B.A.) at 60° C. The sizing solution is allowed to cool, then poured between the moving rollers of a laboratory size-press and applied to a commercial 75 g/m 2 AKD (alkyl ketene dimer) sized, bleached paper base sheet. The treated paper is dried for 5 minutes at 70° C. in a flat bed drier.
[0063] The dried paper is allowed to condition, and then measured for CIE whiteness and brightness on a calibrated Auto Elrepho spectrophotometer. The results are shown in Table 3 and Table 4 respectively and clearly show that the absence of the shading dye has no effect on the brightness build-up, but has a negative effect on the whiteness build-up.
[0000]
TABLE 3
CIE Whiteness
Added OBA solution
Application
Comparative Application
[g/l]
Example 2
Example 2
0
106.8
102.7
10
126.3
123.4
20
134.0
130.5
30
139.0
135.3
40
142.0
138.1
60
144.9
141.8
[0000]
TABLE 4
Brightness
Added OBA solution
Application
Comparative Application
[g/l]
Example 2
Example 2
0
93.1
92.8
10
100.3
100.3
20
103.3
103.1
30
105.2
105.1
40
106.4
106.3
60
107.9
107.9
Application Example 3
[0064] Aqueous sizing compositions are prepared by adding preformed aqueous solution containing compound of formula (3) (14.7% by weight of compound of formula (3), the % by weight being based on the total weight of the aqueous solution containing compound of formula (3)) at a range of concentrations of from 0 to 60 g/l (of from 0 to approx. 9 g/l based on dry compound of formula (3)) to a stirred, aqueous solution containing compound of formula (1) (4.0 mg/l) and an anionic potato starch (75 g/l) (Perfectamyl A4692 from AVEBE B.A.) at 60° C. The sizing solution is allowed to cool, then poured between the moving rollers of a laboratory size-press and applied to a commercial 75 g/m 2 AKD (alkyl ketene dimer) sized, bleached paper base sheet. The treated paper is dried for 5 minutes at 70° C. in a flat bed drier.
[0065] The dried paper is allowed to condition, and then measured for CIE whiteness and brightness on a calibrated Auto Elrepho spectrophotometer. The results are shown in Table 5 and Table 6 respectively and clearly show that the instant invention provides excellent build-ups of both whiteness and brightness.
[0000]
[0066] Comparative Application Example 3
[0067] Aqueous sizing compositions are prepared by adding preformed aqueous solution containing compound of formula (3) (14.7% by weight of compound of formula (3), the % by weight being based on the total weight of the aqueous solution containing compound of formula (3)) at a range of concentrations of from 0 to 60 g/l (of from 0 to approx. 9 g/l based on dry compound of formula (3)) to a stirred, aqueous solution containing an anionic potato starch (75 g/l) (Perfectamyl A4692 from AVEBE B.A.) at 60° C. The sizing solution is allowed to cool, then poured between the moving rollers of a laboratory size-press and applied to a commercial 75 g/m 2 AKD (alkyl ketene dimer) sized, bleached paper base sheet. The treated paper is dried for 5 minutes at 70° C. in a flat bed drier.
[0068] The dried paper is allowed to condition, and then measured for CIE whiteness and brightness on a calibrated Auto Elrepho spectrophotometer. The results are shown in table 5 and table 6 respectively and clearly show that the absence of the shading dye has no effect on the brightness build-up, but has a negative effect on the whiteness build-up.
[0000]
TABLE 5
CIE Whiteness
Added OBA solution
Application
Comparative Application
[g/l]
Example 3
Example 3
0
106.8
102.7
10
125.8
122.7
20
132.9
129.5
30
136.8
133.5
40
138.8
136.4
60
141.4
139.0
[0000]
TABLE 6
Brightness
Added OBA solution
Application
Comparative Application
[g/l]
Example 3
Example 3
0
93.1
92.8
10
100.0
100.3
20
102.9
103.1
30
104.7
104.7
40
105.5
106.0
60
107.0
107.4 | The instant invention relates to liquid sizing compositions comprising shading dyestfuffs, derivatives of diaminostilbene, binders, protective polymers, and optionally divalent metal salts which can be used for the optical brightening of substrates, including substrates suitable for high quality ink jet printing. | 3 |
BACKGROUND TO THE INVENTION
1. Field of the Invention
The invention relates to pistons for internal combustion engines and more particularly to pistons for diesel engines.
2. Review of the Prior Art
Since the fuel in a diesel engine is ignited by the temperature of air compressed in the cylinder prior to injection of the fuel, it is necessary, if combustion is to take place, to compress the air by a predetermined amount to ensure that the required temperature for fuel ignition is reached. The fuel is, however, injected before a piston in a cylinder of the engine reaches top dead centre and so the pressure in the cylinder continues to rise after the fuel has been injected.
In view of the high compression ratios used in diesel engines, the maximum cylinder pressure, reached, at or shortly after top dead centre, can be substantial. This peak pressure imposes loads on the piston which can damage bearings and reduce the effectiveness of lubrication. In addition, it can cause shock waves to pass through the engine block which can in turn cause cavitation in water cooling systems which leads to erosion of metal from the water side of the cylinders. The rate at which the pressure rises also causes fatigue and cracking in the piston and reduces the life of the gudgeon pin bosses. Further, the high rate of pressure rise is an important factor in the noise emission spectrum of diesel engines. The maximum pressure also determines the amount by which the air can be pressurised before entry into the cylinder and affects adversely the equipment for injecting the fuel. In addition, in certain cases, it makes the use of a heater necessary on starting the engine.
SUMMARY OF THE INVENTION
According to the invention there is provided a piston for an internal combustion engine and comprising a crown formed at least partially by a member movable relatively to the remainder of the piston, the member moving in each compression stroke, when the pressure in the associated cylinder reaches a predetermined level, from a first position to a second position in which the combustion chamber volume is increased, the member maintaining said second position until a predetermined pressure is reached on each expansion stroke, when the member returns to said first position.
BRIEF DESCRIPTION OF THE DRAWINGS
The following is a more detailed description of some embodiments of the invention, by way of example, reference being made to the accompanying drawings, in which:
FIG. 1 is a cross-section through a first form of piston for a diesel engine having a combustion bowl of variable volume,
FIG. 2 is a graph showing diagrammatically the variation of pressure within the cylinder of a diesel engine against crankshaft angle for the piston of FIG. 1 and for a piston having a combustion bowl of fixed volume,
FIG. 3 is a cross-section through a modified form of the piston of FIG. 1, and
FIG. 4 is a cross-section through a second form of piston for a diesel engine and having a combustion bowl of variable volume.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring first to FIG. 1, the first form of piston comprises a piston body 10 cast from aluminum or aluminum alloy and formed with a skirt 11 and piston ring grooves 12. The centre of the body is provided with a cylindrical bore 13 terminating at its lower end in an annular radially extending surface 14 provided with a central hole and an annular step 15. The surface 14 is covered with a steel plate 16. A crown 17, of an aluminum or ferrous alloy, is fixed to the body portion 10 by bolts 18 and includes an outer surface 19 contiguous with the skirt 11 and formed, optionally, with a further piston ring groove 12. The crown 17 is generally annular and is provided with a radially inner annular surface 20 which forms an entrance to a combustion bowl 21. An annular bore 22 leads from the radially inner edge of the surface 20. The diameter of the bore 22 is less than the diameter of the bore 13 in the piston body so that a step 23 is formed between the two parts.
A generally cylindrical piston-like member 24 is carried by the piston body 10 and is formed with an upper surface 25 which forms the central portion of the combustion chamber 21. The member 24 has a cylindrical outer surface 26 and is a sliding fit in the crown bore 22. The surface 26 terminates in an annular rabbet 27 which, in the position of the member 24 shown in FIG. 1, is in engagement with the step 23 between the crown 17 and the piston body 10 to prevent axial movement of the member 24 in an upward direction. The cylindrical surface 26 is provided with grooves 28 which receive sealing rings (not shown) for forming a seal between the member 24 and the crown 17.
The member 24 also includes a lower portion 29 of generally cylindrical configuration which is received within the bore 13 in the piston body 10 and which has a diameter substantially less than the diameter of that bore. Within the annular gap between the lower portion 29 and the bore 13 are arranged grouped pairs of plate springs 30, the uppermost bearing against the member 24 and the lowermost bearing against the steel plate 16. The arrangement is such that the plate springs 30 are held under partial compression or preload when the piston is in the position shown in FIG. 1.
The piston is assembled by inserting the plate 16 into the piston body 10 and then placing the plate springs 30 on the plate 16. The member 24 is then inserted with the cylindrical part 29 extending down through the washers into abutment with the plate springs 30. The crown 17 is then placed in position so that the step 23 presses down on the rabbet 27 of the member 24 thus partially compressing the plate springs 30. The bolts 18 are then inserted to fix the crown 17 to the piston body and hold the plate springs 30 under the partial compression.
In use, the piston is inserted into a cylinder of a diesel engine which may be a two-stroke or four-stroke diesel engine and may be either naturally aspirated or preferably pressure-charged. As is well known, a diesel engine works on the principle of compressing a charge of air to a temperature at which diesel fuel will ignite and then, when the requisite compression has been reached, injecting the fuel to produce an expansion and exhaust stroke followed by recompression and combustion. The fuel is injected before top dead centre. In order to achieve the necessary air temperature to initiate combustion, the compression ratio of the engine must be much higher than that in an Otto cycle engine; for example, between 12 and 18:1 with direct injection engines.
After the fuel has been injected, and combustion commenced, the pressure increases to reach a maximum pressure just after top dead centre, before declining in the expansion stroke. This is shown schematically by the broken line 31 in FIG. 2 for a conventional piston not including the member 24. The high maximum pressure has a number of adverse results amongst which are the high stressing of bearings and engine parts, the breaking down of lubrication films, the production of shock waves passing through the engine block which in turn can cause cavitation in a water cooling system leading to erosion of the metal of the engine, and the inability of the engine to withstand high boost for a long periods. Further, this maximum pressure has an adverse effect on the fuel injection equipment, may cause difficulties in starting, and in the attainment of acceptable noise emission and vibration spectrums.
The piston described above with reference to FIG. 1 operates in the following way. As the piston commences the compression stroke to compress the charge of air, the member 24 remains in the position shown in FIG. 1 so that the combustion bowl has a lesser volume. The piston is thus acting in the same way as a conventional piston to compress the air to the temperature necessary to cause combustion of the fuel. Fuel injection then takes place and the plate springs 30 are so preloaded, that, up to the pressure reached at fuel injection, no movement of the member 24 has occurred. At this point, however, the cylinder pressure acting on the combustion bowl surface 25 of the member 24 is sufficient to compress the plate springs 30 to cause the member 24 to slide in the bore 22 in the crown 17 to a second position (not shown) in which the combustion bowl 21 has a much greater volume. The lower end of the member 24 bears aginst the portion of the plate 16 radially inwardly of the step 14. The plate 16 thus prevents the plate springs 30 and the member 24 wearing away the piston body.
The result of this is that the minimum volume of the combustion chamber in the cylinder is increased and the maximum pressure reduced. Once the piston has passed top dead centre and maximum pressure, the cylinder pressure reduces until the limiting pressure is once again reached. The member 24 then moves back to the first position shown in FIG. 1 in which the rabbet 27 abuts against the step 23 and the combustion bowl 21 has its lesser volume.
This is shown schematically in FIG. 2 in the continuous line 32. It will be seen that the curves 31, 32 follow one another until the fuel injection point is reached. The cylinder pressure is then reduced in comparison with the conventional piston until a balancing pressure is reached once again when the two curves virtually regain coincidence.
The piston of FIG. 1 has the following advantages:
1. The peak cylinder pressure is reduced together with the rate of pressure rise following injection. This leads to increased bearing life through reduced loading while assisting in the maintenance of a satisfactory oil film at the crank pin bearing and gudgeon pin bearing surfaces.
2. The cyclic torque characteristics of the engine are improved and some of the energy absorbed around top dead centre is subsequently yielded up on the expansion stroke. Thus the specific output of the engine will remain equal to or slightly better than that of an engine not using the piston described above with FIG. 1, for a given level of fuel input. Thus the need for reduction in specific output to produce smoother and quieter combustion is obviated and there is less shock vibration in the engine structure.
3. The intensity of shock waves is reduced, leading to a decreased tendency to cavitation erosion in water cooled cylinder liners.
4. Because of the increased volume of the combustion bowl 21, the surface 25 should have a longer life with less combustion bowl edge erosion. In addition, gudgeon pin life should be increased by the reduced pressure.
5. The engine will stand higher levels of pressure-charging for longer periods, providing cooling facilities are adequate.
6. Such a piston may simplify fuel injection equipment and the cost of such equipment and, in some cases, may allow the elimination of use of a heater on starting.
7. There may be an ability of the engine to accept differing fuels without redesign.
8. The compression ratio is unaffected at starting and so there will be no adverse effect on the starting characteristics of the engine.
The space within which the springs are located may be supplied with oil, both to cool the springs and to damp the movement of the member 24.
It will be appeciated that the piston need not be provided with a combustion bowl 21. The piston could have a conventional flat crown with the member 24 opening up a recess when the predetermined pressure is reached in closing the recess when the cylinder pressure drops below the predetermined pressure. It will also be appreciated that the piston need not use plate springs 30, any suitable spring means such as coil springs may be used.
Two embodiments using coil springs are shown in FIGS. 3 and 4. In FIG. 3, the piston is constructed generally as the piston described above with reference to FIG. 1 and parts common to FIG. 1 and FIG. 3 will be given the same reference numerals and will not be described in detail. In the piston of FIG. 3, the member 24 is provided on its under surface with a central annular recess 32 and the steel plate 16 is formed with a central upward boss 33. Two co-axial coil springs 34, 35 are arranged between the member 24 and the steel plate 16. The inner coil spring 34 engages the recess 32 and the boss 33 and the outer coil spring 35 engages outer portions of the member 24 and the plate 16. The coil springs 34, 35 have opposite hands.
The piston of FIG. 3 operates in the same way as the piston of FIG. 1 and has the same benefits. The provision of two coil springs 33, 34 allows an increased force to be applied to the member 24 as compared with the FIG. 1 piston. This may be desirable in certain diesel engines where particularly high pressures are generated.
Referring next to FIG. 4, the second form of piston comprises a crown 40 and a body 41 both formed from aluminum or an aluminum alloy. The crown 40 is generally annular and is provided with a ring band 42 including three piston ring grooves 43. The centre of the crown 40 is provided with an annular surface 44 which forms an entrance to a combustion bowl 45. An annular bore 46 leads downwardly from the inner edge of the surface 44.
The body 41 comprises a generally frusto-conical central portion 49 connected by bolts 50 to the crown 40. The upper end of the body is formed with spaced projections 47 which are drawn against the crown 40 by the bolts 50 and which are angularly spaced to form slots between them. Aligned gudgeon pin bores 51 are provided and the lower end of the central portion 49 is connected to an annular skirt 52 having an upper surface lying in a plane normal to the piston axis. A shaped connecting rod 53 has a gudgeon pin bore 54 aligned with the gudgeon pin bore 54 in the body 41 and connected thereto by a pin 60.
A generally cylindrical piston-like member 55 is a sliding fit in the crown bore 46 and is formed with an upper surface 56 which forms the central portion of the combustion bowl 45. The member 55 has downwardly and outwardly extending spider arms 57 which pass through the slots between the projections 47 on the body 41 and carry at their ends an annulus 62 which engages beneath a lower surface 58 of the crown 40. Thus the member 55 is free for sliding movement within the crown bore 56 relatively to the crown 40 and the body 41.
A partially compressed coil spring 59 is arranged between the annulus 62 and a washer 61 provided on the skirt 52. This urges the member 55 into the position shown in FIG. 4.
The piston described above with reference to FIG. 4 operates in the same way as the pistons described above with reference to FIGS. 1 to 3 and has the same benefits. In comparison with the pistons of FIGS. 1 to 3, the piston of FIG. 4 is of light-weight and the increased length of the spring 59 allows it to bear against the member 55 with increased force.
The combustion bowl, where provided, can have any required shape.
Although the pistons of FIGS. 1 to 4 have been described in relation to a diesel engine, it will be appreciated that they may be used in an Otto cycle engine or any other type of engine. | A piston (10) for a diesel engine is formed with a combustion bowl (21) which has a lesser volume until the cylinder pressure reaches that at which fuel ignition takes place. The volume of the combustion bowl is then increased to reduce the maximum pressure in the cylinder. The volume is again decreased during the expansion stroke. This has a number of beneficial effects on the engine including reducing the stress on the engine parts and allowing increased level of pressure-charging. | 5 |
RELATED APPLICATION
This application is a continuation-in-part of application Ser. No. 749,464, filed Dec. 10, 1976, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the removal of carbonyl sulfide from liquid propane utilizing as the principal agent 2-(2-aminoethoxy) ethanol.
2. Description of the Prior Art
Treatment of gasoline plant, refinery, or other processing plant liquid products for removal or conversion of undesirable components including sulfur compounds is a complex and costly necessity for the petroleum fuel processing industry. Such undesirable compounds include, for example, hydrogen sulfide, mercaptans, sulfides and carbonyl sulfide as well as carbon dioxide.
Methods existing prior to the invention described herein for the removal of carbonyl sulfide from natural petroleum fuels have quite often been performed on fuels in a gaseous state. For example, widely relied upon procedures in the natural gas industry for removing sulfide impurities from gaseous state fuels have utilized monoethanolamine (MEA), diethanolamine (DEA), tetraethyleneglycol (TETRA), or diisopropyl amine (DIPA).
It is also well established in the literature that 2-(2-aminoethoxy) ethanol, also known by the trademarked name DIGLYCOLAMINE®, and hereinafter often referred to as DGA, has been used either by itself or in combination with other materials to remove sulfide components from gaseous streams of petroleum fuels and petroleum derived products. Thus, the manufacturer of DGA has stated in a technical bulletin that "the major use of DIGLYCOLAMINE® brand of 2-(2-aminoethoxy) ethanol is for the removal of hydrogen sulfide (H 2 S) and/or carbon dioxide (CO 2 ) from gas streams." Jefferson Chemical Company, Inc., Technical Bulletin, DIGLYCOLAMINE®, Jefferson Chemical Company, Inc., 3336 Richmond Ave., Box 53300, Houston, Tex. 77052.
The use of DGA for removing acid gases from a gaseous mixture stream of wet or dry hydrocarbons is the subject of U.S. Pat. No. 3,712,978 (July 12, 1955) and of Canadian Pat. No. 505,164 (Aug. 15, 1954), assigned to the Fluor Corporation, Ltd., Los Angeles, Cal. This is also described in an article entitled "Acid Gas Removal from Natural Gas Using Diglycolamine" by Howard L. Holder, presented at 45th Annual Convention of The Natural Gas Processors Association.
Additionally, it has been reported that MEA and DGA are substantially equivalent in their effectiveness for removing carbonyl sulfide from gaseous systems. Dingman & Moore, Compare DGA and MEA Sweeting Methods, Hydrocarbon Processing, Vol. 47, No. 7, July, 1968.
Jones and Payne have reported success in using a DGA-water mixture as a solvent in an aromatic extraction treatment of hydrogenated pyrolysis gasoline. They have reported that the DGA-water solvent is more effective for removing benzene-toluene and toluene-xylene mixtures from gasoline than other currently used solvents such as TETRA or DEG-DPG mixtures. Jones and Payne, New Solvent to Extract Aromatics, Hydrocarbon Processing, March, 1973, 91-92.
The Naval Research Laboratory has compared the use of DGA with MEA, N,N' dimethylacetamide (DMAC), and tetramethylene sulfone (TMS) as regenerative carbon dioxide absorbants. It was reported that TMS was superior to the other solvents when employed in CO 2 scrubbers on nuclear submarines. Gustafson and Miller, Investigation of Some New Amines as Regenerative Carbon Dioxide Adsorbants, Naval Research Laboratory, NRL Report 6926, July 23, 1969.
DGA has been used by the El Paso Natural Gas Company for the removal of acid gas impurities from gas streams containing 2% or more of total acid gas. In side-by-side comparisons of a mixture of MEA-DEG solvents with DGA, it was found that DGA was capable of producing approximately a 50% saving in capital investment because the more efficient DGA solvent characteristics resulted in reductions of solution pumping horsepower, reboiler drive steam, cooling tower loads, etc. H. L. Holder, Diglycolamine-A Promising New Acid-Gas Remover, The Oil & Gas Journal, May 2, 1966, 83-86.
The need for complete carbonyl sulfide removal from liquid propane is quite apparent when one considers that hydrolysis of carbonyl sulfide results in the production of carbon dioxide and hydrogen sulfide. The reaction becomes distressingly apparent in petroleum treatment systems which incorporate catalytic dehydrators used to dry purified petroleum products. For example, it was reported in 1962 that propane dehydrators used in a Mobil Oil Company underground storage facility started producing hydrogen sulfide in the effluent stream. Investigations established that the inlet stream of gaseous propane contained trace quantities of carbonyl sulfide. Apparently, activated alumina used in the propane dehydrators catalyzed the hydrolysis of carbonyl sulfide and resulted in hydrogen sulfide contaminated effluent. The problem was solved by Mobil Oil Company not by using a solvent to remove the carbonyl sulfide from the inlet propane stream, but by utilizing a silica-alumina absorbant which had been specially treated to prevent the catalyzed hydrolysis. Fairs and Rumbaugh, Carbonyl Sulfide Hydrolyses in Propane Dehydrator, Hydrocarbon Processes and Petroleum REFINER, 41(11), November, 1962, 211.
Shell Oil Company has suggested a method for the removal of carbonyl sulfide and hydrogen sulfide from liquid propane. This process is known as the ADIP process and is based upon an absorption-regeneration cycle using a circulating aqueous solution of an alkanolamine such as diisopropyl amine. Shell Oil indicates that liquid propane treated by the ADIP process results in a carbonyl sulfide content in liquid propane after the treatment of less than 2 ppm by weight. Shell Oil Company, ADIP, Hydrocarbon Processing, April, 1975, 84.
British Pat. No. 1,513,786 (May 29, 1969) assigned to Shell International Research MAATSCHAPPIJ N.V., teaches the separation of acid gases such as carbonyl sulfide and hydrogen sulfide from gaseous mixtures by means of a selective absorbant of the general formula:
HO--(CH.sub.2).sub.p --O.sub.q --(CH.sub.2).sub.r --NH.sub.2
wherein p, q and r are integers, and p=2 to 3, q=1 to 4 and r=2 to 3
Signal Oil Company has reported on the treatment of gas plant liquids with DGA. Williams, W. W., Treatment of Gas Plant Liquids with Diglycolamine Agent, paper prepared for presentation at Oklahoma Regional Meeting of the Natural Gas Processors Association, Oklahoma City, Okla., Apr. 12, 1973. In that paper, it was reported that a liquid product mixture was treated with DGA prior to fractionation with the intent of minimizing or possibly eliminating the downstream sweetening processes. Initially, an MEA liquid-liquid contact system was constructed. This was subsequently converted to DGA in order to evaluate mercaptan removal with the added advantage that any carbonyl sulfide reaction with DGA produced regenerable degradation products. Table IV of this report, reproduced in part as Table 1 for convenience below, indicates that the raw product sought to be purified was a complex mixture of straight chain hydrocarbons with only approximately 48% of the mixture consisting of liquid propane. Results of chemical analysis after treatment with DGA, also found in Table IV of this report and reproduced in part below, show that only approximately 25% of the carbonyl sulfide found in the untreated raw product was removed after treatment with DGA, whereas significantly higher percentages of the hydrogen sulfide and mercaptan impurities were removed.
Regarding the foregoing, it becomes exceedingly apparent that the prior art usage of DGA has been nearly universally limited to the removal of acid gases from gaseous hydrocarbon streams.
TABLE 1______________________________________ % UNTREATED DGA REMOVAL RAW TREATED OFCOMPONENT PRODUCT PRODUCT IMPURITY*______________________________________Carbon dioxide 10 ppm NIL 100%Hydrogen sulfide 11 ppm 5 ppm 54.5%Carbonyl sulfide 12 ppm 9 ppm 25%Sulfur dioxide 5 ppm 7 ppmCarbon disulfide NIL 1 ppmMethyl mercaptan 27 ppm 20 ppm 25.9%Ethyl mercaptan 32 ppm 29 ppm 9.5%Propyl mercaptan 25 ppm 13 ppm 48%+disulfidesTotal mercaptans 91 ppm 66 ppm 27.5%Total sulfur 122 ppm 86 ppm 29.5%______________________________________ Raw Product Stream Analysis Reproduced from Table IV of Williams, W. W., Treatment of Gas Plant Liquids with Diglycolamine Agent, paper prepared for presentation at Oklahoma Regional Meeting of the Natural Gas Producer Association, Oklahoma City, Oklahoma, April 12, 1973. *This portion of the table was not presented in the original.
The one exception of this use has been the Signal Oil Company treatment of liquid hydrocarbon mixtures with DGA to remove impurities. However, even in this example the effectiveness of removal of carbonyl sulfide from the liquid mixtures has been minimal. Accordingly, prior to the development of the present invention, there has been no commercially acceptable, economically attractive method for substantially reducing the carbonyl sulfide content of liquid propane streams; therefore, the art has long sought a method which can effectively and economically reduce the carbonyl sulfide content absent the disadvantage of low percentage removal of carbonyl sulfide.
Applicant's application Ser. No. 749,464 filed Dec. 10, 1976 discloses an improved method for carbonyl sulfide removal from liquid propane, utilizing DGA as the principal agent in the carbonyl sulfide removal. This present application discloses and claims that same method, the mechanism for carbonyl sulfide removal now being more fully understood and described.
SUMMARY OF THE INVENTION
In accordance with this invention, the foregoing has been achieved through the present method for treating a hydrocarbon stream consisting essentially of liquid propane and containing carbonyl sulfide, and in particular, for the substantially 100% removal of carbonyl sulfide from such liquid propane stream.
The invention is a method for the removal of carbonyl sulfide from liquid propane by mixing under liquid-liquid contact conditions liquid propane containing carbonyl sulfide as an impurity with DGA as the principal agent for carbonyl sulfide removal. The temperature and pressure under which such mixing occurs is such as to retain the liquid propane in the liquid state. After this mixing occurs, the mixture is separated into two components, one being liquid propane substantially free of carbonyl sulfide and the other comprising DGA and DGA degradation products, including H 2 S absorbed by the DGA.
It has now been determined that the principal mechanism of carbonyl sulfide removal using DGA in accordance with the present invention involves a reaction of DGA with carbonyl sulfide to yield the degradation product N,N' bis (hydroxyethoxyethyl) urea (known as BHEEU) according the following equation: ##STR1## where R=HO--CH 2 --CH 2 --O--CH 2 --CH 2
As a result of this reaction the non-propane stream leaving the liquid-liquid contact apparatus will not show any appreciable carbonyl sulfide. Rather this stream will comprise any unreacted DGA, the BHEEU degradation product and hydrogen sulfide absorbed by the DGA. The expression "DGA and DGA degradation products" is therefore meant to embrace this stream which is formed by the reaction of DGA and carbonyl sulfide.
A further characteristic feature of this method is that the above reaction is reversible to the extent that the BHEEU can be reconverted to DGA in a suitable reclaimer, with the off gas of the reclaimer being essentially CO 2 DGA & H 2 O. The DGA can then be used for further carbonyl sulfide removal, thereby making this method extremely commercially attractive.
BRIEF DESCRIPTION OF THE DRAWING
In the drawing, the single FIGURE illustrates a typical flow diagram for DGA removal from liquid propane in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention embodies a method wherein carbonyl sulfide is removed from a liquid propane stream by utilizing certain characteristics of DGA. Sour liquid propane is flowed into intimate contact with DGA which acts to selectively remove the carbonyl sulfide from the liquid propane stream. As used herein, the expression "sour liquid propane" refers to liquid propane which has carbonyl sulfide impurities dissolved within it.
Referring now to the single FIGURE, at the outset of the purification process a stream of sour liquid propane is flowed into a liquid-liquid contactor 1 simultaneously with a stream of unreacted DGA, the flow rate of the DGA merely being such as to provide effective contact between the DGA and liquid propane. The selection of a particular flow rate can be easily carried out by one skilled in the art based on the nature of the liquid-liquid contactor, concentration of DGA, amount of carbonyl sulfide impurity, etc. As used herein, "un-reacted DGA" refers to the DGA prior to reaction with carbonyl sulfide or after regeneration from its degradation products. The unreacted DGA used in this method may be DGA itself, or aqueous solution of DGA. In operation of this method, regeneration of the DGA from BHEEU will not be totally complete. As a result the DGA used for the removal of carbonyl sulfide will generally contain some BHEEU. A typical system for use in this method will therefore comprise from about 5-90% by weight DGA, 10-40% by weight BHEEU and the remainder, if any, water. Aqueous solutions are preferred and it is preferred that the BHEEU concentration be in the range of 10-15% to reduce the viscosity of the treating liquid.
In the liquid-liquid contractor 1, the sour liquid propane stream may be flowed counter-currently to the unreacted DGA stream for the reason that adequate mixing is easily obtainable by such flow. The sour liquid propane stream may also be flowed co-current or cross-current to the unreacted DGA stream if provision is made for adequate mixing of the two liquids in the liquid-liquid contactor 1. The contact and/or mixing time for the liquids in the liquid-liquid contactor 1 is easily determinable through routine experimentation by one skilled in the art. Any commercially available liquid-liquid contactor system may be utilized, using for example, packed columns, bubble-type mixing or stratified plates.
The mixture resulting from this flow is thereafter separated into two components, the first containing DGA and DGA degradation products in water, and the second containing sweet liquid propane including a small amount of DGA soluble in liquid propane and water. As used herein "sweet liquid propane" refers to liquid propane which has been flowed into intimate contact with unreacted DGA, resulting in the removal of carbonyl sulfide from the sour liquid propane stream.
The second of these components is then flowed into a settling tank 2 wherein the DGA and water, both being heavier in weight than sweet liquid propane, migrate to the lower portion of the settling tank 2. Sweet liquid propane containing dissolved water is withdrawn and may be flowed into a propane dehydrator 3. Although not shown in the drawing, the sweet propane stream may be water washed before introduction into the propane dehydrator 3. The water wash system may include a suitable water separator for water removal. Activated alumina, bauxite, silicaalumina gel, molecular seives or similar materials may be present within the dehydrator 3 to act as a catalyst in the following reaction:
COS+HOH .sup.catalyst CO.sub.2 +H.sub.2 S
Thus, any carbonyl sulfide remaining in the water-saturated sweet propane reacts according to this above reaction with the hydrogen sulfide and any remaining unreacted carbonyl sulfide being adsorbed on the surface of the catalyst. After dehydration, the dehydrated liquid propane may be pumped via a line 4 to suitable facilities for storage or sale.
When the propane dehydrator 3 is utilized in the treatment process, it is preferred, for convenience only, that at least two dehydrator units, connected in parallel, be used. Thus, as one of the units is dehydrating the sweet liquid propane and simultaneously causing the above reaction to occur, the remaining unit or units undergo a regeneration cycle in which hot propane vapors may be passed over the surface of the catalyst, thus driving off any adsorbed water, hydrogen sulfide and carbonyl sulfide. These vapors may thereafter be condensed and recycled through the liquid-liquid contactor 1 where the hydrogen sulfide and carbonyl sulfide are removed.
Concurrently with the foregoing, the first stream removed from the liquid-liquid contactor 1 is flowed, preferably along with the DGA withdrawn from the settling tank 2, to a flash drum 5 in which any adsorbed propane is vaporized and removed. The rich DGA stream flows from the flash drum 5 to a carbon filter 6 wherein components such as heavy hydrocarbons and surfactants may be removed. The carbon filter 6 may be of any suitable type such as a model CF-120 made by the Perry Engineering Corporation.
The rich DGA stream from the carbon filter then flows through the tube side of heat exchanger 7 and into still 8. The still bottoms may be flowed through a reboiler 9 in which approximately 20% of the liquid may be vaporized. The reboiler 9 may be of any suitable type including either a steam reboiler or a fired reboiler. Preferably, the steam reboiler is of a standard kettle type having a weir overflow. The vapors from reboiler 9 are flowed back into still 8. The liquid from the reboiler is flowed together with makeup DGA from surge tank 10 through the shell side of heat exchanger 7. The surge tank 10 provides a convenient means for the introduction of make-up DGA and also provides for the continuous flow of lean DGA should the liquid stream from reboiler 9 be interrupted for any reason.
After passing through the shell side of heat exchanger 7 the pressure of the lean DGA stream may be increased by booster pump 11. Approximately 10-40% of the lean DEA stream may be diverted to reclaimer 12. In reclaimer 12 the BHEEU is converted to DGA through the application of heat and the addition of water or steam according to the reaction: ##STR2##
The lean DGA is preferably heated in reclaimer 12 to a temperature of from about 360° to about 400° F. to effect the DGA regeneration. The reclaimer 12 should preferably have a sparging line for the introduction of water from for example reflux accumulator 13, or for the introduction of steam for additional heating and mixing of the lean DGA stream. The vaporized stream from the reclaimer may then be flowed to still 8. It should be apparent that the flow of lean DGA into reclaimer 12 may be controlled by a suitable level controller.
The overhead from still 8 may be passed through a suitable condenser such as fan condenser 14 and may then be flowed to an overhead accumulator 13. The overhead gas from still 8 is generally comprised of CO 2 and H 2 S. Water from the overhead accumulator may be recycled, via pump 13a, to still 8 and may be introduced into the reclaimer 12 through a sparging line.
It should be noted that still 8 and overhead accumulator 13 are shown in a stacked relationship and that this design has obvious advantages which are preferred.
For commercial application of this method, it is important that reclaimer 12 effectively regenerate DGA for reuse from its degradation product BHEEU. In addition to maintaining a sufficiently high temperature for thermal reversion, it is also preferred that reclaimer 12 be sized so as to accommodate the flow of liquid. As previously stated this flow should be approximately 10% to 40% of the total lean DGA flow rate.
The remainder of the lean DGA which is not passed through reclaimer 12 may be passed through a suitable cooler such as fan cooler 15. The lean DGA may then be pumped via pump 16 to the contactor 1.
Throughout the entire treatment process, the pressure and temperature of the system must be compatible to maintain the propane in the liquid state. Through experimentation, it has been established that the most effective treatment temperature range is between 60°-150° F. The pressure of the system is thereby correlated with this temperature range to assure the propane remains in the liquid state throughout the process.
The amount of DGA used in the practice of the present invention is variable depending on the carbonyl sulfide concentration existing in the sour liquid propane and is merely that amount of DGA effective to achieve the desired level of carbonyl sulfide removal. Such amount is easily determined by one skilled in the art through routine experimentation.
Typical liquid-liquid contactors, reclaimers, heat exchangers, other apparatus and the like, such as are commercially available, may be used to perform the invention disclosed herein. It should be understood that the method of the present invention is not be limited to the use of the apparatus as described above, and modifications within the foregoing description can be made while still falling within the spirit of the present invention. For example, it is possible to perform the present invention by simply mixing the unreacted DGA with sour liquid propane in a suitable mixing tank and thereafter separating, by specific gravity differences, the carbonyl sulfide-free liquid propane from the carbonyl sulfide containing DGA.
EXAMPLE
As an example of the effectiveness of the method disclosed herein, two series of experiments were run to determine the efficacy of DGA in the removal of carbonyl sulfide from a liquid propane stream. It should be understood that these procedures are provided simply to show the effectiveness of the present invention and in no way limit the scope of the invention or the procedures as described.
Procedure No. 1
In this series of experiments, 90% by weight liquid propane containing dissolved carbonyl sulfide impurity and 10% by weight of differing DGA concentrations are placed in a high pressure corrosion bomb. The bomb is then vibrated for five minutes to assure adequate mixing, and thereafter, the components are allowed to settle for fifteen minutes. Samples of the liquid propane are then drawn off and are subjected to gas chromatography analysis. Concentration of the DGA solution is varied from 0% DGA to 80% DGA in water. Table 2 lists the results of this experiment. Reference to Table 2 shows that there is a complete 100% removal of carbonyl sulfide from the liquid propane when the concentration of the DGA solution equals or exceeds 15%.
Procedure No. 2
Liquid propane is allowed to flash and is thereafter bubbled through 150 ml of the various aqueous DGA solutions which have previously been placed in 250 ml gas washing bottles. Vapors emanating from the washing bottles are sampled and injected directly into a gas chromatograph. Table 3 provides the results of this procedure. By referring to Table 3, one again sees that there is a complete 100% removal of carbonyl sulfide when the concentration of the DGA solution equals or exceeds 15%.
TABLE 2______________________________________ Carbonyl Sulfide Remaining in Grams Sample after Carbonyl % Carbonyl% DGA Treatment, ppm Sulfide Sulfide Removed______________________________________0 449 28 010 107 6 7915 0 0 10020 0 0 10025 0 0 10050 0 0 10080 0 0 100______________________________________ Results of carbonyl sulfide removal under Procedure No. 1
TABLE 3______________________________________ Carbonyl Sulfide Remaining in Grams Sample after Carbonyl % Carbonyl% DGA Treatment, ppm Sulfide Sulfide Removed______________________________________0 499 28 010 180 10 6415 0 0 10020 0 0 10025 0 0 10050 0 0 10080 0 0 100______________________________________ Results of carbonyl sulfide removal under Procedure No. 2
While the present invention has been described by reference to certain preferred embodiments and examples, it is to be understood that this invention cannot be limited thereto but rather must be construed as broadly as all or any equivalents thereof. | A method for the removal of carbonyl sulfide from liquid propane under liquid-liquid contact conditions by mixing liquid propane containing carbonyl sulfide as an impurity with 2-(2-aminoethoxy) ethanol as the principal agent for the carbonyl sulfide removal. The 2(2-aminoethoxy) ethanol is reclaimed and reused for further carbonyl sulfide removal. | 2 |
BACKGROUND OF THE INVENTION
[0001] The present invention relates generally to storage systems and, more particularly, the rapid deployment of virtual machine pooling volume.
[0002] In a datacenter, the creation and deployment process for virtual machine using a volume on an external subsystem is a time consuming process. A typical procedure involves the following: (1) The virtual machine (VM) user asks the storage administrator to create a volume based on size. (2) The VM user asks the server administrator to discover the created volume on operation. (3) The server administrator discovers the created volume for the target hypervisor on the host. (4) The VM user copies VM images data such as VHD file on the discovered volume (e.g., in Windows Hyper-V world). (5) The VM user runs the image data on the hypervisor. In the copying of VM images data (4), if GUID (globally unique identifier) is duplicated among volumes, some failover clusters keep a state for the duplicated signature disk as reserved disk.
[0003] U.S. Pat. No. 7,555,644 for system and method for operating system image provisioning in a utility computing environment discloses a technique for provisioning OS image a boot up of a computing server using a pool for OS image copied volume. FIG. 1 of that patent shows a procedure of managing the pool based on upper and lower numbers of OS image Boot-up disks as pool threshold. However, that patent does not disclose how to achieve efficient pool management based on customer creation usage and the OS image boot-up disk is fixed in size. The method is not for virtual machine. The VM user cannot select the desired size boot image. Therefore, that patent improves (2), (3), and (4) which we mentioned as customer operation, but not size operation, and it also does not provide efficient control of the pool availability.
BRIEF SUMMARY OF THE INVENTION
[0004] Exemplary embodiments of the invention provide method and apparatus for rapid creation and deployment of virtual machines by reducing or minimizing communication processes between virtual machine user and storage and server administrators. In specific embodiments, the rapid VM creation and deployment method involves the use of an external storage subsystem. The system management server prepares a pool of pre-created virtual volumes with pre-copied images controlling storage subsystem capabilities. On user creation ((1)) and deployment ((2), (3), (4)), the system management server picks a volume from the pool and resizes the volume to a user desired size on deployment. As a beneficial result, from the VM user's perspective, the process makes a short cut for prior (2), (3), and (4). Additionally, regarding the pre-creation, the system management server pre-estimates the number of virtual machines to be created based on the current queuing number of deployed VM or velocity of history for the past deployment. As such, the system avoids the lack of the pre-created volume in the pool and provides continuous, uninterrupted VM deployment. This ensures total system reliability under rapid deployment.
[0005] In specification embodiments, the management server initiates a request to the storage subsystem to create volumes based on the trend of the number of VM deployment in the recent past. Each of the volumes has a pre-copied image which is copied from a golden image. The golden image has GUID's zero field as disk provider on boot record, file system, OS image or data image. On deployment, the management server changes a volume size of the created volume to a volume size calculated based on a customer wanted or preset specified data image. If the calculated volume size is larger than the storage system supported size, the management server returns an error notice to the user via GUI (graphical user interface). Regarding volume deployment on the OS, the Windows failover cluster assigns a new GUID instead of zero GUID; if the GUID is duplicated among volumes, the Windows failover cluster keeps a state for a duplicated signature disk as the reserved disk.
[0006] An aspect of the present invention is directed to a method for deploying virtual machines of one or more host computers which are coupled with a storage subsystem via a network, the storage subsystem providing a pool of pre-created virtual volumes in the storage subsystem prior to deploying the virtual machines, the pre-created virtual volumes having pre-copied images for the virtual machines. The method comprises: selecting one of the pre-created virtual volumes for deploying one of the virtual machines; calculating a volume size for the selected virtual volume based on a specified image size for data and OS image; resizing the selected virtual volume according to the calculated volume size; and requesting one of the host computers to deploy the virtual machine using the resized virtual volume.
[0007] In some embodiments, the method further comprises calculating virtual volumes to be added to the pool of pre-created virtual volumes, wherein a number of the pre-created virtual volumes in the pool to be provided per unit time is determined based on a trend of a past number of virtual volumes used in deploying virtual machines per unit time. The method further comprises requesting the storage subsystem to provide the pool of pre-created virtual volumes; and requesting the storage subsystem to copy a virtual machine file to each of the pre-created virtual volumes to produce the pre-copied images for the virtual machines. A golden image is copied to each of the pre-created virtual volumes to produce the pre-copied images for the virtual machines, the golden image including globally unique identifier's zero field as disk provider on boot record, file system, OS image, or data image.
[0008] In specific embodiments, the method further comprises, after resizing the selected virtual volume and before deploying the virtual machine using the resized virtual volume: expanding a target partition of the resized virtual volume based on a calculated partition size which is calculated based on the specified image size for data and OS image; resizing a file system of the resized virtual volume based on a calculated file system size which is calculated based on the specified image size for data and OS image; resizing a previously created virtual machine file for the resized virtual volume based on the specified image size for data and OS image; and creating a new virtual machine file, based on the specified image size for data and OS image, to replace the previously created virtual machine file for the resized virtual volume.
[0009] In some embodiments, the method further comprises, if the calculated volume size is larger than a maximum size supported by the storage subsystem, then returning an error notice to the user. The volume size, calculated based on the specified image size for data and OS image, includes a sum of: size of MBR, size of partition table, VM configuration size, image file size for OS image and data, margin for VM file for OS image and data, and FS margin; wherein MBR is Master Boot Record, VM is Virtual Machine, OS is Operating System, and FS is File System.
[0010] Another aspect of the invention is directed to a management server in an information system for deploying virtual machines of one or more host computers which are coupled with the management server and a storage subsystem via a network, the storage subsystem providing a pool of pre-created virtual volumes in the storage subsystem prior to deploying the virtual machines, the pre-created virtual volumes having pre-copied images for the virtual machines. The management server comprises a processor; a memory; and a volume management module configured to: select one of the pre-created virtual volumes for deploying one of the virtual machines; calculate a volume size for the selected virtual volume based on a specified image size for data and OS image; resize the selected virtual volume according to the calculated volume size; and request one of the host computers to deploy the virtual machine using the resized virtual volume.
[0011] In some embodiments, the management server further comprises an OS images pool management module configured to request the storage subsystem to create virtual volumes to be added to the pool of pre-created virtual volumes, wherein a number of the pre-created virtual volumes in the pool to be provided per unit time is determined based on a trend of a past number of virtual volumes used in deploying virtual machines per unit time. The management server further comprises a golden image creator module configured to request the storage subsystem to provide the pool of pre-created virtual volumes; and request the storage subsystem to copy a virtual machine file to each of the pre-created virtual volumes to produce the pre-copied images for the virtual machines.
[0012] Another aspect of this invention is directed to a computer-readable storage medium storing a plurality of instructions for controlling a data processor to deploy virtual machines of one or more host computers which are coupled with the management server and a storage subsystem via a network, the storage subsystem providing a pool of pre-created virtual volumes in the storage subsystem prior to deploying the virtual machines, the pre-created virtual volumes having pre-copied images for the virtual machines. The plurality of instructions comprise: instructions that cause the data processor to select one of the pre-created virtual volumes for deploying one of the virtual machines; instructions that cause the data processor to calculate a volume size for the selected virtual volume based on a specified image size for data and OS image; instructions that cause the data processor to resize the selected virtual volume according to the calculated volume size; and instructions that cause the data processor to request one of the host computers to deploy the virtual machine using the resized virtual volume.
[0013] These and other features and advantages of the present invention will become apparent to those of ordinary skill in the art in view of the following detailed description of the specific embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] FIG. 1 illustrates an example of a hardware configuration of an information system in which the method and apparatus of the invention may be applied.
[0015] FIG. 2 illustrates an example of a logical configuration of the invention applied to the architecture of FIG. 1 .
[0016] FIG. 3 shows an example of the port configuration table.
[0017] FIG. 4 shows an example of a flow diagram for creating golden image.
[0018] FIG. 5 shows an example of a Master Boot Record.
[0019] FIG. 6 shows an example of a Partition Table.
[0020] FIG. 7 shows an example of a flow diagram to create VM using storage copy capability.
[0021] FIG. 8 shows an example of a flow diagram for VM deployment.
[0022] FIG. 9 shows an example of the volume size of a volume illustrating the relationship between VM files.
[0023] FIG. 10 shows an example of a procedure of volume size check.
[0024] FIG. 11 shows an example of the volume pool management method to provide volumes in the pool continually.
DETAILED DESCRIPTION OF THE INVENTION
[0025] In the following detailed description of the invention, reference is made to the accompanying drawings which form a part of the disclosure, and in which are shown by way of illustration, and not of limitation, exemplary embodiments by which the invention may be practiced. In the drawings, like numerals describe substantially similar components throughout the several views. Further, it should be noted that while the detailed description provides various exemplary embodiments, as described below and as illustrated in the drawings, the present invention is not limited to the embodiments described and illustrated herein, but can extend to other embodiments, as would be known or as would become known to those skilled in the art. Reference in the specification to “one embodiment,” “this embodiment,” or “these embodiments” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention, and the appearances of these phrases in various places in the specification are not necessarily all referring to the same embodiment. Additionally, in the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that these specific details may not all be needed to practice the present invention. In other circumstances, well-known structures, materials, circuits, processes and interfaces have not been described in detail, and/or may be illustrated in block diagram form, so as to not unnecessarily obscure the present invention.
[0026] Furthermore, some portions of the detailed description that follow are presented in terms of algorithms and symbolic representations of operations within a computer. These algorithmic descriptions and symbolic representations are the means used by those skilled in the data processing arts to most effectively convey the essence of their innovations to others skilled in the art. An algorithm is a series of defined steps leading to a desired end state or result. In the present invention, the steps carried out require physical manipulations of tangible quantities for achieving a tangible result. Usually, though not necessarily, these quantities take the form of electrical or magnetic signals or instructions capable of being stored, transferred, combined, compared, and otherwise manipulated. It has proven convenient at times, principally for reasons of common usage, to refer to these signals as bits, values, elements, symbols, characters, terms, numbers, instructions, or the like. It should be borne in mind, however, that all of these and similar terms are to be associated with the appropriate physical quantities and are merely convenient labels applied to these quantities. Unless specifically stated otherwise, as apparent from the following discussion, it is appreciated that throughout the description, discussions utilizing terms such as “processing,” “computing,” “calculating,” “determining,” “displaying,” or the like, can include the actions and processes of a computer system or other information processing device that manipulates and transforms data represented as physical (electronic) quantities within the computer system's registers and memories into other data similarly represented as physical quantities within the computer system's memories or registers or other information storage, transmission or display devices.
[0027] The present invention also relates to an apparatus for performing the operations herein. This apparatus may be specially constructed for the required purposes, or it may include one or more general-purpose computers selectively activated or reconfigured by one or more computer programs. Such computer programs may be stored in a computer-readable storage medium, such as, but not limited to optical disks, magnetic disks, read-only memories, random access memories, solid state devices and drives, or any other types of media suitable for storing electronic information. The algorithms and displays presented herein are not inherently related to any particular computer or other apparatus. Various general-purpose systems may be used with programs and modules in accordance with the teachings herein, or it may prove convenient to construct a more specialized apparatus to perform desired method steps. In addition, the present invention is not described with reference to any particular programming language. It will be appreciated that a variety of programming languages may be used to implement the teachings of the invention as described herein. The instructions of the programming language(s) may be executed by one or more processing devices, e.g., central processing units (CPUs), processors, or controllers.
[0028] Exemplary embodiments of the invention, as will be described in greater detail below, provide apparatuses, methods and computer programs for rapid deployment of virtual machine pooling volume.
[0029] FIG. 1 illustrates an example of a hardware configuration of an information system in which the method and apparatus of the invention may be applied. This system has personal computers (PCs) including a management server 110 and at least one host 130 , and a storage subsystem 140 . The PCs connect to the storage subsystem 140 via a network 260 such as a SAN (Storage Area Network). The SAN is typically a fiber channel network, and hence includes a Fiber Channel Switch and cables. The SAN may use IP network such as iSCSI. In this case, we use Ethernet cables and Ethernet switch as the network switch. The PCs 110 , 130 and storage subsystem 140 are connected by a LAN (Local Area Network) 270 . The LAN uses Ethernet network in this embodiment, and it includes Ethernet switch and cables.
[0030] Each PC 110 , 130 is a general computer, and includes a CPU, a memory, and a disk. It has a Host Bus Adapter (HBA) for storage to connect to the SAN 260 . The HBA has a unique identifier in the form of world wide name (WWN). The PC also has a Network Interface Card (NIC) to connect to the LAN 270 . The NIC has a MAC address.
[0031] The storage subsystem 140 has storage processors (MPs) 160 , disks 143 , memories 170 , ports 180 to connect to the SAN 260 , and SerVice Processor (SVP) 150 . The ports, MPs, disks, and memories are connected by an internal bus 142 . The memory is NVRAM in this embodiment. The port, memory, disk, MP, SVP, and internal bus can be redundant for system reliability. The MP 160 has a CPU, a local memory, and a NIC. Using this NIC, the MP 160 can communicate with the SVP 150 . The SVP 150 has two NICs for an internal LAN 190 and the external LAN 270 , CPU, memory 170 , and disk 143 .
[0032] FIG. 2 illustrates an example of a logical configuration of the invention applied to the architecture of FIG. 1 . The system has a data center management server or simply management server 210 , at least one virtual machine runnable server 230 , and the storage subsystem 240 . The management server may use the PC 110 in FIG. 1 . It has a Web Portal Server (not shown), an OS Images Pool Management module ( 211 ), a Volume Management module 212 , and a Golden Image Creator 213 . The Portal Server represents GUI for the VM administrator or user to create VM and Deploy VM. Based on user's request, the OS Images Pool Management module 211 executes the Deploy Virtual Machine process (Deploy VM process). The Deploy VM process detaches a volume, which is already a copied golden image, from a dummy port, attaches the volume on the host, and discovers the volume on host's OS, and then the VM runnable hypervisor executes the VM on the volume. The golden image is pre-created by a Golden Image Creator 213 based on the schedule of the OS images Pool Management module 211 . An original model of a virtual server image having a specific set of software such as OS and application software is prepared as “Gold Image” first, and then multiple snapshots of the “Golden Image” are created as bases of virtual server images. The details of the modules in FIG. 2 are discussed below.
[0033] On the hosts 230 , there is operating system OS (not shown), hypervisor, and HA (High Availability) software. On the storage subsystem 240 , there is a port configuration table 242 and a virtual volume pool 241 as the configuration information. The storage subsystem 240 may be runnable with Thin Provisioning Technology. Based on the port configuration 242 , the storage subsystem 240 configures a dummy group on one port and a host group on another port. A host group is a group of hosts which have the host's WWNs that may be mapped to volumes. We discuss later how to configure the ports. On the dummy group, there are several volumes which are golden image and target volumes. On the host group, there are several Host attached volumes. The creation of the target volume from the golden image will be discussed below.
[0034] FIG. 3 shows an example of the port configuration table 242 . The port configuration table 242 has columns of Port Number, Host Group Number, Name for the Host Group Number, LUN, and V-VOL (Virtual Volume) number. The port identified by the Port Number corresponds to the physical port 180 . The Host Group Number (i.e., Host Domain Name in Hitachi products) is on each port to make a group of hosts using the host's world wide name (WWN). The host's WWN is provided by the host's HBA's port in order to specify between the host's port connection and the HBA's port connection. LUNs are on a host group. Therefore, each host group has several LUNs. The LUN is connected to volume (VOL). The VOL number is unique within the storage subsystem. The volume number is shared by several LUNs on different ports' host group to ensure keeping multipath configuration for parallel performance and failover among ports.
[0035] FIG. 4 shows an example of a flow diagram for creating golden image. The process is initiated by the GUI provided by the portal server in the management server 210 and executes on the Golden Image Creator module 213 in the management server 210 . The procedure on the management server 210 is described as follows.
[0036] In step 401 , the management server 210 requests the storage subsystem 240 to create VOL. In step 402 , the storage subsystem 240 creates a volume from the storage page pool 241 . In step 403 , the management server 210 requests the storage subsystem 240 to attach LUN to host on the dummy group. In this embodiment, the LUN is attached to host on dummy group. In other embodiments, another group such as the host group in FIG. 2 may be used instead of the dummy group. In step 404 , the storage subsystem 240 attaches VOL to LUN on the dummy group. In step 405 , the management server 210 requests the host 230 to rescan volume. In this embodiment, the hosts 230 are used as creator of the management server 210 . In other embodiments, the management server is also applicable as creator. In step 406 , the management server 210 executes to rescan new disks (term of disk is in OS world name instead of volume) using disk management tools.
[0037] In step 407 , the management server 210 requests a host 230 to bring a disk online. In OS, the term volume is changed to disk. If the volume is initialized, it may initialize the volume as GPT (GUID Partition Table) or MBR (Master Boot Record) volume and also format the file system on the volume. In step 408 , the host 230 executes to bring the disk online. As an example, in Windows, one may bring the disk online using disk management tools. In step 409 , the management server 210 requests the host 230 to mount the disk on a mount point. In step 410 , the host 230 executes to mount the disk on the mount point using, for instance, a mountvol command. In step 411 , the management server 210 copies a Virtual Machine File such as a VHD file to the mounted disk. In step 412 , the host 230 executes a procedure to copy the VHD images to the disk. In step 413 , the management server 210 requests the host 230 to unmount the disk. In step 414 , the host 230 executes to un-mount the disk. In step 415 , the management server 210 requests to initialize signature. In step 416 , the host 230 initializes signature. This embodiment uses zero. Other embodiments may use other initialization data. In step 417 , the management server 210 requests the host 230 to bring the disk offline. In step 418 , the host 230 brings the disk (e.g., diskpart's disk) offline. In step 419 , the management server 210 requests the storage subsystem 240 to change the attribute to read-only for the volume, which prevents access from the host write.
[0038] Regarding the process of initializing signature in step 415 , FIG. 5 shows an example of a Master Boot Record and FIG. 6 shows an example of a Partition Table. The process initializes signature for disk signature on the MBR in the logical block address 0 in FIG. 5 for the MBR formatted volume. Alternatively, the process initializes signature 8B on the Partition Table Header on LBA 1 in the case of GPT (GUID Partition Table) format. This initialization helps the OS to insert a new signature; otherwise, the HA software reserves the volume which has the same signature volume attached on the same host. To prevent modification of the golden image, step 419 protects the volume from host access as well as storage internal copy operation.
[0039] FIG. 7 shows an example of a flow diagram to create VM using storage copy capability. The process is executed on the Volume Management module 212 . In step 701 , the management server 210 requests the storage subsystem 240 to create a volume. In step 702 , the storage subsystem 240 creates a volume from the storage page pool 241 . In step 703 , the management server 210 requests to attach VOL to LUN on the dummy host group. In step 704 , the storage subsystem 240 attaches VOL to LUN on the dummy host group, changing the port configuration table 242 . In step 705 , the management server 210 requests to copy data from the golden image to the created VOL. In step 706 , the storage subsystem 240 executes to copy data from the specified golden image the created VOL.
[0040] FIG. 8 shows an example of a flow diagram for VM deployment. The VM administrator requests OS imaged volume with specified sizes on VM deployment. The Volume Management module 212 , pursuant to received process by the administrator in management software, performs the following steps.
[0041] In step 801 , the management server 210 selects OS imaged volume which the administrator wants to deploy. In step 802 , the management server 210 calculates new volume size based on the user provided or preset VM image size (a.k.a. Image_File_size). The details of this step are discussed below (see FIG.10). The management server 210 requests the storage subsystem 240 to resize the volume. In step 803 , the storage subsystem 240 resizes the volume based on the management server's request. In step 804 , the management server 210 requests the storage subsystem 240 to detach a target volume from the dummy group. In step 805 , the storage subsystem 240 detaches the target volume from the dummy group based on the management server's request. In step 806 , the management server 210 requests the storage subsystem 240 to attach the target volume to the target host group. In step 807 , the storage subsystem 240 attaches the target volume to the target host group.
[0042] In step 808 , the management server 210 requests the host's OS to rescan volume so as to discover the target volume on the host. In step 809 , the host's OS rescans the disk based on the management server's request to discover the new volume. In sequence, this step executes rescan in diskpart operation and inquires the volume's signature using SCSI page 83 to verify the correct number of the volume. In this step, the OS assigns a new signature to replace the signature initialized in step 416 . In step 810 , the management server 210 requests the host's OS to bring the disk online disk. In step 811 , the host's OS brings the disk online disk. In step 812 , the management server 210 requests the host's OS to expand the target partition based on the calculated partition size. The partition size is as follows using the user desired disk size.
[0000]
Partition
size
=
VM_Configuration
_Size
(
903
)
+
Image_File
_Size
(
OS
(
904
)
and
Data
(
908
)
)
+
Margin_For
_VM
_File
(
OS
(
905
)
and
Data
(
909
)
)
…
+
FS_Margin
(
906
)
[0000] The specific Image_File_size is specified by the user from the management server or preset in the management server or provided from the management server before the start of FIG. 8 by the management server.
[0043] In step 813 , the host's OS expand the target partition based requested size. In step 814 , the management server 210 requests the host's OS to mount the file system on the partition. In step 815 , the host's OS mounts the file system on the partition. In step 816 , the management server 210 requests the host's OS to resize the file system based on the calculated file system size ( 907 in FIG. 9 ). The file system size includes data volume space. The filesystem size is as the same as the partition one. In step 817 , the host's OS resizes the file system based on the requested size from the management server 210 . In step 818 , the management server 210 requests the host's hypervisor to resize the previously created VHD file based on the user desired or preset disk size ( 908 in FIG. 9 ). In step 819 , the host's hypervisor resizes the VHD file based on the requested size. In step 820 , the management server 210 requests the host's hypervisor to create a VHD file for data disk based on the user desired or preset disk size ( 908 in FIG. 9 ). The details of the calculation are discussed below. In step 821 , the host's hypervisor creates the VHD file for data disk based on the requested size. In step 822 , the management server 210 requests the host's hypervisor to start the VM. In step 823 , the host's hypervisor executes to start the VM based on the request from the management server 210 .
[0044] Regarding the size of the volume in #2 (the storage administrator discovering the created volume), one should consider the size of the metadata for the file system on volume, for the virtual machine's configuration, and for the file system on the VM. FIG. 9 shows an example of the volume size of a volume illustrating the relationship between VM files. The calculation of the volume size is as follows.
[0000]
Total
size
of
volume
(
900
)
=
Size_Of
_MBR
(
901
)
+
Size_Of
_Partition
Table
(
902
)
+
VM_Configuration
_Size
(
903
)
+
Image_File
_Size
(
OS
(
904
)
and
Data
(
908
)
)
+
Margin_For
_VM
_File
(
OS
(
905
)
and
Data
(
909
)
)
…
+
FS_Margin
(
906
)
[0045] Regarding the margin for VM image ( 905 or 909 ), the size is calculated as some percentage (e.g., 5% as normal file system) of the total sum of the VM Configuration or Config 903 , for allocating the VM Image as Image_File_Size ( 904 for OS image or 908 for data volume). Regarding the margin for the FS (File System) 906 , the size is calculated by some percentage (e.g., 5% as normal file system) of the total sum of all of the VM Config 903 , for allocating the VM Image File ( 904 or 908 ). The VM margin helps to provide over-allocation for the OS's file system metadata. Based on VM's image, the management software calculates the size of volume using the total size of volume ( 900 ). The management software validates the size of volume to prohibit the provision of LUN by the oversize of the storage subsystem supported. If the user requested size or specified preset size is larger than the hardware limitation (e.g., 2TB per volume), the management server 210 should return an error to the user in process S 802 of FIG. 8 .
[0046] FIG. 10 shows an example of a procedure of volume size check. In step 1001 , the management server 210 calculates the size based on the user wanted or preset specific VM Image's filesystem size 900 . The input for the calculation is VM Image's filesystem system (see FIG. 9 ). In step 1002 , the management server 210 checks if the specified volume size is under the storage limitation size for the LU (e.g., 2TB). If yes, the management server 210 continues to step 1004 . If no, the management server 210 returns an error notice to the user in step 1003 . Moreover, if the volume is a thin provisioning volume, the management server 210 inquiries the storage subsystem 240 regarding the total size of allocated total pages, administrator defined maximum capacity of logical unit (this capacity is defined via SVP from administrator), and the threshold to alert the over-provisioning, and it decides if the total size of allocated total pages is under the threshold of administrator defined total capacity or storage vender defined total capacity for thin provisioning in step 1004 . If yes, the management server 210 continues to volume creation. If no, the management server 210 returns an error notice to the user on the failure of volume creation in step 1003 . By this protection, the customer may create their specified size volume considering the hardware limitation and prevent overuse of the pool in thin provisioning. The benefit of volume size management is that the management server user does not have to recalculate the volume size considering the size of file system, partition table, VM configuration file, and image file (user and data), including the size of FS margin.
[0047] Regarding volume pool management, this embodiment should always be ready to provide volumes in the pool. To avoid the situation where the pool is out of available volumes due to a lack of OS imaged volumes, the embodiment manages the pool in an intelligent way. The embodiment presents a method of pool management, especially lower threshold management and hourly creation of VM's number. The OS Images Pool Management module 211 in the management server 210 has a capability to track the total number of deployed volumes and the maximum number of volumes per operation during a certain term (e.g., hourly). Then the OS Images Pool Management module 211 calculates the average number for both numbers.
[0048] FIG. 11 shows an example of the volume pool management method to provide volumes in the pool continually. In this example, the OS Images Pool Management module 211 executes hourly the Create VM process ( FIG. 7 ) using the hourly number of volume by Create VM 1101 in FIG. 11 . If the hourly number of created volume is below the low water marks number, the OS Images Pool Management module 211 tries to execute the Create VM process to prohibit a lack of volumes in the dummy group. In FIG. 11 , the hourly number (40) is higher than the low water marks number (20). Using this management scheme, the pool may continually provide OS imaged volumes based on VM administrator usages, i.e., utilizing customer usage time-based monitoring to prohibit the lack of volumes in the dummy group.
[0049] According to this embodiment, the VM administrator may deploy user wanted or preset specified sized VM volumes shared by several hosts. Moreover, the VM administrator may improve the availability of the volume pool based on the usage of VM deployment.
[0050] Of course, the system configurations illustrated in FIGS. 1 and 2 are purely exemplary of information systems in which the present invention may be implemented, and the invention is not limited to a particular hardware configuration. The computers and storage systems implementing the invention can also have known I/O devices (e.g., CD and DVD drives, floppy disk drives, hard drives, etc.) which can store and read the modules, programs and data structures used to implement the above-described invention. These modules, programs and data structures can be encoded on such computer-readable media. For example, the data structures of the invention can be stored on computer-readable media independently of one or more computer-readable media on which reside the programs used in the invention. The components of the system can be interconnected by any form or medium of digital data communication, e.g., a communication network. Examples of communication networks include local area networks, wide area networks, e.g., the Internet, wireless networks, storage area networks, and the like.
[0051] In the description, numerous details are set forth for purposes of explanation in order to provide a thorough understanding of the present invention. However, it will be apparent to one skilled in the art that not all of these specific details are required in order to practice the present invention. It is also noted that the invention may be described as a process, which is usually depicted as a flowchart, a flow diagram, a structure diagram, or a block diagram. Although a flowchart may describe the operations as a sequential process, many of the operations can be performed in parallel or concurrently. In addition, the order of the operations may be rearranged.
[0052] As is known in the art, the operations described above can be performed by hardware, software, or some combination of software and hardware. Various aspects of embodiments of the invention may be implemented using circuits and logic devices (hardware), while other aspects may be implemented using instructions stored on a machine-readable medium (software), which if executed by a processor, would cause the processor to perform a method to carry out embodiments of the invention. Furthermore, some embodiments of the invention may be performed solely in hardware, whereas other embodiments may be performed solely in software. Moreover, the various functions described can be performed in a single unit, or can be spread across a number of components in any number of ways. When performed by software, the methods may be executed by a processor, such as a general purpose computer, based on instructions stored on a computer-readable medium. If desired, the instructions can be stored on the medium in a compressed and/or encrypted format.
[0053] From the foregoing, it will be apparent that the invention provides methods, apparatuses and programs stored on computer readable media for rapid deployment of virtual machine pooling volume. Additionally, while specific embodiments have been illustrated and described in this specification, those of ordinary skill in the art appreciate that any arrangement that is calculated to achieve the same purpose may be substituted for the specific embodiments disclosed. This disclosure is intended to cover any and all adaptations or variations of the present invention, and it is to be understood that the terms used in the following claims should not be construed to limit the invention to the specific embodiments disclosed in the specification. Rather, the scope of the invention is to be determined entirely by the following claims, which are to be construed in accordance with the established doctrines of claim interpretation, along with the full range of equivalents to which such claims are entitled. | Exemplary embodiments provide rapid creation and deployment of virtual machines by reducing communication processes between virtual machine user and storage and server administrators. One embodiment is a method for deploying virtual machines of host computers. A storage subsystem provides a pool of pre-created virtual volumes in the storage subsystem prior to deploying the virtual machines, the pre-created virtual volumes having pre-copied images for the virtual machines. The method comprises: selecting one of the pre-created virtual volumes for deploying one of the virtual machines; calculating a volume size for the selected virtual volume based on a specified image size for data and OS image; resizing the selected virtual volume according to the calculated volume size; and requesting one of the host computers to deploy the virtual machine using the resized virtual volume. | 7 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of Invention
[0002] The present invention generally relates to the field of RFID communication systems, and more particularly, to a system and method for detecting an object within an RFID communication system.
[0003] 2. Description of Related Art
[0004] In, for example, retail establishments, it is desirable to know whether objects or persons are passing through portals or close to portals being monitored by RFID transceivers. For example, it is desirable to know whether an object or person is present in the region of an entrance or exit of a retail establishment, and whether an object or person is present in the region of any opening or openings between a frontstore and a backstore where inventory is stored. Additionally, it is desirable to know whether an object or person is present in the region of any loading docks, or other types of portals for bringing inventory into or out of the retail establishment. Furthermore, it is desirable to know whether an object or person is in motion toward or away from any of the forgoing regions, even if the object or person is not in the immediate region.
[0005] It was known in the prior art to use infrared sources and detectors for monitoring the foregoing regions. Infrared detectors used in this manner could detect the motion of an object or person moving either toward or away from a portal. The infrared detectors could provide a detection signal when the motion was detected. Additionally, it was known to use a detection signal from an infrared detector to activate a radar transmission in order to permit further monitoring of the region. The doppler shifts of the radar transmission could then provide further information on the motion in the vicinity of the portal being monitored. Additionally, it was common to use well known light barrier devices to monitor the vicinity of portals. The light barriers could provide a detection signal when an object or person passing through the portal broke a light beam.
[0006] However, the known methods for detecting motion around the RFID transceivers required that a specialized, dedicated device be added to the RFID transceivers. Even the addition of a simple detection device such as an infrared detector or a light barrier added some size and cost to the RFID transceivers. The requirement for additional space for monitoring regions such as the regions around portals is especially problematic in retail applications that have limited and very expensive retail space.
[0007] For example, U.S. Pat. No. 7,023,341 B2 issued to Stilp teaches an RFID reader for detecting motion using doppler in a security network. The RFID reader sent and received RF signals, and measured the reflected pulses relative to the transmitted pulses. Many doppler systems like the one taught by Stilp could easily detect a person walking at a normal speed. The system disclosed by Stilp could also alter the power of its doppler transmissions. By varying the transmission power, the detection range of the RFID readers could be varied. The doppler motion detection in Stilp was performed simultaneously with searching for transponders using conventional tag interrogation techniques.
[0008] U.S. Patent Pub. No. 2008/0318684 A1 by Rofougaran teaches RF position locating in a video gaming system. The teachings in Rofougaran include sweeping an area with RF signals of several different frequency bands, and determining the physical layout of the environment based on reflected, absorbed and refracted signals, angle of incidence and backscatter of the swept signals. The distance to the player, the other objects in the room, the ceiling, the floor, the walls, etc. were determined from the received signals and stored for use during a game. Monitoring of the movements of the player thereafter during the game depended on the player wearing a gaming object.
[0009] U.S. Patent Pub. No. US2008/0001735 A1 by Tran is of general interest for teaching determining when a person passes through a door using a combination of different devices. Tran teaches using radar doppler shift of an RF signal reflected off the person. Tran also teaches using ultrasonic devices and photosensors. The results of the determinations made using the different devices could be combined to distinguish ranges.
[0010] U.S. Pat. No. 5,030,941 issued to Lizzi also teaches a number of different auxiliary detectors for detecting motion near or through RFID portals. The use of photoelectric sensors, body heat sensors and floor switches are taught by Lizzi.
[0011] However, the use of the auxiliary sensors taught by Lizzi, as well as the other systems set forth above, all require a specialized, dedicated device to be added to the RFID transceivers in order to detect the presence or motion of objects or persons in the vicinity of a RFID transceiver monitoring a portal. This increases the size and costs of the RFID transceiver.
[0012] All references cited herein are incorporated herein by reference in their entireties.
BRIEF SUMMARY OF THE INVENTION
[0013] An RFID reader includes a transceiver configured to receive a first radio frequency signal reflected off at least one surface to provide baseline signal information and a second radio frequency signal reflected off the at least one surface and an object to provide further signal information. A comparator is configured to compare the baseline signal information and the further signal information to provide a signal comparison. A processor is configured to detect the presence of the object in accordance with the signal comparison. A determination is made whether the object is in motion in accordance with the signal comparison. The determination whether the object is in motion is made in accordance with a continuous fluctuation of the second radio frequency signal. A determination whether the object is no longer in motion is made in accordance with an ending of the continuous fluctuation of the second radio frequency signal.
[0014] At least one of the first and second radio frequency signals is a simulated electronic product code signal. The comparator is configured to compare received signal strengths. A received signal strength of the first radio frequency signal includes a first sum of signal strengths of a plurality of component signals received by the RFID receiver. A received signal strength of the second radio frequency signal comprises a second sum of signal strengths equal to the first sum of signal strengths and at least one additional signal strength corresponding to a radio frequency signal reflected off the object.
[0015] The comparator is configured to compare a received signal strength of at least one of the first and second radio frequency signals in accordance with a plurality of time samples. The comparator is configured to compare signal phase information. A determination of a signal phase of at least one of the first and second radio frequency signals is made in accordance with a plurality of time samples.
[0016] A tag inventory is performed by the RFID reader. The first radio frequency signal includes a signal with a power level of approximately 30 dBm and the second radio frequency signal includes a signal with a power level less than approximately -5 dBm. The signal comparing and the plurality of tag inventories are interleaved.
[0017] In another embodiment of the invention, a method for detecting the presence of an object having at least one surface in a monitored region in an RFID communication system includes receiving a first radio frequency signal reflected off the at least one surface to provide baseline signal information. The method also includes receiving a second radio frequency signal reflected off the at least one surface and the object to provide further signal information. The baseline signal information and the further signal information are compared to provide a signal comparison. The presence of the object can be detected in accordance with the signal comparison.
[0018] A determination is made whether the object is in motion in accordance with the signal comparison. A determination is made whether the object is in motion in accordance with a continuous fluctuation of the second radio frequency signal. A determination is made whether the object is no longer in motion in accordance with an ending of the continuous fluctuation of the second radio frequency signal.
[0019] At least one of the first and second radio frequency signals is a simulated electronic product code signal. The comparing is a comparing of received signal strengths. A radio signal strength of the first radio frequency signal is a first sum of signal strengths of a plurality of component signals received by an RFID receiver. A radio signal strength of the second radio frequency signal is a second sum of signal strengths equal to the first sum of signal strengths and at least one additional signal strength corresponding to a signal reflected off the object. A received signal strength of at least one of the first and second radio frequency signals is determined in accordance with a plurality of time samples. The comparing is a comparing of signal phase information. A signal phase of at least one of the first and second radio frequency signals is determined in accordance with a plurality of time samples.
[0020] A tag inventory is performed. The first radio frequency signal can be a signal with a power level of approximately 30 dBm and the second radio frequency signal can be a signal with a power level less than approximately −5 dBm. The detecting is interleaved with a plurality of tag inventories.
[0021] The RFID communication system includes a marker tag and the baseline signal information is determined in accordance with the marker tag to provide marker baseline information. The presence of the object is determined in accordance with the marker baseline information. A distance to the object is determined in accordance with the signal comparison. A threshold received signal strength is determined and the distance to the object is determined in accordance with the threshold received signal strength.
[0022] In the RF background object sensing system and method of the invention, a simulated Electronic Product Code (EPC) signal can be transmitted by an RFID transceiver in order to assist in detecting an object or a person that is present in the region of the RFID transceiver. Any radio frequency signal whatsoever can be transmitted by the RFID transceiver and reflected off the object in order to detect the presence of the object. However, the electronic product code signal is preferred because the RFID transceiver is well adapted to detect the signal, and can therefore detect simulated electronic product code signals reflected off the object or person very easily.
[0023] The RF background object sensing system can collect and store information regarding RF reflections of the transmitted simulated electronic product code signal when it is known that no objects or persons to be monitored are in the region of the RFID transceiver. The reflections of the simulated electronic product code signal under these circumstances can depend on the configuration of the surroundings of the transceiver, such as the walls, the ceilings, the floors, any shelves or support beams, etc. This information can be stored as background signal information, or baseline signal information, for later comparisons.
[0024] The simulated electronic product code signal can also be transmitted by the RFID transceiver while the system and method of the invention is monitoring the region of the transceiver for the presence or motion of objects or persons. The simulated electronic product code signal reflects off any object or person moving into the monitored region, thereby providing further signal information. The further signal information regarding the reflections of the transmitted electronic product code signal off the object can be collected while the system of the invention is monitoring the region of the RFID transceiver.
[0025] The further signal information is compared with the baseline signal information that was collected and stored when it was known that no object or person to be monitored was present in the region of the transceiver. Fluctuations between the baseline signal information and the signal information read during monitoring for the presence of an object can indicate the presence of an object. Therefore, based on the comparison of the stored baseline signal information and the further signal information by the system detection logic, a determination can be made whether an object has appeared in the vicinity of the transceiver. If the presence of an object is detected according to the comparison, the transceiver can generate a detection signal. Furthermore, the comparison of further signal information with the baseline signal information can be used to determine whether the object is in motion.
BRIEF DESCRIPTION OF SEVERAL VIEWS OF THE DRAWINGS
[0026] The invention will be described in conjunction with the following drawings in which like reference numerals designate like elements and wherein:
[0027] FIG. 1 shows a schematic representation of an embodiment of a background object sensing system and method according to the present invention.
[0028] FIG. 2 shows a schematic representation of an alternate embodiment of the background object sensing system and method of FIG. 1 .
[0029] FIG. 3 shows a graphical representation of received signal strengths within the system and method of FIG. 1 .
[0030] FIG. 4 shows a graphical representation of received phase shift information within the system and method of FIG. 1 .
DETAILED DESCRIPTION OF THE INVENTION
[0031] Referring now to FIG. 1 , there is shown a schematic representation of an embodiment of the background object sensing system 10 of the present invention, as viewed looking horizontally into a portal. The background object sensing system 10 includes an RFID receiver 16 mounted on a pedestal 12 and an RFID transmitter 18 mounted on a pedestal 14 . The RFID transmitter 18 and RFID receiver 16 can be parts of any known RFID transceiver system. Therefore, while the invention is described with respect to pedestal mounted transmitters and receivers for illustrative purposes, it will be understood that the invention can be practiced using overhead transceiver devices or any other types of transceiver devices. When the RFID transmitter 18 transmits a radio frequency signal it can be received by the RFID receiver 16 . For example, the radio frequency signal 24 transmitted from the RFID transmitter 18 can follow the direct line of sight path to the RFID receiver 16 . The complex attenuation of the radio frequency signal 24 as it travels to the RFID receiver 16 is α 2 .
[0032] The background object sensing system 10 can be located at any area or region where monitoring for the presence of RFID tags is desired. Additionally, it can be located at any area or region where monitoring for the presence or an object of objects or persons is desired, either simultaneously or alternately with the monitoring for RFID tags. For example, it can be placed in the region of the exit or exits of retail establishments, and in the region of the opening or openings between a frontstore and a backstore where the inventory of the retail establishment is stored. It can also be located in the region of any loading docks, or any other types of portals for bringing inventory into or out of the establishment.
[0033] It will be understood by those skilled in the art that the radio frequency signals transmitted by the RFID transmitter 18 can reflect off the surfaces of any objects, floors, walls, ceilings, etc. in the monitored region of the background object sensing system 10 . Furthermore, the RFID receiver 16 can receive all of the reflected signals from the RFID transmitter 18 . Therefore, the RFID receiver 16 can receive multicomponent signals y(t) when the RFID transmitter 18 transmits a signal, wherein each component of y(t) can correspond to one of the surfaces that the transmitted signal bounces off. The multicomponent signal y(t) received by the RFID receiver 16 can be expressed in Eqn. 1 as:
[0000]
y
(
t
)
=
ℜ
[
∑
i
=
1
N
t
α
i
,
t
s
i
(
t
)
j
2
π
f
t
]
(
Eqn
.
1
)
[0000] in the case where the multicomponent signal y(t) has N t components. Since there can be different numbers of multipath components over time N t , is a function of time. The complex attenuation factor of Eqn. 1 can be denoted α i,t if it depends on time.
[0034] In order to detect an object, the multicomponent signal y(t) of Eqn. 1 can be sampled over a period of time. For example, n samples of the multicomponent signal y(t) can be taken, and the received signal strengths, or the amplitudes, can be determined for each of the n samples. The amplitudes of the n samples of the multicomponent signal y(t) can be expressed for each value of time from t 1 to t n as shown in Eqn. 2:
[0000] R A =[|y ( t 1 )|, | y ( t 2 )|, | y ( t 3 )|, . . . | y ( t n )|] (Eqn. 2)
[0035] In addition to determining the signal strength of the samples of the multicomponent signal y(t), it is possible to determine the phase angle information of the received signal y(t) over n samples. The phase samples ∠y(t i ) can be determined for each of the n values of time from time t=t 1 to time t=t n as shown in Eqn. 3:
[0000] R P =[∠y ( t 1 ), ∠ y ( t 2 ), ∠ y ( t 3 ), . . . ∠ y ( t n )] (Eqn. 3)
[0036] Therefore, when no objects or persons to be monitored are in the monitored region of the background object sensing system 10 , Eqns. 1-3 can be used to determine background signal information, or baseline signal information, of the background object sensing system 10 for later comparisons. Furthermore, any other parameters that can be measured by the background object sensing system 10 , in addition to received signal strength and phase angle, can be determined when no objects or persons to be monitored are in the region for later comparison. Fluctuations between the baseline signal information and further signal information read during monitoring for the presence of an object can indicate the presence of an object.
[0037] Additionally, an object 32 can be disposed in the monitored region of the background object sensing system 10 . A radio frequency signal 28 can be transmitted from the RFID transmitter 18 , reflected off the surface of the object 32 , and received by the RFID receiver 16 . The reflected radio frequency signal 28 can have a complex attenuation α 1 . Furthermore, the object 32 in the region of the background object sensing system 10 can move in any direction, including movement in three dimensions. One possible direction of movement for the object 32 is indicated by the dotted arrow 34 . If the object 32 is moving, the attenuation of the radio frequency signal 28 is a complex function of time, α 1,t .
[0038] Assuming that no other objects are in the region of the background object sensing system 10 to reflect radio frequency signals from the RFID transmitter 18 to the RFID receiver 16 , the multicomponent signal y(t) received by the RFID receiver 16 has two components, given as:
[0000] y ( t )= [α 1,t s ( t ) e j2πft +α 2 s ( t ) e j2πft ]. (Eqn. 4)
[0039] In Eqn. 4 the term α i,t s(t)e j2πft represents the component of the multicomponent signal y(t) due to the radio frequency signal 28 reflecting off the surface of the moving object 32 , and α 1,t changes as a function of time. The term α 2 s(t)e j2πft represents the component of the multicomponent signal y(t) due to the direct line of sight radio frequency signal 24 , and α 2 does not change as a function of time.
[0040] Referring now to FIG. 2 , there is shown a background object sensing system 20 . The background object sensing system 20 is an alternate embodiment of the background object sensing system 10 . The background object sensing system 20 includes the RFID transmitter 18 and the RFID receiver 16 as previously described with respect to the background object sensing system 10 . It also includes the line of sight radio frequency signal 24 and the reflected radio frequency signal 28 , which reflects off the moving object 32 , as previously described.
[0041] However, in the background object sensing system 20 the RFID transmitter 18 also transmits reflected radio frequency signals 26 , 30 . The radio frequency signal 26 reflects off a static object 36 , and is received by the RFID receiver 16 . The attenuation of the radio frequency signal 26 is α 3 . The radio frequency signal 30 reflects off a static object 38 , and is received by the RFID receiver 16 . The attenuation of the radio frequency signal 30 is α 4 . Since the objects 36 , 38 which reflect the radio frequency signals 26 , 30 are static, the attenuations α 3 and α 4 , respectively, are not functions of time.
[0042] Under these circumstances, the multicomponent signal y(t) received by the RFID receiver 16 can be expressed in Eqn. 5 as:
[0000]
y
(
t
)
=
ℜ
[
α
1
,
t
s
i
(
t
)
j
2
π
f
t
+
∑
i
=
2
4
α
i
s
i
(
t
)
j
2
π
f
t
]
(
Eqn
.
5
)
[0000] where the term α 1,t s i (t)e j2πft represents the component of the multicomponent signal y(t) due to the radio frequency signal 28 reflecting off the moving object 32 , and the term α i s i (t)e j2πft represents the static components due to the radio frequency signals 24 , 28 , 30 , as i=2 to 4.
[0043] The radio frequency signals generated by the RED transmitter 18 and used for monitoring an area for an object 32 can be transmitted at a very low energy level. Any type of transmitted signal can be used. However, RFID readers are usually designed to decode electronic product code signals, and commonly available RFID readers are well adapted to decode the electronic product code signals. Therefore, the use of simulated electronic product code signals is preferred when performing the method of the invention because no redesign of the RFID readers is required when electronic product code signals are used.
[0044] In one preferred embodiment of the invention, the radio frequency signals used can be less than approximately −5 dBm. Furthermore, they can be transmitted approximately ten times per second, where each transmission can take approximately two milliseconds. Therefore, the duty cycle of the signals can be less than two percent. This is very advantageous because the use of such low transmit power levels minimizes the amount of interference with any other RFID devices that may be nearby.
[0045] In one preferred embodiment, the background object sensing system 20 can detect whether the object 32 is relatively farther away from the portal being monitored, or relatively closer to or within the portal being monitored. In order to determine the distance to the object 32 , different detection thresholds can be provided for the detection logic of the system 20 . The background object sensing system 20 can use a relatively lower detection threshold in order to permit the triggering of an object detection event based on small variations in received radio frequency energy levels. This can permit the detection of an object 32 outside of, or a distance away from, the portal being monitored, depending on how low the detection threshold is set. This type of detection can replace many of the currently available doppler radar sensors. Furthermore, the detection threshold, as well as the energy level of the transmission, can be varied up and down in order to vary the range of detection and localize the object 32 with more accuracy.
[0046] Additionally, the background object sensing system 20 can also use a relatively higher detection threshold, in order to permit the triggering of an object detection event based on relatively larger variations in received radio frequency energy levels. This can permit the detection of an object 32 closer to or inside the portal being monitored, depending on how high the threshold is set. This type of detection can replace many of the currently available light barriers. It will be understood that the relatively lower and relatively higher detection thresholds can be set for any parameters that can be measured by the background object sensing system 20 , including the received signal strength and the phase angle.
[0047] In another preferred embodiment, the background object sensing system 20 can have two modes of operations. The two modes can include the object sensing mode of the invention, in which an object within a monitored region can be detected, and an RFID tag inventory mode. In the RFID tag inventory mode the RFID transmitter 18 transmits a request for RFID tag identifications. The RFID tags within range of the transmission respond by backscattering their electronic product code. The RFID receiver 16 receives the backscattered electronic product code responses, and thereby determines the population of RFID tags within the range of the RFID transmitter 18 and the RFID receiver 16 . A typical power level for transmission of the radio frequency signals in the RFID tag inventory mode can be, for example, 30 dBm.
[0048] When the background object sensing system 20 is not in the RFID tag inventory mode it can enter the object sensing mode. In the object sensing mode, the background object sensing system 20 can reduce the RF power level from a typical value of 30 dBm for the inventory mode, to a much lower value, for example a value in the vicinity of −5 dBm. If the background object sensing system 20 is a multichannel system, the simulated electronic product code can be transmitted and received at the low power level by any one of the transmitter and receiver channels. When an object 32 is detected or another tag inventory is scheduled, the reader can return to the RFID tag inventory mode and perform another inventory round.
[0049] Furthermore, in another preferred embodiment of the invention, the background object sensing system 20 can perform both object sensing and inventory rounds, continuously. One way to accomplish this is to interleave the low power simulated electronic product code object sensing rounds with the normal inventory rounds. For example, one round of normal inventory at approximately 30 dBm can be followed by one round of low power object sensing using a simulated electronic product code at approximately −5 dBm. The round of low power object sensing can then be followed by a round of inventory, etc. This can result in a small drop in the throughput of the inventory operations, since a portion of the time of the system 20 is taken for the object sensing operations rather than for tag inventory. In a typical situation the drop in inventory throughput may be on the order of approximately 0.6% when background object sensing is performed.
[0050] Another way to perform both object sensing and inventory rounds continuously is to place an extra tag, a marker tag, on a surface in the region to be monitored for the presence of an object 32 . For example, the marker tag can be placed in the vicinity of the exit or exits of retail establishments, in the vicinity of the opening or openings between a frontstore and a backstore, or in the vicinity of any loading docks or other types of portals for bringing inventory into or out of the establishment. The baseline signal information of the marker tag can be determined by reflecting simulated electronic product code signals or other signals off the marker tag and any other static surfaces around the marker tag, when it is known that no objects 32 to be monitored are in the vicinity of the marker tag, as previously described. The marker baseline signal information obtained in this manner can be saved for later comparisons.
[0051] During normal inventory rounds, the response of the marker tag can be read in the same manner as any of the tags being inventoried. The readings of the response from the marker tag can be compared with the baseline signal information of the marker tag. Fluctuations between the baseline signal information of the marker tag and further signal information read from the marker during monitoring can indicate the presence of an object 32 . Because there is one additional tag to be read, beyond the tags being inventoried, there may be a small drop in throughput of the inventorying process using this method for detecting the presence of an object 32 in the region of the marker tag. The drop can be approximately the same as described above.
[0052] Referring now to FIG. 3 , there is shown a graphical representation 50 . The graphical representation 50 shows the received signal strength of the multicomponent signal y(t) received by the RFID receiver 16 within the background object sensing systems 10 , 20 , as a function of time. The radio signal strength of a signal transmitted by the RFID transmitter 18 can be calculated, for example, by Eqn. 2 above. This signal can represent the sum of signals reflected off any number of stationary objects such as walls, floors, ceilings, shelves, etc. From time t=0 until time t=t m there are no objects 32 to be monitored in the region of the RFID receiver 16 . Therefore, the values of the received signal strength from time t=0 to time t=t m remain constant at the steady state value R A . Therefore, the value R A can represent the baseline signal information of the monitored region of the RFID receiver 16 .
[0053] At time t=t m , an object such as the object 32 is present in the region of the RFID receiver 16 . This is indicated by the value of the received signal strength fluctuating from R A beginning at time t=t m . The simulated electronic product code signal transmitted by the RFID transmitter 18 reflects off the object 32 , and follows a path to the RFID receiver 16 , such as the path followed by the radio frequency signal 28 in FIG. 1 . Therefore, the value of received signal strength received by the RFID receiver 16 fluctuates from R A when the object 32 is in the region of the background object sensing system 20 .
[0054] Thus, the object 32 in the region of the RFID transmitter 18 can be detected by the background object sensing system 20 according to the monitored value of the received signal strength. Specifically, the presence of the object 32 can be detected when the value of the received signal strength varies from the steady state value R A . A detection signal indicating a detection event can be generated by the background object sensing system 20 in response to the variation in the received signal strength.
[0055] Furthermore, the background object sensing system 20 can distinguish between a case in which an object 32 continues moving after entering the region of the receiver 16 , and a case in which the object 32 stops moving after entering the region. If the object 32 detected by the background object sensing system 20 continues to move after entering the monitored region, the received signal strength can continue fluctuating, as shown by the continuous fluctuation in the graphical representation 50 in the period after time t=t m . The continuous fluctuation of the received signal strength can last as long as the object 32 continues moving through the region. If the object 32 stops moving after entering the region and remains stationary in the region, the received signal strength can reach a new steady state value, different from R A . Additionally, if the object 32 continues to move until it leaves the monitored region, the value of the received signal strength can return to the steady state value R A .
[0056] Referring now to FIG. 4 , there is shown a graphical representation 60 . The graphical representation 60 shows the phase shift information of the multicomponent signal y(t) received by the RFID receiver 16 within the background object sensing systems 10 , 20 , as a function of time. The phase shift information of a signal transmitted by the RFID transmitter 18 can be calculated, for example, by Eqn. 3 above. This signal can represent the sum of signals reflected off any number of stationary objects such as walls, floors, ceilings, shelves, etc. From time t=0 until time t=t m there are no objects 32 to be monitored in the region of the RFID receiver 16 . Therefore, the values of the phase shift information from time t=0 to time t=t m remain constant at the steady state value R P . Therefore, the value R P represents the baseline phase shift information of the region of the RFID receiver 16 .
[0057] At time t=t m , an object such as the object 32 is present in the region of the RFID receiver 16 . This is indicated by the value of the phase shift information fluctuating from R P beginning at time t=t m . The value of phase shift information fluctuates from R P when the object 32 is in the region of the RFID receiver 16 . It fluctuates because the electronic product code signal transmitted by the RFID transmitter 18 reflects off the object 32 , and follows a path to the RFID receiver 16 , such as the path followed by the radio frequency signal 28 in FIG. 1 .
[0058] Thus, the object 32 in the region of the RFID transmitter 18 can be detected by the background object sensing system 20 according to the monitored values of the phase shift information. Specifically, the presence of the object 32 can be detected when the value of the phase shift information varies from the steady state value R P . A detection signal indicating a detection event can be generated by the background object sensing system 20 in response to the variation in the phase shift information.
[0059] Furthermore, using the phase shift information the background object sensing system 20 can distinguish between a case in which an object 32 continues moving after entering the region of the receiver 16 , and a case in which the object 32 stops moving after entering the region. If the object 32 detected by the background object sensing system 20 continues to move after entering the region, the phase shift information can continue fluctuating, as shown by the continuous fluctuation in the graphical representation 60 in the period after time t=t m . The continuous fluctuation of the phase shift information can last as long as the object 32 continues moving. If the object 32 stops moving after entering the region and remains stationary in the region, the phase shift information can reach a new steady state value, different from R P . Additionally, if the object 32 continues to move until it leaves the monitored region, the value of the phase shift information can return to the steady state value R P .
[0060] In another embodiment, the RFID receiver 16 can detect and identify individual tags according to the received electronic product code signals of the tags, for example during an inventory round, as known in the art. Additionally, the RFID reader 16 can repeatedly detect and identify the same individual tags, for example during subsequent inventory rounds. Furthermore, the received signal strength and/or phase information associated with each tag can be determined according to Eqns. 2 & 3, above, and stored each time it is detected. Therefore, for each individual identified tag the stored information can be analyzed in order to determine whether it changes over time.
[0061] If the stored readings of signal strength and/or phase information of an individual tag change over time, a determination can be made that the tag is moving. If the information does not change over time a determination can be made that the tag is not moving. If a tag is determined to be moving in this manner, the RFID reader 16 can continue to interrogate the tag and monitor the received signal strength and/or phase information from the tag in order to monitor its movement. The interrogation can continue until the tag is no longer detected or until the movement of the tag stops.
[0062] The operations of the background object sensing systems 10 , 20 may be implemented in the form of a processing system, or in the form of software executed in a computer processor system. The computer processor system may be located within the RFID reader 16 . Furthermore, the processor system may be implemented by any type of computer system. The processor system may be equipped with a display or monitor, a microprocessor, memories and/or internal or external communications devices (e.g., modem, network cards, etc.) and optional input devices (e.g., a keyboard, mouse or other input device) and wireless devices. Computer program instructions for causing the processor system to implement the operations of the background object sensing systems 10 , 20 may be stored on any recordable medium, e.g., RAM, ROM, magnetic, optical, floppy, DVD, CD, etc.
[0063] The computer program instructions may be stored in a computer readable medium that can direct a computer, other programmable data processing apparatus, or other devices to function in a particular manner. The instructions stored in the computer readable medium can configure the processor to control RFID reader transmit and receive functions, to perform calculations on electronic signals representing radio frequency waves, such as calculations to determine received signal strength and phase information.
[0064] Furthermore, the instructions can configure the processor to perform comparator operations for comparing any parameters within the RFID reader 16 , such as received signal strength and phase information, and to detect an object in the vicinity of the reader 16 based on the comparison. The computer program instructions may also be loaded onto a computer, other programmable data processing apparatus, or other devices to cause a series of operation steps to be performed on the computer, other programmable apparatus or other devices to produce a computer implemented process.
[0065] A processing system suitable for storing and/or executing program code to perform the foregoing operations may be implemented by any conventional or other computer or processing systems. The computer or processing systems may be equipped with a display or monitor and a base, e.g., including the processor, memories and/or internal or external communications. The systems can also include at least one processor coupled directly or indirectly to memory elements through a system bus. The memory elements can include local memory employed during actual execution of the program code, bulk storage, cache memories and any other kind of memories known to those skilled in the art.
[0066] While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof. | An RFD reader includes a transceiver configured to receive a first radio frequency signal reflected off at least one surface to provide baseline signal information and a second radio frequency signal reflected off the at least one surface and an object to provide further signal information. A comparator is configured to compare the baseline signal information and the further signal information to provide a signal comparison. A processor is configured to detect the presence of the object in accordance with the signal comparison. A determination is made whether the object is in motion in accordance with the signal comparison. The determination whether the object is in motion is made in accordance with a continuous fluctuation of the second radio frequency signal. A determination whether the object is no longer in motion is made in accordance with an ending of the continuous fluctuation of the second radio frequency signal. | 6 |
CROSS REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuation of Ser. No. 11/538,956, filed Oct. 5, 2006, entitled “Remote Control Pool Skimmer”, which claims the benefit of U.S. Provisional Application No. 60/731,575, filed Oct. 28, 2005, entitled “Remote Control Pool Skimmer”, both of which are hereby incorporated by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] The present invention relates in general to swimming pool skimmers that are constructed and arranged to collect surface debris from a swimming pool or similar body of water. More specifically, the present invention relates to a remote controlled swimming pool skimmer.
[0003] Swimming pool skimmers have been in use for a number of years as one way to remove surface debris from a body of water. When swimming pools are exposed to nearby deciduous trees and similar vegetation that has a tendency to discharge leaves, seedlings, and other debris, these items can fall into the swimming pool or can be swept into the swimming pool by wind. If not removed promptly, these items of debris typically sink to the bottom of the pool. Debris on the bottom of the pool is more difficult to remove and if not removed, may interfere with the swimming pool filtering system. In the simplest form, such surface debris can be removed from the pool by a net at the end of a long pole. However, this particular approach requires some degree of strength and coordination and constitutes an unpopular chore. While swimming pool services can perform this task for the owners, that comes at an added cost.
[0004] There have been proposals in the past for automatic pool skimmers having some type of buoyant vessel supporting a porous basket. These structures are specifically designed for collecting leaves and other surface debris as the skimmer is propelled through the water, skimming across the surface of the water. However, many of these earlier devices have the disadvantage of having to free themselves when they go into the side of the pool. In addition, some of these prior devices present cumbersome and awkward structural arrangements for removing debris and/or the porous basket.
[0005] While the present invention is described in the context of a swimming pool, the problems and issues described above also exist, at least to some degree, for small man-made lakes and other similar bodies of water where the debris falls along the shoreline. Accordingly, the present invention is directed to providing certain improvements and benefits for such automatic pool skimmers in the form of a device that is remotely controlled, providing another advantage and convenience to the user.
BRIEF SUMMARY
[0006] A remote control pool skimmer for picking up surface debris, according to one embodiment of the present invention, comprises a pair of elongated buoyant hulls spaced from one another, each hull having a bow and a stern, and at least one cross member interconnecting the hulls to one another, a remotely controlled drive system cooperating with the pool skimmer for moving the hulls through the water in a given direction and a collection net spanning the space between the pair of hulls, the net being oriented in order to collect surface debris as the hulls move through the water. In terms of weight distribution from bow to stern, the hulls are weighted non-linearly more toward the stern.
[0007] One object of the present invention is to provide an improved remote control pool skimmer.
[0008] Related objects and advantages of the present invention will be apparent from the following description.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0009] FIG. 1 is a starboard side elevational view of a pool skimmer.
[0010] FIG. 2 is a top plan view of the pool skimmer in FIG. 1 showing a debris collecting net in place.
[0011] FIG. 3 is a front elevational view of the pool skimmer of FIG. 1 .
[0012] FIG. 4 is a rear elevational view of the pool skimmer of FIG. 1
[0013] FIG. 4A is a partial, fragmentary, perspective view of one pontoon with alternative weighting.
[0014] FIG. 5 is a front elevational view of the pool skimmer of FIG. 1 with the debris collecting net removed.
[0015] FIG. 6 is a perspective view of the skimmer of FIG. 1 , showing the debris collecting net in the process of being removed from the pool skimmer.
[0016] FIG. 7 is an exploded view of the FIG. 1 pool skimmer.
DETAILED DESCRIPTION
[0017] For the purposes of promoting an understanding of the principles of the invention, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended, such alterations and further modifications in the illustrated device, and such further applications of the principles of the invention as illustrated therein being contemplated as would normally occur to one skilled in the art to which the invention relates.
[0018] Referring to FIGS. 1-7 , there is illustrated a swimming pool skimmer 10 that is constructed and arranged according to the present invention. Skimmer 10 comprises a pair of spaced pontoons 12 and 14 that are arranged so as to be generally parallel to one another and having tapered bows 16 and 18 respectively. Pontoons 12 and 14 also have sterns 20 and 22 , respectively, as shown in FIG. 4 . A cross member 24 extends between pontoons 12 and 14 at a substantially right angle with respect to the longitudinal axis (line 13 ) of each pontoon 12 and 14 . Cross member 24 provides structural interconnection between the pontoons 12 and 14 by way of flanges 12 a and 14 a and threaded fasteners 21 . The hollow construction of cross member 24 and pontoons 12 and 14 provides a housing for other components, such as, for example, control and propulsion components. Cross member 24 includes an upper surface 26 and fore and aft side walls 28 and 30 , respectively. Sidewalls 28 and 30 are constructed and arranged to reinforce the upper surface 26 . This construction provides the described hollow interior for receipt and/or placement of control and propulsion components.
[0019] The bow ends 31 and 33 of the pontoons 12 and 14 , respectively, are structurally interconnected by a curved frame member 32 secured to an upper housing 34 of pontoon 12 and an upper housing 36 of pontoon 14 by means of screws 38 . Frame member 32 comprises upper and lower walls 40 and 42 , respectively, having a series of recesses 43 between them to accommodate a plurality of rollers 46 . A series of shafts (not shown) extend between walls 40 and 42 and provide a means for journaling the rollers 46 that are uniformly spaced around the circumference of frame member 32 . The rollers 46 are journaled so that at least a portion of their periphery extends forward beyond the outer circumference 45 of frame member 32 .
[0020] Pontoons 12 and 14 may be formed from any appropriate material such as fiberglass, plastics, metal, and the like so long as the pontoons provide buoyancy for the device 10 . The pontoons 12 and 14 each have lower hulls 48 and 50 which mate with upper housings 34 and 36 , respectively. The lower hulls 48 , 50 and upper housings 34 , 36 are fastened together, respectively, by either glue, heat welding or other means to form watertight, buoyant compartments. In one embodiment of the present invention, as shown by dashed lines 56 and 58 , weights are incorporated in the aft end of the pontoons for a purpose to be described later. In another embodiment of the present invention, see FIG. 4A , this “weighting” is achieved by using thicker wall sections 55 and/or by creating added walls or ribs 57 to weight the stern greater than the bow. This weighting is non-linear with a greater proportion of the weight being provided to the stern half of the two pontoons 12 and 14 .
[0021] The back wall 30 of cross support 24 has mounting plates 61 , 63 forming supports for a pair of propulsion units 60 and 62 , respectively secured thereto by suitable fasteners. Propulsion devices 60 and 62 are electrically operated motors with an internal electrical motor driving propellers 64 and 66 through an appropriate power train. It should be apparent to those skilled in the art that the propulsion units 60 and 62 can be provided in a number of forms so long as they have the ability to propel the device 10 through the water at a thrust which can be varied both in absolute magnitude and relative to one another. The electric motors and the propulsion devices 60 and 62 are driven by a controller 68 (shown by a dashed outline) positioned and mounted in the hollow interior of structural cross member 24 . As shown herein, propulsion devices 60 and 62 simulate full-size outboard motors with a small fractional horsepower electric motor used as the prime mover. It should be apparent to those skilled in the art that the number of motors can be varied and the exact means of propulsion can be varied from open propellers as shown herein, to ducted propellers, to jet drive. Furthermore, although the propulsion devices 60 and 62 are shown as fixed in position and the relative speed of the propulsion devices is varied to guide the boat and control its speed, a single motor may be employed with the ability to swivel and thus achieve the directional capabilities.
[0022] The motors 60 and 62 may also be used in conjunction with a rudder or rudders (not shown) which may be fixed or adapted to pivot so as to guide the boat. Propulsion devices 60 and 62 receive electrical power through lines 70 and 72 (shown herein by dashed lines). These lines extend to the power output section 74 of the controller 68 , also indicated by dashed lines. As shown herein, the controller is from a radio controlled model boat that is used to control the relative current to the motors 60 and 62 to control the speed and the direction of the skimmer 10 . Controller 68 receives power from line 76 connected to a battery pack 78 , both shown by dashed lines. As shown herein, the voltage for the battery pack 78 is 9.6 volts and the battery pack 78 is rechargeable. It should be apparent to those skilled in the art, however, that other voltages and other forms of batteries may be employed in the illustrated device. An antenna 80 facilitates reception of signals from a remote control transmitter, not shown in order to provide a more concise description of the present invention. A removable cover 77 provides access for battery pack 78 and a pedestal for a scale size boat pilot 79 . An on-off toggle switch 81 is included.
[0023] The control system and propulsion units are available from a number of outlets including Radio Shack®. It is apparent to those skilled in the art that the system of controlling the speed and direction of the device 10 can take a number of forms to direct movement of pool skimmer 10 through the water.
[0024] As shown particularly in FIG. 2 , the pool skimmer 10 has a skimmer net 82 mounted between pontoons 12 and 14 . Skimmer net 82 comprises a net 84 consisting of an open fabric of appropriate material with suitable porosity to allow flow of liquid but still retain debris of the desired size. Although primarily intended to collect larger natural debris like leaves, the net 84 can be employed to trap smaller items floating on the surface of the water. The net 84 is configured to cover an elongated area between pontoons 12 , 14 . It is in the form of upper and lower walls 86 and 88 , respectively which are secured to each other around the circumference 90 by appropriate gluing, heat welding and the like. Upper and lower walls 86 and 88 may be a single sheet folded over and secured along two edges where they may be made as separate sheets or as a single unit using appropriate manufacturing technology. The walls 86 and 88 , so configured, form an elongated porous pocket extending between pontoons 12 and 14 .
[0025] Walls 86 and 88 are connected at their forward end to a cross frame 92 . Frame 92 may be molded from a single section to embrace and embed in the ends of the net-like walls 86 and 88 . However, it may be formed from a wide variety of materials. Frame 92 has an integral T handle 97 extending vertically from the upper leg 94 for convenient manipulation of the skimmer net 82 . As shown in FIG. 3 , the cross frame 92 is a single piece having an upper leg 94 , a lower leg 96 and curved end sections 98 and 100 to form an open, elongated mouth 95 . As shown particularly in FIG. 5 , the walls 98 and 100 of frame 92 are received within grooves 102 and 104 formed in support webs 106 and 108 , extending towards one another from the in-board side of pontoons 12 and 14 , respectively.
[0026] When the skimmer net 82 is in place, it is held adjacent the front end of the pontoons 12 and 14 with the mouth 95 of frame 92 facing the direction of movement of boat. The water line of the pool skimmer 10 is selected so that it is approximately half way between the upper wall 94 and lower wall 96 of frame 92 . This is to ensure that the skimmer can capture both the exposed and submerged sections of leaves. It should be apparent to those skilled in the art that the design waterline can be manipulated up or down to suit particular requirements.
[0027] As noted, particularly in FIG. 2 and FIG. 4 , the propulsion units 60 and 62 , and more particularly the propellers 64 and 66 , do not extend beyond the stern 20 and 22 of the pontoons 12 and 14 . Furthermore, the propellers do not extend below the lower-most section of pontoons 12 and 14 at the aft end of the pontoons. This is done to protect the propellers 64 and 66 when the unit 10 is placed flat on a surface or placed on end by positioning it on stern 20 and 22 . In order to ensure that the propellers 64 and 66 are sufficiently submerged in the water in spite of having their outer diameter at least as high as the bottom of sterns 20 and 22 , the weights 56 and 58 are positioned to provide a weight distribution of 60 / 40 biased toward the aft end (stern) of device 10 . Approximately the same non-linear weight distribution is achieved if the weights 56 and 58 are replaced with thicker walls 55 and/or added ribs 57 . It is also contemplated that smaller weights could be used in combination with the thicker walls and/or added ribs. This non-linear weight distribution causes a slight positive angle of attack, but more importantly causes the sterns 20 and 22 of pontoons 12 and 14 to be sufficiently immersed in the water to allow optimum propulsion from propellers 64 and 66 . It should be apparent that other weight distributions may be used as needed for particular applications.
[0028] In operation, the pool skimmer 10 is placed in a pool, pond, or other body of water to be cleaned and is operated by an operator on shore or at the edge of the pool to direct the skimmer 10 towards the debris on the surface. As the skimmer proceeds through the water, it is aimed at, and collects the debris in the skimmer net 82 . The above pool skimmer does a very effective job of cleaning debris from the water surface. Since the skimmer 10 has the appearance of a model boat and is radio controlled, it is far more entertaining for a person, and particularly children, to use this device to clear a pool of surface debris.
[0029] When the skimmer net 82 is to be emptied, skimmer 10 is brought to the side of the pool or shoreline and the skimmer net 82 is lifted from the grooves 102 and 104 by means of the T handle 97 on the upper wall 94 . Since grooves 102 and 104 are curved, it allows the frame 92 to be easily withdrawn from the grooves by pivoting the side nearest to the water's edge. This facilitates removal of the debris without the need to remove the entire vessel from the water.
[0030] The curved frame 32 at the bow of the pontoons 12 and 14 not only provides structural interconnection, but allows easy access to the skimmer net 82 . The rollers 46 prevent tearing of vinyl linings in some swimming pools when the pool skimmer is driven into the side. In addition, the rollers 46 allow the pool skimmer to be smoothly guided through a turning maneuver along the side.
[0031] While the invention has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character, it being understood that only the preferred embodiment has been shown and described and that all changes and modifications that come within the spirit of the invention are desired to be protected. | A remote control pool skimmer for picking up surface debris, according to one embodiment of the present invention, comprises a pair of elongated buoyant hulls spaced from one another, each hull having a bow and a stern, and at least one cross member interconnecting the hulls to one another, a remotely controlled drive system connected to the pool skimmer for propelling the hulls across the surface of the water in a selected direction and a collection net spanning the space between the pair of hulls, the net being oriented in order to collect surface debris as the hulls move through the water. In terms of weight distribution from bow to stern, the hulls are weighted more toward the stern. | 4 |
This application is a continuation-in-part application of my co-pending application bearing Ser. No. 11/713,942, filed 5 Mar. 2007, and entitled “Drilling Apparatus and System for Drilling Wells”. This invention relates to a novel drilling device and method of drilling a well. More particularly, but not by way of limitation, this invention relates to a non-reactive torque device that contains an inner bit and a counter-rotating outer bit. This invention also describes a method of drilling the well while utilizing nozzles that aid in the drilling process.
BACKGROUND OF THE INVENTION
In the search for oil and gas, operators have utilized various types of devices in order to drill wells. Operators are continually searching for ways to drill the wells faster and more economically. Traditionally, a specifically designed drill string was used to drill wells. The drill string would have attached thereto a drill bit. In order to drill the well, the driller would cause the drill string to rotate which would in turn cause the bit to rotate, and hence, drill the well. Over the years, various types of drill strings have been developed in order to drill directional, or inclined, well bores.
Further, different types of bottom hole assemblies have also been developed in order to drill these wells. Thus, a typical directional drill string may contain a bottom hole assembly which includes: a bit, bent sub, drilling motor, and measurement-while-drilling surveying and logging tools. With this type of bottom hole assembly, the drill string ideally is held stationary with respect to down hole rotation. The drilling motor generates rotation of the bit via circulation of the drilling fluid through the drilling motor as is well understood by those of ordinary skill in the art. With the drill string held stationary with respect to rotation, the well is drilled in the desired, controlled direction of the bend in the bent sub.
A common problem with this type of drilling assembly is the torque generated by the bit. The bit torque generates an equal and opposite reactive torque that is transferred from the motor into the bottom hole assembly and drill string, causing it to counter-rotate, relative to the bit. Further, the reactive torque, and hence the drill sting counter-rotation, varies due to drilling conditions, such as the weight applied to the bit, properties of the rock being drilled, and hole condition, which all vary independently of each other. As the bent sub is part of the bottom hole assembly being counter-rotated, the direction in which the well is being drilled changes with the changes in reactive torque.
As a result, the directional driller is required to make numerous surface adjustments of the drill string, and hence the bent sub, to maintain drilling in the desired direction. These numerous adjustments cost valuable rig time and reduce the efficiency of the drilling operation. By eliminating, or greatly reducing, the reactive torque in the bottom hole assembly and drill string, drilling can proceed unabated in the desired direction, saving valuable rig time. Other benefits of eliminating, or reducing, reactive torque include the ability to use more powerful motors and more weight on bit to increase drilling rates and drilling a smoother, less tortuous borehole for running logging tools and setting casing. A non-reactive bit apparatus and method were disclosed in U.S. Pat. No. 5,845,721 entitled “Drilling Device And Method Of Drilling Wells”, which is incorporated herein by express reference.
As those of ordinary skill in the art will appreciate, daily rig cost are substantial. In many cases after a well is drilled, the well is prepared for running and cementing a casing string into the well. Hence, any time saved cleaning, running and cementing the casing converts to significant cost savings. Prior art tools have not allowed an operator to effectively drill with a casing string forming a part of the work string due to structural limitations of the casing string and the casing string thread connections. In other words, the casing strings and casing string connections are not structurally designed to handle the stress and strain applied by the numerous torquing requirements for a drill string. However, with the advent of the non-reactive torque drilling device herein described, drilling with an attached casing string is possible. Numerous advantages and features flow from the non-reactive torque drilling device.
Therefore, there is a need for a drilling device that will allow the drilling of a well with a casing string attached thereto. There is also a need for a non-reactive drilling tool with dual bits, and wherein the casing string is left within the well after cessation of drilling operations. Under this scenario, the casing string can be cemented in place and other remedial well work can be performed, wherein the remedial well work includes perforating the casing in order to produce hydrocarbon from a subterranean reservoir.
SUMMARY OF THE INVENTION
An apparatus for drilling a well bore with a down hole motor is disclosed. The down hole motor contains a power shaft for imparting rotational movement. In one preferred embodiment, the apparatus comprises a driver operatively connected to the power shaft, with the driver having a cylindrical body, and wherein an outer portion of the cylindrical body contains a plurality of cogs. The apparatus further contains a first bit having a first end, and wherein the first end is connected to the driver so that rotational movement of the driver is imparted to the first bit, and a sleeve disposed about a portion of the power shaft, with the sleeve having a plurality of openings therein for placement of a plurality of pinions. The pinions have a pin disposed there through, and wherein the sleeve has a radial shoulder for attaching the plurality of pins. A housing is included, and wherein a second bit is formed on a first end, and wherein the housing has an internal portion that contains internal cogs, and wherein said internal cogs engage said pinions so that as said driver rotates in a first direction, rotation is imparted to said pinions which in turn imparts a counter rotation to said second bit.
In one preferred embodiment, the driver contains an outer radial surface that is disposed within the sleeve, and wherein the outer radial surface contains an outer coating material for preventing wear with the sleeve during rotation. The apparatus further comprises thrust bearing means, operatively positioned within the housing, for transferring the axial and lateral loads of the apparatus during drilling. The thrust bearing means generally comprises a thrust mandrel disposed between the housing and the driver, and a plurality of roller bearings operatively associated with the thrust mandrel. A trim spacer may also be included, and wherein the trim spacer is disposed within the housing and abutting the thrust mandrel, for engaging with the thrust mandrel. In the most preferred embodiment, the first bit is offset relative to the second bit so that the first bit extends further into the well bore relative to the second bit.
In one embodiment, the sleeve is attached to a coiled tubing string. In another embodiment, the downhole motor and planetary bit driver is attached to a work string. And, in the most preferred embodiment, the sleeve is attached to a casing string.
A method of drilling a well with a motor having a power shaft is also disclosed. In one preferred embodiment, the method comprises providing a drilling apparatus, with the drilling apparatus comprising a driver operatively connected to the power shaft, with the driver having a cylindrical body containing a plurality of cogs. The drilling apparatus also includes: a first bit having a first end connected to the driver so that rotational movement of the driver is imparted to the first bit; a sleeve disposed about a portion of the power shaft, with the sleeve having a plurality of openings therein for placement of a plurality of pinions, with the pinions having a pin disposed there through, and wherein the sleeve has a radial shoulder for attaching the plurality of pins. The drilling apparatus further includes a housing having a second bit formed thereon, and wherein the housing has an internal portion that contains a plurality of internal cogs engaging the pinions.
The method further comprises providing a casing string concentrically placed within the well, with the casing string being operatively connected to the sleeve, rotating the power shaft via a fluid flow down an internal portion of the casing string and the drilling apparatus, and rotating the first bit in a first direction. The method further includes drilling the well with the first bit, rotating the cogs on the driver, engaging the pinions with the cogs on the driver, and engaging the internal cogs on the housing. The method then comprises rotating the housing in a counter direction relative to the first bit, rotating the second bit in the counter direction, and drilling the well with the second bit. In one embodiment, the first bit is offset relative to the second bit so that the first bit extends further into the well relative to the second bit.
In one embodiment, the method further includes terminating the flow of the fluid down the internal portion of the casing string and the drilling apparatus, and terminating the drilling of the well with the first bit and the second bit. Next, the internal portion of the drilling apparatus, including the first bit, is retrieved from the well. The casing string can then be cemented in place within the well. The method further includes perforating the casing sting so that the inner portion of the casing string is in communication with a subterranean reservoir.
In yet another embodiment, a device for boring a well is disclosed. In this most preferred embodiment, the device is attached to a motor and wherein the motor has a power shaft for imparting rotational movement. The apparatus comprising a driver mandrel operatively connected to the power shaft, with the driver mandrel containing a cylindrical body. Also included is a first bit member having a first end and a second end, and wherein the first end is connected to the driver mandrel so that rotational movement of the driver mandrel is imparted to the first bit member, and wherein the first bit member has an inner bore. A sleeve is disposed about a portion of the power shaft, and wherein the sleeve has a radial shoulder. In this preferred embodiment, a casing string is attached to the sleeve, and wherein the casing string is designed to be permanently placed within the well once the boring is completed, and wherein the inner bore of the casing string is in fluid communication with the inner bore of the first bit. The device further includes a housing disposed about the driver mandrel, a second bit member attached to the housing, and a planetary gear anchored to the radial shoulder and disposed between the driver mandrel and the housing, and wherein the planetary gear is adapted for imparting rotation from the driver mandrel to the housing in a counter radial direction.
The device may further comprise thrust bearing means, operatively placed between the housing and the driver mandrel, for transferring the axial and lateral loads generated during boring. The thrust bearing means comprises a thrust mandrel and a plurality of ball bearings operatively associated with the thrust mandrel. A bearing assembly may also be included, wherein the bearing assembly having a first end and a second end, with the second end of the motor housing being rotatably associated with the first end of the bearing assembly so that rotation of the first bit member and the second bit member is facilitated. Additionally, the first bit includes a first set of cutter teeth positioned to drill the well in the first rotational direction and the second bit includes a second set of cutter teeth positioned to drill the well in the counter rotational direction. Also, in this embodiment, the first bit member is offset relative to the second bit member so that the first bit member extends further into the well relative to the second bit member.
In the most preferred embodiment of this disclosure, an apparatus for drilling a well bore with a down hole motor is disclosed, with the down hole motor having a power shaft for imparting rotational movement in response to a fluid flow. The apparatus comprises a driver operatively connected to the power shaft, with the driver having a tubular body, and wherein an outer portion of the tubular body contains a plurality of cogs and an internal bore for the fluid flow. The apparatus further includes a first bit having a first end connected to the driver so that rotational movement of the driver is imparted to the first bit, a sleeve disposed about a portion of the power shaft, with the sleeve having a plurality of openings therein for placement of a plurality of pinions, with the pinions having a pin disposed there through, and wherein the sleeve has a radial shoulder for attaching the plurality of pins. In this most preferred embodiment, the apparatus also includes a housing having a second bit formed on a first end, and wherein the housing has an internal portion that contains internal cogs, and wherein the internal cogs engage the pinions so that as the driver rotates in a first direction, rotation is imparted to the pinions which in turn imparts a counter rotation to the second bit. The most preferred embodiment also comprises a nozzle disposed within the tubular body and communicating the internal bore of the tubular body to the outer portion of the tubular body, and wherein the nozzle is oriented to deliver the fluid flow to the second bit. The apparatus may further comprise a flow skirt disposed about the outer portion of the tubular body and wherein the flow skirt is configured to receive the fluid flow from the nozzle and deliver the fluid flow to the second bit. In the most preferred embodiment, the flow skirt comprises a conical ring member disposed about the outer portion of the tubular body.
In one preferred embodiment, the driver may contain an outer radial surface that is disposed within the sleeve, and wherein the outer radial surface contains an outer coating material for preventing wear with the sleeve during rotation. The apparatus may further include thrust bearing means, operatively positioned within the housing, for transferring the axial and lateral loads of the apparatus during drilling. The thrust bearing means comprises a thrust mandrel disposed between the housing and the driver and a plurality of roller bearings operatively associated with the thrust mandrel. In this most preferred embodiment, the first bit is offset relative to the second bit so that the first bit extends further into the well bore relative to the second bit. The sleeve may be attached to a coiled tubing string, or work string or casing string.
In the most preferred embodiment, a method of drilling a well with a motor having a power shaft is disclosed. The method comprises providing a drilling apparatus comprising: a driver operatively connected to the power shaft, with the driver having a tubular body containing a plurality of cogs; a first bit having a first end connected to the driver so that rotational movement of the driver is imparted to the first bit; a sleeve disposed about a portion of the power shaft, with the sleeve having a plurality of openings therein for placement of a plurality of pinions, with the pinions having a pin disposed there through, and wherein the sleeve has a radial shoulder for attaching the plurality of pins; a housing having a second bit formed thereon, and wherein the housing has an internal portion that contains a plurality of internal cogs engaging the pinions. The method further comprises providing a casing string concentrically placed within the well, with the casing string being operatively connected to the sleeve, and rotating the power shaft via a fluid flow down an internal portion of the tubular body of the driver. The method further comprises rotating the first bit in a first direction, drilling the well with the first bit, rotating the cogs on the driver, engaging the pinions with the cogs on the driver, and engaging the internal cogs on the housing. The method further comprises rotating the housing in a counter direction relative to the first bit, rotating the second bit in the counter direction, exiting a portion of the fluid flow from a nozzle in the driver, wherein the nozzle is directed to the second bit, and drilling the well with the second bit. In this most preferred embodiment, the first bit is offset relative to the second bit so that the first bit extends further into the well relative to the second bit. Also, the driver may contain a flow skirt disposed on an outer portion of the tubular body and the step of exiting the portion of fluid flow from the nozzle includes directing the portion of fluid flow from the nozzle to the flow skirt and channeling the fluid flow from the flow skirt to the second bit.
The method may further comprise terminating the flow of the fluid down the internal portion of the casing string and the drilling apparatus and terminating the drilling of the well with the first bit and the second bit. The method may further include cementing the casing string in place within the well and perforating the casing sting so that the inner portion of the casing string is in communication with a subterranean reservoir.
In yet another most preferred embodiment, a device for boring a well is disclosed. The device is attached to a motor having a power shaft for imparting rotational movement in response to a fluid flow. The device comprises a driver operatively connected to the power shaft, with the driver containing a tubular body having an internal bore for the fluid flow, a first bit connected to the driver so that rotational movement of the driver is imparted to the first bit, and wherein the first bit has an inner bore, a housing disposed about the driver, and a second bit attached to the housing. The device further comprises a nozzle communicating the internal portion of the tubular with an outer portion of the tubular, and wherein the nozzle is oriented to deliver a portion of the fluid flow to the second bit. In this most preferred embodiment, the device further includes a sleeve disposed about a portion of the power shaft, and wherein the sleeve has a radial shoulder and a planetary gear anchored to the radial shoulder and disposed between the driver and the housing, and wherein the planetary gear is adapted for imparting rotation from the driver mandrel to the housing in a counter radial direction. In one embodiment, the first bit contains a first set of cutter teeth positioned to drill the well in the first rotational direction and the second bit contains a second set of cutter teeth positioned to drill the well in the counter rotational direction. Also in the most preferred embodiment, the first bit is offset relative to the second bit member so that the first bit member extends further into the well relative to the second bit member. The device may contain a plurality of nozzles and wherein the nozzles may be of variable size. Additionally, in the most preferred embodiment, the nozzles are directed in an opposite orientation relative to the fluid flow in the internal portion of the tubular body. In one preferred embodiment, the device further comprises a casing string attached to the sleeve, and wherein the casing string is designed to be permanently placed within the well once the boring is completed, and wherein an inner bore of the casing string is in fluid communication with the inner bore of the first bit.
An advantage of the present invention is the ability to drill with non-reactive torque utilizing a first bit and a second concentric bit. An advantage of the present system is that wells can be drilled and completed faster. Another advantage is that the work string used with the dual bit is a casing string. Yet another advantage is that the casing string can be left in the hole after the intended total depth of the well is reached.
Still yet another advantage is that after drilling the well, the well can be cemented. By cementing the well quicker than prior art methods, the well will experience less skin damage to potential hydrocarbon bearing reservoirs. Another advantage is that operators will realize significant cost savings due to significantly faster completion times. Another feature is that the drilling apparatus can utilize coiled tubing string as a work string, and wherein drilling is possible utilizing the coiled tubing string due to the non-reactive torque produced by the disclosed drilling apparatus.
An advantage of the most preferred embodiment is to maximize the removal of drill cutting by directing drilling fluid flow from the mud supply in the drill string directly to the outer bit. Another advantage of the most preferred embodiment is the placement and direction of the flow nozzles. The upward direction of the nozzles will provide a Venturi effect that will reduce the bottom-hole pressure below the nozzles. The resulting reduction of bottom-hole pressure will improve both the hydraulic and drilling performance of the inner bit.
A feature of the present invention includes the ability to drill-in with the casing string without the need to pull the entire length of casing string from the well. Yet another feature is that the casing string can be cemented into the well. Yet another feature is the option to perforate the casing string to produce hydrocarbon reservoir. Another feature is that the drill-in casing string can employ the same thread connection means used on commercially available casing strings. In other words, commercially available thread means can be used with the drill-in casing. Yet another feature is the pinions are mounted about pins, and wherein the pins are mounted on a radial shoulder of the sleeve, and therefore, the pinions are capable of rotation. Still yet another feature is that the down hole motors used with the disclosed system are commercially available.
A feature of the most preferred embodiment is the placement of the nozzles, which may be in a cross-over sub, between the drive shaft and the inner bit. Another feature may be to add a flow directing skirt to the cross-over sub which will direct drilling fluid flow toward the outer bit and the junk slot area and out into the annulus. The combination of the nozzles and the skirt will help lift the cuttings generated by the inner bit and very efficiently clean the outer bit as it drills. The nozzles will be facing upward at optimal angles and be directed at the point of interaction between the outer bit and the rock. This direction will jet the cuttings away from the outer bit immediately after being cut and keep the outer bit clean to avoid cuttings build-up and keep the annulus moving to efficiently transport cuttings up and out of the hole. Yet another feature of the most preferred embodiment is that the nozzles will include about three separate nozzles angled upwards at an approximate 45 degree angle, aimed at the cutters of the outer bit.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the drilling apparatus of the present disclosure.
FIGS. 2A , 2 B and 2 C are a cross-sectional view of the drilling apparatus of the present disclosure.
FIG. 3 is a cross-sectional view of the drilling apparatus taken from the line 3 - 3 in FIG. 2A .
FIG. 4 is a cross-sectional view of the drilling apparatus taken from the line 4 - 4 in FIG. 2A .
FIG. 5 is a schematic of the drilling apparatus system of the present disclosure disposed within a well.
FIG. 6 is a schematic of the drilling apparatus system cemented within the well with perforations to a hydrocarbon reservoir.
FIG. 7 is a schematic of the drilling apparatus system with the inner bit having been removed.
FIG. 8 is a schematic of the drilling apparatus system drilling a well from a rig.
FIG. 9 is a cross-sectional view of the most preferred embodiment of the drilling apparatus of the present disclosure.
FIG. 10 is a disassembled perspective view of the most preferred embodiment of the drilling apparatus seen in FIG. 9 .
FIG. 11 is a schematic of the most preferred embodiment of drilling apparatus seen in FIGS. 9 and 10 drilling within a well.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1 , a perspective view of the drilling apparatus 2 of the present disclosure will now be described. The power shaft 4 has a first end with external threads 6 and a second end with internal threads 8 . A driver 10 will threadedly connect with the power shaft 4 . The driver 10 has a first end having external threads 12 that will engage with the internal threads 8 and a second end having external threads 14 . As seen in FIG. 1 , driver 10 has a cylindrical body having a plurality of cogs 16 (sometimes referred to as splines 16 ) as well as the raised shoulder 18 . A sleeve 20 is included, and wherein the sleeve 20 has internal thread means 22 on one end and a second end having a plurality of openings, such as seen at 24 . Also, on the radial end, a plurality of indentations have been formed, such as seen at 26 .
FIG. 1 also depicts the pinions 28 , 30 , 32 , and wherein the pins will be disposed there through for rotation. Hence, the pin 34 a will be disposed through pinion 32 as well as the bushings 36 , 38 . The pins (for instance pin 34 a ) will cooperate to engage with a radial shoulder located within the openings of the housing 20 . FIG. 1 also illustrates the housing 40 which will have a first end 42 that will abut the ledge 44 of the sleeve 20 . The housing 40 also contains the external threads 46 on the second end.
FIG. 1 also depicts the thrust pack cylindrical assembly 48 which comprises a plurality of ball bearings (not seen in this view), and wherein the thrust pack assembly 48 (the thrust pack assembly 48 is commercially available) will be disposed about the thrust mandrel 50 . As seen in FIG. 1 , the thrust mandrel 50 has a first end having external threads 52 and a second end having a lip 54 . The trim spacer 56 is included, and wherein the trim spacer 56 is a ring member that cooperates with the thrust mandrel 50 as well as the thrust pack 48 , as seen in FIG. 2A . Returning to FIG. 1 , the outer bit 58 is depicted, and wherein the outer bit 58 has a first end having internal threads 60 and a second end that contains the bit face 62 . As seen in FIG. 1 , bit face 62 contains indentations for allowing fluid and debris circulation, as well understood by those of ordinary skill in the art. The cross-over 64 contains a generally cylindrical body having internal threads 66 that will engage with the external threads 14 . The cross-over 64 will also have internal threads 68 . FIG. 1 also depicts the inner bit 70 , and wherein the inner bit 70 has a first end including external threads 72 that will mate with the internal threads 68 . The second end of the inner bit 70 contains the cutting face 74 for boring the well, as understood by those of ordinary skill in the art.
Referring now to FIGS. 2A , 2 B and 2 C, a cross-sectional view of the drilling apparatus 2 of the present disclosure will now be described. It should be noted that like numbers appearing in the various figures refer to like components. The outer bit 58 is disposed about the cross-over 64 , and wherein the inner bit 70 is threadedly connected to the cross-over 64 . The outer bit 58 is threadedly connected to the housing 40 via the external threads 46 and the internal threads 60 . The driver 10 is threadedly connected to the cross-over 64 on one end and the driver 10 is also connected to the power shaft 4 via internal threads 8 and external threads 12 . The sleeve 20 has a radial shoulder 80 within the previously described openings, and wherein the pin 34 a and pin 34 b are connected to the radial shoulders of the openings so that the pins 34 a , 34 b are held in place as the pinions rotate as per the teachings of this description. Additionally, an indented bottom portion 82 of sleeve 20 is included (which includes the indentation 26 seen in FIG. 1 ), with the indented bottom portion 82 being threadedly attached to the thrust mandrel 50 , and wherein the pins 34 a and 34 b are attached to the indented bottom portion 82 in order to fix the pins 34 a and 34 b in place during operation of the down hole motor.
The power shaft 4 is connected to the down hole motor 84 (also referred to as a mud motor). Down hole motors are commercially available from Robbins and Meyers Inc. under the name positive displacement motors. As seen in FIGS. 2A , 2 B and 2 C, the power shaft 4 is connected to the rotor 86 of the motor 84 . The rotor 86 cooperates with a stator of the motor 84 and the fluid flow in order to impart a rotational movement to the power shaft 4 , as understood by those of ordinary skill in the art. As seen specifically in FIG. 2C , the motor 84 is connected to a cross-over 88 , and cross-over 88 is connected to the casing string 90 as per the teachings of this disclosure.
FIG. 3 is a cross-sectional view of the drilling apparatus 2 taken from the line 3 - 3 in FIG. 2A . Hence, FIG. 3 shows the external cogs 16 of the driver 10 . The pinion 32 is shown with the pin 34 a disposed there through; the pinion 30 is shown with the pin 34 b disposed there though; the pinion 91 is shown with the pin 34 c disposed there through; the pinion 92 is shown with the pin 34 d disposed there through; the pinion 94 is shown with the pin 34 e disposed there through; the pinion 96 is shown with the pin 34 f disposed there through. In operation, as the driver 10 rotates (due to its connection to the rotor), which in turn causes the pinions 28 , 30 , 32 , 91 , 92 , 94 and 96 (due to the engagement of the cogs), which in turn imparts a counter rotation movement to the housing 40 via the engagment of the pinion cogs with the internal cogs 98 located on the housing 40 .
Referring now to FIG. 4 , a cross-sectional view of the drilling apparatus 2 taken from the line 4 - 4 in FIG. 2A will now be described. In this view, the end of pins 34 a , 34 b , 34 c , 34 d , 34 e , 34 f are configured to engage with the indented bottom portion 82 of sleeve 20 , and in particular with a slot within the indented bottom portion 82 . A set screw is used to attach the pin ends to the indented bottom portion 82 . More specifically, the set screw 102 is configured to be inserted into the slot 104 , and wherein the end of pin 34 a is engaged with the set screw 102 so that the pin 34 a is attached to the indented bottom portion 82 . The other set screws include 106 , 108 , 110 , 112 , 114 and their engagement with the pin ends are the same as described with reference to set screw 102 .
Referring now to FIG. 5 , a schematic of the drilling apparatus system of the present disclosure disposed within a well 120 will now be described. The down hole motor 84 is threadedly attached to the cross-over sub 88 as previously mentioned. Fluid flow through the inner bore of the casing string 90 , and into the down hole motor 84 (through the rotor-stator), will produce the rotation of the inner bit 70 in a first direction, which in turn will impart a counter rotational movement to the outer bit 58 , and wherein the action of the two bits in counter directions will produce a non-reactive force. As shown, the bits 70 , 58 will be boring through the subterranean reservoirs. Hence, this non-reactive force allows the drilling of the well 120 with the attached casing string 90 , which heretofore has not been possible due to the extreme torque applied to the casing string thread connections during prior art drilling operations.
As those of ordinary skill in the art will appreciate, many times a well progresses in a series of hole sections which are drilled in progressively smaller hole sizes. Casings are run to consolidate the current progress, to protect some zones from contamination as the well progresses (such as freshwater sources) and to give the well the ability to hold higher pressures. FIG. 6 is a schematic of the drilling apparatus system cemented within the well 120 with perforations 122 to a hydrocarbon reservoir 124 . The cement is denoted by the numeral 126 and has been applied using known techniques to the annulus, wherein the annulus is the area between the outer portion of the apparatus 2 and casing 90 and the inner portion of the well 120 .
Referring now to FIG. 7 , a schematic of the drilling apparatus system with the inner bit (bit 70 ) having been removed is shown. In the position seen in FIG. 7 , the casing string has been cemented in place. As per the teachings of the present invention, a second drilling apparatus system may be run into the hole, down the casing string and through the open end so that drilling may continue. This second drilling apparatus system can also have a casing string as the work string. Note that as seen in FIG. 7 , the casing string 90 may be referred to as intermediate casing. In FIG. 8 , a schematic of the drilling apparatus 2 drilling the well 127 from a rig 128 . The rig is positioned on a drilling platform 130 , and wherein the drilling platform 130 is located in water. FIG. 8 shows an intermediate casing string 132 . The work string is the casing string 134 , and wherein the well 127 can be drilled and subsequently cemented in place as per the teachings of this disclosure. It should be noted that a coiled tubing string can be used as the work string i.e. in place of the casing string. Due to the continuous nature of the tubular of the coiled tubing string, having a non-reactive torque system herein disclosed, allows operators the option of drilling wells utilizing coiled tubing as the work string.
Referring now to FIG. 9 , a cross-sectional view of the most preferred embodiment of the drilling apparatus of the present disclosure will now be described. As mentioned earlier, like numbers refer to like components in the various figures. FIG. 9 depicts the driver 10 being threadedly connected to the cross-over sub 64 , and wherein the sub 64 is threadedly connected to the inner bit 70 . It should be noted that the driver 10 and cross-over sub 64 may be integrally formed as a single member. The housing 40 is threadedly connected to the outer bit 58 . As per the teaching of the present disclosure, the inner bit 70 rotates in a first direction and the outer bit 58 rotates in an opposite direction. FIG. 9 depicts a first passage 140 and a second passage 142 , and disposed within the first passage is nozzle 144 and disposed within the second passage is nozzle 146 . In the most preferred embodiment, the nozzles 144 and 146 are oriented relative to the axial center line 148 at a forty-five (45) degree angle of inclination. The angle of inclination may range from 30 degrees to 75 degrees, upward from horizontal. In the most preferred embodiment, a third passage and third nozzle are provided but not seen in this view. The size (opening) of the nozzle may be selected based on the desired flow rate, as understood by those of ordinary skill in the art. Also, a flow skirt 150 is depicted, and wherein the flow skirt 150 is disposed about the cross-over 64 . In the preferred embodiment, the flow skirt 150 is a ring member formed integrally on the outer portion of the cross-over 64 . As shown, the flow skirt 150 has an angled surface 152 that extends to a radially flat surface 154 . The flow skirt 150 directs drilling fluid flow toward the outer bit and the junk slot area and out into the annulus.
FIG. 10 is a disassembled perspective view of the most preferred embodiment of the drilling apparatus seen in FIG. 9 . Hence, in the view of FIG. 10 , cross-over 64 is shown along with the passages 140 , 142 and the nozzles 144 , 146 . An additional nozzle 156 is also shown. The flow skirt 150 is depicted along with the radially flat surface 154 . As noted earlier, the inner bit 70 threadedly connects with the cross-over 64 , and the cross-over 64 in turn threadedly connects to the driver 10 (not seen in this view).
Referring now to FIG. 11 , a schematic of the most preferred embodiment of drilling apparatus system 2 seen in FIGS. 9 and 10 will be described in the process of drilling within a well 127 . More specifically, the inner bit 70 is drilling the bore hole 158 via the cutters on the bit face 74 and the outer bit 58 is boring the larger hole, which is the well 127 . The drilling fluid is pumped down the drill string, as readily appreciated by those of ordinary skill in the art. A portion of the fluid will exit the nozzles within the inner bit 70 (nozzles in bit 70 not shown), with the fluid flow being represented by the flow arrows “A”. The flow “A” is in the annuluar area 160 and flows generally upward to the surface. As per the teachings of the present disclosure, the remaining portion of the drilling fluid will exit the nozzles within the cross-over 64 , with the fluid flow exiting nozzles 144 and 146 represented by the flow arrows “B”. The flow “B” is in the annular area 162 and flows generally upward to the surface.
In the most preferred embodiment, the nozzles (i.e. nozzles 144 , 146 and 156 ) will be machined into the cross-over sub 64 and threaded to allow different sizes of nozzles to be used, similar to flow nozzles on prior art bits. The nozzles will be supplied with drilling fluid flow from inside the cross-over 64 , which contains all of the drilling fluid from the drill string. Since the inner bit 70 is drilling only part of the entire hole being drilled (for instance, 6¼″, with inner bit versus 8¾ with larger outer diameter bit) more flow is being pumped thru the drill string than is required to adequately clean the inner bit. The nozzles on the inner bit will be selected so that the inner bit will receive the required flow (i.e. flow “A”) to be effectively cleaned during the drilling. The remainder of the flow (i.e. flow “B”) will be used for the nozzles exiting the cross-over sub 64 .
In the most preferred embodiment, the flow skirt 150 will be added as an integral part of the cross-over sub 64 and will cover the entire circumference of the cross-over sub 64 . The flow skirt 150 will direct drilling fluid flow toward the cutters of the outer bit 58 (see arrow “B”) and annulus 162 . The flow being directed will be the continuous flow from the inner bit and from the nozzles, while the continuous flow from the nozzle will strike the bit face intermittently due to the counter rotation. The flow skirt 150 will also prevent drilling fluid and cuttings from being lodged in the bearing area between the cross-over sub 64 and the outer bit 58 . Additionally, the flow skirt 150 can be used as simply a deflector sleeve without the use of the nozzles, in the case where an operator wants to just deflect fluid flow from the bearing area.
In the most preferred embodiment, the upward direction of the nozzles (45 degrees relative to the axial center line in the most preferred embodiment) will provide a Venturi effect that will reduce the bottom-hole pressure below the nozzles. The resulting reduction of bottom-hole pressure will improve both the hydraulic and drilling performance of the inner bit 70 .
Changes and modifications in the specifically described embodiments can be carried out without departing from the scope of the invention which is intended to be limited only by the scope of the appended claims and any equivalents thereof. | A device for boring a well. The device is attached to a motor that has a power shaft for imparting rotational movement. The device comprises a driver operatively connected to the power shaft, with the driver containing a tubular body, a first bit having a first end connected to the driver so that rotational movement of the driver is imparted to the first bit, and a sleeve disposed about the power shaft, and wherein the sleeve has a radial shoulder. The device further comprises a housing disposed about the driver and a second bit attached to the housing. A plurality of nozzles is operatively placed within the driver, and the nozzles deliver fluid flow to the second bit. The device may further include a planetary gear anchored to the radial shoulder, and wherein the planetary gear is adapted for imparting rotation from the driver to the housing in a counter radial direction. | 4 |
This is a continuation of application Ser. No. 07/760,137, filed Sep. 16, 1991, now abandoned.
BACKGROUND OF THE INVENTION
(1) Field of the Invention
This invention relates to a method of the immunoassay, which is applied to the detection of pathogens and disease markers in clinical examinations and to the industrial immunological detection of infinitesimal amounts of target substances. It also relates to a kit for the above-mentioned immunoassay.
(2) Description of the Related Art
The immunoassay using a naturally occuring antibody or an artificially prepared antibody is characterized by a high specificity and a high sensitivity, and is utilized for detecting an infinitesimal amount of a substance. For example, immunoassay is utilized for the clinical examination of detecting disease markers specifically secreted in the case of such diseases as an infectious disease, a tumor, a myocardial infarction and a cerebral thrombosis, or for detecting an infinitesimal amount of a substance in the open air.
As described, for example, in Enzyme Immunoassay (Proteins, Nucleic acids and Enzymes, separate volume, No. 31, pages 13-26, published by Kyoritsu Shuppan K. K.), many methods of the immunoassay have recently developed. Of these methods, the latex agglutination method has been utilized from old for the clinical examination because the operation is simple. However, tile kinds of infinitesimal substances to be tested are now increasing and also the number of items requiring such a high sensitivity as not attainable by the latex agglutination method is increasing.
As the method popularly adopted in these days, there can be mentioned the radio-immunoassay (RIA) and the enzyme immunoassay (EIA). RIA is not favorably used inspite of a high-sensitivity performance, because the assay has a large influence on a human body, and EIA utilizing an enzyme reaction instead of using a radioisotope as the labelled substance is more frequently adopted.
From the viewpoint of the simplicity of the detection system, it is desirable to develop the homogeneous process not requiring B/F separation as a substitute for the conventional heterogeneous process. Ullman et al teach that a fluorescent substance or quencher chemicaly bound to a sandwichable antibody can be used for an immunological reaction [Methods in Enzymology, vol. 74, 28 (1981)]. The taught process is a homogeneous process utilizing a principle that when a sandwich is formed by an antigen-antibody reaction, by an approach of the fluorescent substance and quencher bound to the antibodies to each other, the fluorescent energy of the fluorescent substance is shifted to the exciting energy of the quencher, resulting in reduction of the fluorescence intensity of the fluorescent substance.
As described above, the conventional immunological detection method is complicated because many steps such as the B/F separation step are necessary. Moreover, since the antigen-antibody reaction is carried out in a heterogeneous system where the solid phase and the liquid phase are copresent and the enzyme reaction or the like is used at the final stage, a long time is required for the measurement. In the homogeneous process proposed by Ullman et al, since both of the fluorescent substance and the quencher as the labelled substances are fixed to the antibody, there is a risk of drastic reduction of the performance of the antibody and elevation of sensitivity is limited.
SUMMARY OF THE INVENTION
The present inventors have completed the present invention as the result of investigations made with a view to solving the above-mentioned problems.
More specifically, in accordance with one aspect of the present invention, there is provided a method of the immunoassay comprising the steps of:
binding a fluorescent substance and an antibody reacting specifically with a target substance to be detected, to a fine particle (A);
binding a quencher and an antibody reacting specifically with the target substance to be detected, through a different antigen determinant, to a fine particle (B);
placing said fine particle (A) and said fine particle (B) in contact with the target substance contained in a sample to form an immunoreaction product comprising the target substance sandwiched between the antibody on said fine particle (A) and the antibody on said fine particle (B); and
detecting a quenching of the fluorescence occurring due to the quencher, thus to measure the target substance in the sample.
In accordace with another aspect of the present invention, there is provided a method of the immunoassay comprising the steps of:
binding one member selected from a fluorescent substance and a quencher, and an antibody reacting specifically with a target substance to be detected to a fine particle (C);
binding the other member selected from the fluorescent substance and the quencher to a known amount of the target substance to form a bound product (D);
placing said antibody-bound fine particle (C) and the bound product (D) in contact with the target substance contained in a sample thereby to competitively react the target substance in the sample and the known amount of the target substance with the antibody on said particle (C), thus forming an immunoreaction product comprising the target substance and the antibody on said particle (C); and
(4) detecting a quenching of the fluorescence occurring due to the quencher, thus to measure the target substance in the sample.
In accordance with still another aspect of the present invention, there is provided a kit for the immunoassay comprising a fine particle (A) having bound thereto a fluorescent substance and an antibody reacting specifically with a target substance to be detected, and a fine particle (B) having bound thereto a quencher and an antibody reacting specifically with the target substance through a different antigen determinant.
In accordance with a further aspect of the present invention, there is provided a kit for the immunoassay comprising a fine particle (C) having bound thereto one member selected from a fluorescent substance and a quencher, and an antibody reacting specifically with a target substance to be detected, and a bound product (D) composed of a known amount of the target substance and the other member selected from the fluorescent substance and the quencher.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagram illustrating changes of the fluorescence intensity of fluorescein to the concentration of the IgE antigen in Example 1;
FIG. 2 is a diagram illustrating changes of the fluorescence intensity of fluorescein to the concentration of the FSH antigen of Example 2;
FIG. 3 is a diagram illustrating changes of the fluorescence intensity of fluorescein to the concentration of the FSH antigen in Example 3;
FIG. 4 is a diagram illustrating the relationship of the relative fluorescence intensity to the incubation time in Example 4; and,
FIG. 5 is a diagram illustrating changes of the fluorescence intensity of fluorescein to the avidin antigen concentration in Examples 5 and 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The immunoassay methods and kits of the present invention will be described in detail.
The immunoassay method according to the first aspect of the present invention is now described. The antibody used in the present invention is not particularly limited, as far as it is capable of reacting specifically with a target substance to be detected. Either a monoclonal antibody or a polyclonal antibody may be used. The source material is not particularly limited, and for example, there can be used mouse, rat, sheep, goat, bovine and equine. In the present invention, two kinds of antibodies are used and the reaction is carried out so that the antigen is sandwiched between these two antibodies, and therefore, the two antibodies must be combined so that binding is effected through different antigen determinants. One of the two antibodies is bound together with a fluorescent substance to a fine particle (A), and the other antibody is bound together with a quencher to a fine particle (B).
The size of the fine particles (A) and (B) is larger than the size of the molecule level but cannot be distinguished with the naked eye. For example, various colloidal particles having a diameter of about 10 angstroms to about 5,000 angstroms can be used. More specifically, there can be mentioned polymeric colloids of latexes and synthetic polymers, colloids of noble metals such as platinum, gold and silver, and colloids of inorganic oxides such as aluminum oxide and titanium oxide. A smaller particle diameter is preferable because the fluorescent substance on the fine particle (A) can be approached more closely to the quencher on the fine particle (B).
The binding of the antibody reacting specifically with the target substance to the fine particle (A) or (B) can be carried out by adopting a means customarily used for immunological reactions such as physical adsorption and chemical binding.
The fluorescent substance is bound to a fine particle (A) and the quencher is bound to a fine particle (B). The fluorescent substance and the quencher are not particularly limited, but a preferable fluorescent substance should be selected depending upon the particular quencher. Typical combinations of the fluorescent substance and the quencher include fluorescein and Texas red, pyrene butyrate and β-phycoerythrin, fluorescein and 4',5'-dimethoxy-6-carboxyfluorescein, and fluorescein and rhodamine. The fluorescent substance and the quencher can be bound either directly or indirectly to the fine particles (A) and (B), respectively. In the indirect binding, BSA, polyethylene glycol (PEG) or another substance is adsorbed on a fine particle (A) or (B) and the fluorescent substance or quencher is bound to this adsorbed substance through a covalent bond. Of these bindings, direct binding is preferable because the preparation is simple.
The thus-prepared fine particle (A) having bound thereto the fluorescent substance and the antibody reacting specifically with the target substance, and the thus-prepared fine particle (B) having bound thereto the quencher and the antibody reacting specifically with the target substance through a different antigen determinant, are placed in contact with the target substnce to be detected in the sample. The order of the contact is not particularly limited, and either of the particles (A) and (B) can be contacted at first or they can be simultaneously contacted with the target substance in the sample.
By this contact, the target substance in the sample is sandwiched between the antibody on the particle (A) and the antibody on the Particle (B) to form an immunoreaction product. Before the immunoreaction is caused, since the fluorescent substance and the quencher are separated from each other, they do not influence each other and they have inherent energies, respectively. However, when an immunoreaction product is produced, the fluorescent substance and the quencher are placed very closely to each other and mutually act on each other, a quenching of the fluorescence occurs due to the quencher. Since the quenching of the fluorescence has a correlation to the amount of the immunological reaction product, the target substance contained in the sample can be determined by measuring the degree of quenching.
The immunoassay method according to the second aspect of the present invention will now be described. The same antibody, fine particles, fluorescent substance and quencher as described above with respect to the first aspect of the present invention can be used. Moreover, binding of the antibody, fluorescent substance and quencher to the fine particles can be performed by the same procedure. However, in the second aspect of the present invention, only the fine particle (C) having bound thereto an antibody reacting specifically with a target substance and one of the fluorescent substance and the quencher are used.
Either of the fluorescent substance and the quencher can be bound onto the fine particle (C), but preferably the quencher is bound onto the particle (C). The reason is that the labelled substance can be bound onto the fine particle (C) in an amount larger than the amount bound onto the target substance, and the sensivity is improved.
The other substance selected from the fluorescent substance and the quencher is bound to a known amount of the target substance. Either direct binding or indirect binding through a particle or a polymer can be adopted.
The fine particle (C) to which the antibody and one of the fluorescent substance and quencher are bound and the known amount of the target substance to which the other substance selected from the fluorescent substance and the quencher is bound are placed into contact with the target substance in a sample to effect a competitive reaction, whereby an immunoreaction product comprising the target substance and the antibody on the particle (C), is produced. Before the immunoreaction is caused, the fluorescent substance and the quencher on the particle (C) and the known amount of the target substance are separated from each other, and therefore, they do not influence each other and they exhibit inherent energies, respectively. However, once an immunoreaction is caused, the fluorescent substance and the quencher mutually act on each other and the energy states are changed, and a quenching of the fluorescence occurs. Since quenching of the fluorescence has a correlation to the quantity of the immunoreaction product, the target substance contained in the sample can be determined by measuring the degree of quenching.
According to the present invention, there are provided kits to be used for the above-mentioned two methods of the immunoassay.
The kit used for the first immunoassay comprises a fine particle (A) having bound thereto a fluorescent substance and an antibody reacting specifically with a target substance to be detected, and a fine particle (B) having bound thereto a quencher and an antibody reacting specifically with the target substance through a different antigen determinant.
The kit used for the second immunoassay comprises a fine particle (C) having bound thereto one member selected from a fluorescent substance and a quencher, and an antibody reacting specifically with a target substance to be detected, and a bound product (D) composed of a known amount of the target substance and the other member selected from the fluorescent substance and the quencher.
Respective components constituting these kits are the same as those described above with respect to the immunoassay methods. Furthermore, reagents having no baneful influences on the immunoassay, such as a diluent and a stabilizer, can be incorporated in the kits.
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.
EXAMPLE 1
Synthesis of Fine Particle (A) Having Bound Thereto Fluorescein and Antibody and Fine Particle (B) Having Bound Thereto Rhodamine and Antibody
Two kinds of anti-IgE monoclonal antibodies recognizing different sites, respectively, were fixed to polystyrene latexes A and B having bound thereto fluorescein as the fluorescent substance and rhodamine as the quencher, respectively. More specifically, 100 g of monomeric styrene was dissolved in 500 g of water, and 10 g of SDS was added to the solution and the mixture was stirred and heated. At about 60° C., potassium persulfate was added in an amount of 0.4 g per 100 ml of water to initiate polymerization. The reaction mixture was stirred for three hours and then cooled to stop the reaction. The thus-obtained latex solution was dialyzed for 1 day with pure water. Then 200 mg of fluorescein or rhodamine was added into 10 ml of the obtained 1% solution of the polystyrene latex, and the mixture was treated for 30 minutes by an ultrasonic dispersing device. The obtained solution was dialysed for 1 day with pure water, and thus, the fluorescein- or rhodamine-bound polystyrene latex was obtained.
Then 500 μl of a buffer solution containing 0.1M of sodium bicarbonate, 0.15M of sodium chloride and 0.08% by weight of sodium azide (the pH value was 8.5) was mixed with 500 ul of the fluorescein-bound polystyrene latex (100 times dilution with water), and 4 ml of pure water was further added. Then 40 μl of anti-IgE monoclonal antibody (the antibody concentration was 10 mg/ml) was added to the mixture, and the mixture was stirred. Then 5 ml of 10% polyethylene glycol having a molecular weight of 20,000 was added to the polystyrene latex, and the mixture was allowed to stand for 1 hour to effect blocking. Thus an antibody- and fluorescein-bound polystyrene latex was obtained. Reaction was carried out in the same manner as dscribed above by using the rhodamine-bound polystyrene latex and anti-IgE monoclonal antibody recognizing a different site, whereby an antibody- and rhodamine-bound polystyrene latex was obtained.
Detection of IgE Antigen Concentration
To 50 μpl of each of the fluorescent substance- and antibody-bound latex solution and the quencher- and antibody-bound latex was added 900 μl of standard serum containing 10 to 2,200 IU/ml of IgE antigen as a sample, and incubation was conducted for 10 minutes. Then the fluorescence intensity was measured at an exciting wavelength of 495 nm (the band path was 5 nm) and a flurescence wavelength of 515 nm (the band path was 5 nm) by a fluorescence spectrophotometer. The thus-obtained results are shown in FIG. 1. As is seen from FIG. 1, it was confirmed that the fluorescence intensity was reduced with an increase of the amount of the antigen, and the IgE antigen concentration could be detected from the degree of reduction of the fluorescence intensity.
EXAMPLE 2
Synthesis of Fine Particle (A) Having Bound Thereto Fluorescein Isothocyanate/BSA and Antibody and Fine Particle (B) Having Bound Thereto Rhodamine Isothiocyanate/BSA and Antibody
BSA having bound thereto fluorescein isothiocyanate as the fluorescent substance and BSA having bound thereto rhodamine isothiocyanate as the quencher were fixed respectively to polyethylene latexes having fixed thereto respectively two kinds of anti-FSH monoclonal antibodies recognizing different sites. More specifically, 20 mg of fluorescein isothiocyanate (FITC) was added into 100 ml of PBS buffer containing 100 mg of BSA, and the mixture was stirred for 24 hours and dialyzed for 24 hours to obtain FITC-fixed BSA. Separately, 20 mg of rhodamine isothiocyanate (TMRITC) was added into 100 ml of PBS buffer containing 100 mg of BSA, and the mixture was stirred for 24 hours and dialyzed for 24 hours to obtain TMRITC-fixed BSA.
Separately, 500 μl of a buffer solution containing 0.1M of sodium bicarbonate, 0.15M of sodium chloride and 0.08% by weight of sodium azide (the pH value was 8.5) was mixed with 500 pl of a 1% by weight polystyrene latex solution prepared in the same manner as in Example 1, and 4 ml of pure water was further added. Then 50 μl of anti-FSH monoclonal antibody (the antibody concentration was 0.1 mg/ml) was added, and the mixture was stirred. Then 50 μl of the above-mentioned FITC-fixed BSA was further added to the mixture, and the mixture was allowed to stand for 1 hour to effect blocking, whereby an FITC- and antibody-fixed latex was obtained.
A similar treatment was carried out by using anti-FSH monoclonal antibody recognizing a different site and TMRITC-fixed BSA to obtain a TMRITC- and antibody-fixed latex.
Detection of FSH Antigen Concentration
To 50 μl of each of the thus-obtained FITC- and antibody-fixed latex solution and the TMRITC- and antibody-fixed latex solution was added 900 μl of standard serum containing 1 to 1,000 mIU/ml of FSH antigen as a sample, and incubation was conducted for ten minutes. The fluorescence intensity was measured at an exciting wavelength of 495 nm (the band path was 5 nm) and a fluorescence wavelength of 515 nm (the band path was 5 nm) by a fluorescence spectrophotometer. The thus-obtained results are shown in FIG. 2. As is seen from FIG. 2, it was confirmed that the fluorescence intensity was reduced with an increase of the amount of the antigen, and the concentration of the FSH antigen could be detected from the degree of reduction of the fluorescence intensity.
EXAMPLE 3
Synthesis of Fine Particle (A) Having Bound Thereto FITC/BSA and Antibody and Fine Particle (B) Having Bound Thereto TMRITC/BSA and Antibody
BSA having bound thereto fluorescein isothiocyanate (FITC) as the fluorescent substance and BSA having bound thereto rhodamine isothiocyanate (TMRITC) as the quencher were fixed respectively to platinum fine particles to which two kinds of anti-FSH monoclonal antibodies recognizing different sites were fixed respectively.
Namely, FITC-fixed BSA and TMRITC-fixed BSA were obtained in the same manner as described in Example 2.
Separately, 500 μl of a buffer solution containing 0.1M of sodium bicarbonate, 0.15M of sodium chloride and 0.08% by weight of sodium azide (the pH value was 8.5) was mixed with 500 1μl of a solution of platinum fine particles synthesized according to the conventional method (Chemistry and Applications of Noble Metals, pages.60-71, Kodansha K. K.) and 4 ml of pure water was further added. Then 50 μl of anti-FSH monoclonal antibody (the antibody concentration was 0.1 mg/ml) was added to the mixture, and the mixture was stirred. Then 50 μl of the above-mentioned FITC-fixed BSA was added to the mixture, and the mixture was allowed to stand for 1 hour to obtain FITC and antibody-fixed platinum particles. A similar treatment was carried out by using anti-FSH monoclonal antibody recognizing a different site and TMRITC-fixed BSA to obtain TMRITC- and antibody-fixed platinum fine particles.
Detection of FSH Antigen Concentration
To 50 μl of the thus-obtained FITC- and antibody-fixed platinum fine particle solution and the TMRITC- and antibody-fixed platinum fine particle solution was added 900 μl of standard serum containing 1 to 1,000 mIU of FSH antigen as a sample, and incubation was carried out for 10 minutes. Then the fluorescence intensity was measured at an exciting wavelength of 495 nm (the band path was 5 nm) and a fluorescence wavelength of 515 nm (the band path was 5 nm) by a fluorescence spectrophotometer. The results are shown in FIG. 3. As is seen from FIG. 3, it was confirmed that the fluorescent intensity was reduced with an increase of the amount of the antigen, and the FSH antigen concentration could be detected from the degree of reduction of the fluorescence intensity.
EXAMPLE 4
Synthesis of Fine Particle (A) having Bound Thereto FITC and Antibody and Fine Particle (B) Having Bound Thereto TMRITC and Antibody
In the same manner as described in Example 3, a fine platinum particle having bound thereto TMRITC and an anti-FSH monoclonal antibody and a fine platinum particle having bound thereto FITC and an anti-FSH monoclonal antibody recognizing a different antigen site were prepared.
Detection of FSH Antigen Concentration
The measurement was carried out in the same manner as described in Example 3 except that standard serum containing 387.5 mIU/ml, 775mIU/ml or 1,550 mIU/ml of FSH antigen was used, and the advance of the reaction was examined while adjusting the incubation time to 0.5, 2, 5, 10, 20, 30 or 40 minutes. The results are shown in FIG. 4. In FIG. 4, the incubation time is plotted on the abscissa and the relative fluorescence intensity, calculated based on the supposition that the fluorescence intensity obtained at 0.5 minute's incubation is 100, is plotted on the ordinate. As is seen from FIG. 4, even if the incubation time was short, the reaction was sufficiently advanced. Therefore, it was found that the time required for the detection can be drastically shortened.
EXAMPLE 5
Synthesis of Fine Particle (C) Having Bound Thereto TMRITC/BSA and Antibody
BSA having bound thereto TMRITC as the quencher was fixed to a latex having fixed thereto an anti-avidin antibody. More specifically, 100 μl of a 1/100 dilution of a latex of the reagent class supplied by Sekisui Chemical Co. (the particle size was 0.525 pm and the solid content of 10% by weight) was added to 4.9 ml of 0.1M tris-hydrochloric buffer having a pH value of 8.0, and 50 μl of an anti-avidin antibody (supplied by EY Laboratory, 7.5 mg/ml) was further added to bind it to the latex particles.
To the antibody-fixed latex particles was added 50 μl of TMRITC-fixed BSA obtained in the same manner as in Example 2, and reaction was carried out for 2 hours. Then 500 μl of 10% polyethylene glycol having a molecular weight of 20,000 was added to the reaction mixture and blocking was conducted for 1 hour, whereby an antibody-and TMRITC-fixed latex was prepared.
Detection of Avidin Concentration
To a microtiter plate for the fluorometry were added 50 μl of avidin (supplied by Nakarai Tesque, 0.1 ug/ml to 1,000 μg/ml), 50 ul of FITC-labelled avidin (supplied by Cappel, 0.0259 mg/ml) and 100 μl of the antibody- and TMRITC-fixed latex. Incubation was conducted for 0.5 to 60 minutes, and the fluorescence intensity was measured at an exciting wavelength of 495 nm (the band path was 5 nm) and a fluorescence wavelength of 515 nm (the band path was 5 nm) by a microtiter fluorescence reader. The results are shown by white spots in FIG. 5. As is seen from FIG. 5, it was confirmed that the fluorescence was elevated with an increase of the amount of the antigen, and the avidin concentration could be detected with the degree of this increase.
EXAMPLE 6
Synthesis of Fine Particle (C) Having Bound Thereto TMRITC/BSA and Antibody
BSA having bound thereto TMRITC as the quencher was fixed to ultrafine platinum particles having fixed thereto an anti-avidin antibody. More specifically, 120 ml of 1% by weight citric acid (supplied by Wako Junyaku) and 60 ml of chloroplatinic acid (H 2 PtC 16 6H 2 O supplied by Wako Junyaku) were added into 960 ml of water maintained at 100° C., and the mixture was refluxed and stirred for 3 hours. The mixture was cooled on an ice bath and passed through an ion exchange resin column packed with Amberlite MB-1. It was confirmed that the electric conductivity after the passage through the column was not larger than 5 μS/cm.
To 1 ml of the thus-prepared solution of ultrafine platinum particles was added 4.0 ml of 0.1M tris-hydrochloric acid buffer having a pH value of 8.0, and 50 μl of an anti-avididin antibody (7.5 mg/ml) was added to the mixture to fix the antibody to the platinum particles. Then 50 μl of TMRITC-fixed BSA prepared in the same manner as described in Example 2 was added to the antibody-fixed platnum particles, and reaction was carried out for 2 hours. Then 500 μl of 10% by weight polyethylene glycol having a molecular weight of 20,000 was added to the reaction mixture and blocking was conducted for 1 hour. Thus, antibody- and TMRITC-fixed platinum particles were obtained.
Detection of Avidin Concentration
The measurement was carried out in the same manner as described in Example 5 except that the antibody- and TMRITC-fixed ultrafine platinum particles were used instead of the antibody- and TMRITC-fixed latex. The results are shown by black spots in FIG. 5. As is seen from FIG. 5, it was confirmed that the fluorescence intensity was elevated with an increase of the amount of the antigen, and the avidin concentration.
According to the present invention, a fluorescent substance and a quencher are bound not to an antibody but to fine particles. Therefore, the following effects are attained.
The amounts of the bound fluorescent substance and quencher can be prominently increased, and therefore, detection can be performed at a high sensitivity. The fluorescent substance and the quencher do not inhibit the antigen-antibody reaction, and therefore the antibody is not deactivated.
Since the reaction is conducted in a uniform system, that is, in a liquid phase, there is no need of conducting a complicated operation, such as B/F separation, which is conducted in the conventional method in a solid-liquid heterogeneous system. The time required for the immunoassay, which is about 1 hour in the conventional technique, can be drastically shortened. When the kit for the immunoassay of the present invention is used, the immunoassay can be conveniently effected in a simplfied manner. | A target substance is detected by a sandwich immunoassay using fine particle (A) having bound to it a fluorescer and an antibody reacting specifically with the target substance, and a fine particle (B) having bound to it a quencher and an antibody reacting specifically with the target substance, through a different antigenic determinant. Also disclosed is a competitive immunoassay having a fine particle (C) bound to it a fluorescer or a quencher, and an antibody reacting specifically with the target substance, a bound product (D) composed of the remainder of the fluorescer and the quencher, or a known amount of the target substance. Binding of the fluorescer and the quencher to the fine particle (A), (B) or (C) is affected so that the fluorescer and the quencher are covalently bound to a substance adsorbed on the fine particle. The sandwich immunoassay is advantageously conducted using a kit containing (i) the fluorescer- and antibody-bound fine particle (A) and (ii) the quencher- and antibody-bound fine particle (B). The competitive immunoassay is advantageously conducted by using a kit containing (i) the fluorescer- or quencher-and-the antibody-bound fine particle (C), and (ii) the bound product (D) of the quencher or fluorescer and the target substance. | 8 |
This invention relates to a reel. The invention is directed particularly, but not solely, toward reels having gearing.
BACKGROUND OF THE INVENTION
To operate most take a significant amount of time and effort as the length of wire that forms the fence is normally extremely long which means a huge effort is required to wind or unwind. This effort is time consuming and tiring.
A further problem with current reels is the heaviness of the reel and wire. Other features such as gearing are used in reels to magnify the effort to wind up or unwind. Gearing normally comprises multiple moving parts which can contribute to excessive maintenance requirements and cost, coupled with significant initial manufacturing costs.
Other uses for reels are for example hose reels, fishing reels, electrical conduit reels, kite reels and weather reels. In general the problems described above are also relevant for reels in general.
It is the object of the present invention to provide an improved reel which will obviate or minimise the aforementioned problems in a simple yet effective manner or which will at least provide the public with a useful choice.
STATEMENT OF INVENTION
Accordingly in a first aspect, the invention provides a reel, the reel includes a drum in use to locate a windable material therearound, a rotatable handle and gearing having a ratio greater than 1:1, the gearing connecting the handle with the drum, the gearing including protruding means, wherein rotation of the handle drives the protruding means to rotate the drum.
Preferably the protruding means protrudes from the drum.
Preferably the protruding means includes at least three elongate members having at least one end fixed to the drum.
Preferably the drum comprises a core member fixedly attached to at least one flange, the core member having a central rotational point, a distal end and a proximal end, the at least one flange having an outer surface facing away from the core member.
Preferably the gearing includes a crank face member operatively connected to the protruding means wherein the crank case member is attached to and facing the flange outer surface.
Preferably the fixed end of each elongate member is located in the side of the at least one flange and the other end of each protruding means is located in the crank face member.
Preferably the crank face member comprises a member having an inner face and an outer face and a rotational centre point, the inner face facing the said at least one flange wherein the inner face includes a track for the sliding location of the said other end of each elongate member.
Preferably the track is provided by three slots crossing the rotational centre and radiating in six equidistant positions (60 degrees) from the rotational centre point of the crank face wherein each slot extends from one circumferential edge to the other.
Preferably during rotation of the handle, each elongate member slidably moves from one end of a pair of slots through the crank face member rotational centre point to the other end of the slot of the coincident pair.
Alternatively the protruding means protrudes from the gearing.
Preferably the gearing includes a crank face member operatively connected to the protruding means wherein the crank case member is attached to and facing the flange outer surface.
Preferably the drum comprises a core member fixedly attached to at least one flange, the core member having a central rotational point, a distal end and a proximal end, the at least one flange having an outer surface facing away from the core member.
Preferably the protruding means includes at least three elongate members having at least one end fixed to the crank.
Preferably the crank face member comprises a member having an inner face and an outer face and a rotational centre point, the inner face facing the said at least one flange wherein the inner face includes the protruding means for the sliding location of the said other end of each elongate member.
Preferably the drum is provided with a track for the sliding location of the said other end of each elongate member.
Preferably the fixed end of each elongate member is located in the side of the crank case member and the other end of each protruding means is located in the drum outer surface.
Preferably the track is provided by three slots crossing the rotational centre and radiating in six equidistant positions (60 degrees) from the rotational centre point of the drum outer surface wherein each slot extends from one circumferential edge to the other.
Preferably during rotation of the handle, each elongate member slidably moves from one end of a pair of slots through the drum flange rotational centre point to the other end of the slot of the coincident pair.
Preferably the reel is provided with a locking mechanism located on the handle.
Preferably the locking mechanism comprises a lever pivotally connected to a pawl member being operatively connected to the handle by a ratchet wherein the handle has the ratchet part thereon.
Preferably a frame has one end connected to the handle and another end connected to the distal end of the core wherein the frame is for holding the crank face member to the core and is for supporting the reel when in use.
Preferably the gearing ratio is 2:1.
DRAWING DESCRIPTION
Preferred forms of the invention will now be described with reference to the accompanying drawings.
FIG. 1 is a perspective disassembled side view of the reel of the invention.
FIG. 2 is an opposite end view of the reel of FIG. 1 .
FIG. 3 is a plan view of the flange member.
FIG. 4 is a cross sectional view of the reel.
FIG. 5 is a plan view of the crank face member.
FIG. 6 is a cross sectional view of the crank face member.
FIG. 7 is a cross section of the pins with respect to the crank face member slots.
FIG. 8 is a perspective exploded view of another example of the reel.
FIG. 9 is another view of the reel of FIG. 8 .
FIG. 10 is an assembled perspective view of the reel of FIGS. 8 and 9 .
FIG. 11 is an assembled perspective view of the reel having a locking mechanism.
FIG. 12 show the reel having the locking mechanism in another position on the reel.
FIG. 13 is a perspective view of the reel of FIG. 12 .
FIG. 14 is a close up perspective of a locking mechanism of FIG. 13 .
FIGS. 15 and 16 are end views of the reel of FIGS. 12 - 14 .
DETAILED DESCRIPTION
As shown in FIGS. 1 to 16 there are several views of the reel of the invention. The reel includes a drum 1 with an operating handle 2 and gearing 3 . The gearing can include protruding means 4 which includes elongate members which may comprise for example metal pins or plastic pins P 1 , P 2 , P 3 being formed separately or integrally with the drum 1 . The gearing ratio can be 2:1 or alternatively 1:2.
The drum 1 includes a core portion 5 and at least one flange 6 or 7 . Preferably there are two flanges 6 and 7 . The flanges 6 and 7 serve to assist and hold any windable material in place over the core 5 . For example the windable material can be fencing wire, hosing, cables, string, rope and fishing lines. The core 5 has a core central rotational axis 8 and a distal end 9 and a proximal end 10 . The handle 2 is located on the proximal end of the core 5 . The core can be in one piece or several components. For example the core can comprises two interlocking halves.
The flange 6 has an inner surface 11 and an outer surface 12 and the flange 7 has an inner surface 13 and an outer surface 14 .
The gearing 3 can also include a crank face member 15 having an inner surface 16 and an outer surface 17 . The crank face member 15 has a rotational center or axis 18 . Preferably the face member 15 is circular in shape. The crank face member 15 is operatively connected between the handle 2 and one of the flanges 6 or 7 . The crank face member 15 has a track 19 located on the inner surface 16 which track operatively allows the protruding means 4 to be inserted therein so that with the rotation of handle 2 , the gearing 3 comprising the crank rotates which also rotates the protruding means 4 which in turn turns the reel.
The track 19 can be provided by a slot means or any other shape that allows the protruding means to travel therein. The travel can be a sliding motion. Preferably the slot means consists of three slots made up of six equidistant portions 20 & 21 , 22 & 23 and 24 & 25 that radiate from the crack face member rotation axis 18 . Each of the three slots is made up of a continuous slot that extends from one circumferential edge of the crank face member to the directly opposing circumferential edge. The six slot portions are substantially equally 60 degrees apart. The first slot is 20 & 21 , the second is 22 & 23 and the third slot is 24 & 25 .
Therefore for every one complete rotation of the handle 2 we obtain two complete rotations of the core containing the windable material, it is a doubling of the effort put in. During the rotation of the handle 2 the protruding means 4 (for example pins) travel up and down the individual tracks 19 . The handle 2 has a point of rotation at the center of the crank face 15 which is off-set from the center of the core 5 thus enabling protruding means 4 which for example can be stainless steel pins to travel in the track 19 and double the effort put in. Therefore for every one complete rotation of the handle and crank face member, each pin simultaneously moves from one end of the paired slots or double track and back. For example at an at rest position (see figure 7 ) the three pins which are equidistantly fixedly i.e. radially located on core 5 are located on the slots of the crank face member is whereby one pin is at one end of say slot 21 while the other pins are substantially down slots 22 and 25 . As the crank face member rotates so the position of the pins with respect to the slots with change.
The reel can also include a frame 27 to enable the reel to be located on any support to enable easy unwinding and winding to occur. The frame 27 also serves to hold the crank face member 15 against the protruding means 4 and flange 7 of the core 5 so that the parts of the reel work together to rotate. The frame 27 can have at least two ends 28 & 29 with one end 28 being located at the handle end of the core i.e. 10 and the other end 29 is located at the distal end of the core at point 8 . The frame 27 can also have support means for example at least one hook member 30 to allow location and support during the winding or unwinding operation. Preferably there are at least two hook members 30 .
Optionally the hook can be joined to or extend integrally with a protruding portion. Frame 27 can be fabricated from any suitable cross section that enables it to be joined and hold the rest of the assembly together. For example the cross section can be polygonal or rectangular or circular etc.
The reel can be made up of the following material, the core and flanges may be made up of any suitable plastics with the protruding means 4 being made of stainless steel and fixably attached or being integral with the core 5 . The crank face member 15 may be a different sort of plastics which enables the protruding means 4 to slide through the track 19 . In other examples the handle 2 maybe removable as well as the frame member 27 may also be interchangeable as well.
The reel can also have the protruding means which can act as a holding means 31 whereby the user can grab the holding means which for example can be in the form of a slender member having a gripping portion, while operating the handle 2 or while carrying the reel.
The reel can be provided with a simple locking mechanism as shown in FIGS. 11 to 16 . This mechanism can include an outer operating lever 32 pivotally connected to a pawl member 33 . The pawl member 33 being connected to a ratchet or teeth 34 . The ratchet or teeth 34 being located on the handle 2 or shaft of the handle. The pawl and lever can be one piece or two piece or any number of components necessary to achieve the movement and locking. Other positions for the locking mechanism are also envisaged—see FIGS. 12 to 16 . The locking mechanism can be operated by engaging the lever with the pawl when one does not wish the reel to slip.
In another alternative, the protruding means can be located on crank which can be attached to the handle and the slots 19 can be located on the drum. The outer surface of the core member can also be domed 35 to allow for clearance of the frame members from the drum.
The FIGS. 1 to 16 show the reel in one form of operation but this is not limiting one how the reel can be used. The reel as shown can be orientated as shown or it can be reversed depending on the user's preference and the use in which the reel is being used for.
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 purely illustrative and are not intended to be in any sense limiting.
Throughout the description and claims of this specification the word “comprise” and variations of that word, such as “comprises” and “comprising”, are not intended to exclude other additives, components, integers or steps.
The reel has the following advantages:
1. Few parts. 2. Economic construction. 3. Pleasing appearance. 4. Easy to manufacture. 5. Light weight and tough construction. | A reel consists in a drum in use to locate a windable material therearound, a rotatable handle and gearing having a ratio greater than 1:1. The gearing connects the handle with the drum. The gearing includes protruding means which can protrude from the drum or from the gearing. Rotation of the handle drives the protruding means to rotate the drum. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application relates to U.S. patent application Ser. No. ______ entitled GAS TURBINE FLOATING COLLAR and having Attorney Docket No. 2993-614US, filed simultaneously herewith, the specification of which is incorporated herein by reference.
TECHNICAL FIELD
[0002] The invention relates generally to gas turbine engine combustors and, more particularly, to a floating collar arrangement therefor.
BACKGROUND OF THE ART
[0003] Gas turbine combustors are typically provided with floating collars or seals to permit relative radial or lateral motion between the combustor and the fuel nozzle while minimizing leakage therebetween. The collar is subject to wear and heat, and is therefore cast/machined form a heat resistant material. As fuel nozzles, combustors and related components must be periodically removed for cleaning, inspection, repair and, occasionally replacement, the floating collar arrangement is provided in a manner which facilitates such removal, to thereby facilitate maintenance. Floating collar arrangements have become quite elaborate in the recent art, as designers continuously improve gas turbine efficiency. Such improvement, however, often comes at the expense of economical operation for the operator, as elaborate parts are typically more expensive to repair and replace. Accordingly, there is a need to provide a solution which addresses these and other limitations of the prior art, and in particular, there is a need to provided economical solutions to enable the emerging general aviation very small turbofan gas turbine market.
SUMMARY OF THE INVENTION
[0004] In one aspect, the present invention provides a gas turbine combustor floating collar assembly for receiving a fuel nozzle swirler body, the combustor having a nozzle opening defined in a dome thereof, the swirler body having an abutment shoulder extending therearound, the assembly comprising a mounting arrangement including a mounting flange spaced apart from the dome and circumscribing the opening, the flange fixedly bonded to the dome, and a cap spaced apart in an axial direction relative to the combustor from the mounting flange, the cap fixedly bonded to the mounting flange; and a floating collar slidably trapped between the mounting flange and the cap such that relative axial movement is substantially restrained but relative radial movement is permitted, the collar having a central aperture alignable with the dome opening and adapted for axial sliding engagement with the nozzle body, wherein the floating collar cannot be released from the mounting arrangement and the mounting arrangement cannot be released from the combustor without damaging at least one of the combustor, the mounting arrangement and the floating collar.
[0005] In another aspect, the present invention provides a method of providing a floating collar assembly on a gas turbine engine, the method comprising the steps of providing an assembly having a combustor with a nozzle opening defined in a dome thereof, a mounting arrangement including a sheet metal mounting flange, a sheet metal cap, and a sheet metal floating collar, the mounting flange, cap and floating collar each having a central aperture alignable with the dome opening, the floating collar aperture adapted for axial sliding engagement with a fuel nozzle air swirler body; fixedly bonding the mounting flange to the combustor dome in a spaced apart manner such that the flange central opening is generally aligned with dome opening; inserting the floating collar into the mounting flange; and fixedly bonding the cap to the mounting flange to thereby slidingly trap the floating collar between cap and the mounting flange.
[0006] Further details of these and other aspects of the present invention will be apparent from the detailed description and Figures included below.
DESCRIPTION OF THE DRAWINGS
[0007] Reference is now made to the accompanying Figures depicting aspects of the present invention, in which:
[0008] FIG. 1 is a schematic longitudinal sectional view of a turbofan gas turbine engine;
[0009] FIG. 2 is a partial sectional view of a combustor in accordance with an embodiment of the present invention;
[0010] FIG. 3 is an isometric view of a portion of FIG. 2 ; and
[0011] FIG. 4 is an exploded isometric view of FIG. 3 .
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0012] FIG. 1 illustrates a gas turbine engine 10 of a type preferably provided for use in subsonic flight, generally comprising in serial flow communication a fan 12 through which ambient air is propelled, a multistage compressor 14 for pressurizing the air, a combustor 16 in which the compressed air is mixed with fuel and ignited for generating an annular stream of hot combustion gases, and a turbine section 18 for extracting energy from the combustion gases.
[0013] FIG. 2 shows an enlarged axial sectional view of a combustor 16 having a liner 20 and a dome 22 having an exterior side 24 and a central opening 26 for receiving a air swirler fuel nozzle (depicted in stippled lines in FIG. 2 ) of the type generally described in U.S. Pat. No. 6,289,676 or 6,082,113, for example, and which are incorporated herein by reference. A mounting arrangement 28 is provided as will now be described.
[0014] An annular mounting flange 30 is fixedly bonded, preferably by a weld 32 , to the exterior side 24 of dome 22 , and includes an axially-disposed annular portion 30 a , a radially disposed annular flange portion 30 b , both defining a central aperture 34 therein. Central aperture 44 can be aligned with dome opening 26 when mounting flange 30 is mounted on the combustor. Mounting flange 30 may also include a plurality of legs 36 as will be described further below.
[0015] An annular cap 40 is provided and fixedly bonded, preferably by a weld 42 , to mounting flange 30 , preferably at legs 36 . Cap is provided in a spaced-apart manner relative to mounting flange 30 , as will be described further below. Cap 40 has a central aperture 44 which is aligned with dome opening 26 when mounted on combustor 16 and adapted to receive the fuel nozzle therein.
[0016] A floating collar 50 is provided having a axially-disposed nozzle collar portion 50 a , and a radially disposed annular flange portion 50 b , both surrounding a central aperture 54 , and a smooth transition 50 c joins portions 50 a and 50 b . Central aperture 54 and collar portion 50 a are provided for axially slidingly engaging a circumferential shoulder of the fuel nozzle swirler body (stippled lines in FIG. 2 ). Collar portion 50 a preferably extends to, or inside, dome 22 though opening 26 . Flange portion 50 b is trapped between opposed surfaces of mounting flange 30 and cap 40 , with mounting flange 30 and cap 40 being sufficiently spaced apart to permit radial (relative to the engine axis of FIG. 1 ) sliding motion to occur between floating collar 50 and mounting flange 30 /cap 40 . An anti-rotation tang 56 depends from flange portion 50 b and is likewise trapped between adjacent mounting flange legs 36 , to thereby limit the amount by which floating collar 50 may rotate relative to mounting flange 30 /cap 40 .
[0017] In use, the fuel nozzle air swirler (not shown) is positioned within central aperture 54 and delivers a fuel air mixture to combustor 16 . As forces acting upon the fuel nozzle and the combustor tend to cause relative movement therebetween, floating collar 50 is able to displace radially with the nozzle while maintaining sealing with respect to combustor through maintaining sliding engagement with mounting flange 30 and cap 40 . Welds 32 and 42 ensure that mounting flange 30 and cap 40 maintain their spaced-apart relation and thereby keep floating collar 50 trapped therebetween.
[0018] Referring to FIG. 4 , mounting arrangement 28 is assembled through a process involving at least the following steps: welding mounting flange 30 to combustor dome 22 so that the flange central opening 36 is generally aligned with dome opening 26 ; inserting floating collar 50 into the mounting flange 30 , so that the collar portion 50 a extends through central opening 36 and is generally aligned with dome opening 26 , and preferably also so that anti-rotation tang 56 is trapped between two closely adjacent legs 36 ; and welding cap 40 to mounting flange 30 , preferably at legs 36 , to slidingly trap the floating collar between cap and the mounting flange. The order of operations may be any suitable, and need not be chronologically as described.
[0019] Mounting arrangement 28 and floating collar 50 are preferably provided from sheet metal using a suitable fabrication process. An simplified example process is to provide a sheet of metal, cut a blank, and perform at least one bending operation to provide the floating collar. Referring again to FIG. 2 , it is evident that a sheet metal collar 50 has a continuous transition 50 c is provided as a result of a sheet metal forming operation, such a bending, and helps strengthen the collar 50 . Unlike prior art collars made by investment casting and/or machining processes (see U.S. Pat. Nos. 4,454,711, 4,322,945 and 6,497,105, for example), the present invention's use of sheet metal advantageously permits a very light weight and inexpensively-provided part, due to its simple geometry, and yet provides good performance and reliability.
[0020] Unlike the prior art, the mounting assembly of the present invention is geometrically simple, lightweight, easy to manufacture and east to assemble. Contrary to the prior art which teaches providing a high-cost device which facilitates replacement, the design and method of the present invention instead has relatively low initial cost, which assists in providing a lower-overall cost to the gas turbine engine, thereby facilitating the provision of an affordable general aviation turbofan engine, for example. As well, because the initial cost is lower, the cost of replacement may also be lowered.
[0021] The above description is meant to be exemplary only, and one skilled in the art will recognize that changes may be made to the embodiments described without departing from the scope of the invention disclosed. For example, the present invention may be applied to any gas turbine engine, and is particularly suitable for airborne gas turbine applications. The means by which flange 30 is mounted to cap 40 may be different than that described. For example legs 36 may be replaced or supplemented with a continuous or discontinuous flange or lip, and/or may extend from flange 30 , cap 40 or both. The mode of anti-rotation may be any desirable. Though welding is preferred, brazing or other bonding methods may be used. Other modifications which fall within the scope of the present invention will be apparent to those skilled in the art, in light of a review of this disclosure, and such modifications are intended to fall within the equivalents accorded to the appended claims. | A simplified floating collar mounting arrangement is provided comprising a collar mounted between spaced-apart mounting flanges. The arrangement offers reduced part count and simplicity, and therefore improves reliability. | 5 |
BACKGROUND OF THE INVENTION
AND DESCRIPTION OF RELATED ART, INCLUDING INFORMATION DISCLOSED UNDER 37 C.F.R. 1.97-1.99
Power door drives or operators for mass transit vehicles are in widespread use throughout the world. The systems now in use can be broadly divided by the specific energy source for the system prime mover or door drive. The invention disclosed herein pertains generally to door drives employing electrically powered devices as prime movers.
Generally speaking, electrical drives utilize highly reliable rotary electric motors operating doors through intermediate devices. These intermediate devices convert rotary motion of the drive motor to linear and/or other movement required to move the vehicular door panels. Intermediate devices as contemplated herein can further be categorized as mechanical linkages or rotary helical drive systems.
While reliable and reasonably cost effective, a major shortcoming of the above described drive systems lies in need for an intermediate component between the prime mover and door panel. At a time where system reliability is an increasingly important factor in choosing door systems, the use of a prime mover such as a linear induction motor which directly drives the panels, essentially eliminates much of the intermediate linkages, thereby substantially increasing the reliability of the overall system.
Linear induction motor (LIM) drives have been proposed as door panel drives for some time. U. S. Pat. No. 1,950,627 discloses and claims such a system. However, as disclosed in U.S. Pat. No. 1,950,627 the system as disclosed, generally speaking, would be inoperative and/or impractical due to the space and power limitations currently present in mass transit vehicles.
Further, previous innovations disclosed under prior art patents using LIM drives did not contemplate other requirements mandated by public transportation car manufacturers and municipal or federal authorities. Additional requirements such as: reliable mechanical lock device, immunity against iron dust with simplified mechanical design resulting in reduced maintenance, ability to conform to a restricted mounting space and envelope, door panel obstruction detection capability, reliable emergency door opening mechanism and smooth door opening and closing speed profile.
Applicant, however, has discovered an approach to integrating presently available linear induction motors into modern complex door control systems required by today's transit authorities.
It is, therefore, an object of the invention disclosed herein to provide a door control system for mass transit vehicles wherein the combination of electrical control and door drive components has high reliability through reduction in the number of components employed.
It is an additional object of the invention to provide a door drive wherein the prime mover drive forces are directly applied to the drive panel.
It is a further object of the invention disclosed herein to provide a door drive prime mover wherein components intermediate the prime mover energy source and drive door panel are reduced to one moving part.
It is yet an additional object of the invention to provide an electronic control for a linear induction motor door drive wherein door edge force and door speed are controlled with direct electromechanical devices.
It is an additional object of the invention to provide a door drive incorporating a LIM motor having drive powered door opening lock.
SUMMARY OF THE INVENTION
A double side linear induction motor is used to move a public transportation car door. A closed control loop via a variable voltage, variable frequency inverter and a computerized algorithms or other suitable control modes, including pulse width modulation of the LIM prime mover, achieve the desired speed/travel profile of the door panel motion. The total weight of the door is supported by a linear bearing hanger. A sealed rotary incremental optical encoder actuated by the LIM motor transport part or rod indicates, through use of algorithms, the instantaneous door panel position. Door signals from the encoder are processed to get the door panel speed information.
A mechanical device integrated into the LIM transport rod assembly ensures locking the door panel at fully closed position. Unlocking this latter mechanism is achieved by the further motor transport part movement. A mechanical limit switch is mounted on the lock mechanism to inform the control algorithms on the door status.
A double side linear induction motor is mounted overhead of, and magnetically coupled to, a movable door panel. The panel is independently attached to a suitable hanger and the hanger in turn is journaled for motion along a door panel support.
The linear induction motor stator or stationary component is suitably attached to the car structure overhead and adjacent to the door hanging system. The linear induction motor transport rod or movable armature is attached to the above described hanger. Since the transport rod moves only parallel to the half of the door traveled, efficiency of the drive is high and requires no intermediate components.
As coupling between the linear induction motor stator and transport rod is magnetic, door panel breakaway force is limited and controllable independent of the door speed. This feature reduces potential passenger hazards and mechanical wear on the overall drive system.
Movement and location of the transport rod is sensed and indicated by a simple counter operated by a portion of the transport rod. Operation of the door drive by the linear induction motor drive is therefore controllable by relative simple, highly reliable electrical components including relays and/or power electronic devices.
A novel lock secured to the linear induction transport rod secures the rod and thereby the door panel to the operator base plate through the action of a spring latch carried on the transport rod and a lock pin on the baseplate after panel locking. Unlocking is achieved by lost motion of the latch in relation to the transport rod when driven in the door opening direction after locking has been completed.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects and advantages of the invention will become apparent upon reading the following detailed description and upon reference to the drawings in which:
FIG. 1 is a pictorial block diagram showing a configuration of the invention utilized to drive by-parting sliding doors, including a diagrammatic showing of the location of the door locks and door position sensor for a door closed condition.
FIG. 2 is a pictorial block diagram particularly showing a view of the left hand door of FIG. 1 with the operator in place, particularly showing a complete hanger.
FIG. 3 is a perspective view of the door drive of the invention in situ, partially showing a transit vehicle wherein the door drive is located in the transit car overhead.
FIG. 4 is a partial or tearaway section of FIG. 3 showing the operator of the invention in position over the door of FIG. 2 for a door closed condition, particularly showing the linear induction motor, its transport rod and associated motion sensor, attached to one door panel in a door closed and locked condition.
FIG. 5 is a partial section along line 5--5 of FIG. 3, particularly showing the guide/support structure for sliding doors as disclosed.
FIG. 6 is a partial view of the door drive of the door system of FIG. 1, particularly showing the relationship between the linear induction motor drive transport rod and lock members for a single door panel in a door open position.
FIG. 7 is a further view of the door panel of FIG. 6 in a door closed position.
FIG. 8 is a partial view of the door system panel lock and manual panel release assemblies showing the panel lock components as associated with the LIM transport rod and operator baseplate for a panel unlocked condition.
FIG. 9 is a view of the panel lock components of FIG. 8, for a closed panel condition with lock components immediately prior to a fully locked condition.
FIG. 10 is a further view of the lock components of FIG. 9, particularly showing the lock in an engaged condition.
FIG. 11 is a further partial view of the lock components of FIG. 10, particularly showing operation of the emergency cable release from a locked condition.
FIG. 12 is an additional partial view of the lock components of FIG. 11, particularly showing unlocking by action of the emergency cable.
FIG. 13 is an exploded partial tearaway view of the lock and emergency release mechanism, particularly showing spatial relationship of lock components and the operator baseplate.
FIG. 14 is a further partial tearaway view of the emergency mode of components, particularly showing emergency unlocking.
FIG. 15 is a sectional view of the operator of the invention in place above the opening of FIG. 3, and along line 15--15 of FIG. 7, particularly showing door hanger, LIM components, and transfer rod.
FIG. 16 is a further sectional view of the operator along line 16--16 of FIG. 7, particularly showing the LIM transfer rod operator baseplate and lock components.
FIG. 17 is a further sectional view of the operator along line 17--17 of FIG. 7, particularly showing the LIM transfer rod attached to the door hanger.
DETAILED DESCRIPTION OF THE INVENTION
In reference to FIGS. 1 and 2, there is shown in semi-diagrammatic form a door drive system 1 including a door controller 5 having a logic unit 12 and individual panel drive controllers 9. The drive unit 5 provides controlled power to a linear induction motor door drives 16, thereby moving door panels 17 and 18, over and away from an aperture in a car body 3 (reference FIG. 3). Panels 17 and 18 include windows 14 and sealing edges 19. Panels 17 and 18 are further slidably mounted for motion over and away from an aperture in the car body through upper end attachment via door hangers 24 to a door hanger rod 20. The door hanger rod 20 is attached to the car body 3 via hangers 21.
Reciprocal motion of doors 17 and 18 over an aperture 4 in the car body 3 is obtained through force exerted by linear induction motor (LIM) actuator assemblies 16 via a LIM transfer rod 26, also attached to door hanger 24. Information relating to the position of each door panel 17 or 18 is transmitted to the logic unit 12 via a suitable distance measuring transducers 22 and 23, thereby supplying the controller 5 with information describing door panel travel when powered by LIM actuators 25 and 30.
In more particular reference to FIGS. 4, 5 and 6, the lower edge of door panels 17 and 18 is slidably contained in a slot (reference FIG. 5) in the car body 3. In reference to FIG. 4, with the door panel 17 in a fully closed position, the transfer rod 26 of LIM actuator 25 has moved door lock assembly 40 into a locked condition, securely maintaining panel 17 in a door closed position. Similarly, (reference FIG. 7) right hand LIM actuator 30 has, in moving panel 18 to a closed position, extended LIM transfer rod 26 and actuating lock assembly 34, thereby maintaining door panel 18 in a securely closed position.
Incorporated and adjacent to lock assembly 34 is a manual door lock release assembly 50 (reference FIGS. 6 and 11). Since the operation of the manual door release assembly involves operating elements of the primary door lock assembly 40, description of the interaction will proceed as adjunct to operation of the primary lock assembly 40. It should be noted that as the right hand and left hand lock assemblies are identical, other than a reversal of parts for each individual LIM door drive, the following description will proceed by following movement of the right hand panel 18 from a fully opened position (reference FIG. 6) to a fully closed position (reference FIG. 7).
It should also be noted that positioning of door lock and manual unlock components on opposite sides of the LIM actuator transfer rod 26 require occasional referral to exploded and detailed drawings of the lock components and interrelations depicted on FIGS. 11, 12, 13, and 14.
Door lock and manual unlock assemblies 34 and 50 for panel 18 in a fully opened position are best shown in FIG. 8 with further reference to exploded and detailed component drawings shown in FIGS. 13 and 14. With reference to FIG. 8, there is shown lock pawl 42 mounted for rotatable movement on and along lateral movement of transfer rod 26 by pivot pin 43. Additional movement of lock cam 42 around pivot pin 43 is restrained by unlock pin 44 acting through aperture 48 in transfer rod surface 27 (partially shown). Lock cam 42 is also controlled by spring 46 affixed to the lower end of lock cam 42 and attached to transfer rod 26 so as to maintain a predetermined rotational force bias on the position of lock cam 42 as retained by the combination of pin 44 and slot 48 (as shown in FIG. 8).
Adjacent the opposite end of transfer rod 26, lock pin 41 is suitably attached to the operator base plate 29 (reference FIGS. 13 and 16). Also attached to base plate 29 (reference FIG. 13) is limit switch bracket 39 and limit switch 38 (as shown). Limit switch 38 includes a suitable operating arm in order to co-act with the lock cam 42, thereby signaling the door in a fully closed position.
The manual release assembly 50, essentially attached to base plate 29 includes a door release actuating arm 52 mounted for pivotal motion around pin 53. Pivotal motion of arm 52 is controlled by bias spring 58, maintaining the arm in an unactuated position. Located at an appropriate position along arm 52 there is a bracket 54 rotatably attached to arm 52 by pivot 59. Bracket 54 is contained in baseplate slot 60. The opposite end of bracket 54 has one end of release cable 56 attached thereto. Slot 61 in baseplate 29 is provided for adjustment of the manual release assembly operation. Similarly, slot 48 in baseplate 29 is provided for adjustment of the operating position of lock pin 41 when coacting with lock cam 42. The significance of this will be discussed below.
Turning to FIG. 8, operating elements of primary lock assembly 34 are shown in door open, unlocked condition. Lock cam 42 is shown with its unlock pin 44 engaged in the furthermost left hand position of slot 48. Spring 46 provides a predetermined amount of force maintaining cam 42 (as shown) and ensuring that future lock condition is maintained.
Turning now to FIG. 9 where the transfer rod 26 has moved the left hand panel into a door closed position by actuation of the LIM actuator 25, lock pin 41 has rotated cam 42 around pivot 43 in a counterclockwise direction allowing lock pin 41 to enter lock pin slot 49. In FIG. 10, the locking action has been completed with lock pin 41 securely held in slot 49 through the action of spring 46. Note that unlock pin 44 has returned to its initial position shown in FIG. 8. This essentially completes the locking action of the door drive system.
Unlocking of the previously locked door panel is obtained by energizing the LIM actuator so as to propel the transfer rod 26 in a direction 62 opposite to that shown in FIG. 9. Movement of transfer rod 26 in a direction 62 (reference FIGS. 9 and 10) exerts a force against lock pin 41 and the left hand edge of slot 49 in lock cam 42. When the force 62 exceeds a predetermined value, a force couple developed between lock pin 41 affixed to the operator baseplate and pivot 43 affixed to the transfer rod 26 provides counterclockwise rotation of cam 42 such that pin 44 moves to the right hand portion of slot 48 in transfer rod 26 (reference FIG. 9). The counterclockwise rotation of cam 42 disengages lock pin 41 and slot 49, thereby allowing transfer rod 26 to move toward an open position (reference FIG. 6). Operation of the right hand or opposite panel of the door system of the invention is identical and will not be separately described.
Operation of the manual door lock release is accomplished through the action of pivoting lever 52 (reference FIG. 11) in response to a force exerted on member 54 contained in slot 60 for limited movement therein (reference FIG. 13) and pivotally attached to lever 52 at pivot 54. On application of force from cable 56 through handle sufficient to overcome the force exerted on the lower end of lever 52 by spring 58, lever 52 rotates around pivot 53 attached to baseplate 29, into a position where it contacts unlock pin 51 (reference FIGS. 13 and 14). Further movement of cable 56 at a predetermined force rotates lock cam 42 around pivot 43 within the limits provided by slot 48 in the transfer rod 26. Movement of unlock pin 51 such that door unlock pin 44 occupies the position shown in FIG. 9, wherein lock pin 41 and slot 49 are disengaged, allowing manual movement of door panels to an open position. | Automatic door system for mass transit vehicles utilizing a linear induction motor for powering door panels from open to closed. A power actuated panel lock provides positive panel locking and unlocking through actuating the prime mover. | 4 |
CLAIM OF PRIORITY
[0001] The present application claims priority from Japanese application JP 2004-112654 filed on Apr. 7, 2004, the content of which is hereby incorporated by reference into this application.
BACKGROUND OF THE INVENTION
[0002] 1. Field of Invention
[0003] The invention relates to a track forming method for forming a substantially spiral information track on an disc-shaped information recording medium, and a information recording method for recording information on an information recording medium.
[0004] 2. Related Art
[0005] Various methods for forming tracks on an optical disc have been proposed, such as those disclosed in JP Patent Publication (Kokai) No. 60-50733 A (1985) and JP Patent Publication (Kokai) No. 61-13458 A (1986), for example. In these known examples, the light emitted by a laser light source 1 is separated by a beam splitter 2 into guide groove recording light 100 and header recording light 200 , as shown in FIG. 4 . These beams of light are composed after being intensity-modulated in accordance with relevant signals by optical modulators 4 and 3 driven by signals G and H, respectively, sent from a signal source 15 . The composed beam of light irradiates a photosensitive layer 13 formed on a disc 12 via a lens 9 and a recording lens 10 so as to record the signals on the photosensitive layer. In order to form a header signal between guide grooves, guide groove recording light 100 is tilted by mirrors 8 and 8 ′ by a required angle such that the guide groove recording light 100 is incident on the lens 9 at an angle with respect to the header recording light.
Patent Document 1: JP Patent Publication (Kokai) No. 60-50733 A (1985) Patent Document 2: JP Patent Publication (Kokai) No. 61-13458 A (1986) Patent Document 3: JP Patent Publication (Kokai) No. 63-308745 A (1988)
SUMMARY OF THE INVENTION
[0009] In the aforementioned track forming method, a spindle 14 is moved by a distance corresponding to the track pitch before the disc makes a complete rotation. In order to obtain a uniform track pitch, it is necessary to control the amount of movement in a continuous (smooth) and highly accurate manner. For this purpose, a dedicated master manufacturing machine with a highly accurate feed capability has been employed. Such a machine, however, is very expensive. Therefore, the tracks formed by the aforementioned method are typically transferred to a plastic substrate, for example, by injection molding or the 2P process. However, injection molding requires a substrate with a thickness of 0.1 mm or more, with the result that when substrates formed by injection molding are stacked into a multilayered laminate, the thickness of the laminate becomes too large. Furthermore, the 2P process requires performing the transfer of the tracks for individual layers, resulting in an increase in manufacturing cost. It is also difficult to achieve a high positioning accuracy.
[0010] Another technique is disclosed in JP Patent Publication (Kokai) No. 63-308745 A (1988) whereby, after the recording grooves are formed, a photosensitive agent is reapplied, and then the grooves are further processed while performing a tracking with reference to the initially formed grooves. In this method, the required accuracy is not so high because the cutting is performed while tracking the initially formed grooves during the second processing. However, this is after all a technique whereby the initially recorded regions are further processed into more complex shapes, so that it does not help reduce the labor and cost involved in the initial processing (cutting).
[0011] Namely, this technique also involves the transfer of the tracks onto a plastic substrate or the like by injection molding or the 2P process, as in the earlier example, and it does not solve the aforementioned problems of the prior art.
[0012] Referring to FIG. 3 , an example of a conventional optical recording system for recording and reproducing an optical disc with tracks formed by the conventional method will be described.
[0013] FIG. 3 shows a block diagram of a conventional optical recording and reproducing apparatus. A laser light source 25 (with the wavelength of approx. 660 nm in the case of DVD-RAM), which forms a part of a head 19 , emits light. The light is collimated into substantially parallel optical beams 22 by a collimating lens 24 . The optical beams 22 irradiate an optical disc 18 via an objective lens 23 , forming a spot 21 . Thereafter, the beams are guided to a servo detector 26 and a signal detector 27 via a beam splitter 28 and a hologram element 29 , for example. The signals from each detector are summed or subtracted to produce servo signals, such as a tracking error signal and a focus error signal, which are then inputted to a servo circuit. The servo circuit, using the obtained tracking error signal and focus error signal, controls a drive means 31 for the objective lens 23 or the position of the entire optical head 2 such that the optical spot 21 can be positioned at a target recording or reproducing region. A sum signal from the detector 27 is fed to a signal reproduction block 41 . The input signal is filtered and frequency-equalized by a signal processing circuit and is then digitally processed. The digital signal is then processed by an address detection circuit and a demodulation circuit. Based on an address signal detected by the address detection circuit, a microprocessor calculates the position of the optical spot 21 on the optical disc 18 and then controls an automatic position control means, such that the optical head 2 and the optical spot 21 are positioned at a target recording unit region (sector).
[0014] In the case where a higher-level device directs the optical recording and reproducing apparatus to record, the microprocessor receives recording data from the higher-level device and stores it in a memory, while controlling the automatic position control means to position the optical spot 21 at a target recording region. The microprocessor, after confirming that the optical spot 21 has correctly been positioned at the recording region based on the address signal from the signal reproduction block 41 , controls a laser driver, for example, to record the stored data in the target recording region.
[0015] As described above, in accordance with the conventional cutting method, the manufacturing cost increases if the recording layers are to be multilayered for greater capacities, and it is difficult to reduce the eccentricity among the layers due to their relative positioning errors.
[0016] It is an object of the invention to provide a track manufacturing method capable of forming a tracking groove or mark with hardly any increase in cost when the number of recording layers is five or more.
[0017] In order to achieve the aforementioned object, the invention provides the following means.
(1) A disc-shaped optical recording medium is irradiated at least with a first optical spot and a second optical spot, and a tracking mark or a guide groove is formed using said second spot while performing a tracking using said first optical spot. In this way, tracks can be formed accurately using the second spot while using the first spot as a guide. Thus, it becomes possible to manufacture media with narrow-pitched tracks without requiring a highly accurate cutting device as in the conventional, thereby reducing manufacturing cost.
[0019] This feature is particularly advantageous in the case of multilayered media, as it reduces the eccentricity between layers. Although the above means makes reference to the formation of tracks, the step of forming tracks may comprise the recording of information if the track formation and the recording mark formation are performed in the same step, as in the cases of the pits in ROMs or write-once media, for example.
(2) The same recording surface is irradiated with said first optical spot and said second optical spot, and the distance between the first spot and said second spot in the radial direction is substantially equal to an integer multiple or ½ of an integer multiple of the track pitch. In this way, a spiral track can be formed continuously. (3) A tracking mark or guide groove is formed on a recording surface of the medium in advance, making at least one complete rotation. The optical recording medium comprises a plurality of recording surfaces, and different recording surfaces are irradiated with said first optical spot and said second optical spot. In this way, the medium can be shipped after recording it with only the initial, complete-circled track, so that the media manufacturing cost can be significantly reduced. (4) A tracking mark or a guide groove is formed in advance on only one of the multiple recording surfaces.
[0023] In this way, the need to form the guide groove in all of the layers in a multilayered medium in advance can be eliminated, thereby reducing the media manufacturing cost.
(5) Address data or user data is recorded simultaneously with the formation of the tracking mark or guide groove. (6) A track forming method for a disc-shaped optical information recording medium, comprising forming a spiral or concentric track making at least one complete rotation, and then forming the remaining tracks using the earlier-formed track for tracking purposes. In this way, the optical disc manufacturing cost can be significantly reduced.
[0026] Although the aforementioned means involve the formation of two spots, tracks can be easily formed using a conventional apparatus.
[0027] In accordance with the invention, prewriting of the media prior to shipping can be performed in a short time, so that the media manufacturing cost can be significantly reduced.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 shows the principle of forming a track in an embodiment of the invention.
[0029] FIG. 2 shows a recording medium in an embodiment of the invention.
[0030] FIG. 3 shows an example of a conventional recording apparatus.
[0031] FIG. 4 shows an example of a conventional disc manufacturing apparatus.
[0032] FIG. 5 shows the principle of another embodiment of the invention.
[0033] FIG. 6 shows a block diagram of an apparatus according to an embodiment of the invention.
[0034] FIG. 7 shows the shapes of tracks in examples of the invention.
[0035] FIG. 8 shows an example of an optical head in an embodiment of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Embodiment 1
[0036] FIG. 1 (left) shows an initially prewritten track 182 formed on a disc. The track may be formed by a variety of ways, as descried in the subsequent embodiments. The following description is based on the assumption that there is the prewritten track on the disc. The track 182 that has been prewritten is tracked using a first optical spot 211 so that the first optical spot 211 and a second optical spot 212 can be disposed on the track 182 . When the radial distance between the first and the second optical spots is equal to the track pitch, which is approximately 0.32 μm in the present embodiment, the second spot would be automatically disposed on the prewritten track 182 . As the disc rotates, the optical spots 211 and 212 move relative to the disc in the direction indicated by the arrow, and the second spot 182 comes to a region where no tracks are formed. By irradiating the medium with a light beam with an intensity such that a recording mark can be formed on the medium, a track 181 is additionally formed. By repeating this process, tracks can be formed sequentially up to the periphery of the disc.
[0037] FIG. 2 shows an optical disc 18 with an inner region 181 where tracks are formed and a peripheral region 180 where no tracks are formed.
[0038] Although in the present embodiment it is assumed that the disc is recorded from the inner side thereof sequentially, the same effect would be obtained when recorded from the peripheral side. In the latter case, the first optical spot would be disposed towards the radially peripheral side of the disc. The radial distance between the first and second optical spots is equal to the track pitch, or 0.32 μm. The circumferential distance between them, which is not so important, is typically on the order of 10 μm so that they can be sufficiently resolved on a detector.
[0039] FIG. 6 shows a block diagram of an embodiment of an optical recording apparatus adapted to the invention. A laser light source 25 (with the wavelength of approx. 405 nm in the present embodiment), which forms a part of a head 19 , emits light that is collimated into substantially parallel optical beams 22 by a collimating lens 24 . The beams of the first-order diffracted light are then slightly deflected by a blazed diffraction grating 29 . Thereafter, the optical beams 22 irradiate the optical disc 18 via an objective lens 23 , thereby forming two spots on the optical disc 18 . The ratio of intensity of the first optical spot 211 and the second optical spot 212 was adjusted to be approximately 1:10. This ensures that the intensity of the first spot is sufficiently small when recording with the second spot, thus preventing the destruction of the tracks that have been previously formed. Thus, the intensity of the second spot is preferably smaller than that of the first spot. Reflected light from the two optical spots is guided to a servo detector 26 and a signal detector 27 or the like via a beam splitter 28 , for example. Although not shown in the drawing, there are actually two sets of the servo detector 26 and signal detector 27 , one set detecting information in the reflected light from the first optical spot and the other from the second optical spot.
[0040] Immediately prior to recording, namely, in the state shown to the left of FIG. 1 , the servo signal is derived from a signal detected from the first optical spot, while a read signal is derived from a signal obtained from the second optical spot, so that the data that is recorded using the second spot can be timed with the immediately preceding data. Once the recording starts, the signal detector 27 is switched to the first optical spot. In this way, the information in the immediately prior track (one track earlier) can be read, and it can be confirmed continuously that the recording is taking place correctly and that the right track is being recorded. Thus, a highly reliable recording can be performed. Should the immediately earlier track be unable to be normally read due to fingerprints or a scratch on the disc surface, the recording apparatus shown in FIG. 3 reports it to the higher-level device as a recording error. If it turns out, based on the immediately subsequent reading, that reading is possible but the recording power is rather lacking, for example, the recording power is corrected. This means that a real-time power control can be made using the immediately subsequent optical spot. In the illustrated example, however, because the first and second optical spots utilize the light emitted by the same laser 25 , the second optical spot is modulated in one way or another during recording. Therefore, detection of the address information would become easier if it is superposed on the data signal as a low-frequency component. It goes without saying that the reliability would be further improved by simultaneously recording the address signal as normal data.
[0041] The servo detector detects the servo signal obtained from the first optical spot. Signals from the individual detectors are summed or subtracted to produce servo signals, such as a tracking error signal and a focus error signal, which are then fed to a servo circuit. The servo circuit, using the tracking error signal and focus error signal, controls a drive means 31 for the objective lens 23 and the position of the entire optical head 2 , such that the first optical spot 211 can be positioned at the target recording or reproducing region. A sum signal from the detectors 27 is fed to a signal reproducing block 41 . The thus input signal is filtered, frequency-equalized, and then digitalized by a signal processing circuit. The digitally processed signal is further processed by an address detection circuit and a demodulation circuit. Using the address signal detected by the address detection circuit, the microprocessor calculates the position of the optical spot 21 on the optical disc 19 and controls an automatic position control means such that the optical head 2 and the optical spot 21 can be positioned at the target recording unit region (sector).
[0042] In the case where the instruction from the higher-level device to the optical recording and reproducing apparatus is that for recording, the microprocessor receives recording data from the higher-level device and stores it in memory, while controlling the automatic position control means such that the optical spot 21 can be positioned at the target recording region. The microprocessor, after confirming from the address signal from the signal reproducing block 41 that the optical spot 21 has correctly been positioned at the recording region, controls the laser driver or the like, thereby recording the stored data in the target recording region.
Embodiment 2
[0043] FIG. 5 shows the arrangement of the optical spots in another embodiment of the invention. In this embodiment, the optical recording medium is a multilayered recording medium. In this case, a pre-pit or a pre-groove is formed with an irregular pattern or the like in one of the layers of the multilayered recording surface, in the form of a (initial) servo plane. The first spot is focused on the servo plane for tracking, while the second spot is focused on another plane. At this point in time, the servo plane is used for tracking. Then, the information recorded on the plane opposite to that for the reading is tracked. Tracking is performed based on the information in the tracks formed on the plane because the information on the servo plane and that on the data plane might be displaced should the disc be tilted, for example, as shown in the right hand side of FIG. 5 . In consideration of the possibility that the disc could be warped by heat, for example, during recording, the present method is preferably combined with the method of Embodiment 1. Namely, after forming several to several dozens of tracks on a separate plane by utilizing the servo plane, additional tracks are formed while preferably performing tracking based on the data in adjacent tracks on the same plane, as in Embodiment 1.
Embodiment 3
[0044] FIG. 7 shows an example of tracks formed in accordance with the present invention.
[0045] FIG. 7 ( a ) shows a case where data is recorded in the form of a string of completely randomly modulated marks, as in CDs or DVD-ROMs, in which tracking is performed by DPD or the push-pull method. In this case, because data is recorded in the form of sector IDs in the address data mark string, for example, the first optical spot and the second optical spot must be each positioned at the center of a particular track. Thus, the spot intervals in the radius direction would be an integer multiple of the track pitch.
[0046] FIG. 7 ( b ) shows another case where servo regions 500 aligned in the radial direction are allocated, in which tracking can be performed using a sample servo. The address information is read in the form of a gray code or CAPA (Complimentary Allocated Pit Address). Thus, the spot intervals of the first optical spot 121 would be a half-integer multiple of the track pitch.
[0047] FIG. 7 ( c ) shows an example where a continuous groove tracking is performed. In this case, two methods can be employed. Namely, in a first method, a continuous groove 510 and an address portion 501 are formed by a leading spot (second spot 212 ), and thereafter, the trailing spot (first spot 211 ) is used for forming a mark 511 . In a second method, the continuous groove 510 and the address portion 501 are formed by the leading spot (second spot 212 ) and a formatting is performed, followed by the recording of data in the form of the mark 511 . In the case of the first method, although it is required that both optical spots can be modulated independently, formatting and recording can be performed simultaneously. In the case of the second method, recording can be performed solely with the leading spot, so that the aforementioned method whereby the intensity ratio of leading spot and trailing spot is fixed by the diffraction grating can be adopted. In the second method, there is a degree of freedom for the apparatus manufacturer to choose the same formatting depending on the apparatus cost and application. In this case, the address portion 501 may simply employ CAPA.
Embodiment 4
[0048] In the present embodiment, methods of pre-writing are described. In a first method, the medium is preformatted using an apparatus similar to the conventional, so-called cutting machine shown in FIG. 4 at the factory, for example, prior to shipping. In this case, only several to several dozens of tracks are preformatted per disc, so that each disc requires several seconds for processing, and the increase in cost by introducing the machine into the production line would be minimum. In another method, the prewriting is performed on the drive on the user's end.
[0049] This method requires a mechanism for dynamically adjusting the intervals of the two spots in the radial direction (such as a diffraction grating rotating mechanism). In a first step, a complete track is formed using only the leading spot without tracking. In a second step, the thus formed concentric track is tracked using the first spot (trailing spot), while controlling the radial distance between the first spot and second spot to be increased by the track pitch, in synchronism with the single rotation of the disc. By so doing, a complete spiral track can be formed. In this case, the first spot and the second spot are spaced apart by more than one track. Furthermore, since there is the possibility that the initial concentric track cannot be formed properly due to vibrations or the like, the quality of the track is preferably checked by way of the tracking signal quality after the formation of the track.
[0050] In the case of concentric tracks, instead of spiral tracks, although tracks can be formed by jumping from one complete concentric track to another without utilizing the spot interval adjusting capability, such a process is not suitable for continuous or high-speed recording because it would result in overhead costs for the track-jumping procedure.
Embodiment 5
[0051] In the present embodiment, tracks are formed using two beams from two independent laser light sources. FIG. 8 shows an optical system equipped with the relevant capability. The disc is irradiated with two beams, namely, left-hand and right-hand circularly polarized light. Two semiconductor laser light sources 611 and 612 emit linearly polarized light beams, which are passed through diffraction gratings 641 and 642 . One of the beams has its plane of polarization rotated by 90° by a ½ wavelength plate 651 . The two beams of light are composed into a substantially single luminous flux by a polarizing beam splitter (PBS) 66 . The polarizing beam splitter (PBS) 66 has a property such that it reflects the light with the polarization direction of laser 612 while letting through the light with the polarization direction that has been rotated by the wavelength plate 651 . By “substantially single” above is meant that the angles of the two luminous fluxes are slightly different. When the composed light is converted into circularly polarized light by a ¼ wavelength plate 69 , because the polarized planes of the light coming from the light source 611 and that from the light source 612 are perpendicular to each other, they are converted into different, namely, left and right, circularly polarized light. The light is shone on the medium 18 via a foldup mirror 67 and an objective lens 68 , thereby forming two circularly polarized light spots. These circularly polarized light spots are slightly displaced by the aforementioned slight angular difference. Even where they are superposed, their polarization states are different, such that there is no possibility that the spot shapes might be deformed by interference. Thus, the distance between the spots can be determined arbitrarily. When reflected by the recording medium 18 , the right-circularly polarized light is converted into left-circularly polarized light, while the left-polarized light is converted into right-polarized light by the mirror effect. Thus, once the reflected light passes through the ¼ wavelength plate 69 , its polarization is perpendicular to the original polarization. As a result, the light is caused by the polarizing beam splitter (PBS) to travel back in a different direction from the original direction of the light source. The returning light is then guided by the diffraction gratings to the multi-segment detectors 621 and 622 , from which servo signals for auto-focusing or tracking, as well as a read signal and push-pull signal, are produced. In the present embodiment, the positional relationship between the two spots was adjusted at a position that is slightly rotated from the original position of the ¼ wavelength plate 9 . In this way, the return light beams can be caused to be incident on the same detector without being completely separated. Thus, by adjusting the position of the beams on the detector, the two beams can be accurately positioned. In practice, the amount of displacement of the two spots can be calculated from the amplitude of a push-pull signal that is obtained when the two beams are turned on and off alternately on a push-pull detector. This technique was adopted in the present embodiment for automatic adjustment purposes.
[0052] In the present embodiment, the light source consists of two semiconductor lasers with a wavelength of 405 nm. Light emitted by the light source is focused by an objective lens with the aperture ratio (NA) of 0.85 on the recording medium, thereby forming two adjacent optical spots thereon, each spot measuring approximately 450 nm in diameter. | The increase in manufacturing cost that would result if a tracking pattern is transferred to all of the layers of a multilayered recording medium is prevented. A servo pattern is formed in a part of the medium in advance, and then servo patterns are additionally formed with one of two optical spots while performing a tracking using the other optical spot. Prewriting of the media prior to shipping can be performed in a short time, so that the manufacturing cost of the media can be significantly reduced. | 6 |
BACKGROUND OF THE INVENTION
Various methods are proposed for manufacturing optical fiber glass in a continuous process. One method is that disclosed in U.S. Pat. No. 3,957,474 assigned to Nippon Telegraph and Telephone Public Corp. This method involves the deposition of the glass forming ingredients on a heated mandrel to form a fiber optic preform.
The method described in U.S. Pat. No. 3,614,197 assigned to Semiconductor Research Foundation describes the process of using a multi-stepped funnel-shaped heating vessel to form a solid glass rod which is subsequently heated and drawn into an optical fiber. Both the heated mandrel and the heated crucible process provide continuous means for forming optical fiber glass into a solid glass preform but do not suggest forming the optical fiber per se in an in-line continuous process where the raw materials are fed into one end of the process while a finished optical fiber is continuously drawn from the other end.
It was first believed that the formation of a solid optical fiber preform as a separate step in the fiber manufacturing process provided certain beneficial results. The rod could be tested for optical transmission properties as well as geometric uniformity before being drawn into a fiber. These measurements could be used to select the best candidates from a number of fiber optical preforms before investing time and effort into drawing large quantities of the resultant optical fibers.
The purpose of this invention is to provide methods and apparatus for forming high strength and high purity optical fibers in a single continuous manufacturing operation.
SUMMARY OF THE INVENTION
Starting materials for high purity, high strength optical fibers are distilled into a specially designed high temperature container which allows the materials to be co-deposited without intermixing in a continuous flow. The materials are distilled into a vapor phase and are rapidly deposited by a localized R.F. glow discharge. The energy is also provided to heat the ingredients to a liquid state for drawing through a controlled orifice into an optical fiber within an enclosed chamber. The fiber is optionally treated by a filtered oxygen jet stream to cool the liquid and to exclude any air borne dust particles from the solidified fiber surface. Other features include the use of a fluorine gas flow to prevent any water from reacting with the finished fiber structure. The fiber is coated with a soft plastic film before leaving the environmental enclosure and exposure to air in the fiber drawing process.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of one type of apparatus used in the continuous fiber making process of this invention;
FIG. 2 is a sectional view of another apparatus used with the fiber making process of this invention; and
FIG. 3 is a cross-section of an optical fiber manufactured by the apparatus shown in FIGS. 1 and 2.
DESCRIPTION OF THE INVENTION
Since a great deal of time and equipment is required for manufacturing optical fibers by means of a fiber optic preform various attempts were studied in a search for a continuous and economically feasible fiber drawing process. In order to determine whether increased fiber drawing speeds could be realized without affecting the quality of the resultant optical fiber experiments were performed by drawing fibers on existing equipment using fiber optic preforms at increasing drawing speeds. Evaluating the resultant fibers for optical and strength properties surprisingly revealed that the increased drawing speeds rather than adversely affecting the optical properties of the fiber produced fibers having lower optical loss. The reason for the improved optical properties with optical fibers drawn at fast drawing rates is not well understood but it is believed due to the decrease in Rayleigh scattering losses possibly caused by the more uniform glass density in the fibers drawn at increased drawing rates.
In order to utilize the added benefits accompanying the fast fiber drawing rates in a continuous fiber making process without the use of fiber optic preforms various methods were considered for producing the starting materials at a sufficient rate to supply the faster fiber drawing process.
The high purity deposition of chemicals from the vapor phase process was selected as the best source of high purity material but was discounted as too slow for use with high speed fiber drawing apparatus. However, when depositing the core and fiber materials simultaneously and using a method of distillation such as chemical vapor disposition sufficient fiber material can be produced to sustain the faster fiber drawing speeds when a glow discharge is utilized.
The use of a localized R.F. field to create a glow discharge results in a material deposition rate 10 times as fast as the deposition rate which occurs when electric heaters are employed in the deposition process. The material deposits uniformly and rapidly upon the surface of the crucible. The R.F. generated glow discharge may be introduced to the region within the crucible through the use of a plasma jet arrangement. The crucible may be heated by R.F. heating to ensure that the glass deposited will be kept at a molten state and flow into the orifice.
The method of chemical vapor deposition by means of an R.F. glow discharge is described in U.S. patent application Ser. No. 696,991, filed June 17, 1976 (Uffen-2Y) and assigned to the assignee of the instant invention. The R.F. glow discharge in the aforementioned application was used for forming layers of core and cladding materials on the inner surface of a silica tube. The silica tube was subsequently collapsed to form a preform and the preform was heated and drawn into an optical fiber.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The continuous high strength, low loss fiber of this invention can be processed on the apparatus of FIG. 1 which consists of an enclosure 10 completely enclosing crucible 15. Extending through enclosure 10 are a series of nozzles generally designated as 11 which introduce the fiber making materials in gaseous form upon the inner surface of crucible 15. Crucible 15 is surrounded by R.F. coils 16 for crucible heating. An R.F. glow discharge is introduced through plasma jets 2, 2' and the material for depositing is emitted from nozzles 11 in a vapor form. The vapor particles 9 reacts in the plasma and forms glass which rapidly deposit upon the surface of the crucible 15 in a series of uniform glassy layers. For the purpose of this embodiment three of the nozzles 11 are described, however, since each of the individual nozzles contributes to a separate layer of material any number of nozzles can be provided depending upon the number of layers desired. Here the first nozzle 12 contributes to the first layer of material 21, the second nozzle 13 provides the material for the second layer 22 and the third nozzle 14 provides the third and innermost layer 23. A corresponding series of nozzles 11' designated respectively as 12', 13' and 14' are used to insure that the resulting layers will be uniformly distributed around the circumference of the crucible 15. Once the material is deposited upon the heated crucible 15 the resultant glass layers 21, 22 and 23 flow through orifice 17 under the tension exerted by take-up reel 27. The fiber 24 therefore concentrically contains each of the corresponding glass layers 21, 22 and 23 with the innermost layer 23 constituting the core.
Since the entire glass deposition process occurs within the enclosure 10 various elemental gases can be introduced to the fiber in order to control the fiber chemistry. Oxygen, for example, can be introduced through the oxygen intake nozzle 18 where the oxygen is directed upon the fiber surface to cool and chill the fiber 24 and to exclude any air borne dust particles from the surface of the fiber 24 and further to insure that the fiber 24 remains dust-free while within the enclosure 10. Additional chemicals can be introduced during the fiber drawing process as desired. A fluorine intake nozzle 19, for example, can provide a steady stream of fluorine gas in order to terminate surface bonding and prevent moisture attack and the formation of OH radicals. Exhaust fan 20 insures that the by-products of the chemical vapor deposition process will be continuously removed from the enclosure 10 and that high concentrations of oxygen and fluorine do not build up at any time during the fiber drawing process.
In order to insure that the drawn fiber 24 remains dust-free and mositure free, fiber 24 is exited from the enclosure 10 by means of orifice 38 through which the fiber 24 traverses into a container 25 of plastic 26. The fiber 24 is completely wet and coated by the plastic 26 before exposure to the atmosphere and before being wound on take-up reel 27.
When doped core optical fibers are manufactured by the apparatus of FIG. 1, the third layer 23 forms the doped core of the resultant optical fiber 24. The second layer 22 provides a low refractive index cladding layer and the first layer 21 provides the outer optical cladding. Suitable materials for forming the doped core optical fiber are provided by the halides of the desired materials since the halides can be readily transferred in vapor form entrained within a carrier gas such as oxygen. When silicon tetrachloride is entrained within oxygen then the silicon tetrachloride-oxygen mixture when introduced to crucible 15 by means of nozzle 12 forms a glow discharge under the influence of a strong R.F. field produced by R.F. coil 16 and produces a first layer 21 consisting essentially of silica. When boron trichloride and silicon tetrachloride vapors are entrained with oxygen and transported into crucible 15 by means of nozzle 13 then, in a similar manner, the second layer 22 consists essentially of borosilicate glass. Using germanium and silicon tetrachloride vapor within a stream of oxygen gas and transporting the mixture within crucible 15 by means of nozzle 14 the third layer 23 consists essentially of germanium silicate glass.
FIG. 3 shows a cross-section of the coated fiber 7 which consists of a core 23' formed from the third layer 23, an interface layer 22' formed from second layer 22 and a cladding layer 21' formed from the first layer 21. The soft plastic layer 26' can be overcoated with a hard plastic layer 35 if desired. The core can, of course, have a graded profile.
Although R.F. glow discharge techniques provide separate layers within a common crucible as described for the embodiment of FIG. 1, multi-component optical fibers can also be manufactured by a multi-layered crucible technique as described in FIG. 2. Since some of the elements of the apparatus of FIG. 1 provide a similar function in the apparatus of FIG. 2, common reference numberals will be employed wherever possible. In the embodiment of FIG. 2 the enclosure 10 having exhaust 20 and intake nozzles 18 and 19 includes a multi-layered crucible generally designated as 6 and containing a first concentric crucible 29, a second crucible 31 and a third crucible 33. R.F. coils 16 concentrically extend around multi-layered crucible 6 for the purpose of providing crucible heating. The R.F. glow discharge is introduced in a manner similar to that described for the embodiment of FIG. 1 through plasma jets 2, 2' and 2". The materials for generating the optical fiber glass enter the crucible 6 by means a first inlet 30, a second inlet 32 and a third inlet 34. Each of these inlets communicate respectively with corresponding first crucible 29, second crucible 31 and third crucible 33. The materials entering each of these crucibles provides a vapor 9 within the R.F. glow discharges generated as shown in FIG. 2 and become deposited on the inner surface of the respective crucibles in a manner similar to that described for the R.F. glow discharge of the embodiment of FIG. 1. Heating the multi-layered crucible 6 by R.F. coils 16 causes the material to flow through the series of corresponding orifices 5, 4 and 3 to produce a continuous fiber 24 having a concentric layered structure corresponding to the materials selected for each of the crucibles 29, 31 and 33. The advantage of the multi-layered crucible 6 of the embodiment of FIG. 2 over the single crucible of FIG. 1 is the generation of the vapor material 9 in separate enclosures for the embodiment of FIG. 2 to insure that the individual components of the vapor material 9 will not mix while in the gaseous state. This is particularly important when graded index optical fibers are formed where each of the concentric layers of the fiber cross-section contain very carefully determined variations in material concentration. The embodiment of FIG. 2 contains an in-line plastic extruder 36 containing a hard plastic material 35. This combination of the outer hard plastic layer 35 and soft plastic layer 26 as shown in FIG. 3 greatly improves the resistance of the coated optical fiber 7 to stress when subjected to sharp bends.
The combination of a plurality of optical fiber component materials simultaneously deposited by a radio frequency glow discharge process combined with a fast fiber drawing mechanism can produce a strong optical fiber having a low optical loss. The choice of the chemical vapor deposition method to continuously distill high purity materials avoids the losses due to absorption caused by hydroxyl and transitional metal ion impurities while the fast fiber draw mechanism decreases losses caused by Rayleigh scattering. The use of the controlled environmental enclosure along with continuous oxygen flow across the fiber surface during the fiber drawing operation insures that air borne dust particles will not be present on the fiber surface when the fiber is being encapsulated in a protective plastic coating.
The glow discharge-chemical vapor deposition method deposits the glass at a rate substantially faster than standard thermal methods of decomposition and is an important factor in the development of the inventive fiber drawing process. R.F. excitation is employed to create an electrodeless discharge which efficiently deposits the glass components onto the surface of the crucible without the need for auxiliary electrodes. However, D.C. type glow discharges may be employed for the deposition process but require electrodes for setting up an electric field to cause the plasma to occur. Plasma torches are used to heat the glass forming components when an R.F. field is used for crucible heating.
Although fibers produced by the method of this invention find application in the field of optical communications, this is by way of example only. The fibers produced by the method of this invention may be used wherever fibers having high tensile strengths and good optical transmitting properties may be required. | A continuous optical fiber manufacturing process utilizes the method of chemical vapor deposition of the glass forming materials within an R.F. excited glow discharge. The rapid deposition rate within the discharge provides a sufficient stream of glass material for winding into a finished fiber on a synchronous take-up mechanism. Alternate embodiments include an oxygen air stream to remove dust particles from the fiber surface and an in-line fluorine stream to terminate surface bonding and reduce moisture attack on fiber surfaces. | 8 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to an image forming apparatus such as a copying machine, a printer, a facsimile machine, etc. for forming an image by electrophotography. Particularly, it relates to an image forming apparatus using toner for forming an image.
[0003] 2. Description of the Related Art
[0004] In electrophotography, a charging unit such as a charging roller is used for giving electric charge on a photosensitive member evenly. An exposure unit is used for forming an electrostatic latent image corresponding to image data on the photosensitive member to which electric charge is given. Toner which is powder electrostatically charged in accordance with the charge pattern of the electrostatic latent image is deposited on the photosensitive member to thereby form a toner image on the electrostatic latent image. The toner image is transferred onto a recording medium such as a sheet of paper directly or through an intermediate transfer belt as an intermediate transfer member to thereby form an image.
[0005] Because electric charge remains on the photosensitive member after toner is transferred onto the recording medium, the residual electric charge is erased by an erasing unit before an image is formed again. A method of erasing electric charge by light irradiation or a method of erasing electric charge by an electrically conducting brush etc. brought into contact with the photosensitive member has been proposed as the erasing unit.
[0006] For formation of a color image, color toners such as yellow (Y), magenta (M), cyan (C), black (K), etc. are superposed on one another to form an image.
[0007] The color image forming method is roughly classified into two techniques. One is a repetitive development technique for forming a color image by repetitively developing the respective color toners on one photosensitive member. The other is a simultaneous development technique for forming a color image by simultaneously developing the respective color toners on a plurality of photosensitive members.
[0008] The repetitive development technique uses one photosensitive member for forming a color image. An intermediate transfer technique is an example of the repetitive development technique. The intermediate transfer technique is a technique in which developers that develops different color toners and a medium conveyance member are disposed around a photosensitive member so that toner images formed on the photosensitive member are color by color transferred onto the medium conveyance member successively, for example, as described in JP-A-8-137179. After this operation is repeated color by color so that the toner images of the different colors are superposed on the medium conveyance member, the superposed color toner image formed on the medium conveyance member is transferred onto a sheet of paper to thereby output a color image.
[0009] In this technique, for example, toner images of the four colors of yellow, magenta, cyan and black are color by color formed on the photosensitive member successively and then superpositively transferred onto the medium conveyance member. After all the toner images are transferred onto the medium conveyance member, the superposed color image formed on the medium conveyance member is transferred onto a medium such as a sheet of paper. Because colors are superposed successively in this manner, a time about four times as much as the printing time in the case of formation of a monochrome image from a color of black is required for forming an image.
[0010] It is however possible to reduce the number of parts because a charging unit, an exposure unit, a transfer unit, a cleaner unit and an erasing unit necessary for printing and developers corresponding to the four colors can be formed around one photosensitive member.
[0011] On the other hand, in the simultaneous development technique, photosensitive members corresponding to colors are provided as described in JP-A-5-35097. Toner images are almost simultaneously formed on the photosensitive members. The toner images are transferred in accordance with conveyance of a sheet of paper to thereby form a color image. This technique is also called “tandem electrophotographic”.
[0012] In the tandem electrophotographic, image forming section each having a photosensitive member, a charging unit, an exposure unit, a developing unit and a cleaner unit are provided independently in accordance with the colors. Accordingly, when a color image is formed from toners of the four colors of yellow, magenta, cyan and black, it is necessary to provide four image forming sections.
[0013] After toner images are almost simultaneously formed by the independent image forming section corresponding to the four colors, the toner images are transferred onto an intermediate transfer medium or a medium such as a sheet of paper. Because colors are superposed simultaneously in this manner, a color image can be formed in a time approximately as much as the printing time in the case of formation of a monochrome image from a color of black. This technique is suitable for high-speed printing of a color image.
[0014] It is however necessary to increase the number of parts because all printing processes required for forming images corresponding to the colors must be prepared.
[0015] A method of detecting the amount of toner remaining in a developer has been described in JP-A-5-35097. A residual toner amount detection unit includes a toner sensor, and toner detection windows. The toner sensor is disposed in an image forming apparatus and has a light-emitting element, and a light-receiving element. The toner detection windows are provided in the developer.
[0016] When there is no toner in the developer, light emitted from the light-emitting element is transmitted through one of the toner detection windows in the developer and further transmitted through the other toner detection window on the opposite side via the inside of the developer so that the light is received by the light-receiving element.
[0017] When there is toner in the developer, light emitted from the light-emitting element is blocked by the toner in the developer so that the light cannot reach the light-receiving element on the opposite side. On this occasion, the presence of toner can be detected because the light-receiving element outputs a voltage or the like proportional to the quantity of light received by the light-receiving element.
[0018] A method of erasing residual electric charge has been described in JP-A-11-344909. In this method, a light-emitting element such as an LED lamp or a fluorescent lamp is disposed between a transfer unit and a charging unit so that electric charge remaining on a photosensitive member can be erased by application of light on the photosensitive member.
[0019] In recent years, color printers have become widespread rapidly and reduction in cost of the printers has advanced because of increasing demands for colorization of documents in offices. In addition, tandem color printers have attracted notice because of demands for increase in printing speed.
[0020] It is however difficult to reduce the size of the tandem printer because the tandem printer must have four image forming sections as descried above. The tandem printer requires a large number of parts. Accordingly, the size of the tandem printer and the cost of parts in the tandem printer must become larger than those of a printer using the repetitive development technique. Above all, the residual toner amount detection unit needs light-emitting element and light-receiving element pairs, light-emitting element drive circuits and light-receiving element receiving circuits in accordance with the four colors, so that increase in production cost is brought.
SUMMARY OF THE INVENTION
[0021] The present invention has been made in view of above circumstances and provides an image forming apparatus and an image forming unit. According to an aspect of the invention, the number of constituent parts in the image forming apparatus or the image forming unit can be reduced to thereby reduce the cost of production.
[0022] According to a first aspect of the invention, there is provided an image forming apparatus including: an image forming section and a residual toner amount detection unit. The image forming section includes a photosensitive member having a photosensitive layer in its surface; a charging unit that gives electric charge to the photosensitive member, the charging unit disposed on the photosensitive member; an exposure unit that exposes the photosensitive layer to light based on image data to form an electrostatic latent image; a developing unit that deposits toner on the electrostatic latent image formed on the photosensitive member to form a toner image; and a toner storage unit that stores toner used in the developing unit; wherein the toner image formed on the photosensitive member is transferred onto a recording medium conveyed by a medium conveyance member directly or through an intermediate transfer member to form an image. The residual toner amount detection unit detects an amount of toner remaining in the developing unit. The residual toner amount detection unit includes a light-emitting element and a light-receiving element. After the toner is deposited on the photosensitive member to form the toner image until electric charge is given onto the photosensitive layer by the charging unit again, the light-emitting element removes electric charge remaining on the photosensitive layer.
[0023] According to a second aspect of the invention, there is provided the image forming apparatus according to the first aspect, wherein at least one of the photosensitive member, the developing unit and the toner storage unit is formed as an detachable image forming unit which is detachable to a main body of the image forming apparatus; and wherein the light-emitting element is provided in the main body of the image forming apparatus. In this configuration, not only can the number of parts be reduced but also the detachable image forming unit can be repaired and exchanged easily.
[0024] According to a third aspect of the invention, there is provided the image forming apparatus according to the first aspect, wherein at least one of the photosensitive member, the developing unit and the toner storage unit is formed as an detachable unit which is detachable to a main body of the image forming apparatus; and wherein the light-emitting element is provided in the detachable unit. In this configuration, not only can the number of parts be reduced but also the optical element can be repaired and exchanged easily.
[0025] According to a fourth aspect of the invention, there is provided the image forming apparatus according to the first aspect, wherein light emitted from the light-emitting element is led to the photosensitive member through a light guide unit in order to remove electric charge remaining on the photosensitive layer. In this configuration, the light-emitting element can be arranged in an appropriate position.
[0026] According to a fifth aspect of the invention, there is provided the image forming apparatus according to the first aspect, further including: an emission amount adjusting unit that changes an amount of light emitted from the light-emitting element. In this configuration, the quantity of light emitted from the light-emitting element is reduced or emission of light is forbidden so that a good image quality can be always provided to a user.
[0027] According to a sixth aspect of the invention, there is provided an image forming unit including: a light-emitting element. The image forming unit further includes at least one of: a photosensitive member having a photosensitive layer in its surface; a developing unit that deposits toner on an electrostatic latent image formed on the photosensitive member to form a toner image; and a toner storage unit that stores toner used in the developing unit. The light-emitting element detects a residual toner amount in cooperation with a light-receiving unit of a residual toner detection unit and removes electric charge remaining on the photosensitive layer after the toner is deposited on the photosensitive member to form the toner image until electric charge is given onto the photosensitive layer by a charging unit again. In this configuration, it may be possible to provide an image forming unit in which the number of parts can be reduced.
[0028] According to a seventh aspect of the invention, there is provided the image forming unit according to the sixth aspect, wherein the image forming unit is equipped with the light-receiving element. In this configuration, it may be possible to provide an image forming unit in which not only can the number of parts be reduced but also the light-receiving element can be repaired and exchanged easily.
[0029] According to above configuration, a light-emitting element serves as the light-emitting element used in the erasing unit that erases electric charge remaining on the photosensitive member and serves also as the light-emitting element used in the residual toner amount detection unit that detects the residual amount of toner. Accordingly, the number of parts such as the light-emitting element and a drive circuit for the light-emitting element can be reduced to attain reduction in cost.
BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Embodiments of the present invention will be described in detail based on the following figures, wherein:
[0031] FIG. 1A is a schematic sectional view of an image forming apparatus according to Embodiment 1 of the invention; and
[0032] FIG. 1B is a schematic sectional view of a printing unit according to Embodiment 1;
[0033] FIG. 2 is a schematic sectional view of an image forming apparatus according to Embodiment 2 of the invention;
[0034] FIG. 3 is a schematic sectional view of an image forming apparatus according to Embodiment 3 of the invention;
[0035] FIG. 4 is a schematic sectional view of an image forming section according to Embodiment 4 of the invention;
[0036] FIG. 5 is a sectional view taken along the line A-A′ on the image forming section depicted in FIG. 4 ;
[0037] FIG. 6 is a schematic sectional view of an image forming section according to Embodiment 5 of the invention;
[0038] FIG. 7 is a sectional view taken along the line B-B′ on the image forming section depicted in FIG. 6 ;
[0039] FIG. 8 is a schematic sectional view of an image forming section according to Embodiment 6 of the invention;
[0040] FIG. 9 is a schematic sectional view of an image forming section according to Embodiment 7 of the invention;
[0041] FIG. 10 is a schematic sectional view of a developer according to Embodiment 8 of the invention;
[0042] FIG. 11 is a schematic sectional view of a developer according to Embodiment 9 of the invention;
[0043] FIG. 12 is a schematic sectional view of an image forming apparatus according to Embodiment 10 of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0000] Embodiment 1
[0044] An embodiment of an apparatus according to the invention will be described with reference to FIGS. 1A and 1B . FIG. 1A is a schematic sectional view showing the overall configuration of an image forming apparatus using printing units as image forming section. FIG. 1B is a schematic sectional view showing one of the printing units. The image forming apparatus and the printing unit will be described below.
[0045] Sheets of printing paper 19 and a pickup roller 18 for picking up the sheets of printing paper 19 are provided in a lower portion of the image forming apparatus.
[0046] As shown in FIG. 1B , each of the printing units 11 a, 11 b, 11 c and 11 d has a photosensitive member 2 , a charging roller 6 , an exposure device 5 , and a developer 4 . The photosensitive member 2 is provided as an endless cylinder having a photosensitive layer in its surface. The charging roller 6 , the exposure device 5 and the developer 4 are disposed around the photosensitive member 2 . The charging roller 6 gives electric charge onto the photosensitive layer of the photosensitive member 2 . The exposure device 5 applies light based on image information on the electric charge given onto the photosensitive layer of the photosensitive member 2 to thereby form an electrostatic latent image. The developer 4 develops toner on the electrostatic latent image. The printing units 11 a, 11 b, 11 c and 11 d, which are units ( 11 a to 11 d ) corresponding to the four colors of yellow, magenta, cyan and black necessary for forming a color image, are detachably attached to the image forming apparatus body 1 successively.
[0047] As shown in FIG. 1B , the developer 4 which is one of image forming section has a developer casing 20 , a developing roller 8 , a supply roller 9 , and a toner vessel 21 . The developing roller 8 , the supply roller 9 and the toner vessel 21 are surrounded by the developer casing 20 . The developing roller 8 is used for developing toner on the electrostatic latent image. The supply roller 9 is used for supplying toner to the developing roller 8 . The toner used for development is stored in the toner vessel 21 . Incidentally, the reference numeral 7 in FIG. 1B designates a photosensitive member cleaner.
[0048] As shown in FIG. 1A , in this embodiment, a light-emitting element 14 and a light-receiving element 15 for detecting the residual amount of toner are attached to the image forming apparatus body 1 so as to be separate from the printing units ( 11 a to 11 d ).
[0049] The photosensitive members 2 of the printing units 11 abut on a medium conveyance member 3 . Each transfer roller 10 is disposed so that the medium conveyance member 3 is put between the transfer roller 10 and the photosensitive member 2 .
[0050] The medium conveyance member 3 is an endless belt. The medium conveyance member 3 is disposed horizontally in the apparatus body 1 in the condition that the medium conveyance member 3 is laid on a drive roller 24 and a driven roller 25 circularly. Incidentally, the positional relation between the drive roller 24 and the driven roller 25 may be reversed or two or more rollers may be provided.
[0051] In this embodiment, the image forming apparatus has printing units ( 11 a to 11 d ) corresponding to the four colors of yellow, magenta, cyan and black necessary for forming a color image. The colors of yellow, magenta, cyan and black are developed in the printing units 11 a to 11 d respectively. Toner images thus formed are successively transferred to the medium conveyance member 3 used as an intermediate transfer belt. A second transfer roller 17 transfers the toner images onto a sheet of paper 19 fed by the pickup roller 18 . Thus, an image is formed.
[0052] The sheet of paper 19 having the toner images transferred thereon is ejected after toners are fixed by a fixing device 16 under heat and pressure.
[0053] Each residual toner amount detection unit is constituted by a combination of a light-emitting element 14 such as an LED and a light-receiving element 15 such as a photo diode. Light emitted from the light-emitting element 14 passes through the developer casing 20 so as to be incident on the light-receiving element 15 . When the amount of toner remaining in the developer casing 20 is small on this occasion, a large part of light emitted from the light-emitting element 14 becomes incident on the light-receiving element 15 .
[0054] On the other hand, when the developer casing 20 is filled with toner, the quantity of light incident on the light-receiving element 15 is reduced. The residual amount of toner is detected on the basis of the difference between quantities of light incident on the light-receiving element 15 .
[0055] Next, the erasing unit will be described. A part of light emitted from the light-emitting element 14 is led to a light guide plate 12 disposed between the transfer roller 10 and the cleaner 7 , via an end portion of the photosensitive member 2 by a light guide path 13 . The light emitted from the light-emitting element 14 and led to the light guide plate 12 is diffused and applied on the photosensitive member 2 to thereby erase electric charge remaining on the photosensitive member 2 .
[0056] It is preferable that light emitted from the light-emitting element 14 contains the wavelength of sensitivity characteristic of the photosensitive layer on the photosensitive member 2 and the wavelength of sensitivity characteristic of the light-receiving element. When, for example, the photosensitive layer on the photosensitive member 2 has sensitivity at a wavelength of 780 nm and the light-receiving element 15 has sensitivity at a wavelength of 880 nm, light emitted from the light-emitting material 14 contains light in a range of emission wavelengths of 780 nm and 880 nm.
[0057] In this embodiment, the number of parts such as a drive circuit belonging to the light-emitting element can be reduced because the light-emitting element 14 serves as the light-emitting element of the residual toner amount detection unit and also as the light-emitting element of the erasing unit. Incidentally, the reference numeral 22 in FIG. 1A designates a belt cleaner.
[0000] Embodiment 2
[0058] Another embodiment of the invention will be described below with reference to FIG. 2 . FIG. 2 is a sectional view showing the overall configuration of an image forming apparatus in which one 11 a of printing units ( 11 a to 11 d ) corresponding to the four colors of yellow, magenta, cyan and black necessary for forming a color image is separated.
[0059] The arrangement and functions of various kinds of parts constituting the image forming apparatus are the same as those in the image forming apparatus described above in Embodiment 1. Although Embodiment 1 shows the case where the light-emitting element 14 used in common to the residual toner amount detection unit and the erasing unit is attached to the image forming apparatus body 1 , this embodiment shows the case where the light-emitting element 14 is attached to the developer 4 .
[0060] For this reason, the light-emitting element 14 together with the developer 4 can be exchanged for a new one. In this configuration, not only can the number of parts shown in Embodiment 1 be reduced but also electric charge erasing failure in the erasing unit can be prevented from being caused by reduction in quantity of light due to deterioration of the light-emitting element 14 with the passage of time.
[0000] Embodiment 3
[0061] A further embodiment of the invention will be described below with reference to FIG. 3 . FIG. 3 is a sectional view showing the overall configuration of an image forming apparatus in which one 11 a of printing units ( 11 a to 11 d ) corresponding to the four colors of yellow, magenta, cyan and black necessary for forming a color image is separated.
[0062] The arrangement and functions of various kinds of parts constituting the image forming apparatus are the same as those in the image forming apparatus described above in FIGS. 1A and 1B or FIG. 2 . Although Embodiment 2 shows the case where the light-receiving element 15 of the residual toner amount detection unit is attached to the image forming apparatus body 1 , this embodiment shows the case where the light-receiving element 15 together with the light-emitting element 14 is attached to the developer 4 .
[0063] For this reason, the light-emitting element 14 and the light-receiving element 15 together with the developer 4 can be exchanged for new ones. In this configuration, not only can the same improvement effect as in Embodiment 2 be obtained but also residual toner amount detection failure etc. can be prevented from being caused by deterioration of the light-receiving element 15 with the passage of time etc.
[0000] Embodiment 4
[0064] A further embodiment of the invention will be described below with reference to FIGS. 4 and 5 .
[0065] FIG. 4 is a view showing a state in which only the printing unit 11 described in FIG. 2 or 3 is removed. FIG. 5 is a sectional view taken along the line A-A′ in FIG. 4 , as seen from the upper surface.
[0066] The printing unit 11 shown in FIGS. 4 and 5 operates in the same manner as in the image forming apparatus described in Embodiments 1 to 3. In this embodiment, light emitted from the light-emitting element 14 braches into an optical path for the erasing unit and an optical path for the residual toner amount detection unit, so that the light-emitting element 14 can be incorporated in the developer 4 easily.
[0067] The reference numerals 30 and 31 in FIG. 5 designate through-holes which are formed in the developer casing 20 so that light emitted from the light-emitting element 14 toward the light-receiving element 15 can be transmitted. Transparent plastic sheets 32 are stuck to inner surfaces of the though-holes 30 and 31 respectively in order to prevent toner from scattering from the casing 20 .
[0068] Although this embodiment shows the case where the transparent plastic sheets 32 are used, the plastic sheets need not be provided and lenses or the like may be joined to the through-holes so that light emitted from the light-emitting element 14 can converge or diverge.
[0000] Embodiment 5
[0069] A further embodiment of the invention will be described below with reference to FIGS. 6 and 7 .
[0070] FIG. 6 is a view showing a state in which only the printing unit 11 described in FIG. 2 or 3 is removed. FIG. 7 is a sectional view taken along the line B-B′ in FIG. 6 , as seen from the upper surface.
[0071] The printing unit 11 shown in FIGS. 6 and 7 operates in the same manner as in the image forming apparatus described in Embodiments 1 to 3. In this embodiment, light emitted from the light-emitting element 14 is guided by the light guide plate 12 used as an erasing unit so that a part of the emitted light is applied on the photosensitive member 2 . A part of the emitted light is transmitted through the light guide path 13 as light for the residual toner amount detection unit so that the light is guided to the light-receiving element 15 .
[0072] In this configuration, loss in quantity of light at the time of splitting light emitted from the light-emitting element 14 can be reduced.
[0073] The reference numeral 33 in FIG. 7 designates a through-hole which permits insertion of a front end of the light guide path 13 and through which light emitted from the front end of the light guide path 13 is applied on the light-receiving element 15 .
[0000] Embodiment 6
[0074] A further embodiment of the invention will be described below with reference to FIG. 8 . FIG. 8 is a view showing a state in which only the printing unit 11 described in FIG. 2 or 3 is removed.
[0075] The printing unit 11 shown in FIG. 8 operates in the same manner as in the image forming apparatus described in Embodiments 1 to 3. In this embodiment, the light-emitting element 14 and the light guide plate 12 are disposed in a lower portion of the developer 4 so that the light-emitting element 14 and the light guide plate 12 can be incorporated in the developer 4 easily.
[0000] Embodiment 7
[0076] A further embodiment of the invention will be described below with reference to FIG. 9 . FIG. 9 typically shows paths of light emitted from the light-emitting element 14 .
[0077] Light emitted from the light-emitting element 14 splits into two optical paths. One is an optical path 34 which leads to the light-receiving element 15 via the developer casing 20 and which is used for the toner detection unit. The other is an optical path 35 which leads to the photosensitive member 2 after diffused by the light guide plate 12 via the light guide path 13 and which is used for the erasing unit.
[0078] The light guide path 13 is made of a transparent material such as polycarbonate, polyester, acrylic resin, glass, etc. The light guide path 13 leads light emitted from the light-emitting element 14 to the light guide plate 12 . The light guide plate 12 is made of a transparent light-diffusing material such as polycarbonate, polyester, acrylic resin, glass, etc. The light guide plate 12 plays a role of reflecting/diffusing the emitted light to apply the light on the photosensitive member 2 .
[0000] Embodiment 8
[0079] A further embodiment of the invention will be described below with reference to FIG. 10 . FIG. 10 is a typical view of a controller for controlling the quantity of light emitted from the light-emitting element 14 .
[0080] The developer 4 shown in FIG. 10 operates in the same manner as in the image forming apparatus described in Embodiments 1 through 3. In this embodiment, a current control circuit 23 for controlling the quantity of light emitted from the light-emitting element 14 is attached to the image forming apparatus body 1 . When, for example, the developing ability of the developer 4 is lowered because of the expiration of its life, the current control circuit 23 applies an overcurrent to the light-emitting element 14 to disable the light-emitting element 14 from emitting light.
[0081] By this measure, the image forming apparatus is informed of the time of exchange of the developer 4 having the developing ability lowered, so that a good image quality can be always provided to the user.
[0000] Embodiment 9
[0082] A further embodiment of the invention will be described below with reference to FIG. 11 . FIG. 11 is a typical view of a controller for controlling the quantity of light emitted from the light-emitting element 14 . The developer 4 shown in FIG. 11 operates in the same manner as in the image forming apparatus described in Embodiments 1 through 3.
[0083] In this embodiment, a current control circuit 23 for controlling the quantity of light emitted from the light-emitting element 14 is attached to the developer 4 . When, for example, the developing ability of the developer 4 is lowered because of the expiration of its life, the current control circuit 23 controls the current applied to the light-emitting element 14 so that the quantity of light emitted from the light-emitting element 14 can be reduced or light emission can be forbidden.
[0084] By this measure, the light-emitting element 14 can be recycled while the same effect as in Embodiment 8 can be obtained.
[0000] Embodiment 10
[0085] A further embodiment of the invention will be described below with reference to FIG. 12 . FIG. 12 is a sectional view showing the overall configuration of a printing unit and an image forming apparatus using the printing units.
[0086] The arrangement and functions of various parts constituting the image forming apparatus are the same as those of the image forming apparatus described in Embodiment 1. Although Embodiment 1 shows the case where the light-emitting element 14 used in common to the residual toner amount detection unit and the erasing unit is provided for each of the printing units ( 11 a to 11 d ) of the four colors of yellow, magenta, cyan and black, this embodiment shows the case where the light guide path 13 is used so that one light-emitting element 14 can be used for all the printing units.
[0087] For this reason, the number of parts belonging to the light-emitting element 14 can be reduced compared with the image forming apparatus described in Embodiment 1.
[0088] Although each of the embodiments of the invention exemplifies the image forming apparatus using the medium conveyance member 3 as an intermediate transfer medium, the medium conveyance member 3 may be constituted by a paper conveyance member or the like.
[0089] Although each of the embodiments of the invention exemplifies the image forming apparatus provided with the printing units 11 disposed horizontally, the printing units 11 may be disposed vertically or obliquely.
[0090] Although each of the printing units 11 has been described on the case where a roller coated with an elastic material is used as the charging roller 6 , a brush roller coated with a brush or a non-contact charger may be used as the charging roller 6 .
[0091] For example, a device which is an array of LEDs arranged in one row in the widthwise direction of the photosensitive member and which has 600 to 1200 light-emitting diodes arranged per 1 inch (25.4 mm) so that each diode can be turned on and off at predetermined timing may be used as the exposure device 5 . As another example, a device constituted by a combination of a laser and a rotary mirror or an exposure device constituted by a combination of a light-emitting device and an optical switch such as a micro-mirror may be used.
[0092] Although each of the embodiments of the invention shows the case where the light-emitting element 14 as the erasing unit applies light on the photosensitive member 2 through the light guide plate 12 , light may be applied on the photosensitive member 2 directly without interposition of the light guide plate 12 or the light-emitting element 14 may apply light on the light-receiving element 15 without use of the light guide path 13 .
[0093] The case where the light-emitting element 14 is formed to apply light on the photosensitive member 2 or the light-receiving element 15 through the light guide unit such as the light guide plate 12 , the light guide path, etc. as shown in each of the embodiments of the invention is however preferred because not only a small light-emitting element 14 can be used but also there is room for arrangement of other units.
[0094] Although each of the embodiments of the invention shows the case where a sheet of paper which is a paper member is used as the printing medium used in the image forming apparatus, a plastic material such as a plastic sheet may be used as the printing medium.
[0095] Although each of the embodiments of the invention shows the case where printing units ( 11 a to 11 d ) corresponding to the four colors of yellow, magenta, cyan and black necessary for forming a color image are used as the printing units, one printing unit corresponding to only a color of black may be used or a repetitive development technique using four rotations may be used.
[0096] Although each of the embodiments of the invention shows the case where printing units ( 11 a to 11 d ) each having all of the photosensitive member 2 , the developing unit 4 and the toner storage unit 21 (Embodiments 1 and 10) or printing units ( 11 a to 11 d ) each having the developing unit 4 and the toner storage unit 21 (Embodiments 2 to 9) are used as the printing units ( 11 a to 11 d ) which are image forming sections, the invention is not limited thereto. For example, at least one of the photosensitive member 2 , the developing unit 4 and the toner storage unit may be used as a unit which can be separated from the apparatus body 1 .
[0097] The image forming apparatus according to the invention can be applied not only to the color printer shown in the aforementioned embodiments but also to a copying machine, a printer, a facsimile machine, etc. for forming an image by electrophotography.
[0098] The entire disclosure of Japanese Patent Application No. 2005-062431 filed on Mar. 7, 2005 including specification, claims, drawings and abstract is incorporated herein be reference in its entirety. | An image forming apparatus comprising: an image forming section and a residual toner amount detection unit. The image forming section includes a photosensitive member, a charging unit, an exposure unit, a developing unit, and a toner storage unit. The residual toner amount detection unit detects an amount of toner remaining in the developing unit. The residual toner amount detection unit includes a light-emitting element and a light-receiving element. After the toner is deposited on the photosensitive member to form a toner image until electric charge is given onto a photosensitive layer of the photosensitive member by the charging unit again, the light-emitting element removes electric charge remaining on the photosensitive layer. | 6 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates generally to remediation of toxic organic compounds in the aqueous phase. More specifically, this invention relates to processes and reaction vessels that use simultaneously ultraviolet light (UV) and ultrasonic waves (US) to destroy organic pollutants, typically halogenated organic compounds in water.
[0003] 2. Related Art
[0004] Widespread water contamination with, for example, chlorinated volatile organic compounds (VOCs) has motivated research on photosonocatalysis technology for destroying VOCs, as an alternative to currently available remediation technologies such as air stripping and carbon adsorption processes.
[0005] Researchers have studied the effects of simultaneous and combined treatment of materials with ultraviolet light (“photolysis”) and ultrasonic waves (“sonolysis”).
[0006] Photolysis is a photochemical cleavage reaction initiated by the action of radiant energy in the UV/visible region of the electromagnetic spectrum. When light hits the molecule and the molecule absorbs its energy, the energy content of the molecule is increased and the molecule reaches an excited electron state. Photolysis is one deactivation process in which the unstable excited state molecule comes down to a stable ground-level energy state.
[0007] Photolysis occurs competitively with the radiation and radiationless reactions. In the former reaction, the molecules's extra energy is released through emission of light (e.g., fluorescence). In the latter reaction, its extra energy is converted to thermal energy and dissipated. The absorption of light energy by the molecule may occur directly or indirectly. When the molecule itself directly adsorbs light energy and is degraded, the reaction is direct photolysis, while light energy is transferred from other substances, the resulting reaction is indirect or sensitized photolysis. When photons of light strike a semiconductor, they are either absorbed or scattered. The absorbed photons with energy greater than or equal to the semiconductor band gap energy excite electrons from the valence band to the conduction band. The excitation generates electron-hole pairs (e − +h + ) on semiconductors, which can either recombine and release heat, or cause oxidation and reduction reactions by charge transfer to species adsorbed to the semiconductor (Lau, 1996).
[0008] Sonolysis is a physical/chemical reaction initiated by implosion of cavitation bubbles in liquid, induced by ultrasound. Ultrasound can create powerful rarefaction waves to develop a negative pressure in liquid. If the waves are powerful enough to overcome the intermolecular forces of bonds in liquid, the liquid molecules will be torn apart from each other to form microbubbles in liquid. The cavitation bubbles are formed at the weak spots in the liquid. Once a microbubble is formed, it rapidly grows until it reaches the critical size at which the bubble can no longer sustain itself and results in an implosion instantaneously releasing a large amount of energy (Bhatnagar and Cheung, 1994).
[0009] The energy generated by the compression of gas and vapor inside is released as intense heat at a local hot spot. Suslick (1990) reported that these hot spots (imploding bubbles) would reach temperature of 5000° C., pressure of 500 atmospheres, and heating and cooling rates greater than 10 9 K/sec. Thus, the reaction that takes place in aqueous solution may be direct bond cleavage, or thermal reaction similar to combustion. The extreme conditions may also produce reactive species (e.g., H 2 O 2 ., HO 2 .H, .OH) in aqueous solution, and result in hydrolysis and oxidation-reduction reactions with these species.
[0010] Photosonolysis is the use of photolysis and sonolysis in combination. Initial studies on the use of photosonolysis were reported by Toy and Stringham (1984, 1985). They used ultraviolet light (UV) and ultrasonic waves (US) for the synthesis of 1,2,4-tris (methylthio)-3-H-hexafluoro-n-butane from methyl disulfide and hexafluorobutadiene. Photosonolysis was later applied in numerous additional synthetic applications, and has also been applied to polymer degradations (Toy and Stringham, 1985; Toy et al., 1990).
[0011] Toy and Stringham's photosonosynthesis work has been expanded by other researchers to the applications to waste remediation technologies. Sierka and Amy (1985) studied the composite effects of ultraviolet light (UV), ultrasound (US), and ozone oxidation (O 3 ) to reduce the trihalomethane formation potential and maximize the destruction of nonvolatile total organic carbons. They found that concurrent use of UV, US, and ozone provided the most effective combination in the performed experiments.
[0012] Johnston and Hocking (1991, 1993) studied the combined use of UV (with 0.5-2 g/L TiO 2 ) and ultrasonic irradiation to degrade various chlorinated organics including pentachlorophenol (PCP, 2.4×10 −4 M); 3-chlorobiphenyl (PCB, 4×10 −4 M); 2,4-dichlorophenol (2,4-DCP, 1×10 −3 M); and 4-chlorophenol (4-CP). The chlorinated compounds were more rapidly degraded by the combination of ultrasound and ultraviolet light irradiation than with any other combination (i.e., UV or US treatment with or without TiO 2 ) studied.
[0013] Toy et al. (1990) studied photosonocatalysis on decomposition of ethylene glycol and urea in aqueous solutions, and reported that photosonocatalytic decomposition is more aggressive than with either sonolysis or photolysis individually. Toy et al. (1990) also performed experiments on the photosonochemical decomposition of aqueous 1,1,1-trichloroethane (TCA), and reported that the combined use of photolysis and sonolysis causes a greater decomposition than if each technique were used separately.
[0014] Muzzoli et al. (1994) studied the effects of ultrasound and ultraviolet radiation on vitamin E and its pharmacological excipient, olive oil. The vitamin E appeared to be inactivated and behaved as a radical species, while olive oil appears unaffected by treatment either with ultrasound or with ultraviolet radiation.
[0015] Other inventors have developed methods and reactors for carrying out these treatments on liquids. See, for example, U.S. Pat. No. 3,672,823 (Boucher, issued Jun. 27, 1972), and U.S. Pat. No. 5,130,031 (Johnston, issued Jul. 14, 1992).
[0016] Still, there is a need for an easily constructed, simply operated, portable UV/US reactor design. Also, there is still a need for such a UV/US reactor design with increased flexibility and capability of responding effectively to variable water flow and quality conditions without the need for necessarily added chemicals or catalysts. Also, there is a need for a process to destroy halogenated organic pollutants using UV/US. This invention addresses these needs.
SUMMARY OF THE INVENTION
[0017] The present invention is a process and reactors for simultaneous ultraviolet light/ultrasound (UV/US) treatment of pollutants (e.g., halogenated organic compounds) in water. This process and these reactors use an advanced oxidation process (AOP) for the treatment of waters (e.g., surface water, groundwater). The process and reactors are designed to combine photolysis/photocatalysis and sonolysis, induced by ultraviolet light (UV) with/without photocatalyst (e.g., TiO 2 ) and ultrasound (US), respectively. The process and reactors are preferably circular, cylindrical-shaped reaction vessels that accept a central ultrasonic horn. UV light is provided by lamps placed generally parallel to the reactor walls, either external to the walls when a material transparent to UV is used for the reactor walls, or centrally provided in a transparent immersion well. Between, for example, the UV immersion well near the top of the reactor, and the ultrasonic horn near the bottom of the reactor, a horizontal, hollow metal partition with reactant flow-through holes is installed. This way, simultaneous UV/US energy may be effectively provided to the reactors for the remediation of pollutants in the water in the reactors. Also, this way, compact and portable reactors may be constructed to permit mobile applications of the UV/US processes. Because the units may be made mobile, they can be used for military applications, for remote or temporary communities or for emergency responses, as after natural disasters or accidental contaminations of water supplies.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIGS. 1 (A-B) are schematic diagrams of two embodiments of the present invention, showing the systems in which the present invention is used.
[0019] [0019]FIG. 2 is a schematic depiction for the batch photosono reactor embodiment of the present invention.
[0020] [0020]FIG. 3 is a schematic depiction for one embodiment of the flow-through photosono reactor of the present invention.
[0021] FIGS. 4 A-a and 4 A-b are side and top view schematic depictions, respectively, for another embodiment of the flow-through photosono reactor of the present invention. FIGS. 4 B-a and 4 B-b are side and top view schmatic depictions, respectively, for another embodiment of the flow-through photosono reactor of the present invention.
[0022] [0022]FIG. 5 is a schematic depiction for yet another embodiment of the flow-through photosono reactor of the present invention.
[0023] FIGS. 6 - 9 are graphical depictions of the results from the EXAMPLE I of this application.
[0024] [0024]FIG. 10 is a schematic depiction of a flow-through photosono reactor embodiment with a horizontal, hollow metal partition.
[0025] [0025]FIGS. 11A and B are top and side detail views, respectively, of the embodiment of the metal partition of FIG. 10.
[0026] [0026]FIGS. 12 and 13 are graphical depictions of the results from EXAMPLE II of this application.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0027] As shown in FIGS. 1 A-B, the present invention is a UV/US reactor primarily for the remediation of toxic organic compounds in the aqueous phase. By simultaneously exposing the toxic organic compounds to both ultraviolet light and ultrasonic waves, the compounds are remediated into less toxic and nontoxic compounds.
[0028] [0028]FIG. 1A shows a general schematic diagram of one embodiment of the invented process and apparatus. Contaminated water (e.g., VOC aqueous solution) stored in a container 110 is pumped, using a pump 120 , into a heat exchanger 130 . Cooled water (preferably 10±5° C.) from chiller 140 is supplied to the heat exchanger 130 and recirculated through a recirculation system and stored in a vessel 150 . This results in the temperature of the contaminated solution being reduced to preferably 10±5° C. This cooled contaminated solution is then processed through this embodiment of the present invention 100 A.
[0029] [0029]FIG. 1B also shows a general schematic diagram for another embodiment of the invented process and apparatus. Contaminated water (e.g., VOC aqueous solution) stored in a container 110 is pumped, using a pump 120 , into the present invention 100 B. Cooled water (preferably 10±5° C.), cooled by a chiller 140 , is supplied to a water jacket #a of the reactor from an inlet port #b, removed from an outlet port #c, and recirculated through a recirculation system and vessel 150 . This results in the reactor temperature being maintained to preferably 20±5° C.
[0030] The basic UV/US reactor generally comprises a quartz or equivalent photo-reaction vessel, UV lamp(s), and an ultrasonic (US) liquid processor. The four, preferred, basic UV/US reactor designs according to the present invention are described in detail below. The preferred design of these four is the Type- 3 A and B reactor(s) (shown in FIGS. 4 A-B).
[0031] The reactors may be made by conventional construction techniques with conventional materials. Scaled-up versions of the reactors may be designed by conventional engineering techniques. Components, equipment and accessories for scaled-up designs may be obtained from commercial vendors or custom-designed by conventional techniques. Preferably, the scaled-up designs will be modular units with accompanying inventory tanks, pumps, compressors, if necessary, separator vessels, level, flow and pressure controllers, electrical power supply and analytical instruments on a truck body or trailer for transport to the application site.
[0032] For experimental work, the preferred ultrasonic liquid processor is a Model XL2020, Misonix Inc. processor for a source of ultrasound. This processor is used to produce ultrasonic waves of 20-kHz frequency, preferably conducted in a pulse (5-sec on/off) mode. The XL2020 sonicator is capable of delivery 550 W of ultrasonic power.
[0033] 1. Batch System Reactor
[0034] a. The “Type- 1 ” Reactor
[0035] The preferred embodiment of the Type- 1 reactor system is a batch system, as shown in FIG. 2. For experimental work, this reactor system 100 comprises of a quartz reaction vessel 50 , a photochemical reactor chamber 60 (such as a Rayonet Photochemical Mini-Reactor Model RMR-600), and an ultrasonic liquid processor or “sonicator” (such as the preferred Misonix Model 2020) that has a ½-inch diameter titanium horn tip with a flat radiating surface. If no cap, which is optional, is placed on the reaction vessel 50 , this permits background loss of volatile constituents (such as tetrachloroethylene (“PCE”), for example) in the reactor.
[0036] The quartz reaction vessel 50 is custom built with the following preferred specifications: a height of 317.50 mm, an inner diameter of 76.20 mm, inlet 52 and outlet 54 tubes of 4-mm diameter and a height of 241.30 mm from the reactor bottom. Solution to be treated is preferably placed within the reaction vessel 50 to a solution level 51 , thereby resulting in a 1-liter open photosono reactor, when no cap, which is optional, is placed on the reaction vessel.
[0037] The input 52 and output 54 tubes are used to facilitate recirculation of the solution and keep the TiO 2 particles in suspension when TiO 2 powder is added. Such recirculation is preferably done by a peristaltic pump, such as a Flex-Flow model 7553-70, having a recirculation rate of 250 mL min −1 . It is preferred that the temperature of the solution be kept at 10±5° C. through the use of a chiller, as shown in FIG. 1.
[0038] The sonicator horn tip 72 is submerged into the quartz reactor vessel 50 placed inside the photoreactor chamber 60 . The contaminated solution to be treated is placed within the quartz reaction vessel 50 . The preferred photo-reactor 80 is placed outside the quartz reactor vessel 50 . This photo-reactor 80 contains light sources (4 watts per lamp, 32 watts total), power consumption of about one ampere per lamp at 110/120 volts (50/60 Hz A.C.).
[0039] Thus, the solution to be treated is UV-irradiated from UV radiation from the outside of the reactor vessel (the photoreactor), and the solution is exposed to ultrasonic (US) waves from within the reactor vessel (from the submerged sonicator horn tip).
[0040] The photoreactor's UV lamps are preferably turned on for at least 15-30 minutes before the contaminated solution is added to the reactor vessel. This 15-30 minutes warm-up period allows the lamps to reach a standard operating temperature. A cooling system comprising an internal fan and an external air source are also preferably employed to keep the lamps from overheating.
[0041] 2. Flow-Through Reactors
[0042] The preferred flow-through reactors comprise a reaction vessel, a UV lamp(s), and an ultrasonic liquid processor (e.g., Misonix Model 2020). This is a closed vessel, designed for a continuous flow mode.
[0043] a. The “Type- 2 ” Reactor
[0044] Referring to FIG. 3, the Type- 2 reactor system is a continuous, flow-through reactor system 100 . For experimental work, the photosono reactor comprises a double wall quartz photoreaction vessel 50 , a UV lamp 80 , and an ultrasonic liquid processor 70 (Misonix Model 2020) with a custom designed (modified) cuphorn having a titanium tip with a flat radiating surface of 64 mm (2½ inches) diameter.
[0045] The double wall quartz vessel 50 was designed by the inventor, custom built with the following approximate preferred specifications: a height of 250 mm, an outer diameter of 120 mm, inlet-outlet port of a 7-mm outside diameter and 4-mm inside diameter at a height of 250 mm from the reactor bottom. The inner diameter of the immersion well is approximately 40 mm. Thus, the total volume available for the reaction is approximately 1840 mL. This is a closed vessel, designed for a continuous flow mode.
[0046] The preferred UV light source 80 used is a 100-watts mercury-vapor lamp with the following preferred specifications: 90-110 lamp volts, 1.2 lamp amps,arc length of 69.86 mm, distance from lamp to bottom is 42.86 mm, total length of 155.58 mm. The silicone lead wires, fitted with pin jacks for connecting to power supply, permit lowering of the lamp for vertical location in an immersion well.
[0047] b. The “Type- 3 ” Reactor
[0048] Referring to FIGS. 4 A, the Type- 3 reactor system is a modified version of the Type- 2 flow-through reactor system. The modification was made to improve its efficiency. The reactor was modified from a commercially available cuphorn 77 (Model 431, Misonix) by increasing the depth, placing an immersion well 60 for a UV lamp and sealed the cup with a plexiglass plate 57 , resulting in an approximately 2.8 L photosono reactor.
[0049] A titanium tip 72 with a flat radiating surface of 64 mm (2½ in.) diameter was used in the Type 3 system. The design of the reactor 100 allows the UV lamp to be placed into the cuphorn of the reaction vessel 77 . A single immersion lamp (Model 7825, ACE Glass Inc.) is employed as a source of ultraviolet light. The UV light source used is a 100-watts, mercury-vapor lamp with the following specifications: arc length of 69.86 mm, distance from lamp to bottom is 42.86 mm, total length of 155.58 mm. The silicone lead wires, fitted with pin jacks for connecting to power supply, permit lowering of the lamp for vertical location in an immersion well 60 .
[0050] Referring to FIG. 4B, the Type- 3 B reactor system is modified version of Type- 3 A reactor system by adding a water jacket #a, an inlet port #b, and an outlet port #c. Cooled water (preferably 10±5° C.), cooled by the chiller 140 and the recirculation vessel 150 (in FIG. 1B) is supplied to an outer water jacket #a from an inlet port #b, and removed from an outlet port #c. This results in the temperature of the reactor solution being reduced to preferably less than 25° C.
[0051] c. The “Type- 4 ” Reactor
[0052] As shown in FIG. 5, the Type- 4 reactor system 100 is a modified version of the Type- 1 batch reactor system 100 . This reactor system 100 comprises a quartz reaction vessel 50 , a photochemical chamber reactor 60 (Rayonet, Model RPR-100), and an ultrasonic liquid processor 70 (Misonix, Model 2020) with a ½ (one-half) inch diameter horn. The preferred quartz vessel was custom built with the following specifications: a height of 315 mm, an inner diameter of 90 mm, inlet and outlet tubes of 4 mm diameter at a height of 241.3 mm from the reactor bottom. The sonicator horn tip is submerged into the immersion well about 25.4 mm from the solution surface in the quartz reactor vessel. Total volume available for the reaction is approximately 1680 mL. This is a closed vessel, designed for a continuous flow mode. The top of the quartz reactor is sealed with a Teflon sheet. The quartz vessel is placed inside the photochemical chamber (Rayonet, Model RPR-100). The solution to be treated is UV-irradiated from the outside, and exposed to acoustic waves from inside (in the solution to be treated).
EXAMPLE I
Experimental Section
[0053] The primary objective of this study was to evaluate the combined effect of UV and US on the degradation of VOC compounds by quantifying their effects in terms of degradation rate and removal efficiency. In the present study, photolysis, sonolysis and photosonolysis of TCA, TCE, and PCE were comparatively investigated using two different types of flow-through photosonolysis reactor systems.
[0054] Materials and Solution Preparation
[0055] All chemicals used were of analytical reagent quality. 1,1,1-Trichloroethane (99+%), trichloroethylene (99.5+%), tetrachloroethylene (99.9+%), and titanium dioxide (99.9+%, anatase) were obtained from Aldrich Chemical Co. All aqueous solutions were prepared in water purified with a Barnstead Milli-Q/RO system (R=18 MΩ-cm).
[0056] Prior to each experimental run, an 18-L solution of simulated groundwater was prepared according to Hardy and Gillham by adding the following reagent-grade salts to deionized water: 0.100 g of MgSO 4 , 0.124 g of CaCl 2 , 0.187 g of NaCl, and 0.303 g NaHCO 3 . Expected concentrations of the ions are given in Table 1. For the experiments with TiO 2 , 1.8 g of TiO 2 was added to 18 L of simulated groundwater, resulted in a concentration of 100 mg/L TiO 2 .
TABLE 1 Composition of Simulated Groundwater Concentration Parameter (mg/L) (mM) Na + 8.69 0.378 Mg 2+ 1.12 0.046 Ca 2+ 2.48 0.062 Cl − 10.67 0.301 SO 4 2− 4.41 0.046 HCO 3 − 12.24 0.201
[0057] Equipment
[0058] Two types of photosono reactor systems, a cup-horn reactor and a probe-horn reactor, were constructed for the experiments. For both reactor systems, an ultrasonic liquid processor (Model XL2020, Misonix), capable of delivering 550 W of ultrasonic energy and producing ultrasonic waves of 20-kHz frequency was used. All of the tests were conducted in a pulse (5-sec on/off) mode. The sonicator was allowed to warm-up for 30 min prior to increasing the power to the operating frequency. The cup-horn reactor system consisted of a 2850-mL vessel equipped with ultraviolet light and ultrasound sources, a feed pump, a recirculating chiller, a cooling unit, and two collapsible containers. FIGS. 1 (A-B) shows a schematic diagram of the cup-horn reactor system. A custom cup-horn vessel (Misonix) with 140-mm I.D. and 220-mm depth was modified to accomodate a UV lamp. A 100-W medium pressure, quartz, mercury-vapor lamp and a power supply (Model 7830, ACE Glass) were used as the UV source. The UV lamp was placed inside the quartz immersion well. UV intensity was measured at outer surface of the immersion well at three positions (60, 140, and 250 mm from the bottom of the well) using a UVX digital radiometer (UVP Inc.). The average radiation intensity measured at λ=253.7 nm was 5.6 mW/cm 2 . Of total energy radiated, approximately 40 to 48% is in the ultraviolet, 40 to 43% in the visible, and the balance in the infrared portion of the spectrum. Ultrasonic waves were generated from a titanium horn with a flat 64-mm diameter radiating surface. The sonicator was operated at its maximum output setting and was typically delivering 70% of its rated power to the reactor (385 W). The UV lamp was allowed to warm up for 30 min before each experimental run. Throughout the cup-horn reactor experiment, the influent was kept at a constant temperature of 16° C. by using a recirculating chiller (Model CFT-33, Neslab) and a cooling unit. The flow rate of 100 mL/min, corresponding to a hydraulic retention time of 28.5 min, was selected.
[0059] The probe-horn reactor system consisted of a custom quartz vessel (1680 mL), a photochemical chamber, a sonicator with a probe horn, a feed pump, and two collapsible containers. FIG. 2 shows the reactor setup and the schematic of the system. The top of the custom quartz vessel was sealed with a Teflon sheet. A 12.7-mm diameter probe horn (Misonix) was placed in a solution at a depth of 25 mm from the solution surface. The photochemical chamber (Model RPR-100, Rayonet) is equipped with 16 UV light sources (peak intensity at 253.7 nm, 35 W per lamp) and a cooling fan. Only 8 lamps (total 280 W) were used in the probe-horn experiments. The lamps were allowed to warm up for 30 min before each experimental run. The intensity of UV radiation was measured at the inner surface of the empty quartz vessel at various locations using the digital radiometer. An average radiation intensity from the eight UV lamps was 4.76 mW/cm at λ=253.7 nm. The ultrasonic power output was 193 W (35% of its rated power to the reactor). The probe-horn reactor system was operated at retention times of 26 and 60 min.
[0060] Experimental Procedures
[0061] Prior to each experimental run, simulated contaminated groundwater was mixed on a shaker at 100 rpm for 1 hr. The reactor was filled with the solution and allowed to recirculate for at least 30 min to equilibrate the reactor system. A dark condition was maintained in the laboratory room by turning off all external lights and placing a cover (aluminum foil) over the whole reactor system.
[0062] After the equilibration, the effluent tubing was connected to a receiving container, and a timer was set to zero. During the course of experiments, a 20-mL sample was periodically withdrawn from the influent and effluent sampling ports for the analyses of VOCs, chloride, pH, and temperature. Of the total sample volume, 5 mL was used for pH measurement, 5 mL for chloride analysis, and three 1.5 mL samples were used for the VOC analysis.
[0063] The VOC analyses were performed using a headspace technique described by various investigators. The 1.5-mL samples were transferred into each of three 2-mL vials, followed by shaking for 20 min on a shaker. The samples were then allowed to equilibrate for 20 min in a temperature controlled chamber (Revco) at 20° C. After the equilibration, 50 L of the gas phase sample was injected into a GC. A HP 5890 Series II gas chromatograph with a Supelco SPB-5 capillary column (dia. 0.53 mm, length 30 m, and film thickness 3.0 m) was used for the analysis of each VOC constituent.
[0064] Chloride was analyzed by a chloride ion selective electrode (Fisher Accumet Model 915 pH/ISE Meter). The chloride ICE meter was calibrated daily using Cl − standard solutions. An Orion pH/ISE meter (Model 250A) was used to detect the changes in pH in inflow and effluent. All the samples were analyzed immediately following the sampling. The temperature of the influent and effluent was monitored by means of a digital thermometer (Monitoring Thermometer, Fisher Scientific).
[0065] It should be noted that the selected experimental conditions (e.g., power of ultraviolet light and ultrasound, and reactor retention time) were not intended to demonstrate high process efficiencies, but were chosen so that the individual and combined effects of UV and US could be evaluated comparatively. Since ultrasound was emitted in a 5 sec on/off pulse mode, the net US irradiation time is half of the total run time or UV irradiation time.
[0066] Results and Discussion
[0067] Photolysis, sonolysis, and photosonolysis of the VOC compounds are evaluated using the first-order degradation rate constant (k) and the removal efficiency (E). In a UV-TiO 2 study using a recirculating photoreactor, Glaze et al. reported that PCE and TCE degradation can be expressed using first-order kinetics. Our preliminary studies with a batch system suggested that the VOC degradation with UV and US follows pseudo first-order kinetics. A continuously stirred tank reactor (CSTR) system was assumed because the lamp emits UV light in all directions and ultrasound provides intensive mixing in the reactor vessel. A general equation at a constant flow rate may be given as:
C t + ( 1 t d + k ) C = C in t d ( 1 )
[0068] where C in and C are the constituent concentrations (mg L −1 ) in influent and effluent, respectively. t d and k are the reactor retention time (min) and first-order degradation rate constant (min −1 ), respectively. At steady state with constant C in , solution of Eqn (1) is given as:
C ss = C in 1 + k t d ( 2 )
1 C ss = 1 C in + k t d C i n ( 3 )
[0069] where C ss is the steady-state effluent concentration. The value of k can be determined from the slope of the1/C ss versus t d /C in plot, or calculated using Eqn (4):
k = ( C i n C ss - 1 ) / t d ( 4 )
[0070] The combined effect of UV and US can be additive, antagonistic, or synergistic. The additive effect of UV and US is assumed to be summation of the k values obtained from the UV and US runs:
k ad =k uv +k us (5)
[0071] where k uv and k us are the first-order degradation rate constants (min −1 ) observed for UV and US, respectively.
[0072] The UV, US, or UVUS efficiencies for the contaminant removal may be given as:
E =( C in −C ss )/ C in (6)
[0073] where E is the observed efficiency for a given process (UV, US, or UVUS). C in and C ss are respectively the steady-state concentrations of VOC constituent in influent and effluent. The additive effect of the UV and US may also be evaluated using the removal efficiencies by UV and US as:
E ad =E uv +E us (1 −E uv ) (7)
[0074] where E uv and E us are the removal efficiencies (fraction) with UV and US, respectively. E ad is the additive efficiency (fraction). It is postulated that, for defining the additive efficiency, a UV reactor and a US reactor are situated in series. In this study, the combined effects are defined as follows:
[0075] if k uvus =k ad and E uvus =E ad , the combined effect is additive
[0076] if k uvus <k ad and E uvus <E ad , the combined effect is antagonistic
[0077] if k uvus >k ad and E uvus >E ad , the combined effect is synergistic
[0078] where k uvus and E uvus are, respectively, the first-order degradation rate constant and removal efficiency exhibited by the UVUS run. If the observed k uvus value was larger than the calculated additive rate (k ad ) and the observed removal efficiency (E uvus ) was larger than the additive efficiency (E ad ), then a synergistic effect between UV and US would exist.
[0079] [0079]FIGS. 6 through 9 show the results of one experiment using the cup-horn photosono reactor (FIGS. 1 A-B). In this experiment, simulated groundwater containing TiO 2 at 100 mg/L was spiked with a mixture of TCA, TCE, and PCE (VOCs). The aqueous VOC solutions were then treated with UV, US separately, and UV and US simultaneously (UVUS). The VOC compounds, chloride, and pH in influent and effluent were monitored over a 90-min run period. In the control run (FIG. 6), the concentrations of the VOC compounds in the effluent were slightly lower than those in the influent, indicating possible background losses of these compounds. Since there were little differences in the influent and effluent chloride concentrations and pH, the VOC losses were likely due to transport phenomena, probably a gas phase leakage from the reactor. In this particular experiment, US had scant effect on the degradation of the VOC compounds (FIG. 7). Although the differences in the concentrations of the VOC constituents in the influent and effluent were small, the effluent VOC concentrations were consistently lower than the influent concentrations. The slightly elevated chloride concentration and decreased pH in the effluent suggest some degradation (sonolysis) of the VOC compounds had occurred. UV had marked effects on the degradation of TCE and PCE, but little effect upon TCA (FIG. 8). The elevated chloride concentration and decreased pH in the effluent are most likely due to the degradation (photolysis or photocatalysis) of TCE and PCE. UVUS affected, to the largest extent, the decomposition of the VOC compounds, as seen in the effluent as significant decreases in the TCA concentration and pH, and an increase in the chloride concentration (FIG. 9). Results from other experiments are generally in good agreement with the above observations, and all available data were used in the evaluation of the first-order degradation rate constant (k) and the removal efficiency (E).
[0080] The values of k and E for the VOC compounds were evaluated as follows. First, a steady state period in which the influent and effluent VOC concentrations are stable was selected. Then the average influent (C in ) and effluent (C ss ) concentrations were calculated for the observed steady state period. The values of k and E for each VOC constituent and experimental condition were calculated using Eqns (4) and (6), respectively. The net removal efficiencies and degradation rate constant values were calculated by subtracting the background losses from the UV, US, and UVUS experimental results. The additive degradation rate (k ad ) and removal efficiency (E ad ) were calculated using Eqns (5) and (7), respectively, as summarized in Table 2, below.
TABLE 2 Summary of the VOC Degradation Rate Constants and Removal Efficiencies for the Cup-Horn Reactor System. Influent Degradation Rate Removal Conc. Const. Efficiency Constituent Process Cin (mg/L) k (per min) E (fraction) Comment TCA UV 139 0.002 0.043 K UVUS > K td in VOC US 68 0.005 0.102 E UVUS > E td mixture UVUS 138 0.012 0.209 UV&US Additive n/a 0.007 0.140 TCA UV 221 nil nil K UVUS > K td in VOC US 68 0.005 0.102 E UVUS > E td mixture UVUS 182 0.006 0.128 UV&US Additive n/a 0.005 0.102 TCE UV 73 0.078 0.601 K UVUS < K td in VOC US 37 0.002 0.036 E UVUS < E td mixture UVUS 87 0.076 0.598 UV&US Additive n/a 0.079 0.615 TCE UV 145 0.024 0.347 K UVUS > K td in VOC US 37 0.002 0.036 E UVUS > E td mixture UVUS 86 0.039 0.450 UV&US Additive n/a 0.026 0.371 PCE UV 21 0.068 0.547 K UVUS > K td in VOC US 9 nil nil E UVUS > E td mixture UVUS 22 0.071 0.556 UV&US Additive n/a 0.068 0.547 PCE UV 58 0.023 0.319 K UVUS > K td in VOC US 9 nil nil E UVUS > E td mixture UVUS 42 0.048 0.475 UV&US Additive n/a 0.023 0.319 TCE UV 46 0.031 0.416 K UVUS > K td US 45 0.013 0.235 E UVUS > E td UVUS 36 0.059 0.565 UVUS 0.24 0.178 0.764 UVUS 0.04 0.278 0.815 UV&US Additive n/a 0.044 0.553 PCE UV 13 0.103 0.680 K UVUS > K td US 10 0.015 0.264 E UVUS > E td UVUS 10 1.481 0.906 UVUS 0.03 1.593 0.908 UV&US Additive n/a 0.118 0.764
[0081] The background losses of TCA, TCE, and PCE in the three-component mixture observed in the control run were respectively 9, 10, and 13% of the influent VOC concentrations, and occurred at rates of 0.004, 0.004, and 0.005 min −1 . Slight degradation of TCA was shown by UV (k uv =nil, 0.002 min −1 ; E uv =nil, 4.3%). TCA was degraded by US with k us value of 0.005 min −1 and E us value of 10.2%. UVUS yielded the considerably larger TCA degradation rates (k uvus =0.006 and 0.012 min −1 ) and removal efficiencies (E uvus =12.8 and 20.9%). The k uvus and E uvus values are somewhat larger than the calculated additive rate constants (k ad =0.005 and 0.007 min −1 ) and efficiencies (E ad =10.2 and 14.0%), suggesting a possible synergistic effect of UV and US on the decomposition of TCA.
[0082] TCE was degraded by UV yielding k uv values of of 0.024 and 0.078 min −1 and E uv values of 34.7 and 60.1%. Slight decomposition of TCE was shown by US with k us value of 0.002 min −1 and E us value of 3.6%. With UVUS, the degradation rate constant values (k uvus =0.039 and 0.076 min −1 ) and removal efficiencies (E uvus =45.0 and 59.8%) evaluated for TCE are comparable with the calculated additive rate constants (k ad =0.026 and 0.079 min −1 ) and efficiencies (E ad =37.1 and 61.5%). The observed UVUS effect on the TCE degradation is observed to be additive of the UV and US effects, although it could be smaller than the additive effect under certain conditions.
[0083] PCE in the three-constituent mixture was degraded by UV with k uv values of 0.023 and 0.068 min −1 , yielding E uv values of 31.9 and 54.7%. An extent of PCE degradation with US was nearly a background loss level. UVUS gave k uvus values of 0.048 and 0.071 min −1 and E uvus values of 47.5 and 55.6%. These values are somewhat larger than the calculated additive values (k ad =0.023 and 0.068 min −1 ; E ad =31.9 and 54.7%). Although US alone exhibited little effect on PCE degradation, it enhanced the photolysis of PCE, suggesting a possible synergistic effect of UV and US on the decomposition of PCE.
[0084] Simulated groundwater solutions containing TCE or PCE at two different concentrations were exposed to UV, US, and UVUS. TCA was not selected for the single-constituent experiments because of its poor degradability with UV, as previously shown. The results from the single-constituent runs are also presented in Table 2. Approximately 7% of the inflow TCE was lost during the control run at a rate of 0.003 min −1 . TCE was degraded by UV at a photolysis rate, k uv , of 0.031 min −1 yielding E uv value of 41.6%, while it was degraded by US at a sonolysis rate, k us , of 0.013 min −1 with E us value of 23.5%. The UVUS runs were carried out at three different concentrations. At 36, 0.24, and 0.04 mg/L TCE, the values of k uvus are respectively 0.059, 0.178, and 0.278 min −1 , and E uvus are of 56.5%, 76.4%, and 81.5%. The observed k uvus and E uvus values are consistently larger than the calculated additive rate (k ad ) of 0.044 min −1 and the additive efficiency (E ad ) of 55.3%. Thus, the results suggest synergistic effect of UV and US on the decomposition of TCE. It should be noted that for the UVUS runs, decreasing influent concentration increased the degradation rate constant and the VOC removal efficiency. Similar trends were reported by Glaze et al. in their study with TiO 2 -mediated photolysis of TCE and PCE.
[0085] The background loss of PCE was evaluated to be 7% of its influent concentration and occurred at a rate of 0.003 min −1 . Photolysis of PCE took place at a rate (k uv ) of 0.103 min −1 , giving a removal efficiency (E uv ) of 68.0%. PCE was degraded with US at k us of 0.015 min −1 and E us of 26.4%. The UVUS runs were carried out at 10 and 0.03 mg/L PCE, and yielded k uvus value of 1.48 and 1.60 min −1 , respectively. Both the runs yielded the removal efficiency values (E uvus ) of approximately 91%. Since E uvus and k uvus values are substantially larger than what would be expected for an additive effect of UV and US (k ad =0.118 min −1 , E ad =76.4%), the combined effect of UV and US on the decomposition of PCE is shown to be synergistic.
[0086] Experimental results from the probe-horn reactor study are fundamentally consistent with the cup-horn reactor results. A summary of their data analysis is given in Table 3, below.
TABLE 3 Summary of the VOC Degradation Rate Constants and Removal Efficiencies for the Probe-Horn Reactor System. Influent Degradation Rate Removal Conc. Const. Efficiency Constituent Process Cin (mg/L) k (per min) E (fraction) Comment TCA UV 53 0.003 0.006 K UVUS > K td (t d = 26 min) US 53 0.007 0.127 E UVUS > E td UVUS 54 0.019 0.275 UV&US Additive n/a 0.010 0.176 TCA UV 46 nil nil K UVUS > K td (t d = 60 min) US 43 0.004 0.113 E UVUS > E td UVUS 43 0.009 0.218 UV&US Additive n/a 0.004 0.113 TCE UV 29 0.055 0.431 K UVUS > K td (t d = 26 min) US 42 0.005 0.071 E UVUS > E td UVUS 34 0.106 0.556 UV&US Additive n/a 0.059 0.471 TCE UV 26 0.035 0.480 K UVUS > K td (t d = 60 min) US 33 nil 0.008 E UVUS > E td UVUS 24 0.058 0.566 UV&US Additive n/a 0.035 0.484 PCE UV 7 0.524 0.663 K UVUS < K td (t d = 26 min) US 11 nil nil E UVUS < E td UVUS 6 0.422 0.649 UV&US Additive n/a 0.524 0.663 PCE UV 5 4.973 0.618 K UVUS > K td (t d = 60 min) US 11 nil nil E UVUS > E td UVUS 8 8.307 0.620 UV&US Additive n/a 4.973 0.618
[0087] Note that TiO 2 was not used in all the probe-horn experiments. As expected from the previous cup-horn experiments, TCA was not effectively degraded with UV. US affected slightly the degradation of TCE. TCE was degraded more effectively by UV than US, and most significantly by UVUS. PCE was most effectively degraded by UV, while it was not affected by US. For all the cases with the probe-horn experiments, except for the PCE run at t d =26 min, the k uvus values are greater than the k ad values, and the E uvus values are greater than the E ad values. The combined effect of UV and US is seen to fall in the additive to synergistic range depending on the conditions.
[0088] For both the cup-horn and probe-horn systems which were run under the various conditions (with or without TiO 2 ), the order of degradability given by the values of the degradation rate and removal efficiency are PCE>TCE>TCA with UV, TCA>TCE>PCE with US, and PCE>TCE>TCA with UVUS. A photocatalysis study with a mixture of chlorobenzene, PCE, and TCA found in the literature reports that the order of degradation was chlorobenzene >PCE>TCA. The explanation given to the order was that the higher electron density of the aromatic and unsaturated compounds led to stronger adsorption on electrophilic sites at the TiO 2 surface. In our experiments with UV, the degradation rates of PCE and TCE were greater than that of TCA with and without TiO 2 , suggesting that the degradation reaction that occurred in the reactors was predominantly non-catalytic photolysis.
[0089] As was mentioned earlier, experimental conditions were chosen to allow the comparisons between UV, US and UVUS. Optimization to increase reactor efficiency and obtain higher degradation rates was beyond the scope of the present work. It is expected that increasing the power of the UV and US sources will result in higher degradation rates and removal efficiencies. Significantly high concentrations of TiO 2 can result in lower photocatalysis efficiency due to the interference of the solid catalyst with light penetration. Particle size and concentration of TiO 2 also affect the sonolysis rate. Orzechowska et al. suggested that the fine particles may enhance the rate by providing additional nuclei for bubble formation and large particles may decrease the rate because of sound attenuation. They found, however, that sand particles at various sizes and concentrations had a negligible effect on the degradation rate.
[0090] The mechanism of ultrasonic enhancement, when used in combination with TiO 2 -photocatalysis, is thought to be due to acoustic and/or cavitational effects at the semiconductor-solution interface. At the microscopic level, the implosion of vapor bubbles near the semiconductor particle may enhance mass transport at solid surfaces, and aid in surface adsorption of the substrate. Local region of high temperature and pressure can also result in the acceleration of reactions between free radicals and the substrate. Microjets induced by cavitation may act to cleanse the catalyst surface which may become poisoned by inert byproducts. This mechanism may allow more effective adsorption and radical production, and may decrease the effective diffusion zone thickness for reactants and products. In our study, however, enhancement of the VOC photolysis by US was observed in the experiments with and without TiO 2 particles, suggesting that direct- or noncatalytic-photolysis was the predominant reaction. If the photolysis rate (k) is a direct function of the light intensity (I λ ) molar absorbtivity (E λ ) at wavelength λ, and quantum yield (φ) of the compound of interest, the quantum yield might possibly be a cause for the observed synergism. It can be postulated that photolysis, in combination with sonolysis, initiated a chain reaction for the VOC degradation, resulting in increased quantum yield. Without more evidence, the ultrasonic enhancement mechanisms that produce the synergistic effect in the photolysis of VOC compounds remains an open question.
[0091] Since the observed effluent chloride concentrations are considerably lower than those estimated assuming complete mineralization of the VOC compounds, the dechlorination reaction is unlikely the initial step of the degradation pathways, and the possible formation of chlorinated byproducts is suggested. According to the photocatalytic mineralization pathway model for TCE and PCE, dechlorination occurs in later stages of the degradation pathway. During the photocatalysis experiments, dichloroacetic acid, dichloroacetaldehyde, trichloroacetaldehyde, and trichloroacetic acid were formed as byproducts of TCE, and dichloroacetic acid and trichloroacetic acids as byproducts of PCE. Although elucidation of photosonolysis pathway is beyond the scope of this application, the presently available results lead us to suggest that the halogenated sites of some of the target compounds are less reactive than the nonhalogenated sites, and that the reaction scheme does not lead to the immediate release of chloride ion. In our study, the GC/MS analysis indicated formation of methylene chloride and chloroform or structurally similar compounds during the photosonolysis of PCE and TCE, suggesting double-bond cleavage as one of the primary degradation pathways. Elucidation of the degradation pathway of these compounds is underway to gain a better understanding of photosonocatalysis.
[0092] In summary, this study demonstrated photosonolysis of TCA, TCE, and PCE in simulated groundwater using the cup-horn and probe-horn reactor systems. The values of the first-order degradation rate constant (k uv , k us , k uvus ) and the removal efficiency (E uv ,E us , E uvus ) for the VOC compounds were evaluated for the UV, US, and UVUS treatments. The k uvus values were compared to the k ad values calculated from the sum of the rate constants under the individual UV and US irradiation (k ad =k uv +k us ), and the E uvus values were compared to the calculated E ad values, E ad =E uv +E us (1−E uv ). The concurrent use of UV and US increased, in most cases, the VOC degradation rate constant and removal efficiency beyond the additive effect of UV and US. The results suggest that the combination of UV and US can create synergistic effects on the decomposition of VOCs in water.
EXAMPLE II
[0093] Introduction
[0094] This section reports findings by the inventor that: 1) an aluminum partition installed in the UVUS reactor increases the efficiency of the VOC (PCE, TCE) removal relative to a stainless steel partition; and 2) the aluminum partition enhances synergistic effect of UV and US on the removal of VOC relative to a stainless steel partition.
[0095] The newly developed reactor vessel consists of a UV lamp compartment, a US horn compartment, and a partition compartment. The partition compartment is a removable compartment made of either aluminum (AL) or stainless steel (SS). Data on photosonolysis of VOC obtained from the experiments using the reactor having the AL partition are compared to those from the experiments using the reactor with the SS partition. Stainless was used as control material.
[0096] This paper adapts the following notation: PCE=tetrachloroethylene, TCE=trichloroethylene, VOC=chlorinated volatile organic compounds (particularly PCE and TCE in this paper), UV=ultraviolet light or the ultraviolet light run, US=ultrasound or the ultrasound run, UVUS=the combination of UV and US, AL=aluminum or the reactor with the aluminum partition, SS=stainless steel or the reactor with the stainless steel partition, and UP=upflow scheme.
[0097] Experimental Methods
[0098] The reactor system setup is illustrated in FIG. 10. The UVUS reactor system consists of a three-compartment reactor vessel, a feed pump, two collapsible containers, and a shaker.
[0099] Design of the Three-Compartment UVUS Reactor
[0100] A 4.1-L reaction vessel was custom designed and manufactured by commercial Plastics & Supply Co. (Salt Lake City, Utah). The vessel can be separated into a UV compartment and a US compartment by installing the partition. The partition was made by welding two round sheets (of aluminum or stainless steel) together (see FIG. 11). The dimension of each sheet was 200-mm diameter and 3.2-mm thickness. The conduit height in the plate was 60 mm and the volume of the inner space between the two sheets (i.e., the partition compartment volume) was 90 mL.
[0101] A cup-horn ultrasonic liquid processor (LX 2020, Misonix, Farmingdale, N.Y.) was used as US source. The rated maximum ultrasonic power was 550 W at 20 kHz output frequencies. A model 7825 medium pressure, quartz, mercury-vapor immersion lamp (100 watts) with a power supply (7825-30 power supply, ACE Glass Inc., Vineland, N.J.) was employed as a UV source. The total radiated energy was 11.49 watts. Approximate 40% is located in the ultraviolet region of the spectrum, 41% is in visible region, and the remaining belongs to infrared region. Irradiance was measured by a UVX digital radiometer (UVP Inc., San Gabriel, Calif.).
[0102] A Masterflex Pump (Model 7553-71, Cole-Parmer Instrument Company, Niles, Ill.) was used to feed aqueous solution into the reactor. Two collapsible containers (Cole-Parmer Instrument Co., Vernon Hills, EL) were used as a reservoir for the feed solution and a container to receive treated solution. A shaker (Model G-33, New Brunswick Scientific Company, Edison, N.J.) was used to agitate feed solution for obtaining uniform constituent concentration.
[0103] Experimental Conditions
[0104] All experiments were carried out using a flow-through UVUS reactor with a partition made of AL or SS. Using the partition, the reactor was divided into a UV lamp compartment, a US horn compartment, and a partition compartment; thus, the investigations of the effects of UV and US can be conducted either separately, series, or concurrently. In this study, all experimental runs were conducted in an upflow, from the US compartment to the UV compartment (US→UV), scheme.
[0105] The sonicator was operated in a pulse (5-second on/off) mode. The ultrasonic power delivered into the aqueous solution was approximately 330 W (delivered 60% of the rated power) at 20 kHz output frequencies. The power of the UV lamp employed was 100 watts. The average radiation intensity employed at λ=253.7 nm was 16.1 mW/cm 2 for the TCE experiment and 10.6 mW/cm 2 for the PCE experiment. The flow rate of 100 mL/min, corresponding to the total hydraulic retention time of 41 min (30 min for the UV compartment, 11 min for the US compartment, 50 sec for the partition compartment), was maintained for all experimental runs.
[0106] Experimental Procedures
[0107] The experiments consisted of TCE and PCE runs. All the chemicals were used as received. A 20-L solution containing TCE or PCE was prepared in a feed solution container and uniformly mixed for 30 min on the shaker at 100 rpm. The solution was filled into the reactor system and allowed to recirculate until the system reached equilibrium (about 60 min). After the equilibration period, the effluent was discharged into a receiving container. The flow rate was adjusted to 100 mL/min. When the UV lamp, the US sonicator, or both were turned on (except for the control run), the timer was set to zero for each experiment.
[0108] During each experimental run, a 20-mL sample was withdrawn at times 0, 3, 5, 10, 20, 30, 60, 90 min from the influent and effluent sampling ports for the analyses of TCE, PCE, chloride, and pH. Temperatures of influent and effluent solutions were recorded at each sampling time. All samples from the experiments were analyzed in the lab immediately after each sampling (or experimental run). Analysis of TCE and PCE was performed using a BP 5890 Series II gas chromatograph (GC) with a DB-624 capillary column (diameter 0.32 mm, length 30 m, and film thickness 1.8 μm, J&W Scientific, Folsom, Calif.) and an Electron Capture Detector (ECD).
[0109] Results
[0110] The effect of the partition material on the photosonolysis of PCE and TCE in the UVUS reactor, was examined. The reactor efficiencies (E 3 =Euvus) for the removal of VOC in the UVUS runs are computed using Eqns. (1)′ and (2)′.
E 3 C i n C ss3 C i n 1 C ss3 C i n ( 1 ) ′ E 3 = [ 1 - 1 ( 1 + k 1 t d1 ) ( 1 + k 2 t d2 ) ( 1 + k 3 t d3 ) ] ( 2 ) ′
[0111] where E 3 =Euvus=the removal efficiencies based on the effluent of the third compartment of the reactor at steady state; t d1 , t d2 , and t d3 =the mean retention time (min) for the first, second, and third compartment, respectively; k 1 , k 2 , and k 3 =the degradation rate constants (min −1 ) in the first, second, and third compartment, respectively(=k us , k pc , and k us , respectively). The effect of the partition compartment on the overall efficiency was assumed to be insignificant due to its small retention time (t d2 =50 sec).
[0112] The theoretical additive removal efficiencies (E ad ) were calculated using Eqn. (3)′
E ad E us (1 E us )E uv (3)′
[0113] where E ad =the additive removal efficiency; E uv =the removal efficiency with UV irradiation; and E us =the removal efficiency with US irradiation. If E uvus =E ad , the combined effect is additive; if E uvus >E ad , the combined effect is synergistic; if E uvus <E ad , the combined effect is antagonistic. E uvus =the removal efficiency with UVUS irradiation.
[0114] The reactor efficiencies (E uvus ) for the removal of PCE and TCE are presented in Table 1′ and shown graphically in FIG. 12 As seen, for both PCE and TCE, the combined effect of UV and US is greater with the AL partition than that with the SS partition (control).
[0115] The observed removal efficiencies (E uvus ) and the theoretical additive efficiency (E ad ) for the removal of PCE and TCE are presented in Table 2′. FIG. 13 gives a comparison between E uvus and E ad obtained from the AL-UP and SS-UP runs with PCE and TCE. It is seen for both PCE and TCE that the observed removal efficiencies (E uvus ) are greater than the corresponding theoretical additive removal efficiency (E ad ) in both the AL and SS runs. The difference between E uvus and E ad is more distinct with the AL partition. The result suggests that the synergistic effect of UV and US on the decomposition of VOC is enhanced by the AL partition.
[0116] Conclusions
[0117] 1) An aluminum partition increases the UVUS reactor efficiency for the removal of VOC (PCE, TCE) relative to a stainless steel partition.
[0118] 2) An aluminum partition enhances synergistic effect of UV and US on the removal of VOC in the UVUS reactor relative to a stainless steel partition.
TABLE 1 Reactor efficiencies (Euvus) for the removal of PCE and TCE Efficiency, Euvus Experimental Run (fraction) PCE-AL 0.884 PCE-SS 0.867 TCE-AL 0.951 TCE-SS 0.897
[0119] [0119] TABLE 2 Comparison between the observed efficiency (Euvus) and the theoretical additice efficiency (Ead) for the decomposition of PCE and TCE Experimental Run Euvus Ead PCE-AL 0.884 0.843 PCE-SS 0.867 0.859 TCE-AL 0.951 0.881 TCE-SS 0.897 0.892
[0120] Although this invention has been described above with reference to particular means, materials and embodiments, it is to be understood that the invention is not limited to these disclosed particulars, but extends instead to all equivalents within the scope of the following claims. | The invention is a process and reactors designs for simultaneous ultraviolet light/ultrasound(UV/US) treatment of halogenated organic compounds contaminants in water. The reactors are preferably circular cylindrical reaction vessels that accept a central ultrasonic horn. UV light is provided by lamps placed generally parallel to the reactor walls. Or, UV light may be centrally provided in an immersion well near the ultrasonic horn. Also, preferably a hollow metal partition with a reactant flow-through hole is placed in the reactor between the UV light source and the ultrasonic horn. This way, simultaneous UV/US energy may be effectively provided to the reactors for the remediation of toxic compounds in the water in the reactors. Also, this way, compact and portable reactors may be constructed to permit mobile applications of the UV/US processes. | 2 |
BACKGROUND OF THE INVENTION
The present invention relates to the reduction of sulfur-containing emissions (e.g., SO 2 and SO 3 gases, particulate sulfates, and H 2 SO 4 mist) from a large scale, continuous, flat glass melting operation. The term flat glass refers to glass commercially produced by the float process, plate rolling and grinding, and sheet drawing. Flat glass generally conforms to a relatively narrow composition range as follows:
SiO 2 : 69-75% by weight
Na 2 O: 12-16% by weight
K 2 o: 0-2% by weight
CaO: 8-12% be weight
MgO: 2-5% by weight
Al 2 O 3 : 0-2% by weight
So 3 : 0.15-0.5% by weight
Fe 2 O 3 : 0-0.7% by weight
Commercial production of flat glass conventionally involves feeding raw glass batch materials into an opening at one end of an elongated melting furnace while withdrawing melted glass through an opening at the opposite end of the furnace and forming it into a continuous flat ribbon. Flat glass batches typically include sand (silica), soda ash (sodium carbonate), limestone (calcium carbonate), dolomite (calcium carbonate and magnesium carbonate), rouge (iron oxide), a source of sulfate such as salt cake, gypsum, etc., and sometimes the raw materials aplite, feldspar, or nepheline syenite. It is also known to use caustic soda in place of soda ash. Minor amounts of additional materials such as colorants may sometimes be used as well. These batch ingredients, in finely divided, dry, particulate form, are blended together and usually wetted with water prior to being introduced into the furnace. Additionally, a substantial amount of cullet (crushed glass) is mixed with the batch ingredients, in amounts usually ranging from about 20% to about 60% of the total glassmaking materials being fed to the furnace.
When introduced to the high temperature conditions within the melting furnace, the raw ingredients undergo chemical reactions and dissolution which, in a continuous flat glass furnace, normally take place within the first half of the furnace or less. The remainder of the furnace is devoted to "fining" (or "refining") and conditioning the glass melt. The process of fining is the removal of gaseous products of reaction from the melt by providing conditions which cause the gas bubbles to rise to the surface and burst or to redissolve in the glass. In a continuous glassmaking operation it is very important that conditions be maintained to enable fining of each portion of the melt to take place within its limited residence time in the fining zone of the furnace. Any gaseous inclusions which are carried out in the product stream form the defects known as "bubbles" (those having diameters larger than 0.25 mm.) or "seeds" (those having diameters smaller than 0.25 mm.) in the glass.
The problem of obtaining adequate fining is especially acute in a flat glassmaking operation since the standards for bubbles and seeds for flat glass are much more stringent than other types of glass such as bottle glass. For example, flat glass having one seed per square foot (0.09 square meter) would be considered rejectable for most flat glass applications, whereas what would be regarded as a very good grade of bottle glass may have on the order of 500 seeds per square foot (0.09 square meter) if formed into a sheet of the same thickness. In order to obtain adequate fining within a reasonable length of furnace, the flat glass industry has heretofore relied on the inclusion of large amounts of salt cake (sodium sulfate) and coal (carbon) in the batch as fining agents. The salt cake reacts to form substantial volumes of gaseous products which accelerate the movement of bubbles and seeds to the surface of the melt and help to homogenize the glass. Thus, it has long been the standard practice in the commercial production of flat glass to include substantial amounts of salt cake and coal in the batch ingredients fed to continuous melting furnaces. The customary use of salt cake and coal has also been based on other widely-held beliefs in the glassmaking art, such as the necessity for preventing "silica scum" (see "Handbook of Glass Maufacture," p. 66, F. V. Tooley, Ogden Publishing Co., N. Y., 1953) and for aiding the dissolution of sand grains (see Ceramic Bulletin, Vol. 54, No. 6 (1975), pp. 262-4).
Unfortunately, the use of salt cake as a fining agent has serious drawbacks. At glass melting temperatures salt cake dissociates or volatilizes, resulting in the emission of sulfur-containing gases. These may recombine with water vapor or sodium vapor within the furnace to form sulfuric acid mist or particulate sodium sulfate, which are not only air pollutants, but have a detrimental effect on the checker-packing in the regenerators of the furnace. Many widely varying proposals for reducing sulfur-containing emissions, have been made in the prior art, but none is entirely satisfactory.
One commonly proposed solution is to treat the effluent gas stream to remove the sulfur compounds. However, such an approach is costly and does not reduce the detrimental effects of the emissions on the regenerators. U.S. Pat. Nos. 3,788,832 and 3,880,639 disclose examples of the recovery and recycling of sulfur compounds from the exhaust gas stream by contacting the exhaust gas with incoming batch materials.
Elimination of salt cake is proposed in U.S. Pat. No. 3,846,143 by using in place thereof the reaction product of an alkali hydroxide and a source of alumina. It would be preferred that such an added pre-treatment step be avoided. Moreover, alkali hydroxides are generally a more costly batch material than salt cake and the seed counts reported in the patent appear to be much higher than permitted for flat glass. Substitution of SO 2 gas for some or all of the salt cake as a source of sulfate is taught in U.S. Pat. No. 3,375,095 for the purpose of reducing deposition of sodium sulfate in the regenerators, but apparently without alleviating overall sulfur-containing emissions. Also, the use of SO 2 gas as a sulfate source would usually be more costly.
Many other materials have been suggested for use as fining agents in addition to or as a substitute for salt cake, but without addressing the problem of sulfur emissions. In U.S. Pat. No. Re. 26,328 the use of calcium fluoride, gypsum, and slag are suggested as fining agents in a bottle glass operation. But gypsum and slag are both sulfur-containing, and the fluoride content of calcium fluoride can also be an air pollution problem. U.S. Pat. No. 3,589,885 discloses the use of carbonaceous material impregnated with a sulfate as a fining agent along with calcium fluoride for making bottle glass. U.S. Pat. No. 3,615,767 teaches the use of sodium sulfite as a fining agent. In U.S. Pat. No. 3,511,629 a frit containing sodium or barium sulfide is used as a fining agent. An article in "Ceramic Industry," Feb. 1972, page 31, suggests the use of elemental sulfur or slag in addition to salt cake as fining agents. The use of slag is also suggested in U.S. Pat. No. 3,725,022. None of these alternate fining agents is purported to alleviate sulfur-containing emissions problems, and for the most part appear to be merely substituting one source of sulfate for another in the batch.
It has also been previously suggested that pelletizing the batch as taught in U.S. Pat. Nos. 3,542,534 and 3,969,100 and the abovementioned U.S. Pat. No. 3,880,639, while intended primarily to ease melting, may have as a secondary advantage a lower salt cake requirement. The substantial capital investment and increased operating costs entailed by a pelletizing operation, however, make such an approach impractical in many cases. Moreover, since the presence of salt cake in these patents is said to be as a melting aid, and not as a fining agent, it is unclear what effect the reduction of salt cake would have on defect levels in a large scale, continuous, flat glass melting furnace employing pelletizing.
In U.S. Pat. No. 3,833,388 there is disclosed a glass composition differing from that of conventional flat glass, and which is said to require less salt cake, with a resulting reduction in sulfur-containing emissions. But because such a glass has properties which are slightly different from those of conventional flat glass, which properties are important in subsequent processing such as tempering, its use is preferably avoided.
Reduced amounts of salt cake are employed in the manufacture of one type of flat glass: colored glasses which incorporate selenium, cobalt, and nickel oxides, such as those disclosed in U.S. Pat. Nos. 3,296,004 and Re. 25,312. In glasses of this particular type, development of the desired coloration requires that oxidizing conditions be maintained and, therefore, salt cake and coal are minimized and alternate fining agents which act as oxidizing agents are employed, such as sodium nitrate or sodium chloride. The present invention, on the other hand, deals only with glasses which may be categorized as clear, or which contain iron oxide as the essential colorant. Since the refining agents used in the melting of the selenium, cobalt, and nickel colored glasses are more costly, and since the high oxidizing conditions are not required for conventional clear and iron tinted glass, the use of such alternate fining agents is preferably avoided when possible. Other alternate fining agents which are known in the art, but which are also preferably avoided, are arsenic oxide, antimony oxide, cerium oxide, and manganese oxide.
Other ways of reducing sulfur-containing emissions may be apparent to those of skill in the art, but each has serious drawbacks. For example, volatilization of salt cake may be reduced by lowering the melting furnace temperature, but the output of the furnace would be reduced and completeness of melting may suffer. Another possibility would be to reduce the amount of salt cake employed and compensate by increasing furnace temperatures. But the result would be shorter furnace life and greater fuel consumption. Yet another approach would be to increase the relative amount of cullet charged to the furnace along with the batch materials. This latter approach has been considered by some in the glass industry to be best solution to the emissions problem as evidenced by Business Week, Mar. 31, 1976, pp. 66B, 66H. But reliance on large amounts of cullet is preferably avoided because adequate supplies of suitable cullet are not always available in the flat glass industry, and excessive use of cullet represents inefficient utilization of a flat glass melting furnace in that more fuel is consumed to yield a net amount of glass. Thus, it would be desirable if sulfur-containing emissions could be reduced without altering the usual temperature conditions in a melting furnace, while at the same time using a high batch-to-cullet ratio.
SUMMARY OF THE INVENTION
The present invention relates to a method of operating a continuous flat glass melting furnace so as to reduce sulfur-containing emissions. This is achieved by the present invention without sacrificing glass quality and without the use of substitute fining agents, and yet permits the use of high batch-to-cullet ratios while operating at normal furnace temperatures and throughputs.
It has been discovered that a relatively small, specifically defined amount of salt cake employed in the batch results in reduced emissions without sacrificing glass quality. More specifically, it has been found that the sulfur content of the batch (expressed as SO 3 ) which includes both the salt cake in the batch as well as SO 3 in the cullet, should be less than about 2.25 (preferably less than 2.0) times the amount of SO 3 retained in the final glass product. In other words, for a given tonage of throughput, an optimum amount of salt cake has been found which is independent of the batch-to-cullet ratio. This is contrary to the prior art belief that inclusion of salt cake in an amount proportional to the sand in the batch was necessary. It has been found that this prior art practice of maintaining a fixed amount of salt cake for a given amount of sand in the batch can lead to excessive sulfur-containing emissions and to the production of excess foam on the surface of the melt and associated defects, particularly at high batch-to-cullet ratios, such as 70 parts by weight batch to 30 parts by weight cullet or higher. But by utilizing a batch with a total SO 3 content of no more than about 2.25 times that of the outgoing glass stream, it has been found that batch-to-cullet ratios higher than 70/30 may be used with reduced sulfurous emissions, while at the same time maintaining the usual low defect densities of flat glass.
It has additionally been discovered that even greater improvements can be obtained if the conventional inclusion of coal in the glass batch is reduced or essentially eliminated. Coal has long been considered an essential ingredient in the glass batch for the purpose of aiding melting. It was believed that the coal serves to break down salt cake into sodium oxide and sulfur dioxide, and that the sodium oxide then serves to dissolve sand grains. It has now been found, however, that such a reaction results in premature volatilization of the sulfur dioxide, with the result that less of the salt cake is available for fining at the subsequent fining stage of the continuous melting process and that excess foam is produced on the surface of the melt, particularly at high batch-to-cullet ratios. By eliminating coal, the salt cake is not so rapidly broken down, so that a greater portion of the salt cake may be retained in the glass melt so as to act as a fining agent in the fining zone of the melting furnace. While the fining ability of a given amount of salt cake is thus enhanced, it has been found quite suprisingly that no difficulty in melting sand grains and producing homogeneity is caused thereby in a flat glass melting operation. As a result, considerable less salt cake is needed to produce glass of a given quality and the amount of sulphurous emissions is reduced. Additionally, even though less salt cake is used, it has been found that fining is improved and that the final glass composition includes slightly more SO 3 than with previous practice. Also, the amount of foam in the furnace is reduced.
DETAILED DESCRIPTION
The invention will be illustrated herein by a number of specific examples of preferred embodiments, and these examples all relate to a large-scale, commercial glassmaking operation employing the float process, with an output of about 400 to 550 tons (360 to 500 metric tons) per day of flat glass. The glasses produced in the examples have the following average compositions, with only very minor variations:
______________________________________ Tinted Standard Clear______________________________________SiO.sub.2 72.80 73.10Na.sub.2 O 13.63 13.66K.sub.2 O 0.02 0.02CaO 8.80 8.85MgO 3.85 3.90Al.sub.2 O.sub.3 0.10 0.10SO.sub.3 0.25 0.25Fe.sub.2 O.sub.3 0.55 0.12______________________________________
TABLE I__________________________________________________________________________ Example 1* Example 2 Example 3 Example 4 Example 5__________________________________________________________________________Batch formula:Sand, kg. 1000.0 1000.0 1000.0 1000.0 1000.0Soda ash, kg. 298.4 311.75 315.96 313.7 316.26Limestone, kg. 84.0 84.0 84.0 84.0 84.0Dolomite, kg. 242.0 242.0 242.0 242.0 242.0Salt cake, kg. 35.0 17.0 11.5 14.3 11.1Coal, kg. 0.861 0 0 0 0Rouge, kg. 0 9.04 10.2 7.75 0Cullet, kg. 553.0 554.8 708.5 184.6 0Batch/cullet ratio 75/25 75/25 70/30 90/10 100/0SO.sub.3 in batch + cullet, kg./2000 kg. glass 21.78 11.3 7.9 10.87 9.05SO.sub.3 retained in glass, kg./2000 kg. glass 5.0 5.0 5.0 5.0 5.0SO.sub.3 lost, kg./2000 kg. glass 16.78 6.3 2.9 5.9 4.05SO.sub.3 added/SO.sub.3 retained ratio 4.35 2.26 1.58 1.85 2.23Glass type Clear Tinted Tinted Tinted ClearGlass thickness, mm. 10 5.5- 6.4 5.5- 6.4 4.8 19Defects:Stones, knots, bubbles & blistersper square meter 0.076 0.037 0.068 0.025 0.38Bubbles per square meter 0.051 0.027 0.009 0.002 0.19Seeds per square meter 3.65 2.63 2.40 0.60 9.1__________________________________________________________________________ *Typical prior art practice.
In Table I a number of batch formulae are shown which illustrate the present invention alongside a typical prior art formula. Example 1 is a batch formula typical of commercial flat glass practice prior to this invention, and which previously would have been considered to have a relatively low salt cake content. Example 2 shows a marginally acceptable set of operating conditions with the ratio of SO 3 added to SO 3 retained slightly higher than that found to be most advantageous. Examples 3 through 5 are illustrative embodiments of the present invention wherein the sulfur content (calculated as SO 3 ) in the raw materials is less than 2.25 times the SO 3 retained in the glass leaving the melting furnace, more specifically, the ratios in Examples 3 and 4 are in the preferred range of less than 2.0. From the data in the table, it can be seen that the operations in Examples 3 through 5 resulted in reduced sulfur-containing emissions, and that, unexpectedly, the reductions in emissions were proportionately greater than the reductions in salt cake. Additionally, the Table shows that defect densities were not detrimentally affected, but were maintained within the high standards for flat glass. But perhaps most significantly, the production runs represented by Examples 3, 4 and 5 were at advantageously high batch-to-cullet ratios of 70/30, 90/10, and 100/0 respectively, which in accordance with prior art practice would have entailed increased emissions rather than the reduction achieved by the present invention. Examples 3, 4, and 5 presented no foam problems.
A furnace employing the batch of Example 1 was found to exceed applicable state standards for particulate emissions, and the operation of Example 2 was marginally out of compliance, whereas Examples 3, 4, and 5 were well within the standards. Maximum allowable particulate emissions are calculated differently in different jurisdictions; the standard to which the examples were subjected was calculated by the following formula:
e.sub.max = 4.1p.sup.0.67
where:
e max = maximum allowable particulate emissions, kg./hour
p = process weight input (total feed to the furnace up to 27.3 metric tons per hour), 2000 kg./hour
It should be understood that the sulfur content of the batch, cullet, glass produced, and emissions in Table I have been expressed as SO 3 for the sake of convenience. The sulfur in the cullet and product glass are analyzed as SO 3 , but the SO 3 content of batch is usually provided by salt cake, but could also be supplied by other sources such as gypsum, barytes, or SO 2 gas as in U.S. Pat. No. 3,375,095. The emissions may include primarily Na 2 SO 4 particles, H 2 SO 4 mist, and small amounts of SO 2 and possibly some SO 3 . What constitutes particulate emissions under governmental air pollution standards depends upon the method of sampling the effluent gas. One type involves filtering particles from the effluent stream, dissolving the contents of the filter in water, and then analyzing the solution. When such a type of sampling is employed, it has been found that, prior to this invention, particulate emissions were usually about 75% by weight sulfur compounds; when operating in accordance with the present invention, sulfur compounds have been found to constitute only about one-third by weight of the particulate emissions. An empirically derived relationship between total particulate emissions and the calculated value for SO 3 lost, as reported in Table I, has been found to be:
x = 0.196y + 1.083
where:
x = total particulate emissions, kg./1000 kg. glass produced
y = SO 3 lost, kg./1000 kg. glass produced
The amount of SO 3 in the batch and cullet may be calculated by the following formula:
S = (0.673YB + 20ZC)/(0.825B + C)
where:
S is kilograms of SO 3 per 2000 kg. glass produced.
B is the fraction of batch in the feed.
C is the fraction of cullet in the feed.
Y is the kilograms of salt cake per 1000 kg. sand in the batch.
Z is weight percent SO 3 in the cullet.
The concentration of SO 3 in the final glass product will vary slightly in accordance with the glass composition, the furnace temperature, and the amount of salt cake used. Flat glass typically includes about 0.15 to 0.50 percent by weight SO 3 . The glasses produced in Examples 1 through 5 may have undergone maximum fluctuations in their SO 3 contents from about 0.20 to about 0.30 percent by weight, but in calculating the amount of SO 3 retained in each glass, an approximate average of 0.25 percent by weight SO 3 was assumed.
The ratio of SO 3 added to SO 3 retained must logically be no less than 1.0, but because some volatilization of SO 3 is necessary for fining of the glass, the ratio should be at least slightly greater than 1.0. It has been estimated that a minimal fining effect for flat glass entails the volatilization of about one-half part by weight SO 3 for each 1000 parts by weight of glass produced. If, for example, 0.25 percent by weight SO 3 is retained in the glass, the approximate minimum ratio of SO 3 added to SO 3 retained would be about 1.2.
The present invention permits the inclusion of coal (carbon) in the batch, but it has been found preferable to minimize or essentially exclude coal in order to attain the lowest emission levels. The essential exclusion of coal is intended to mean that the batch is free of any deliberate addition of coal, but does not exclude trace amounts which may be present as impurities. In some cases, such as with glasses colored with iron, it may be necessary to include some coal to maintain a certain oxidation state in the melt. In such cases, a minimal inclusion of coal would be an amount sufficient to maintain a maximum ferrous/total iron ratio of about 0.35 for clear glass or about 0.30 for tinted glass. The amount of coal that this represents depends upon the particular operating conditions in a specific furnace. In Table II, Examples 6 through 10 each show the operation of a different large scale, continuous, flat glass melting furnace within the scope of the invention. Examples 6 through 9 include coal in the batch while Example 10 is free of coal; all show improved emissions at high batch-to-cullet ratios.
TABLE II__________________________________________________________________________ Example 6 Example 7 Example 8 Example 9 Example 10__________________________________________________________________________Glass type Clear Clear Clear Clear ClearCoal, parts by weight 0.96 0.53 0.93 0.97 0per 1000 parts by weight sandSalt cake, parts by weight per 14 14 15 15 121000 parts by weight sandBatch/cullet weight ratio 73/27 73/27 73/27 72/28 80/20SO.sub.3 retained in glass, 0.27 0.27 0.27 0.27 0.25weight percentSO.sub.3 in batch + cullet, 9.56 9.56 10.12 10.05 8.68kg./2000 kg. glassSO.sub.3 lost, kg./2000 kg. glass 4.16 4.16 4.72 4.65 3.68SO.sub.3 added/SO.sub.3 retained ratio 1.77 1.77 1.87 1.86 1.74__________________________________________________________________________ | Conventional flat glass compositions are melted in a continuous melting process with lowered sulfur-containing emissions and with improved fining at high batch-to-cullet ratios by controlling the amount of SO 3 included in the batch materials and cullet. This is accomplished while maintaining high throughputs and without using substitute fining agents. Preferably, the amount of carbon in the batch is maintained at a minimal level or eliminated. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not applicable.
BACKGROUND OF THE INVENTION
[0003] The present invention relates to site and building selection methods and apparatus and more specifically to software that accounts for various disparate selection criteria or factors such as business drivers, intended business uses, the industry associated with a building project, construction costs, personnel costs when determining the overall costs associated with constructing and operating a facility at a particular location.
[0004] Whenever an employee of a business is charged with real estate decisions (hereinafter a “real estate decision maker”) decide to design/locate a new building, the decision maker should account for many different factors or business drivers (e.g., factors that affect new building location and design) to optimally complete the design and locating process. Exemplary business drivers that may be associated with a new building include but are not limited to drivers related to employee productivity, customer experiences, availability and cost of different types of labor, environmental impact, first time cost to build, real estate related energy costs, the affect on recruiting, training and retaining employees, etc.
[0005] Public databases have been developed that can be used by real estate decision makers to develop a general understanding of how different building locations may impact certain business drivers. To this end, public databases currently exist that store statistical information related to various labor related business drivers such as average employee salaries, skill sets of potential employees within geographic regions, employee retention rates, unemployment rates, etc. Similarly, databases exist that store statistical data regarding construction material costs and construction labor costs based on geographic regions.
[0006] While public statistical labor and construction databases exist, currently there is no known way to easily access existing data regarding building construction costs and labor related factors in a format that would be meaningful/useful to a real estate decision maker. For this reason, in many building design and locating endeavors, location related cost and rate data may be only anecdotally considered because of its format and an inability to translate the existing data into building specific information. Thus, while data may exist that indicates that a software engineer can be hired for 30% less in Detroit, Michigan than in San Diego, Calif. while widget assemblers can be hired for 10% less in San Diego than in Detroit Mich., translating that information into labor cost savings associated with a specific building in each of the two locations where it is anticipated that 20% of the employees will be software engineers and 80% will be widget assemblers it not an easy task and therefore, in many cases, is simply not done. Instead, because 80% of employees are to be widget assemblers a decision maker may simply look to San Diego as the location where widget assembler wages are low and opt for that location over Detroit.
[0007] When real estate decision makers require more geographically specific information to make building decisions, many real estate decision makers rely on design, construction and human resource consultants to provide advice. These consultants develop valuable expertise in their respective fields and can typically customize statistical information for decision makers so that decisions are made in a more informed environment.
[0008] While building design and location selection processes have been developed by consultants, unfortunately, there are several shortcomings in the current building locating and designing processes that result in less than optimal decisions.
[0009] First, while design, construction and human resource consultants each have developed various skills that are useful when selecting the location for a new building or for designing a building to meet a client's needs, typically these consultants work separately and in a vacuum (i.e., generally not knowing what other consultants are doing). For instance, human resource consultants may provide specific labor related statistical information (e.g., unemployment rate, average wages for different types of employees, turnover rates, typical educational background, etc.) for different locations to help a client select a location for a new building but typically have no special knowledge regarding building design or construction costs and do not care much about those statistics. In contrast, design consultants typically design a building that is consistent with business drivers related to building design and have no special knowledge about labor statistics or, in many cases, even costs associated with constructing the building that is being designed. In fact, in many cases design consultants are hired to design a building without even knowing where the building will ultimately be located and therefore the design consultants cannot know how much it will cost to construct the designed building as costs can vary appreciably as a function of location. Similarly, construction consultants typically bid on a building designed by a design consultant without any special labor related knowledge and with little or no input into the building design.
[0010] Moreover, even where design, construction and human resource consultants do share information or all share information with a decision maker, there is no known way to quickly and relatively inexpensively integrate data from the various consultants to help real estate decision makers make well informed decisions. Thus, decision makers typically approach the location, design and construction portions of the decision making process in stages, first selecting a small number of possible building locations, then designing a building and thereafter selecting a final location at least in part based on location related construction costs for the designed building.
[0011] While the location-design-construction cost progression may seem logical, such a sequential regimen can have unintended consequences. For instance, in some cases a decision maker may use labor related costs in an initial process to identify two possible building locations. After the two locations are identified and a building design has been selected, the decision maker may use construction costs to select one of the two locations as a final location for the building. In this case it may be that third, fourth and fifth locations have better overall mixes of construction and labor costs which could have reduced the long term costs associated with the building appreciably and therefore the sequential process results in a less than optimal decision.
[0012] Second, in many cases real estate decision makers and their consultants never clearly define which of the business drivers are driving the design and location processes and/or the relative importance of the drivers. To this end, typically different business drivers are important to each of the different consultants used by real estate decision makers. For instance, human resource consultants are primarily interested in labor related business drivers like recruiting, retention and training of employees, wage rates, skill sets within specific geographical regions, etc., and are generally not concerned with design related factors such as how a building affects customer experiences, how a building fosters employee communications, employee cooperation, employee innovation, employee productivity or flexibility of a workplace. In contrast, a design engineer typically has no interest in labor related business drivers and instead is completely focused on design related drivers like how a building affects customer experiences, how a building fosters employee communications, employee cooperation, employee innovation, employee productivity and flexibility of a workplace. Similarly, construction consultants are typically interested only in cost related business drivers and have very little interest in the labor related and design related business drivers.
[0013] Each consultant, having his or her own area of focus, naturally stresses the importance of the business drivers that are important in the consultant's field of expertise. The real estate decision maker often gets lost in the middle of the consultants and usually cannot even articulate a possible list of business drivers much less rank drivers in the order of importance for a specific building endeavor. In many cases the consultant that makes the greatest impression on the decision maker can end up driving the entire process such that drivers that are not related to the consultant's field but that should have been important to the decision maker are relegated to a secondary status at best.
[0014] Third, because some of the business drivers are relatively easy to generate metrics for while others are difficult to quantify, many decision makers and consultants are inclined to simplify the decision making process by focusing only on easily quantifiable business drivers. For instance, it is generally accepted that a well designed and aesthetically appealing building can enhance employee recruitment, training efforts, collaborative activities and productivity and can increase employee retention rates. Nevertheless, because the degree to which building design affects employee factors is not easily quantifiable, often design takes a back seat to easily quantified construction costs. For example, where construction costs can be reduced by 10% by eliminating half of the planned windows in a building and there is no hard metric indicating how such a change would affect employee related factors, it is difficult to argue against the window cost reduction. In short, while cost and employee related factors may both be important business drivers for a building, in many cases building decisions are reduced to abbreviated decision processes wherein cost is a primary consideration while employee related factors are either not considered or are only secondarily considered.
[0015] Abbreviated decision processes have short term appeal as they provide comfort to decision makers and consultants that, at least regarding the easily quantifiable metrics, the right decisions are being made. Unfortunately, in the long term, in many cases, abbreviated processes do not yield optimal results and can increase costs appreciably. For instance, it is generally known that building costs are a fraction of employee costs (e.g., wages, recruiting, training, insurance, retention, etc.). It is also generally accepted that when employees find the spaces in which they work appealing, employee costs can be reduced appreciably as the space aides recruiting and retention efforts, may increase productivity, may increase collaboration, etc. In this example it will be assumed that construction costs are only 10% of anticipated yearly employee costs. Here, if an initial construction cost increase of 10% for better furniture or building design results in a 1% employee retention rate increase, the 10% increase in construction costs can be offset in one year by the reduced employee turnover rate alone. In addition, recruiting and training costs may be reduced and collaborative activity may be enhanced by the increase in furniture costs and/or better building design so that the increase in construction costs is offset even faster. In this example, if construction costs are viewed in a vacuum without considering effects on employees, the end result is appreciably more costly in the long term.
[0016] Fourth, even when a real estate decision maker is sawy enough to clearly understand which business drivers are driving the decisions to design and locate a building, because of the nature of the decision making process, the process itself often takes on a life of its own and begins to constrain the decision maker and consultants to other than optimal designs and locations. For instance, once the location selection and design processes have progressed and the decision maker and consultants have all spent substantial time and effort in moving a building project toward an end goal, obviously the costs associated with a decision maker's time and effort in considering specific designs and locations cannot be recouped. In addition, most consulting costs cannot be recouped when a real estate decision maker decides not to pursue an initial design direction or location (i.e., when a design change or building location change is made).
[0017] For these reasons, at some point during the design and locating process, decision makers and consultants often feel compelled/constrained to continue along the path already started even after the decision maker and/or consultant suspects that the path is no longer optimal. As a simple example, consider a case where a decision maker initially contemplates constructing a building to house a customer call center in San Diego and only later, after extensive efforts related to a San Diego site, recognizes that there may be some advantages to placing the call center in Kansas City. While there may in fact be many advantages to the Kansas City location, the decision maker and/or consultant may be compelled to stick with the San Diego site in order to justify costs already incurred. Once again, here, the process leads to a less than optimal building location decision.
BRIEF SUMMARY OF THE INVENTION
[0018] It has been recognized that many different rules of thumb can be developed and stored in a database that relate default/common facility characteristics to user specifiable factors. Here, after at least a small subset of factors related to an anticipated building have been specified by a user, a processor can use the rules of thumb to generate and render accessible a subset of facility characteristics related to an anticipated facility. In at least some embodiments the default building characteristics can be altered by the user to customize the facility subset and when at least some of the default characteristics are altered, the alterations ripple through the other characteristics in the facility characteristic subset.
[0019] Exemplary factors related to an anticipated facility that may be provided by the user include but are not limited to any subset of business drivers, the number and types of employees that are expected to use the building, the location of the building, physical characteristics of the building, the industry in which the building is to be used, the location of the building and characteristics regarding labor expectations (e.g., turnover rate, wage rate, etc.). Exemplary business drivers include productivity related factors, customer/client related factors, real estate energy costs, availability and cost of labor, capital investment factors, environmental impact factors, factors related to communication with employees, factors related to customer service, factors related to construction costs, factors related to innovation fostering, factors related to recruiting, training and retention of employees, factors related to speed of construction, factors related to workplace flexibility and factors related to workplace culture. In at least some embodiments relative importance of the business drivers may be specifiable and the building characteristic subset may be selected as a function of the relative importance as specified.
[0020] In at least some embodiments, after a small number of facility characteristics have been specified and during a characteristics customization process, a user can jump to a summary page independent of how much customization has occurred to get a quick summary of estimate of facility construction and furnishing costs, estimated labor costs, location related costs and workspace characteristics.
[0021] In some embodiments it is contemplated that the system will be capable of identifying likely useful modifications to a facility specified by a system user and will render helpful suggestions to the user. For instance, where a user indicates that first time cost to build a facility is the only important factor to be considered but then specifies a relatively expensive building the system may identify a subset or all of the building characteristics that could be altered to reduce costs and may present that information in any of several different forms to the user.
[0022] In some embodiments it is contemplated that the system will be able to identify cost differences other than construction cost differences associated with different building types. For instance, where a first building will reduce energy costs by $0.50 per square foot when compared to a second building, the system may be able to estimate the $0.50 cost savings. As another instance, where a first building will reduce churn (i.e., reconfiguration costs) costs by $0.60 per square foot per year, the system may be able to estimate the $0.60 cost savings. Where other than construction costs can be determined by the system, the system may also generate and present other useful metrics including but not limited to a net effective rent (NER) value which is the triple net lease cost of a facility minus other costs (e.g., the $0.50 and $0.60 energy and churn savings above) that would be incurred if a different type of facility were constructed.
[0023] In some embodiments the system may also be able to identify estimated profit increases as a function of different building characteristics and report those increases either as raw data or reflect those increases in an NER value.
[0024] To the accomplishment of the foregoing and related ends, the invention comprises the features hereinafter described. The following description and the annexed drawings set forth in detail certain illustrative aspects of the invention. However, these aspects are indicative of but a few of the various ways in which the principles of the invention can be employed. Other aspects, advantages and novel features of the invention will become apparent from the following detailed description of the invention when considered in conjunction with the drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0025] FIG. 1 is a schematic view illustrating a computer and communication system according to at least some embodiments of the present invention;
[0026] FIG. 2 is an exemplary building type/default employee database that may be included as a portion of the proprietary database shown in FIG. 1 ;
[0027] FIG. 3 is a primary operations center database that may be included as a primary operations center database of FIG. 1 ;
[0028] FIG. 4 is a flow chart illustrating at least one method that may be performed by the server of FIG. 1 that is consistent with at least some aspects of the present invention;
[0029] FIG. 5 is a flow chart illustrating a subprocess that may be substituted for a portion of the process shown in FIG. 4 ;
[0030] FIG. 6 is a screenshot that may be provided by the server of FIG. 1 via the display shown in FIG. 1 to enable the system user to rank or bucket various business drivers as mission critical, core drivers, drivers to be considered or not important;
[0031] FIG. 7 is a similar to FIG. 6 , albeit showing a summary of how different business drivers have been bucketed or ranked by a user;
[0032] FIG. 8 is screenshot showing tools that allow a system user to select one of several different types of facilities to be constructed and to provide additional information related to the number of seats to be provided within a facility and the number of employees that it is anticipated will use a facility;
[0033] FIG. 9 is a screenshot including tools that allow a system user to input targets and assumptions for a facility to be constructed;
[0034] FIG. 10 is a screenshot including tools that allow a system user to input location related information corresponding to a facility to be constructed and also includes a subwindow that provides some summary information related to employees expected to use a facility;
[0035] FIG. 10A is an exemplary subwindow that provides summary information related to a building;
[0036] FIG. 10B is similar to FIG. 10A , albeit providing workspace related summary information;
[0037] FIG. 11 is a screenshot including tools that enable a system user to view default employee characteristics and wages and to alter those characteristics and wages;
[0038] FIG. 12 is a screenshot including tools that enable a system user to view exemplary building shapes and to select one of the building shaped for a facility to be constructed;
[0039] FIG. 13 is similar to FIG. 12 , albeit allowing a system user to view and select building entry type;
[0040] FIG. 14 is similar to FIG. 12 , albeit allowing a system user to view and select roof types for a building to be constructed;
[0041] FIG. 15 is similar to FIG. 12 , albeit allowing a system user to view arid select different mixes of exterior skins for a building to be constructed;
[0042] FIG. 16 is a screenshot allowing a system user to view and specify various characteristics related to a building and the location at which the building is to be constructed;
[0043] FIG. 17 is a screenshot including tools that allow a system user to view and edit at least a subset of core choices for a building to be constructed;
[0044] FIG. 18 is a screenshot including information related to user workspaces within a facility to be constructed;
[0045] FIG. 19 is a screenshot including tools to allow a system user to view a basic image of individual workspaces and to specify various characteristics of individual workspaces;
[0046] FIG. 20 is a summary screenshot including information related to the location at which a building is to be constructed, the employees that it is anticipated will use the building, building characteristics and characteristics of individual workspaces to be included in a building;
[0047] FIG. 21 is similar to FIG. 20 , albeit including highlighting boxes indicating building characteristics that are inconsistent with the way in which a system user has bucketed business drivers; and
[0048] FIG. 22 is a screenshot showing an NER tool.
DETAILED DESCRIPTION OF THE INVENTION
[0049] Referring now to the drawings where in similar reference numerals correspond with to similar elements throughout the several views and, more specifically, referring to FIG. 1 , the present invention will be described in the context of an exemplary computer and communication system 550 that includes, among other things, at least one server/processor 552 , one or more interface devices 554 (only one shown in FIG. 1 ) and a plurality of databases 556 , 558 and 555 . Server 552 is linked or linkable via a communication network 551 to each of the databases 556 , 558 and 555 and also to interface device 554 . At least some of the databases in some of the embodiments will be public databases while other are proprietary.
[0050] In FIG. 1 , exemplary databases 556 and 558 are public meaning that the data stored therein can be accessed either free of charge or for a small fee by members of the public. Exemplary public databases in FIG. 1 includes a cost construction database 556 and a human resource database 558 . Cost construction database 556 , as the label implies, includes various statistical information related to the cost of constructing various types of buildings. For example, database 556 may include geographically specific information related to the cost of labor to construct buildings, the cost of specific materials to construct buildings, permit and regulatory costs associated with building specific types of structures, real estate costs including the costs of buying property within geographic areas, etc. In many cases construction cost types of information are maintained by municipalities/governmental agencies which render the information accessible via the internet or the like.
[0051] Human resource database 558 , as the label implies, may include periodically collected information related to employees within specific geographic areas. For example, employee related data in database 558 may include data related to unemployment rate, educational statistics for people living within specific regions including percent that have college educations, percent that have high school educations, percent that have masters degrees, percent that have doctorates, percent that are trained as managers, percent that are trained as scientists, etc., average hourly rates for employees within particular regions, average hourly rates for employees having specific skill sets within particular regions, retention rates for employees with particular skill sets within particular regions, etc. While databases 556 and 558 are described herein as being public, in at least some embodiments it is contemplated that one or both of databases 556 and 558 may be proprietary or at least supplemented by proprietary databases. Moreover, databases 556 and 558 may comprise a single database or may each comprise two or more public databases.
[0052] Referring still to FIG. 1 , proprietary database 555 includes one or more software programs 557 and a default database 560 . Programs 557 are various programs that are run by server 552 to perform various inventive methods and processes as described below.
[0053] Default database 560 , as the label implies, includes a plurality of default settings usable by server 552 for specifying various characteristics of buildings/facilities/employees. To this end, default characteristics have been and are continuing to be generated where the characteristics include default or benchmark percentages of employees that work in different types of facilities, typical or common building and workspace features and choices given different building types, different business drivers associated with specific buildings and the number of employees that are expected use a building. The default database 560 includes two sub-databases, a building type/default employee database 562 and a facility characteristics default database 564 .
[0054] Referring still to FIG. 1 and also to FIG. 2 , building type/default employee database 562 relates bench mark employee statistics to four different facility/building types. In the illustrated example, database 562 includes a facility/building type column 565 , a staff column 569 , a support staff column 573 , a manager column 575 and a senior management column 577 . Facility/building type column 565 , as the label implies, includes a list of different facility types including a primary operation center, a regional operations center, a general office/headquarters and a regional office/headquarters. Here, it is assumed that any new building to be constructed or occupied will be used as either a primary or regional operations center or as a general or regional office/headquarter and therefore the building can be categorized as one or the other of the four types in column 565 .
[0055] For each of the facility types in column 565 , corresponding entries in columns 569 , 573 , 575 and 577 indicate the percentage of total employees at the facility type that can be categorized as staff, support staff, managers and senior management, respectively. Thus, as shown in FIG. 2 , at a primary operations center it may be that statistical information derived from prior project experience has shown that 75% (e.g., 0.75) of the total number of employees will likely be staff employees (e.g., see the entry in column 569 that corresponds to the primary operations center type in column 565 ). Similarly, at a primary operation center, 10% of the total number of employees will typically or commonly be support staff, 10% will be managers and 5% will be senior managers as indicated in column 573 , 575 and 577 , respectively, in the row associated with the primary operations center type in column 565 . Thus, for example, if a primary operations center is to have 500 employees, given the bench mark defaults in database 562 , 375 of the employees will be staff (i.e., 0.75×500=375), 50 of the employees will be support staff, 50 of the employees will be managers and 25 of the employees will be senior managers. In contrast, given the employee breakdown bench mark data in database 562 , if 500 employees were to work at a general office headquarters, 225 of the employees would be staff, 100 of the employees would be support staff, 75 of the employees would be managers and 100 of the employees would be senior managers.
[0056] Here, it should be appreciated that, while four different facility types are listed in FIG. 2 , in other embodiments, more or less facility types may be listed, depending upon what is reasonable given how buildings are used in an industry. In addition, facility types and benchmark employee breakdowns may be different for different industries. For example, while the statistics and facility types in FIG. 2 may be appropriate in the case of a manufacturing industry, entirely different facility types and benchmark employee breakdowns may be more appropriate in the health care industry, education industry, etc.
[0057] Referring still to FIG. 2 , in addition to the bench mark employee breakdown data provided in columns 569 , 573 , 575 , and 577 , bench mark turnover rates are provided for each of the facility/building types in column 565 which can be used to develop relatively sophisticated statistics related to employee or labor costs. In this regard, column 567 includes a separate entry for each one of the facility/building types in column 565 . For instance, for a primary operations center, the bench mark annual turnover rate in column 567 is 10% meaning that, where 500 employees work at a primary operations center, 50 of the those employees will turnover on an annual basis. Similarly, for a regional operations center the data in column 567 indicates that 15% annual turnover should be expected while only 5% annual turnover should be expected for an general or regional office/headquarters.
[0058] Referring once again to FIGS. 1 and 2 , building characteristics default database 564 includes a separate default database for each one of the facility/building types listed in column 565 of database 562 . Thus, database 564 includes a primary operations center database 566 , a regional operations center database 568 , a general office/headquarters database 570 and a regional office headquarters database 572 . Each of the databases 566 , 568 , 570 and 572 is similar in construction and is used or operates in a similar fashion and therefore, in the interest of simplifying this explanation, only primary operations center database 566 will be described here in any detail. The main differences between the databases 566 , 568 , 570 and 572 are the characteristics specified by the different databases. For example, comparing a regional operations center database to a general office/headquarters database, because headquarters buildings are often designed to be relatively more aesthetically impressive for recruiting and for customer relations purposes, the headquarters database may include defaults that require the best possible signage, wall coverings, furniture, relatively large executive management offices, etc., whereas the regional operations center database 568 may specify lower quality materials, design, relatively smaller executive management offices, etc.
[0059] Referring still to FIG. 1 and now to FIG. 3 , an exemplary and simplified primary operations center database 566 is shown in FIG. 3 . Database 566 includes a facility characteristics column 602 and a plurality of additional column 604 , 606 , 608 , etc., that specify default facility characteristics. As the label implies, column 602 includes a list of facility characteristics which, as shown, are broken down into sub-groups of characteristics including a building sub-group 609 , an individual space sub-group 614 , a team space sub-group 611 , a technology sub-group 613 , a communications/branding sub-group 616 , an amenities sub-group 615 and an “other” sub-group 617 . Under the building sub-group, labels beginning with the first label 610 include shape, level, entry, roof type, exterior skin, parking ratio, parking level, stairs-communicating, etc.
[0060] The “shape” label in column 602 corresponds to the general shape of a building to be constructed or occupied. To this end see FIG. 12 where a screen shot 218 shows various general building shapes including a rectangular shape 222 , a gull-wing type shape 226 and various other shapes. The “levels” label corresponds to the number of levels (e.g., 1 , 2 , etc.) of a building to be constructed or occupied. The “entry” label corresponds to the type of entryway into a building to be constructed or occupied. To this end, see FIG. 13 where a screenshot 250 shows various building entry types including, among others, a simple entry 254 , an integrated porch entry 258 , an extended canopy entry, etc. The “roof type” label corresponds to the type of roof to be included on a building to be constructed or occupied. To this end, see FIG. 14 that shows a screenshot 270 illustrating exemplary roof types including, among others, a flat roof type 274 , a barrel vault roof type 278 , etc.
[0061] Referring still to FIG. 3 , the “exterior skin” label in column 602 corresponds to the material used on the exterior of a building to be constructed or occupied. In this regard, see FIG. 15 where a screenshot 290 shows images of different types of materials to be used on the exterior surface of a building including concrete, masonry, panelized metal, windows and curtain wall. Under the exterior skin label in column 602 a separate label for each of the types of exterior skin is provided, the separate labels collectively identified by numeral 612 in FIG. 3 . The “parking lot ratio” label indicates a parking space ratio to be used to determine the number of parking spaces to be included around a building to be constructed. The “parking level” label indicates the number of parking levels to be included if a parking structure is to be constructed. For example, where a parking structure is to have three levels, a parking levels value would be 3. The “stairs/communicating” label indicates the number of stairwells to be included in common or customer related areas to be constructed.
[0062] Referring yet again to FIG. 3 , under the individual space portion 614 of column 602 , different labels are provided for different types of offices including senior manager, manager, support staff and staff. Although not illustrated, the individual space portion of column 602 may also include labels related to individual space or office amenities such as desk, a chair, side chairs, lighting, wall coverings, computer type, monitor type, file cabinets, bins, shelving, side tables, a credenza, etc.
[0063] Under the communications/branding portion 616 of column 602 , labels are included that are related to “applied digital imagery wall covering”, “entry signage”, “individual name plaques”, and “information flat screens”. While no labels are shown under the team space, technology, amenities, and “other” portions of column 602 , it should be appreciated that various labels corresponding to various features will be provided under each one of those portions. Moreover, many other labels are contemplated that will be provided under the facility characteristics, the individual space and the communications/branding portions of column 602 .
[0064] In at least some embodiments, it is contemplated that a list of business drivers may be provided for a system user that can be ranked in terms of their importance in relation to a facility to be constructed and furnished or fitted out for use. Here, the term “business driver” is used to refer to things that may be considered important to a real estate decision maker when going through the process of searching for a location for a building, designing the building and furnishing different parts of the building. To this end, referring now to FIG. 7 , sixteen exemplary business drivers that may be provided for ranking by a system user are shown including “productivity effectiveness workflow”, “compelling customer experience”, “energy costs of real estate”, “changes in organization”, “availability and cost of labor”, “new service, new product”, capital investment”, “impact on the environment”, “communication with employees”, “customer service”, “first time cost to build”, “foster innovation”, “recruit, train, retain”, “zero down time”, “flexibility of work space” and “cultural change”.
[0065] As shown in FIG. 7 , in the illustrated example, a system user can bucket the business drivers into any of four different buckets to rank the importance thereof. In this regard, the four buckets of importance in the present example include a “mission critical” bucket 102 , a “core driver” bucket 104 , a “consider” bucket 106 (also referred to hereinafter as a “to be considered” bucket), and a “not important” bucket 108 .
[0066] In at least some embodiments it is contemplated that the default facility characteristics that may be provided in the facility characteristics default database 564 (see again FIG. 1 ) may depend upon the importance of the different business drivers to a system user. For example, where a compelling customer experience is the most important or most mission critical business driver, facility characteristics may be very different than in a case where the first time cost to build a building is the most important or mission critical of the business drivers. For instance, where a compelling customer experience is the only mission critical business driver for a particular building and where first time cost to build is not important, the facility defaults in database 564 may be consistent with a far more expensive building than in a case where the first time cost to build is mission critical and a compelling customer experience is not important.
[0067] Referring once again to FIG. 3 , each of the columns 604 , 606 , 608 , etc., in the primary operation center database corresponds to a unique group bucketing of the business drivers shown in FIG. 7 . In FIG. 3 , the abbreviated labels “MC”, “CD”, “C” and “NI” correspond to the mission critical, core driver, consider and not important buckets shown in FIG. 7 , respectively. Thus, the information in column 604 corresponding to the labels 600 indicates that the characteristic values in column 604 correspond to the case where business drivers have been bucketed such that the first time cost to build is the only mission critical driver and all of the other business drivers (BDs) are not important (i.e., are in the NI row). Similarly, the information in column 606 corresponding to labels 600 indicates that the only mission critical business driver is a compelling customer experience and that all of the other business drivers are not important. In column 608 , the information related to the labels 600 indicates that a compelling customer experience is mission critical, the first time cost to build is a core driver (i.e., is in the CD row) and that all other business drivers are not important.
[0068] Referring yet again to FIG. 3 and specifically to column 604 , where the first time cost to build is the only mission critical business driver and all other business drivers are not important, it can be seen that, in general, a relatively inexpensive facility is specified by the facility characteristics values. To this end, the shape of the default building in column 604 is a rectangle which is generally the least expensive shape in which to construct a building. Only a single facility level is indicated in column 604 . The default entry in column 604 is a simple entry and the roof type is flat, both inexpensive options. Consistent with a relatively inexpensive building, the exterior skin is 90% panelized metal and only 10% windows in column 604 . Similarly, consistent with a relatively inexpensive building, the offices specified are relatively small and the communications/branding components and materials are indicated as good which is, in the present example, a relatively low cost indicator (e.g., better and best indicators correspond to relatively more expensive materials and building techniques than the good indicator throughout this description).
[0069] Referring yet again to FIG. 3 , in contrast to the low cost building defaults in column 604 , in column 606 where customer experience is the only mission critical business driver and all other business drivers are not important, a more expensive building is specified by the default values. In this regard, in column 606 , the shape of the building is a gull wing type shape as opposed to the simpler rectangular shape in column 604 , the building has two levels, the entry of the building includes a relatively expensive integrated canopy, the roof type is a barrel vault, the exterior skin of the building includes much more concrete and many more windows as well as a curtain wall, the offices specified under the individual space portion in column 606 are larger than the offices specified in column 604 and the communication/branding features and materials are indicated as being the best so that a compelling customer experience is more likely.
[0070] Referring still to FIG. 3 , in column 608 where a compelling customer experience is mission critical, first time cost to build is a core driver and all other business drivers are not important, the default values specify a building that is relatively high quality and is aesthetically pleasing in all areas where customers are expected to function and that is relatively inexpensive in other spaces where customers are not expected to function (e.g., any individual spaces, amenities, etc.).
[0071] Referring once more to FIG. 3 , it should be appreciated that the database 566 illustrated is extremely simplified and that, in most cases, a much more complex database is anticipated. In this regard, as shown, database 566 includes only three columns 604 , 606 and 608 that correspond to three different ways of bucketing or ranking the business drivers. It should be appreciated that there are several thousand different combinations of the 16 business drivers shown in FIG. 7 and that, in at least some embodiments, a database 566 would include a separate column for each one of the different possible ways of bucketing the business drivers. It should also be appreciated that while 16 business drivers are shown in FIG. 7 , embodiments with fewer business drivers or a larger number of business drivers or indeed with completely different sets of business drivers are contemplated. Moreover, while four buckets are provided in FIG. 7 , and in the example here, in other embodiments, fewer buckets or a larger number of buckets may be used for ranking business driver importance.
[0072] In at least some embodiments, instead of providing a separate column in the primary operations center database 566 for each one of the different possible ways of bucketing the business drivers, it is contemplated that one or a subset of the business drivers may be associated with a specific set of facility characteristics such that only the subset of business drivers and how those business drivers are bucketed affect those facility characteristics. For example, in at least some embodiments the compelling customer experience business driver may be the only driver that affects the communications/branding portion of the default facility characteristics. Thus, for instance, regardless of how other business drivers are bucketed, a “best” value may be provided for each of the communications/branding labels in column 602 whenever a compelling customer experience is mission critical, a “better” value may be provided for each of the communications/brandings labels whenever a compelling customer experience is a core driver and a “good” value may be provided for each of the communications/branding labels when a compelling customer experience is either not important or only a consideration. Similarly, other single business drivers or subsets (e.g., two or three, etc.) of business drivers may drive subsets of the facility characteristics independent of how the other business drivers are bucketed so that a simplified primary operations center database can be constructed.
[0073] Moreover, in at least some embodiments, some type of equation may be formulated that combines different business driver rankings to generate a single business driver value where the value then dictates which of several sets of facility characteristics to select as default. For instance, in some embodiments there may be one hundred different sets of facility characteristics where the 1 st set corresponds to an inexpensive building, the 100 th set corresponds to an expensive building and the sets between the 1 st and 100 th set increase in cost progressively. Despite there being thousands of ways to bucket the sixteen business drivers into the four buckets in FIG. 7 , the equation may result in a second level of bucketing where each of the different ways of ranking the drivers corresponds to one of the 100 sets of facility characteristics and therefore corresponds to one of 100 different sets of facility benchmarks.
[0074] Referring once again to FIG. 1 , interface device 554 may take any of several different forms including a personal computer, a laptop computer, a palm-type computing device, a server, a workstation, a thin client type computing device, etc. In the illustrated embodiment, device 554 includes a keyboard or other input type device 549 such as a mouse and a display screen 557 for receiving output from server 552 and for providing input to server 552 .
[0075] Referring now to FIG. 4 , an exemplary method 640 that is consistent with at least some embodiments of the present invention is illustrated. Referring also to FIGS. 1 through 3 , at process block 642 , default databases 560 are provided which are accessible by server 552 . At block 644 , a system user provides input regarding business drivers, anticipated facility type and anticipated number of employees to occupy a building to be constructed using interface device 554 . To this end, referring also to FIG. 6 , a screen shot 50 that may be provided by server 552 via display screen 547 is shown. Screen shot 50 includes a graphical interface display having a primary navigation tool bar 54 along the lower edge thereof and a secondary navigation toolbar 52 along the top edge thereof. Between the primary and secondary tool bars, a data entry space 98 is provided. The exemplary primary navigation tool bar 54 includes a utilities icon 51 , a notepad icon 53 and a forward arrow icon 69 . Each of icons 51 , 53 and 69 is selectable by moving a mouse controlled cursor there over and clicking one of the mouse buttons in a conventional manner. When utilities icon 51 is selected, a pop-up menu (not shown) including mouse selectable labels for various software features appears. When notepad icon 53 is selected, a window opens up in which a user can take notes by typing with keyboard 549 or the like to memorialize thinking during use of the inventive system. Forward arrow icon 69 is selectable to move to a next screen shot shown in FIG. 7 after a user is done using the input tools in space 98 of screen shot 50 .
[0076] Referring still to FIG. 6 , secondary navigation tool bar 52 includes five separate mouse selectable icons including a “drivers” icon 58 a “location” icon 60 , a “people” icon 62 , a “building” icon 64 and a “workspace” icon 66 . Each of the icons 58 , 60 , 62 , 64 and 66 is usable to enter different types of information to be associated with a building to be constructed and/or to navigate back and forth among different screen shots supported by the system. In this regard, it has been recognized that an optimal set of information needed when making a real estate decision can be broken down into several different categories and that the information entry tool can be arranged so that data entry progresses along a logical flow based on those categories. In the illustrated example, the information categories include the categories corresponding to the secondary tool bar 54 icons.
[0077] As the label implies, “drivers” icon 58 is selectable to allow a user to enter information related to business drivers associated with a building to be constructed. “Location” icon 60 is selectable to allow a user to access various location related construction and labor statistics and to specify an anticipated location for a new facility. “People” icon 62 is selectable to allow a user to access and alter employee breakdowns for a facility. “Building” icon 64 is selectable to allow a user to examine and specify building characteristics and “workspace” icon 66 is selectable to allow a user to examine and specify characteristics of individual workspaces for a facility.
[0078] Referring still to FIG. 6 , when “drivers” icon 58 is initially selected, the information shown in space 98 of screen shot 50 is initially provided. Tools are provided in space 98 for considering different business drivers and bucketing those drivers as mission critical, core, to be considered or not important. To this end, a business drivers wheel 56 is provided along with a mission critical bucket 68 , a core driver bucket 70 , a to be considered bucket 72 and a not important bucket 76 .
[0079] Referring to FIGS. 6 and 7 , while there are 16 different business drivers in the illustrated example, the business drivers in this example have been subdivided into four separate business driver sets labels a “people in process” set, a “service the customer” set, a “reduce expenses” set and a “business dynamics” set, each of the separate sets provided with a mouse selectable arrow icon 78 , 80 , 82 and 84 , respectively, in space 98 . In the present example, each of the separate business driver sets includes four of the business drivers shown in FIG. 7 . For example, the “people in process” set includes the “productivity effectiveness work flow” driver, the “communication with employees” driver, the “availability and cost of labor” driver and the “recruit, train, retain” driver. As shown in FIG. 6 , when the people in process icon 78 is selected, the four drivers associated therewith are provided within a circular space defined by arrow icons 78 , 80 , 82 and 84 . Similarly, although not separately illustrated, the “compelling customer experience” driver, the “customer service” driver, the “new service, new product” driver and a “zero down time” driver in FIG. 7 are all included in the “serve the customer” set associated with icon 80 so that when icon 80 in FIG. 6 is selected, the four related drivers appear within the circle formed by icons 78 , 80 , 82 and 84 . In a similar fashion, when the “reduced expenses” icon 82 or the “business dynamics” icon 84 are selected, the four business drivers related to each of those icons would appear within the circle defined by icons 78 , 80 , 82 and 84 .
[0080] Referring still to FIG. 6 , after the people in process icon 78 is selected, the four drivers related thereto are provided as mouse selectable icons within the circular space defined by icons 78 , 80 , 82 and 84 . The icons in FIG. 6 include the “productivity effectiveness work flow” icon 86 , the “recruit, train, retain” icon 88 , and “availability and cost of labor” icon 90 and the “communication with employees” icon 92 . When one of icons 86 , 88 , 90 or 92 is selected, additional information explaining the nature of that icon and that business driver is provided in space 59 to the left of tool 56 and the selected icon is highlighted. Thus, when icon 86 is selected, icon 86 is highlighted and information related thereto is provided in space 59 .
[0081] To rank or bucket the business drivers corresponding to icons 86 , 88 , 90 and 92 , a user can select the icon associated therewith via a mouse controlled cursor and drag the icon to one of the mission critical, core driver, to be considered or not important buckets 68 , 70 , 72 or 76 , respectively. After all four drivers associated with the people in process icon 78 have been bucketed, the user can select one of the other arrow icons 80 , 82 or 84 to access other business drivers and to bucket those drivers in a similar fashion.
[0082] After at least one of the business drivers has been bucketed, a user can select forward arrow icon 69 to move to the next screen shot shown in FIG. 7 . Referring now to FIG. 7 , a next screen shot 100 provides a summary page indicating how business drivers have been bucketed. To this end, separate mission critical, core driver, to be considered and not important icons 102 , 104 , 106 and 108 are provided in space 98 along with lists of the business drivers that have been bucketed and associated therewith. In the illustrated example, a list 110 of four drivers have been bucketed as mission critical, a list 112 of four drivers have been bucketed as core drivers, a list 114 of four drivers have been bucketed as to be considered and a list 116 of four drivers have been bucketed as not important. At this point, it should be noted that, while four separate drivers have been bucketed in each one of the different buckets, fewer or greater numbers of drivers could have been put in any one of the buckets. In addition, it should be noted that while there are 16 drivers and while all of those drivers have been bucketed in the present example, a user may choose to only bucket a subset of the total number of drivers in which case drivers that are not bucketed are considered to be not important in at least embodiments. At this point, primary navigation tool bar 54 includes both forward and backward arrow icons 120 and 118 , respectively, so that a user can, if necessary, back up to screen shot 50 shown in FIG. 6 to modify the way in which business drivers have been bucketed or can move forward to a next screen shot.
[0083] Referring once again to FIG. 1 and now also to FIG. 8 , after business drivers have been bucketed and forward icon 120 (see again FIG. 7 ) has been selected, server 552 in the present example provides a screen shot 130 which allows the system user to indicate a type of building to be constructed and to indicate the total number of employees to use the building and the number of seats or independent work spaces to be included in the building. To this end, screen shot 130 provides four facility or building type options in space 98 including a primary operations center, a regional operations center, a general office/headquarters and a regional office/headquarters. Binary mouse selectable buttons are provided next to each one of the building types including buttons 132 , 134 , 136 and 138 . A system user can select one of the binary buttons to place a dot (see button 132 ) therein to indicate selection of one of the building types for the building to be constructed. Note that the building type options in space 98 correspond to the default databases 566 , 568 , 570 and 572 in FIG. 1 . Seat and employee number fields 140 and 142 are also provided in space 98 where a user can input the number of work spaces that should be included in the new building and the anticipated number of employees to work in the new building, respectively. After the information required in space 98 has been provided, a user can select forward arrow icon 120 to go to the next screen shot.
[0084] Referring to FIG. 1 and now also to FIG. 9 , a next screen shot 150 allows the user to provide target and assumption information regarding project cost, anticipated or desired total square footage and an expected move in date. In this regard, cost, square footage and move in date fields 152 , 154 and 156 are provided. Pull down menus like menu 158 may be provided to allow a user to qualify information in any one of the fields 152 , 154 and 156 . Here, inputting information into fields 152 , 154 and 156 is optional. To move to the next screen shot, a user selects forward arrow 120 or may select the “Location” icon 60 from bar 54 .
[0085] Referring once again to FIG. 4 , after block 644 , control passes to block 646 where a user uses device 554 to input location selection information indicating the location at which the user would like to construct a facility. Referring also to FIG. 10 , a screen shot 170 to help a user select a location for a building is shown. Here, location specifying tools include a state/province field 172 and a city field 174 in which, as the labels imply, state/province and city names can be entered or selected from pull down menus (not illustrated) to specify a specific location for a building. In the illustrated example, the state/province and city selected are California and Fresno, respectively. When a state/province and city are selected, referring also to FIG. 1 , server 552 accesses the public cost of construction and human resource databases 556 and 558 to obtain information therefrom related to cost of construction, unemployment, wage rates, energy costs, etc. General or basic cost and related types of information is immediately provided within space 98 as shown collectively by numeral 176 in FIG. 10 .
[0086] Referring still to FIG. 10 , once a location has been specified via fields 172 and 174 , a summary icon 175 , a drivers icon 177 , a dashboard icon 179 and a scenarios icon 178 are provided along with other icons in primary tool bar 54 . Summary icon 175 , as can be selected at any point after which a location has been selected for a building in order to jump to a summary page (see FIG. 20 ) for a building project. Here, in general, it has been recognized that, after the limited amount of information described above with respect to FIGS. 6 through 10 has been specified by a system user, facility default characteristics and default employee mixes for specific building types can be used to generate a complete set of building summary information. In fact, in at least some embodiments, after location has been selected at block 646 in FIG. 4 , control passes to block 648 where server 552 accesses the building type/default employee database 562 in FIG. 2 and determines default quantifies of different employee types as a function of building type and anticipated number of employees. To this end, in the present example where 500 employees were specified in field 142 in FIG. 8 and the building type is a primary operation center, referring to FIG. 2 , the default employee mix would include 375 staff, 50 support staff, 50 managers and 25 senior managers.
[0087] 1 After block 648 , control passes to block 650 where server 552 accesses the building facility default characteristic database 564 and identifies default building characteristics based on business drivers, building type and default quantities of different employee types. Thus, for instance, referring once again to FIG. 3 , where a compelling customer experience is the only mission critical business driver as shown in column 606 , all of the building characteristics in column 606 would be specified. Here, consistent with the above example, where there are 25 senior managers, as shown in column 606 , 25 private medium-sized senior manager offices would be specified as defaults for the building. Similarly, where the building is to house 50 managers, 50 private small offices would be specified as defaults for the new building as indicated in column 606 , and so on. At block 652 , location related labor and construction costs are accessed, and at block 654 , the default quantities of employee types and location related labor data are used to generate labor estimates that may include estimated wages, turnover rates, turn over costs, etc. At block 656 , default building characteristics and location related construction data are used to generate default construction cost estimates. After block 656 , all information needed to provide a summary as shown in FIG. 20 has been generated. At block 658 , the default building and labor characteristics are presented to the system user. In the illustrated example, default characteristics are provided in the summary form when icon 175 is selected and, if not selected, are provided in a tabular fashion that allows a user to edit the default characteristics as shown in exemplary FIGS. 11 through 19 . Here, a first screen shot 190 showing a portion of the default characteristics as in FIG. 11 can be accessed by selecting forward arrow icon 120 or the “People” icon 62 in FIG. 10. 100881 Referring still to FIG. 10 , driver icon 177 can be selected to access information in a pop-up window (not illustrated) similar to the information shown in FIG. 7 so that a user can refresh memory regarding how business drivers were bucketed. After refreshing memory, the drivers window can be closed. To edit how business drivers were bucketed, a user can reselect “drivers” icon 58 to go back to screen shot 100 shown in FIG. 7 .
[0088] Referring yet again to FIG. 10 , dashboard icon 179 can be selected at any time after a building location has been specified in fields 172 and 174 to cause a dashboard window like window 482 shown in FIG. 10 to pop up which provides summary information similar to the information in the executive summary shown in FIG. 20 ., albeit in an abbreviated form. To this end, dashboard window 482 includes a mouse selectable people icon 484 , a building icon 486 and a workspace icon 488 , along with an abbreviated summary space 490 . When the people icon 484 is selected, information related to labor or employees to be associated with the building is provided in space 490 including information corresponding to an annual estimated salary 473 , turnover 475 and building costs 477 as shown in FIG. 10 . Here, the annual estimated salary is determined by using public wage information for different types of employees and the number of staff, support staff, managers and senior management that it is anticipated will work in a building based on default employee numbers or user specified numbers.
[0089] Referring to FIG. 10A , the dashboard window 482 is shown after the building icon 486 has been selected and building related information is provided in space 490 . The building related information includes general building specifying information 481 and a speedometer icon 483 that indicates the relationship between a target cost and a cost estimate. Similarly, in FIG. 10B , dashboard window 482 is shown after workspace icon 488 has been selected and workspace related information is provided in area 490 . The information subsets in area 490 are only exemplary and other information subsets may be provided in other embodiments.
[0090] Referring yet again to FIG. 10 , scenario icon 178 is selectable to allow a user to move between any of three different building and location scenarios so that different building and location scenarios can easily be compared to each other. To this end, it has been recognized that system users like to be able to “game” the building and location selection process changing different business driver rankings, facility location and various facility and employee characteristics and to see how those changes effect the ultimate construction, furnishing and labor costs.
[0091] In the present embodiment, when a first building and location scenario is specified, second and third scenarios that are identical to the first scenario are automatically specified and can be selected by selection icon 178 . Here, as shown in FIG. 10 , initially a label “1” is provided in icon 178 indicating a first scenario. To flip to a second scenario, a user clicks on icon 178 once which changes the “1” label to a “2” label. Similarly, to change to the third scenario, the user clicks on icon 178 until a “3” label appears therein. When the user changes from one scenario to another, the user can change the location of a building via fields 172 and 174 , can go back to the driver's information by selecting icon 58 and change the bucketing of the business drivers, can change building or facility type by going to the screen shot corresponding to the other scenario as shown in FIG. 8 and so on. In addition, in any of the scenarios, the user can customize the default facility characteristics in a fashion similar to that shown in FIGS. 11 through 19 .
[0092] This process of automatically creating multiple identical scenarios simultaneously where each scenario can then be customized is particularly advantageous as in most cases, where a real estate maker may want to compare very similar scenarios where only one or a small number of factors are different among the scenarios. For instance, in many cases anticipated number of employees and facility characteristics between two scenarios may be identical, the only difference between the two scenarios being location. Here, instead of requiring a user to specify all scenario characteristics two or three times, a single specification process is required where customization only requires selection of a second location for the second scenario.
[0093] Referring still to FIG. 10 and also FIG. 11 , once forward arrow icon 120 or “People” 62 is selected, screen shot 190 is provided in the illustrated embodiment. As shown and consistent with the example above, where 500 employees are to use a building and where 75% of the employees will be staffed, 10% of the employees will be support staff, 10% will be managers and 5% will be senior managers, the information provided in space 98 includes an employee type column 192 , a percent of staff column 194 and a number of staff column 196 that indicates the percentages and numbers of each of the different types of employees. Thus, for the staff label in column 192 , column 194 indicates that 75% of the employees are staff. Column 196 indicates that the number of staff is 375 . Similarly, column 194 indicates that 10% of the employees are support staff and column 196 indicates that the number of support staff is 50 . Column 198 is an average hourly wage column and includes information obtained via the public human resource database 558 as shown in FIG. 1 . Here, the average hourly wages for Fresno, Calif. (see again FIG. 10 ) are shown for each of a staff employee, a support staff employee, a manager and senior management. Serve 552 automatically determines the total annual wage cost given the number of employees, types of employees and the average hourly wages for the location of the facility selected and provides the total cost at 206 . The default turnover rate from database 562 in FIG. 2 is provided at 204 and a turnover cost estimate is provided at 210 . An annual base of employee cost including the wage cost and the turnover cost is provided at 208 . Here, a user can change the percentages in column 194 or the average hourly wage rates in column 198 and/or the turnover rate at 204 to customize the estimates.
[0094] When default values are altered, the changes to the default values can have a rippling affect throughout other defaults and in general can affect the building and labor summary results. To this end, referring again to FIGS. 3 and 11 , where the percentage of staff in field 201 corresponding to senior management is changed from 5% to 25% so that there are 125 senior managers instead of 25, an additional 100 senior manager offices have to be constructed which totally affects other building characteristics and the ripple affect occurs.
[0095] Referring again to FIG. 11 , after forward arrow icon 120 or “Building” icon 64 is selected, screen shot 218 in FIG. 12 is provided. In FIG. 12 , the default building is indicated by a dot provided in a binary button spatially associated with an image of the default building shape. In FIG. 12 , the dot appears in button 220 associated with the default rectangular shape 222 . To change the default shape, a user simply clicks on one of the binary buttons corresponding to one of the other building shapes such as button 224 to select a gull wing building shape as illustrated at 226 . After building shape has been selected or accepted, a user selects forward arrow icon 120 and screen shot 250 in FIG. 13 is provided.
[0096] As in FIG. 12 , images showing building entries are provided along with binary mouse selectable buttons where a default button initially includes a dot as shown at 252 . Other entries such as the integrated porch entry shown at 258 can be selected by clicking on the associated buttons (e.g., 256 ). After an entry has been selected or accepted, a user selects forward arrow icon 120 which causes screen shot 270 in FIG. 14 to be shown.
[0097] In FIG. 14 , roof types are selectable by selecting binary buttons. Exemplary buttons 272 and 276 correspond to images of buildings having different types of roofs 274 and 278 , respectively. After a roof type has been selected or accepted, a user selects forward arrow icon 120 and the system provides screen shot 290 as shown in FIG. 15 .
[0098] Screen shot 290 allows a user to either view default exterior building skins or to view and edit those default values by changing default percentages. To this end, default exterior skin percentages shown include 45%, 15%, 25% and 15% of concrete, panelized metal, windows and curtain wall, respectively. In addition to the percentages, images showing the different types of skins are provided including a concrete image 294 and a windows image 298 . To change the default exterior skin percentages, the user changes the value in a field corresponding to the specific skin type. Exemplary fields include a concrete percentage field 292 and a windows percentage field 236 . After skin selections have been made or accepted, a user selects forward arrow icon 120 and screen shot 310 shown in FIG. 16 is provided where additional building default characteristics and some calculated values are shown.
[0099] In FIG. 16 , one calculated value includes the square feet of an anticipated facility given the previously specified information which is shown at 312 . Here, the square feet of the building is determined by adding the square feet of workspaces, conference spaces, circulating spaces, stairwells, restrooms and other spaces required in specific building types. A sliding button 316 is provided for changing the number of levels in the building at 314 . A sliding button is provided to adjust the parking ratio at 318 . Parking levels can be changed at 320 . At 322 , a balance for setbacks in green area square feet 330 is provided which, in the present example, cannot be changed because it is typically mandated by local municipalities. An average cost per acre 324 is provided in field 326 which is based on public information. The cost per acre in field 326 can be altered by a user to accommodate special circumstances. Calculated required acreage is provided at 328 and a total cost of land is provided at 332 . After a user is done using the tools associated with screen shot 310 , forward arrow icon 120 can be selected after which screen shot 350 in FIG. 17 is provided.
[0100] In FIG. 17 , screen shot 350 includes core building choices in column 352 , quality columns including a good column 354 , a better column 356 , and a best column 358 , a quantity column 360 , a square foot column 362 and a total square foot column 364 . In column 352 , core choices for a building include restrooms, stairs, elevators, HVAC equipment, etc. Each of the good, better and best columns 354 , 356 and 358 includes a column of binary mouse selectable buttons that can be selected to indicate whether or not one of the choices in column 352 associated therewith should be good, better or best quality. The quantity column 360 includes a number that indicates the quantity of each choice in column 352 . For example, column 360 indicates that five restrooms are required (see 366 ) and that six HVAC system or units are required (see 370 ). The square foot column specifies square feet for each one of the choices in column 352 . The total square foot column 364 includes an entry indicating the total square feet required for the quantity of specific choices specified in columns 360 and 352 .
[0101] Referring still to FIG. 17 , here, it should be appreciated that some of the quantities in column 360 may be altered while others cannot be changed. This is because municipalities routinely require specific numbers of the choices in column 352 and those numbers typically represent more than required resources so that it would be a very rare circumstance where a system user would want to increase the number of specific choices. For instance, five restrooms as indicated at 366 is generally a large number of restrooms given other default building characteristics and, to minimize costs of the building, most users would not opt to increase the number of restrooms. While some quantities in column 360 cannot be changed, other quantities can such as, for instance, the number of communicating stairs in field 368 , can be altered. Many other building related screen shots may be provided for examining default building characteristics and customizing those characteristics. After a user is satisfied with the information provided by screen shot 350 and other building characteristic screen shots, the user can select forward icon 120 or “workspace” icon 66 to access screen shot 380 shown in FIG. 18 .
[0102] In FIG. 18 , screen shot 380 provides default information related to workspaces. Here, an additional toolbar 369 is provided that includes mouse selectable icons labeled “individual space” 382 , “team space” 384 , “technology” 386 , “communication/branding” 388 , “amenities” 390 and “other” 394 . A user can select any one of icons 382 , 384 , 386 , 388 , 390 or 394 to jump to either default or currently specified workspace characteristics and features related to the selected icons. Thus, for instance, individual space icon 382 can be selected to examine current characteristic settings for workspaces as shown in screen shot 380 . Screen shot 380 includes a workspace column 381 , a level of quality column 396 , a quantity column 398 , a square foot column 400 and a total square foot column 402 . In the illustrated example, it is assumed that a user has already modified the quantities in column 398 so that default values no longer apply. Thus, while the example above associated with FIGS. 2 and 3 requires 25 private small offices, column 398 in FIG. 18 indicates that only four private small offices are required. Other user specified customizations are reflected in screen shot 380 . Although not shown, various tools like those described with respect to FIG. 17 will be provided to allow a user to alter default or current individual space settings. In at least some embodiments, information related to any one of the work place types such as the six by seven space at 410 in FIG. 18 may be accessed by simply clicking on the workspace label 410 . To this end, referring to FIG. 19 , when the label 410 in FIG. 18 is selected, screen shot 420 may be provided to allow a user to see an image 422 of an exemplary default workspace type, to change quantity via a field box 424 , to select workspace quality via binary mouse selectable buttons 426 , 428 and 430 and to save 432 or cancel 434 modifications.
[0103] Although only a few screen shots are shown for viewing and altering default values, it should be appreciated that in complex systems several hundred different screens may be provided for altering and viewing default values.
[0104] Referring now to FIG. 20 , as indicated above, at any point during the process of examining default or currently set building characteristics or altering default or currently set characteristics, a user can select summary icon 175 causing server 552 to generate a summary page as shown in screen shot 450 . The summary page 450 includes five different sections including a short executive summary at 452 , location based information at 454 , employee information at 456 , building information at 458 and workspace information at 460 .
[0105] After viewing a summary page, a user can select backward arrow icon 119 to move back through the default and customized data. In addition, once a user moves back to a screenshot that includes secondary tool bar 54 (see again FIG. 19 ), the user can select any one of the bar 54 icons 58 , 60 , 62 , 64 , or 66 to access specified information related thereto and to alter that information when necessary. Different summaries 450 can be printed out or saved in a database by selecting print and save icons 461 and 463 , respectively (see again FIG. 20 ).
[0106] In at least some embodiments, it is contemplated that programs 557 would allow a user to specify business driver ranking and building/facility characteristics and, as part of the summary screenshot, may provide feedback to the user indicating the specified characteristics that are inconsistent with the driver rankings.
[0107] For instance, where first time cost to build and furnish a facility is mission critical and all other drivers are not important, if a system user specifies an extremely complex and expensive building, the summary screenshot 450 may indicate ways to reduce building costs in some fashion to bring the building more into alignment with the way the drivers were ranked.
[0108] Referring now to FIG. 21 , one way to indicate facility characteristics that are not consistent with how drivers were ranked may be to highlight or otherwise visually distinguish various characteristics on the summary page 450 . In the illustrated example boxes 722 , 720 , 724 , 726 and 728 are shown around different summary characteristics to signify highlighting. Here, in at least some embodiments, it is contemplated that a user may place a mouse controllable pointing icon over any one of the highlight boxes causing a pop-up window to appear in which suggested changes to the information in the selected box are provided. For instance, where a pointing icon hovers over box 726 , a pop-up window could suggest that branding space be increased to 7% of the total space where a compelling customer experience is mission critical. In addition to including suggestions, the pop-up windows could include a “Accept” icon which, when selected, causes the server 552 to replace the information in the box 726 with the suggested value.
[0109] Although not illustrated, in other cases suggested facility characteristics that are consistent with business driver ranks could be presented along with the default and customized characteristics on the summary screenshot 450 . In some cases suggested characteristics may be able to be toggled on and off via a mouse selectable icon (not illustrated).
[0110] In still other cases where a specified facility is inconsistent with the way in which business drivers were bucketed by a user, server 552 may identify different levels of inconsistency and may only specify the most egregious inconsistencies for a user's consideration. For instance, where first cost to build is mission critical and all other drivers are not important but a user specifies a 100% window exterior skin, while other user specified characteristics may be inconsistent with a low first time cost to build, server 552 may be programmed to only suggest that the skin type be changed to a less expensive material.
[0111] Referring now to FIG. 5 , a subprocess 690 that may be substituted for a portion of the process 640 of FIG. 4 is shown where modifications to user specified facility characteristics are identified and presented to a user to bring a facility more in line with business drivers. Referring also to FIGS. 1 and 4 , after block 656 , server control may pass to block 692 where a user specifies building preferences and anticipated employee types and quantities. At block 694 , server 552 uses the user specified labor and location information to generate labor estimates associated with the user input.
[0112] Referring still to FIGS. 1 and 5 , at block 698 , a summary akin to summary 450 in FIG. 21 is provided that is based on the user specified information. At block 700 , server 552 compares presented data and estimates with default data and estimates to identify inconsistencies and at block 702 , server 552 indicates inconsistencies and provides suggestions to the user in some fashion.
[0113] In addition to the features described above, in at least some embodiments, new real estate and real estate to labor metrics are contemplated that it is believed will be particularly useful to real estate decision makers. To this end, it is known that specific facility designs can result in energy savings to run the facility. For instance, by using a concrete skin as opposed to sheet metal, heating costs may be able to be reduced by 5% for a facility. As another example, by using an open office plan where windows allow natural light to shine into 95% of all individual workspaces, lighting costs may be able to be reduced by 15%.
[0114] Similarly, it is generally known that it is far more expensive to reconfigure drywall type office delineating structure than to reconfigure partition wall systems. It is also known that most all facilities are “churned” over time. Here, the term “churn” means inevitable relocating of personnel and equipment and related structural changes to a facility to accommodate the relocation. A typical churn rate may be 20% meaning that 20% of facility space has to be reconfigured on an annual basis. While partition wall type space delineating systems may be more expensive than drywall structures, the cost associated with churn may be substantially less in both materials and labor in the case of a partition wall system.
[0115] Here, one interesting real estate related metric is referred to herein as “net effective rent” (NER) which means the triple net lease rate per square foot minus the other costs that would be incurred if a facility had some other baseline type characteristics. For instance, in some cases the cost of churn may be reduced by 0.94 cents per square foot per year and providing additional windows in a facility may reduce lighting cost by 0.38 cents per square foot per year. In this case, if the triple net lease rate is $14.50 per square foot per year, the NER would be $13.18 (i.e., $14.50−0.94−0.38=$13.18).
[0116] To facilitate the NER calculation, referring again to FIG. 1 , database 555 also includes an NER database 700 that stores data related to benchmark churn and energy savings statistics related to different facility characteristics. Although not shown in detail, it is contemplated that database 700 would include statistics related to percentage of exterior building skin formed by windows and related lighting cost savings, percentage of skin formed by concrete and heating cost savings, average churn cost savings when different building techniques are employed, etc. In addition, to support the NER calculation, in at least some embodiments, a third public database 702 may be accessible by server 552 to access geographically associated energy cost information.
[0117] In addition to the NER metric, other potentially interesting metrics include a labor-to-NER ratio (e.g., employees/NER), a seat-to-NER ratio, a turnover-to-NER ratio and an amenity cost/seat ratio. Each of these metrics can be determined by server 552 and provided via display 547 .
[0118] One other feature that is contemplated is one where benchmark retention costs are tied loosely to facility characteristics so that a real estate decision maker can gain insight into how facility changes can affect labor and overall operating costs. For instance, it is generally known that people like to work in workspaces that are at least in part illuminated via natural light. Thus, it is entirely possible and seems likely that retention rate can be increased by increasing the amount of natural light in a facility. A facility characteristics/retention database is contemplated that will include real life statistical information to show the relationship between natural light in a workspace and retention of employees. For instance, the database may indicate that where natural light in a facility is increased by 20% (e.g., exterior skin includes more windows), retention rates goes up 2%. In other cases the facility characteristics/retention database may not be based on actual statistics and instead may reflect knowledgeable perceptions such as an assumption that an increase in natural light of 20% will increase retention rate by at least 1% where the 1% value is at the low end of an expected range.
[0119] In FIG. 1 an exemplary facility characteristics/retention database is shown at 704 . It is contemplated that database 704 may include many other benchmark or assumed relationships between building characteristics and retention rates. Similarly, database 555 may include other facility characteristics/results databases (not shown) that relate characteristics to benchmark results or assumptions. For instance, data may be developed for medical facilities that indicates that repeat business can be increased by 15% by increasing the quality of certain facility spaces from good to better and by another 10% by increasing space quality from better to best. have realized that patients increasingly select medical facilities as a function of the amenities provided to patients. Thus, where patient rooms in a first hospital are private, include private high end spa type rest rooms and entertainment centers as well as high end decorations (e.g., wall coverings, furniture, artwork, etc.) and in a second hospital rooms are shared, have utilitarian rest rooms and minimal other amenities, patients will routinely prefer the first hospital. In this case the inventive system can he used to show how increases in construction and furnishing costs can directly increase profits.
[0120] All of the assumptions made when generating benchmark data can be used to generate other useful information for a system user and to affect the NER metric when appropriate. Thus, while increased construction and furnishing costs will increase a triple net lease cost per square foot, much if not all of the increase in triple net cost will often be offset by reduced turnover; increased work efficiency, increased profitability due to additional and more satisfied clients (e.g., patients), etc.
[0121] Referring now to FIG. 22 , an exemplary screenshot 750 is shown that can be used to see how an exemplary high end facility, when compared to a more traditional type of facility, can affect NER. Screenshot 750 and related tools may be accessible via the pop-up menu (not illustrated) associated with utilities icon 51 (see FIG. 6 ). In FIG. 22 , the high end facility is referred to as a “workstage” facility (see 774 ). In the illustrated example, it is assumed that facility quality and amenities only affect energy costs and the costs associated with churn. Consistent with the above comments it should be recognized that many other costs and sources of revenue (e.g., turnover rate, work efficiency, client satisfaction, full use of resources, etc.) may also be associated with facility quality and amenities and that those costs and revenue sources could be included in the NER calculation (see NER result at 770 ).
[0122] As shown, exemplary screenshot 750 includes data entry tools and various output fields that report calculated costs and savings associated with the data input via the input tools. The input tools include a building size field 756 , a geographical location field 758 , a churn rate slider button and a triple net lease rate field 764 . A user can specify building size, location, anticipated churn rate and anticipated triple net lease rate via fields and button 756 , 758 , 762 and 764 , respectively. When a location is selected via field 758 , server 552 accesses the public energy cost database 702 , obtains an energy cost value for the specific location and provides the cost value in an energy cost field 760 . Once location specific energy cost has been determined and churn rate has been specified, server 552 generates energy savings and churn savings values per square foot and populates fields 766 and 768 , respectively. The values in fields 766 and 768 are subtracted from the triple net rate in field 764 to generate the NER metric in field 770 .
[0123] Referring still to FIG. 22 , comparison data for a traditional facility and the high end facility is provided in a table including a “traditional” column 772 , a “workstage” column 774 , a “%” savings column 780 and a “cost” savings column 782 . In the illustrated example, energy savings is divided into lighting in table row 784 and heating/cooling in row 786 while churn savings is divided into labor and material rows 790 and 792 , respectively. As values in fields 756 , 758 and 770 and the churn rate specified by button 762 are altered, the resulting numbers output change in real time. Thus, for instance, where the location in field 758 is changed, the energy cost value in field 760 will automatically be changed which ripples through the data in fields 766 and 770 and rows 784 and 786 in the results table. Similarly, if the churn rate is altered via button 762 , data in fields 768 and 770 and in rows 790 and 792 is automatically altered.
[0124] Referring yet again to FIG. 23 , while a user can specify values/information in fields 756 , 758 , 762 and 764 , it should be appreciated that all of that data may simply be imported from default values generated by server 552 in the manner described above. Thus, for instance, a default building size for field 756 will result after a user has ranked business drivers (see FIGS. 6 and 7 ) and identified building type and numbers of seats and employees (see FIG. 8 ). Similarly, after a location has been selected (see FIG. 10 ), the electrical cost for field 760 can be populated.
[0125] One or more specific embodiments of the present invention have been described above. It should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation-specific decisions must be made to achieve the developers' specific goals, such as compliance with system-related and business related constraints, which may vary from one implementation to another. Moreover, it should be appreciated that such a development effort might be complex and time consuming, but would nevertheless be a routine undertaking of design, fabrication, and manufacture for those of ordinary skill having the benefit of this disclosure.
[0126] For instance, while databases 556 , 558 and 702 have been described above as being public and in some cases proprietary, in some embodiments the public databases may routinely (e.g., every week) be downloaded into private databases for subsequent use. As another instance, embodiments are contemplated where business drivers are not ranked or even considered by a user and/or where facility types are not considered.
[0127] Thus, the invention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the following appended claims. For example,
[0128] To apprise the public of the scope of this invention, the following claims are made: | A site/building decision facilitating apparatus including a database that correlates building characteristics with business driver factors, a processor linked to the database and running a program to perform the following acts: receiving business driver factor information for a first building project via an input device and identifying a subset of default building characteristics for the first building project using the database and the received business driver factor information | 6 |
BACKGROUND OF THE INVENTION
Embodiments of the invention relate generally to turbine blades and, more particularly, to the formation of cooling channels on a surface of a turbine blade and turbine blades including such cooling channels.
Turbine blades employed in high-temperature applications are typically a nickel-based super alloy and covered with a metallic bond coat and a ceramic thermal barrier coating. Embodiments of the invention facilitate improved cooling of a turbine blade, as compared to known configurations and methods of forming cooling channels. In turn, this enables use of the turbine blade in hot gas paths having a higher temperature, the use of a thinner thermal barrier coating, and a reduced cost, as compared to the use of nickel alloys. In some cases, cooling passages within the turbine blade may be simplified, since more of the active cooling of the turbine blade occurs at the blade surface. In addition, all cooling channels may be fabricated simultaneously, which reduces expense as compared to known methods of cooling channel formation, such as by water jet or electro-discharge machining.
BRIEF DESCRIPTION OF THE INVENTION
In one embodiment, the invention provides a method of forming a cooling channel along a surface of a turbine blade, the method comprising: applying a first mask material to a first portion of a surface of a turbine blade; forming a first barrier layer atop the first mask material and atop a second portion of the surface of the turbine blade; removing the first mask material and the barrier layer atop the first mask material to expose the first portion of the surface of the turbine blade; and etching the first portion of the surface of the turbine blade to form a cooling channel along the surface of the turbine blade.
In another embodiment, the invention provides a method of coating a turbine blade, the method comprising: aluminizing a metal layer of the turbine blade surface; converting the aluminized metal layer to an aluminide layer; and removing aluminum from the aluminide layer, forming a porous metal layer.
In still another embodiment, the invention provides a turbine blade comprising: a nickel-based superalloy airfoil; an oxidized porous metal layer on a surface of the airfoil; and a thermal barrier coating over the oxidized porous material.
BRIEF DESCRIPTION OF THE DRAWINGS
These and other features of this invention will be more readily understood from the following detailed description of the various aspects of the invention taken in conjunction with the accompanying drawings that depict various embodiments of the invention, in which:
FIG. 1 shows a perspective view of a turbine blade according to an embodiment of the invention.
FIG. 2 shows a flow diagram and cross-sectional side views of a method according to an embodiment of the invention.
FIG. 3 shows a flow diagram and cross-sectional side views of a method according to another embodiment of the invention.
FIGS. 4 and 5 show schematic top views of cooling channels formed according to embodiments of the invention.
FIG. 6 shows a cross-sectional side view of a step of a method according to an embodiment of the invention.
FIGS. 7-9 show schematic top views of cooling channels formed according to embodiments of the invention.
FIG. 10 shows a flow diagram of a method according to another embodiment of the invention.
It is noted that the drawings of the invention are not to scale. The drawings are intended to depict only typical aspects of the invention, and therefore should not be considered as limiting the scope of the invention. In the drawings, like numbering represents like elements between the drawings.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a cross-sectional side view of a portion of a turbine blade 1 according to an embodiment of the invention. Turbine blade 1 includes a leading surface 8 and a trailing surface 10 . A plurality of cooling channels 20 have been formed along trailing surface 10 according to one method of the invention. A bond coat layer 70 and thermal barrier coating layer 72 are formed atop trailing surface 10 and cover the plurality of cooling channels 20 . Although cooling channels 20 are shown only along trailing surface 10 in FIG. 1 , it should be appreciated that cooling channels may similarly be placed along leading surface 8 rather than or in addition to trailing surface 10 .
FIG. 2 shows a flow diagram and accompanying cross-sectional side views of a method according to one embodiment of the invention. At S 1 , a first mask material 30 is deposited atop a surface 10 of a turbine blade. Mask materials suitable for use according to embodiments of the invention include, for example, photoresist or a polymer material. First mask material 30 may be deposited using a number of methods or techniques, including, for example, dipping, spraying, or vapor deposition. The particular method or technique employed will depend, at least in part, on first mask material 30 . First mask material 30 may be discretely deposited or may be deposited across a larger area and then patterned. As shown in FIG. 2 , first mask material 30 covers a first portion 12 of surface 10 , leaving a second portion 14 exposed. First portion 12 includes an area or areas of surface 10 in which cooling channels are to be formed. Second portion 14 includes areas of surface 10 in which cooling channels are not to be formed and may comprise some or all of surface 10 other than first portion 12 . One skilled in the art will recognize, of course, that materials and deposition techniques other than those disclosed may be employed.
At S 2 , a first barrier layer 40 is formed atop surface 10 , covering both first mask material 30 and second portion 14 of surface 10 . First barrier layer 40 may include, for example, Titanium oxynitride, TiO 2 , TaO 2 , TiN, SiO 2 , and high melting point oxides, such as aluminum oxide. First barrier layer 40 may be formed using any number of methods or techniques, including, for example, chemical vapor deposition, sputtering, or reactive sputtering. The particular method or technique employed will depend, at least in part, on first barrier layer 40 . At S 3 , first mask material 30 is removed, along with the portion of barrier layer 40 atop first mask material 30 , exposing first portion 12 of surface 10 . First portion 12 may then be etched at S 4 to form cooling channel 20 in surface 10 . Etching first portion 12 may include any number of methods or techniques, including, for example, liquid chemical etching and reactive ion etching.
In some embodiments of the invention, cooling channels 20 may be further processed to form overhanging structures above the cooling channels 20 . This effectively reduces an opening to the cooling channel 20 , which may be desirable in some circumstances. FIG. 3 shows a flow diagram and accompanying cross-sectional side views of a method of forming such overhanging structures. At S 5 , cooling channel 20 is filled with a second mask material 32 . Second mask material 32 may be the same as first mask material 30 ( FIG. 2 ) or may be a different mask material. Similarly, second mask material 32 may be deposited using the same method or technique as first mask material 30 or by a different method or technique.
At S 6 , a high-temperature metal layer 50 is deposited, formed, or applied atop second mask material 32 and first barrier layer 40 . High-temperature metal layer 50 may include, for example, a nickel-based super alloy or a refractory metal and may be deposited, formed, or applied using any number of methods or techniques, such as vapor deposition, sputtering, or electrochemical deposition.
A third mask material 34 and second barrier layer 42 are then deposited or formed atop high-temperature metal layer 50 at S 7 . As can be seen in FIG. 3 , third mask material 34 is deposited such that, in at least one dimension, its width is less than that of cooling channel 20 . The deposition or forming of third mask material 34 and second barrier layer 42 are similar to the deposition or forming of first mask material 30 and first barrier layer 40 in FIG. 2 . Third mask material 34 may be the same as first mask material 30 or second mask material 32 or may be a different mask material and may be deposited using the same or a different method or technique. Similarly, second barrier layer 42 may be the same as first barrier layer 40 or may be a different mask material and may be deposited using the same or a different method or technique.
At S 8 , third mask material 34 and the portion of second barrier layer 42 atop third mask material 34 are removed, similar to the removal of first mask material 40 and a portion of first barrier layer 40 at S 3 of FIG. 2 . At S 9 , high-temperature metal layer 50 is etched where exposed by the removal of third mask material 34 and second barrier layer 42 , forming an opening 22 through which second mask material 32 is removed from cooling channel 20 . As can be seen in FIG. 3 , the smaller dimension of third mask material 34 , as compared to cooling channel 20 , results in overhangs 60 , 62 of high-temperature metal layer 50 and second barrier layer 42 above cooling channel 20 .
FIG. 4 shows a top view of a cooling channel 20 according to one embodiment of the invention. For ease of illustration and explanation, only second barrier layer 42 is shown. One skilled in the art will recognize, however, that high-temperature metal layer 50 lies below second barrier layer 42 . In FIG. 4 , overhangs 60 , 62 reside adjacent opening 22 and over a portion of cooling channel 20 . Other configurations are possible. In FIG. 5 , for example, overhang 60 is continuous around a substantially square opening 22 .
FIG. 6 shows a cross-sectional view of another embodiment of the invention. Here, opening 122 is offset and substantially flush with a wall 121 of cooling channel 120 . As such, a single overhang 160 is formed above cooling channel 120 . FIGS. 7-9 show top views of various arrangements of opening 122 relative to cooling channel 120 according to such an embodiment.
In FIGS. 3-9 , opening 22 , 122 is shown as being substantially square- or rectangular-shaped. This is neither necessary nor essential, however, and openings formed according to the various embodiments of the invention may have any number of two-dimensional shapes.
In any of the embodiments of the invention, once surface 10 , 110 is etched to form cooling channel 20 , 120 , a metallic bond coat, such as MCrAlY, may be applied in a manner that is sufficient to cover first barrier layer 40 or second barrier layer 140 , as well as to cover the surfaces of, but not fill, cooling channel 20 , 120 . Similarly, in any of the embodiments of the invention, the cooling channel 20 , 120 formed may be joined to a source of cooling fluid, such as air or steam, for example, within the turbine blade 1 ( FIG. 1 ). For example, once cooling channel 20 , 120 is formed, a passage may be formed, such as by drilling, from a bottom surface of the cooling channel 20 , 120 through to a source of cooling air in the center of the turbine blade.
In some embodiments of the invention, high-temperature metal layer 50 , 150 includes a porous metal layer. Use of such a porous metal layer reduces stress in a thermal barrier coating (TBC) applied to the turbine blade during later processing steps, since it is more compliant than either the turbine blade itself or the TBC. Porous metal layers also reduces the thermal diffusivity, as compared to a similar non-porous metal layers. This increases the temperature drop between the hot gas and the turbine blade.
FIG. 10 shows a flow diagram of a method of forming a porous metal layer on a turbine blade according to an embodiment. At S 10 , a metal layer, for example, 42 in FIG. 3 , is aluminized. This may be achieved using any number of methods or techniques, including, for example, dipping the metal layer in an aluminum bath, spray depositing aluminum onto the metal layer, or vapor depositing aluminum onto the metal layer.
At S 11 , the aluminized metal layer is converted to an aluminide layer. Typically, this is achieved by heating the aluminized metal layer to a temperature between about 660° C. and about 1200° C. in the absence of oxygen.
At S 12 , aluminum is removed from the aluminide layer to form a porous metal layer. The aluminum may be removed using any number of methods or techniques, but is typically removed by applying a caustic solution to the aluminide layer. Where the metal layer was a nickel alloy, the porous metal layer thus formed comprises a porous nickel alloy layer.
A number of additional processes may be carried out on the porous metal layer. For example, at S 13 , the porous metal layer may optionally be passivated by oxidation. This may be desirable, for example, where the metal layer will be exposed to high temperatures, since the high surface area of the porous metal layer is likely to be pyrophoric. Oxidizing the porous metal layer may be achieved by, for example, heating in air around 400 C.
At S 14 , a bond coat and/or thermal barrier coating may optionally be applied to the porous metal layer formed at S 12 or the oxidized porous metal layer formed at S 13 .
As described herein, the porous metal layer is formed from high-temperature metal layer 50 , 150 , although other metal layers may similarly be made porous to provide increased compliance. For example, the nickel-based superalloy of the turbine blade itself may be made porous using the method described above or a similar method. In addition, the turbine blade may be coated with a layer of a nickel-based heat resistant alloy which is then made porous using the method described above or a similar method.
In any case, additional layers may be deposited atop the porous metal layer to complete the finishing of the turbine blade. For example, in some embodiments of the invention, a turbine blade comprises a nickel-based superalloy airfoil, an oxidized porous metal layer on a surface of the airfoil, a bond coat, and a thermal barrier coating over the oxidized porous material.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used herein, the singular forms “a”, “an” and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms “comprises” and/or “comprising,” when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to practice the invention, including making and using any devices or systems and performing any related or incorporated methods. The patentable scope of the invention 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 if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal language of the claims. | Embodiments of the invention relate generally to turbine blades and, more particularly, to the formation of cooling channels on a surface of a turbine blade and turbine blades including such cooling channels. In one embodiment, the invention provides a method of forming a cooling channel along a surface of a turbine blade, the method comprising: applying a first mask material to a first portion of a surface of a turbine blade; forming a first barrier layer atop the first mask material and atop a second portion of the surface of the turbine blade; removing the first mask material and the barrier layer atop the first mask material to expose the first portion of the surface of the turbine blade; and etching the first portion of the surface of the turbine blade to form a cooling channel along the surface of the turbine blade. | 5 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a method of determining the travel time of an elastic signal from a predetermined point of a drill string to a transducer spaced on the drill string from the predetermined point.
2. Description of the Related Art
During the drilling of a well, it is useful to know the time taken by an elastic wave to travel from one part of the drill string to another, for instance from the bit to a transducer placed near the top of the drill string. Although an estimation of the travel time may be made on the basis of the length of the drill string and the speed of propagation of the energy in the material of which the drill string is constructed, such an estimation does not correlate with actual travel times. This is because the drill string is made up of a plurality of sections with impedance discontinuities between the sections. The impedance discontinuities create energy reflections which interact with each other and with the direct upwardly propagating energy to alter the effective velocity of propagation of the energy within the drill string.
Knowledge of propagation time along the drill string is particularly useful for the technique known as "checkshot while drilling". According to this technique, the energy generated by the drill bit and propagating into the earth is used as a seismic source. Direct and reflected energy is detected by a transducer such as a geophone, for instance located on the surface of the earth some distance away from the drill string. A further transducer is mounted near the top of the drill string. The outputs from the transducers may then be processed to reveal information, for instance about the strata through which the drill bit is passing or ahead of the drill bit. However, in order to make use of the transducer output signals, it is required to know the time taken by the acoustic energy generated at the drill bit to travel up the drill string to arrive at the transducer on the drill string.
The applicants are presently aware of the following prior art, none of which is considered relevant to the present invention: EP-A-0409304; U.S. Pat. No. 4,926,391; U.S. Pat. No. 4,718,048; U.S. Pat. No. 4,829,489; and "The Use of Drill-Bit Energy as a Down Hole Seismic Source" by J. W. Rector III and B. P. Marion, Geophysics, Vol 56 No 5 (May 1991), pp 628-634.
SUMMARY OF THE INVENTION
According to one aspect of the invention, there is provided a method of determining the travel time of an elastic signal from a predetermined point of a drill string to a transducer spaced on the drill string from the predetermined point, the method comprising: modeling the drill string as a one dimensional layered medium of equal travel time layers; generating vibrational energy in the drill string by means of a vibrational energy source on the drill string; deriving from an output signal of the transducer a reflection coefficient series corresponding to the modeled drill string each reflection coefficient of which corresponds to an impedance discontinuity in the drill string; identifying one reflection coefficient of the series with the predetermined point of the drill string and a further reflection coefficient with a known structure in the drill string spaced from the predetermined point; and determining the travel time from the positions of the one reflection coefficient and the further reflection coefficient in the reflection coefficient series.
According to a second aspect of the invention, there is provided a method of determining the travel time of an elastic signal from a predetermined point of a drill string to a transducer spaced on the drill string from the predetermined point, the method comprising: modeling the drill string as a one dimensional layered medium of equal travel time layers; generating vibrational energy in the drill string by means of a vibrational energy source on the drill string, deriving from an output signal of the transducer a reflection coefficient series corresponding to the modeled drill string; each reflection coefficient of which corresponds to an impedance discontinuity in the drill string identifying at least one reflection coefficient corresponding to a structure in the drill string; determining the rate of change of position of said at least one reflection coefficient in the reflection coefficient series as the length of the drill string; increases and determining the velocity of the signal from the rate of change of position, and determining the travel time from the velocity and the length of the drill string.
By modeling the drill string as a one dimensional layered medium it is possible to process the transducer output signal to derive reflection coefficients related to the drilling structure. It is thus possible to provide a method which permits accurate estimation of travel times in a drill string. Such a method may be employed in any application where drill string travel times are required, such as in checkshot while drilling.
In the first aspect of the invention, the predetermined point of the drill string is preferably the drill bit or a connection between a bottom hole assembly and an adjacent section of the drill string. The known structure is typically the transducer or a structure at the point in the drill string where the transducer is located.
In the second aspect of the invention, it is preferred that a plurality of reflection coefficients, typically all relating to one structure such as the bottom hole assembly, are monitored and a rate of change is determined which provides the best fit for the coefficients.
The vibrational energy source is usually the interaction of the drill bit with the formation in drilling. Rollercone bits are preferred as vibration sources. The transducer is conveniently located at or near the top of the drill string such as on the traveling block and can respond to force, displacement velocity or acceleration.
The reflection coefficient series can be derived by determining the filter coefficients of a filter model, such as an auto-regressive filter model, by fitting the filter output signal to the transducer output signal and deriving the reflection coefficients from the filter coefficients.
Typically this is achieved by correcting the filter coefficients of a lattice filter representing the reflection coefficient series. Where the transducer is spaced from the traveling block, an auto-regressive moving average model of the transducer output signal is calculated, the reflection coefficient series being derived from the auto-regressive part of the model. In this case it is preferred that the power spectrum of the transducer output signal is divided by the moving average model to form a quotient, the reflection coefficient series is derived from the quotient. The reflection coefficient series can be derived from the auto-correlation function of the transducer output signal.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be further described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 illustrates schematically part of a drill string bottom hole assembly;
FIG. 2 illustrates schematically a typical drill string interface;
FIG. 3 illustrates a series of drill string layers of equal travel time;
FIG. 4 shows a drill string with an impulse applied to a bit thereof;
FIG. 5 illustrates at (a) an artificial reflection coefficient series and at (b) the
spectrum of upgoing waves measured just below a traveling block of the drill string;
FIG. 6 illustrates an original reflect:ion coefficient series and an estimated series;
FIG. 7 illustrates at (a) a reflection series showing tooljoints and at (b) a system frequency response;
FIG. 8 illustrates a reflection series using part of a spectrum;
FIG. 9 shows at (a) a spectrum after low pass filtering and at (b) a reflection series calculated from the filtered spectrum;
FIG. 10 shows a reflection series calculated using a first half of a filtered spectrum;
FIG. 11 shows at (a) the spectrum of a signal measured just below a drill string swivel and at (b) a reflection coefficient series calculated from a first half of the accelerometer spectrum;
FIG. 12 shows at (a) a first half of an accelerometer spectrum and a spectrum of an MA (3) model and at (b) a reflection series calculated from the ratio of the spectra shown at (a);
FIG. 13 shows at (a) the measured output of a swivel-mounted accelerometer and at (b) the power spectrum of the measured output;
FIG. 14 shows a set of reflection coefficient series for increasing well-depth; and
FIG. 15 shows a reflection series for an actual drill string.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A drill string consists of a series of steel cylinders of different lengths and cross sectional areas joined together. Such a drill string can be modeled as a layered impedance system for instance as disclosed by J. F. Claerbout in "Fundamentals of Geophysical Data Processing", Blackwell Scientific Publications, California, 1985. The drill string is divided into a number of sections or layers, the thicknesses of which are such that it takes the same amount of time for an axial wave to travel across each section. Within each layer, the cross sectional area and material properties remain constant. This model is similar to the lossless tube model used in speech processing as disclosed by L. R. Rabiner and R. W. Schafer in "Digital Processing of Speech Signals", Prentice, N.J., 1978.
FIG. 1 shows pan of the bottom hole assembly (BHA) of a typically drill string. The interface 11 between two sizes of drill collars 12 and 13, for an elastic wave traveling upwards, can be characterized by two coefficients, names a reflection coefficient c d and a transmission coefficient t u . Thus, for a unit amplitude incident wave, the amplitude of the transmitted part of the wave is t u and that of the reflected part is c d . For reasons of continuity, the wave amplitudes must be the same of either side of the interface 11. This gives rise to the relationship:
t.sub.u =1+c.sub.d (1)
Similarly for a unit impulse traveling downwards:
t.sub.d =1+c.sub.u (2)
where C u and t d are the reflection and transmission coefficients, respectively, for a downward traveling wave.
The energy in the wave is equal to the wave amplitude squared multiplied by a proportionality factor which depends upon the material properties. For example if the amplitude measured is velocity, then the proportionality factor is impedance I. If the impedance in the upper drill collar 12 is I 1 and that in the lower collar 13 is I 2 , then energy conservation before and after incidence gives:
I.sub.2 =I.sub.2 C.sub.d.sup.2 +I.sub.1 t.sub.u.sup.2 (3)
for an upward traveling wave. Substituting equation (1) in equation (3) gives: ##EQU1##
The reflection coefficient depends upon the size of the impedance change across the interface. Using the same argument gives: ##EQU2## hence:
C.sub.u =--c.sub.d (6)
The general case of an interface 21 in a drill string is illustrated in FIG. 2. The upward and downward going waves in the upper layer 22 are represented by U' and D' respectively, while the upward and downward waves in the lower layer 23 are shown as U and D, respectively. The reflection coefficient at the interface is c for an upward traveling wave while the transmission coefficients are denoted as t u and t d .
Thus:
U'=t.sub.u U--cD'D+t.sub.d D'+cU (7)
or, in matrix form: ##EQU3##
Premultiplying by the inverse of the left: hand matrix and simplifying gives: ##EQU4## For a series of layers as illustrated in FIG. 3, equation (9) can be rewritten as: ##EQU5## for the interface between each k th and (k+1)th layer.
The travel time across each layer is T /2, where T is the data sampling interval. This means that travel across a layer can be indicated by multiplication by √Z where Z is the unit delay operator. To make the notation simpler, the transmission coefficient t u will be referred to as t. Therefore, in the k th layer: ##EQU6##
Substituting equation (11) into equation (10) and simplifying gives the layer matrix: ##EQU7##
This layer matrix can be used to extrapolate the signal measured in one layer to that measured in another. For example, to extrapolate from layer k to layer k+2: ##EQU8##
In general, from Claerbout (see above), the form of the product of k layer matrices is given by: ##EQU9## where F(Z) and G(Z) are polynomials in Z. These polynomials are related to each other. Their coefficients are determined by the values of the reflection coefficients. A more detailed investigation of their structure can be found in Claerbout.
For the drill string 41 shown in FIG. 4, if an impulse is applied to the bit 42, then an axial wave will propagate through the drill string, reflecting from all the impedance changes. This will give rise to a wave P(Z) scattered back from the drill string. Assuming that there is a perfect reflector 43 at the top of the drill string which has a reflection coefficient of -1 for waves traveling upwards, then if the upgoing waves just below this top reflector are designated as X(Z), then the downgoing waves must be --X(Z). The product of the layer matrices can be used to determine the waves in terms of the reflection coefficients: ##EQU10##
From the first part of equation (15): ##EQU11## X(Z) is an auto-regressive (AR) process. If a sensor were placed just below the second reflector 44 shown in FIG. 4, it would measure the sum of the upgoing and downgoing waves U 3 and D 3 . Equation (12) gives: ##EQU12##
From this, the measured signal is given by: ##EQU13##
This is an auto-regressive moving average (ARMA) process and the AR part is the same as in equation (16). This procedure can be continued to see what would be measured further down the drill string. At each successive layer, the AR part of the signal is the same but the moving average (MA) part changes. For U 4 +D 4 the MA part is given by:
[Z.sup.0 (1+c.sub.3)+0Z.sup.1 -Z.sup.2 (1+c.sub.3)] (19)
and for U 5 +D 5 it is: ##EQU14##
Further down, the MA part becomes larger and more complicated. However certain things about the nature of this MA signal may be observed. First, it depends only on the reflectors above the measurement point. This is important when it comes to deciding where to place the sensor on a real drill string. Second, there is a symmetry to the coefficients of the MA polynomial. For a polynomial that extends to Z k , the coefficient of the highest power of Z is equal to the coefficient of Z 0 multiplied by -1. Similarly the coefficient of Z k-1 is equal to -1 times the coefficient of Z 1 , and so on, i.e.:
a.sub.1 Z.sup.0 +a.sub.2 Z.sup.1 +a.sub.3 Z.sup.2 +K-a.sub.3 Z.sup.k-2 -a.sub.2 Z.sup.k-1 -a.sub.1 Z.sup.k (21)
If k is even then the coefficient of Z k/2 is zero (see equation (19)). One consequence of this is that the roots of the MA polynomial must always lie on the unit circle.
Synthetic data were used to determine how to calculate the reflection coefficients from measurements made near the top of the drill string. The effects of anti-alias filters and sensor position were also considered.
FIG. 5(a) shows a reflection coefficient series intended to represent a typical drill string. The reflection coefficient due to the effective top of the drill string, the traveling block (TB), is assumed to have a value of -1 for upward traveling waves, and is not shown. The first few reflectors represent such things as the hook, swivel, kelly spinner, etc. The reflector at position 70 represents a change from drill pipe to heavyweight drill pipe. The remaining reflectors below position 120 represent changes in section in the BHA. The bit is at position 156.
If this drill string is excited by a white noise input at the bit (representing the bit/rock interaction) and the upgoing waves are measured just below the TB, a signal is obtained whose spectrum is shown in FIG. 5(b). This signal is equivalent to the signal X(Z) defined hereinbefore. As can be seen, it is an AR process. The AR parameters of this signal are the coefficients of the Z polynomial on the bottom line of equation (16). These coefficients depend upon the reflection coefficients. There are many ways to determine both the AR parameters and the reflection coefficients. These divide into two main categories namely block data methods and sequential data methods. Block data methods divide the available data into sections which are processed independently. The most widely known technique for estimating the AR parameters and reflection coefficients from a finite set of time samples is the Burg algorithm. If a large number of time samples is available, then the Yule-Walker method may be used. Sequential data algorithms may be applied to a continuous stream of time data samples. These algorithms update estimates of the AR parameters (or reflection coefficients) as new data samples become available. Examples of such techniques are least mean square (LMS), recursive least squares (RLS) and least squares lattice (LSL) filters. These techniques are well known and may be found, for instance, in "Adaptive Filter Theory" by S Haykin, Prentice Hall, New Jersey, 1986, "Modern Spectral Estimation: Theory and Application" by S. M. Kay, Prentice Hall, New Jersey, 1983, and "Digital Spectral Analysis with Application" by S. L. Marple Jr., Prentice Hall, New Jersey, 1987.
To obtain both the AR parameters and the reflection coefficients, the Yule-Walker approach will be described.
Basically the approach is to make some estimate of the auto-correlation sequence (ACS) of the measured signal and then to use the Levinson recursion to determine both the AR parameters and the reflection coefficients. If the data set is large, then the estimate of the ACS can be easily obtained using the fast Fourier transform (FFT).
Applying the Yule-Walker approach to the signal shown in FIG. 5(b) yields the set of reflection coefficients shown in FIG. 6. The solids line shows the original reflection coefficient series (offset for clarity), while the dashed line is the Yule-Walker estimate. Agreement between the two is very good.
As disclosed above, the reflection coefficients represent the boundaries between impedance layers with the layers defined such that the travel time across each is equal to T /2, where T is the data sampling interval. For example, if the signal X(Z) is sampled at 500 Hz, then the sampling interval is 0.002 seconds. The travel time across each layer is then 0.001 seconds. Hence, if the bit can be identified as being represented by reflection 156 then the direct travel time of a signal from the bit to the measurement point is 0.156 seconds.
The resolution in terms of length depends upon the velocity of sound in the drill string. If the sampling frequency is increased then the spatial resolution is increased. The limits of this resolution depend on the frequency content of the signal. For example, if there is no energy in the signal above 200 Hz then sampling at 1000 Hz will not increase the useful resolution of the derived reflection coefficients. There are three things which control the frequency content of the measured signal:
the bit/rock interaction. This is the (assumed) white noise driving process. If this is bandlimited, then the measured signal will be bandlimited;
attenuation. The higher the frequency of vibration, the more energy is lost (radiated to the mud, lost to string/borehole interactions, etc.);
the drill string. Due to its periodic structure, the drill string contains stop bands in its transfer function. For a typical drill string, the first stop band is between 200 and 300 Hz and is several tens of Hz wide.
One effect of the limit on the resolution is that drill string features are smaller (shorter in travel time) than the limit of resolution cannot be resolved. This is the case for tooljoints. The typical magnitude of the reflection coefficient for the impedance contrast between the body of a drillpipe and a tooljoint is about 0.5, but such a reflector is followed almost immediately by another reflector of equal magnitude but opposite sign. Because the two reflectors are so close together it would be necessary to sample at a very high frequency to resolve them.
For a reflection coefficient series shown in FIG. 7(a), the alternating reflection coefficients represent the tooljoint/drill pipe boundaries. In addition there are some smaller reflection coefficients which represent changes in the average impedance of the drill string (e.g. between the different grades of drill pipe). The frequency response of this system is shown in FIG. 7(b).
The stop bands can be clearly seen. If, however, the reflection coefficients are calculated using only that part of the data before the first stop band, then the result is as shown in FIG. 8. The reflectors due to the average impedance changes are visible, but hose due to the tooljoints are not.
In practice, when data from an accelerometer or other sensor are gathered, analogue low pass filtering is used to prevent aliasing of the signal. FIG. 9(a) shows the effect of a low pass filter on the spectrum of the signal X(Z). If this spectrum is used to generate the ACS and then the reflection coefficients, the result is as shown in FIG. 9(b). The solid line shows the original series (offset for clarity) and the dashed line shows that derived from the filter spectrum.
Obviously the low pass filter has a detrimental effect on the processing. The reflectors are much less distinct and appear to have shifted towards the top of the drill string. This is because, after filtering, the measured signal is no longer an AR process and therefore cannot be adequately modeled as such.
The low pass filter is designed to attenuate the high frequency part of the signal, and it should have little effect on the low frequency part. By using the first half of the spectrum in FIG. 9, the set of reflection coefficients shown in FIG. 10 can be calculated. Although the resolution has been halved, the reflectors are in the correct position and are quite distinct.
The preceding description has dealt with how to process the upgoing waves measured just below the TB. In reality, it is not possible to measure just the upgoing part of the signal. Usually the sum of the up and downgoing waves is measured at some point below the TB, but not just below. As described above, such a signal is an AR/VIA process in which the MA part depends only upon the reflectors above the measurement point and the AR part is the same as that of the upgoing waves measured just below the TB.
Referring to FIG. 5, if an accelerometer is placed just below reflection 5 (which represents the bottom of the swivel) then, for the same white noise excitation as before, the spectrum shown as the solid line in FIG. 11(a) should be measured. The dashed line shows the same signal after low pass filtering. The zeros are due to the MA part of the signal.
In order to recover the reflection coefficients, both the low pass filter and the MA part of the signal must be dealt with. If the reflection coefficients were merely calculated from the first half of the spectrum as before, then the result shown as the dashed line in FIG. 11(b) would be obtained. The solid line shows the results first seen in FIG. 10 for comparison. The effect of the MA part is obvious.
There are many ways to estimate the MA part of an ARMA process for instance as disclosed by Kay or Marple (see above). One simple way is to evaluate the inverse Fourier transform of the reciprocal of the accelerometer power spectrum and then to apply the Levinson recursion to the resulting ACS. To do this successfully, the order of the MA process must be known. This can be determined by counting the zeros in the spectrum. In the first half of the spectrum shown in FIG. 11 there is one obvious zero at a normalized frequency of about 0.13. There is also half a zero at 0. Each full zero required 2 MA parameters to define it, so in this case 3 MA parameters are needed.
FIG. 12(a) shows both the first half of the accelerometer spectrum (solid line) and the spectrum of a MA(3) model (dashed line) evaluated from the reciprocal of the accelerometer spectrum. If the accelerometer spectrum is divided by the MA(3) spectrum and the reflection coefficients calculated from the result, then the series shown as the dashed line in FIG. 12(b) is obtained. Once again the solid line is from FIG. 10.
The data set used in the following example was obtained while drilling with 171/2 inch rollercone bits. An accelerometer was mounted on the swivel. The data were logged at 500 Hz.
FIG. 13 shows a typical section of time data from accelerometers, and the power spectrum calculated from that data. The amplitude variations in the time data are due to stick slip motion at the bit.
Calculating the reflection coefficients for the drill string at increasing depths (using only the first 130 Hz and a MA order of 6) gives FIG. 14. The x-axis is drill string length. The BHA components can clearly be seen moving to the right as the drill string length increases. Since the make-up of the drill string is known, particularly reflection coefficients can be identified with particular parts of the BHA. FIG. 15 shows the reflection series for a drill string length of 1001 meters. The reflector at position 84 is the change from drill pipe to heavyweight drill pipe (HWDP), the change from HWDP to 8 inch drill collars (DC) is at 90, and the change from 8 to 91/2 inch DC is at 97. The bit is at position 110. Since a MA(6) model was needed to correctly process the data, the accelerometer is at position 6. Remembering that only the first 130 Hz of the spectrum was used to calculate the reflection coefficient series (which implies a sampling rate of 260 Hz), the travel time from bit to accelerometer is calculated as: ##EQU15##
If the bit has been correctly identified, this travel time is accurate to within ±0.00096 seconds (i.e. half of the travel time across one layer of the layered impedance model, which is defined such that the travel time across each layer is equal to half the sampling interval).
If the bit is difficult to identify, another method may be used to determine travel time. The acoustic velocity in the drill pipe is less than that for a uniform steel pipe, because of its periodic structure. The reflection coefficient image may be used to determine this velocity. As shown in FIG. 14(a), the BHA components move to the right as the drill string gets longer, i.e. as more drill pipe is added. If a feature is chosen in the BHA part of the image which is clearly visible in most of the traces, and a best fit straight line is drawn through the position of this feature on all traces, then the slop of this line gives the acoustic velocity in the drill pipe. Where several features are taken, the least squares fit gradient of all of these can be used to obtain the acoustic velocity.
Doing this for FIG. 14(a) gives a velocity in the drill pipe section of 4930 meters/sec. The BHA section is much shorter than the drill pipe section and is more uniform in structure. If the BHA velocity is assumed to be the same as for uniform steel pipe (i.e. 5150 meters/see) then, for a drill string length of 1001 meters, the travel time from bit to accelerometer is:
.increment.t.sub.ds =0.201 sec
The accuracy of the estimation of drill pipe velocity will improve as the well gets deeper, i.e. as the best fit straight line is calculated on more points. The assumption that the BHA velocity is similar to that of a uniform pipe may be wrong, especially if the BHA contains such components as shock subs and jars. However, the length of the BHA is usually small compared to the overall drill string length; so that the error introduced by this assumption will be small. | During a drilling operation, the vibrational energy produced by a drill bit cutting through the earth excites a drill string and the energy near the top of the drill string is mounted by a transducer. A reflection coefficient series is derived from the transducer output such that each reflection coefficient corresponds to a drill string impedance discontinuity. One of the reflection coefficients is identified with a predetermined point of the drill string and energy travel time in the drill string is determined from the position of the one reflection coefficient in the series to the position in the series of a further coefficient. | 4 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a one-way clutch for a torque converter used as a part for torque transmission, back stop, etc., in the driving apparatus of,-for example, an automobile, and more particularly to an improvement in a sprag.
2. Related Background Art
Generally, a one-way clutch comprises an inner race and an outer race radially spaced apart from each other and concentrically disposed for rotation relative to each, and a torque transmitting member disposed between the inner race and the outer race for transmitting torque, and the cam surface of a sprag meshes with the raceway surfaces of the inner and outer races to thereby transmit the torque.
In order to form an oil film, it is preferable that the cam surface of the sprag be as smooth as possible, but in order to give predetermined surface roughness to the cam surface, there is a sprag in which as described in Japanese Patent Application Laid-open No. H6-313445, minute unevenness is formed on a meshing surface to improve the forming rate of oil film on the cam surface.
The sprag, however, if the viscosity of lubricating oil becomes high under a very low temperature environment (e.g. −20° C. to −40° C. or lower), does not normally mesh but continuously causes slip when shift is made from idle rotation to meshing, and there may occur the inconvenience that the meshing of a sprag clutch does not function. When as in Japanese Patent Application Laid-open No. H6-313445, minute unevenness is formed on the surface, there is the possibility that lubricating oil of high viscosity collects in the unevenness and becomes oil film to thereby cause continuous slip.
To overcome these problems, it is conceivable to increase a ribbon spring force which applies a load in a meshing direction to the sprag, but an increase in the ribbon spring force may increase the drag during idle rotation, and may cause the aggravation of fuel consumption in a one-way clutch used in an automatic transmission.
SUMMARY OF THE INVENTION
Accordingly, it is the object of the present invention to provide a one-way clutch which eliminates the above-noted problems and is greatly improved in meshing during a low temperature, and a sprag for use in the one-way clutch.
In order to achieve the above object, the one-way clutch of the present invention is a one-way clutch comprising an inner race and an outer race radially spaced apart from each other and concentrically disposed for rotation relative to each other, and a sprag disposed between the inner race and the outer race for transmitting torque, wherein the cam surface of the sprag which contacts with the inner race and the outer race is formed with a plurality of axially extending grooves.
Also, the sprag of the present invention is a sprag used in a one-way clutch comprising an inner race and an outer race radially spaced apart from each other and concentrically disposed for rotation relative to each other, and disposed between the inner race and the outer race for transmitting torque, wherein a cam surface contacting with the outer peripheral surface of the inner race is formed with a plurality of axially extending grooves.
According to the present invention, there is obtained the following effect.
Since the meshing surface of the sprag which is adjacent to the inner race is formed with a plurality of axially extending grooves, a sufficient meshing property can be secured even during a low temperature at which the viscosity of lubricating oil rises. This is because the grooves formed in the cam surface of the sprag eliminates oil film between the sprag and the inner race which has become high in viscosity during the low temperature, during meshing, and the sprag and the inner race achieve metal-to-metal contact and mesh with each other.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a sprag used in a one-way clutch according to an embodiment of the present invention.
FIG. 2 is a fragmentary front view of the sprag of FIG. 1 .
FIG. 3 is a partly broken-away front view of the one-way clutch.
FIG. 4 is a front view of a one-way clutch of other type to which the present invention is applicable.
FIG. 5 is a front view of a sprag used in the one-way clutch as shown in FIG. 4 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will hereinafter be described in detail with reference to the drawings. The embodiment hereinafter described illustrates the present invention by way of example, and of course does not restrict the present invention. Also, throughout the drawings, like portions are designated by like reference characters.
FIG. 1 is a perspective view of a sprag 3 used in a one-way clutch 10 ( FIG. 3 ) according to an embodiment of the present invention, and FIG. 2 is a fragmentary front view of the sprag 3 of FIG. 1 . While here is shown an example in which a gourd-shaped sprag 3 is used as a torque transmitting member, the present invention can also of course be applied to a one-way clutch using other form of sprag.
As shown in FIG. 1 , the sprag 3 has a plurality of axially extending substantially parallel grooves 20 in a cam surface 21 . The grooves 20 extend from one axial edge portion 3 a to the other edge portion 3 b of the sprag 3 . That is, the grooves 20 extend over the entire axial width of the cam surface 21 of the sprag 3 .
The depth and pitch of the grooves 20 will now be described with reference to FIG. 2 . The depth of the grooves 20 in about 0.005 mm or greater and 0.05 mm or less for the durability of the sprag, but may desirably be within the amount of elastic deformation of the surface during a maximum load, and may more preferably be about 0.015 mm or greater and about 0.03 mm or less.
Also, the pitch between adjacent ones of the grooves 20 can be arbitrarily set, but may desirably be about 0.5 mm or less to secure a meshing property. In FIG. 1 , and particularly FIG. 2 , for the convenience of illustration, the grooves 20 are depicted at a size larger than the actual size thereof. Also, when the sprag 3 is used in a one-way clutch, the cam surface 21 of the sprag 3 is opposed to the outer peripheral surface of an inner race and therefore, the grooves 20 shown in FIGS. 1 and 2 are located in the lower portion of the sprag 3 . That is, in order to show the grooves 20 , the sprag 3 is shown as being inverted relative to a state in which it is actually used.
Description will now be made of the construction of a one-way clutch 10 using the sprag 3 formed with the grooves 20 in the cam surface 21 . FIG. 3 is a partly broken-away front view of the one-way clutch 10 .
In FIG. 3 , the one-way clutch 10 is provided with an outer race 1 and an inner race 2 . The outer race 1 is provided with a substantially completely round inner peripheral surface la. Also, the inner race 2 is provided with a substantially completely round outer peripheral surface 2 a. The outer race 1 and the inner race 2 are disposed for rotation relative to each other with the inner peripheral surface la and the outer peripheral surface 2 a thereof opposed to each other.
In an annular space defined by the outer race 1 and the inner race 2 , a plurality of torque transmitting members for transmitting torque between the two races, i.e., ground-shaped sprags 3 , are equally arranged in the circumferential direction of the annular space, and transmit the torque between the inner and outer races. The sprags 3 are held in substantially rectangular windows 8 provided in a pair of holders, i.e., an outer holder 5 and an inner holder 6 .
A ribbon spring 4 is disposed between the outer and inner holders 5 and 6 , and gives the sprags 3 a rising moment in a direction to mesh with an engagement surface. The grooves 20 shown in FIGS. 1 and 2 are formed in the cam surface 21 by which the sprags 3 mesh with the outer peripheral surface 2 a of the inner race 2 .
It is preferable in terms of cost that the grooves 20 be formed at a time when the sprags 3 are manufactured at the drawing-out step, but the grooves 20 can also be formed after the completion of the sprag 3 . Also, the grooves 20 are formed so as to extend over the entire axial width of the cam surface 21 of each sprag 3 , whereas they need not always be formed over the entire width, but can also be formed so as not to extend to the axial opposite ends of each sprag 3 .
Also, if a desired meshing property is obtained under a very low temperature, the number of the grooves 20 is arbitrary, and is not restricted to the shown number.
While the present invention has been described with respect to a one-way clutch having two holders, i.e., the outer holder and the inner holder, the present invention can also of course be applied to a one-way clutch of a type having a single holder.
FIGS. 4 and 5 show a case in which the present invention is applied to a one-way clutch of other type. FIG. 4 is a front view of one-way clutch of other type to which the present invention is applicable and FIG. 5 is a front view of a sprag used in the one-way clutch as shown in FIG. 4 . The one-way clutch 30 comprises a sprag 33 provided between inner and outer races to transmit torque, a wire gauge 32 for retaining the sprag 33 , a garter spring 31 fitted in a circumferential groove 35 (in FIG. 5 ) formed in the sprag 33 and a side plate 34 for supporting the sprag 33 in an axial direction. The inner and outer races are not shown.
As shown in FIG. 5 , the sprag 33 is provided with a plurality of grooves 37 extending in the axial direction on a cam surface 36 which is in contact with the inner race (not shown). Pitch and depth of the grooves 37 can be designed as in the grooves 20 , and the grooves 37 have substantially the same function as the grooves 20 . | A one-way clutch comprising an inner race and an outer race radially spaced apart from each other and concentrically disposed for rotation relative to each other, and a spray disposed between the inner race and the outer race for transmitting torque is characterized in that the cam surface of the sprag which contacts with the outer peripheral surface of the inner race is formed with a plurality of axially extending grooves. | 5 |
PRIORITY INFORMATION
[0001] This application claims priority to U.S. Provisional Patent Application No. 60/916,089 filed May 4, 2007, entitled “Garment Stain Treatment Bag,” the disclosure of which is incorporated by reference herein.
BACKGROUND
[0002] Embodiments of the present invention relate, in general, to a device for pre-treating a stain on fabric, and more particularly, to a portable enclosure for treating and transporting a garment.
[0003] Clothes can be easily stained from food, drink, oils or the like. In the past, soiled clothes may have been permanently stained unless they were immediately washed. There are now a number of commercial detergents and stain-removing formulas capable of removing stains from soiled clothes. However, it may not always be practical to immediately wash clothes. When traveling away from home, it can be even more impractical to immediately wash soiled clothes. In addition, if soiled clothes are not immediately washed, garments which come into contact with the soiled clothes may also be permanently stained.
[0004] Even with access to a sink and/or a washing machine, removing a stain from a soiled garment may be an unsanitary and unpleasant activity. For example, it may be preferred not to expose a kitchen sink to certain kinds of biological stains that may be on garments. As another example, the cleansers may irritate the skin, especially when kitchen gloves are not readily available.
[0005] While several devices and apparatuses have been made and used for pre-treating a stain on fabric, it is believed that no one prior to the inventors has made or used the invention described in the appended claims.
BRIEF DESCRIPTION OF THE FIGURES
[0006] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention, and, together with the general description of the invention given above, and the detailed description of the embodiments given below, serve to explain the principles of the present invention.
[0007] FIG. 1 is a front view of an exemplary embodiment of a stain treatment bag with graphical indicators prompting optimum treatment parameters.
[0008] FIG. 2 is a diagrammatic depiction of an alternate exemplary embodiment of a stain treatment bag with treatment regimes selected for the appropriate type of stain.
DETAILED DESCRIPTION
[0009] Turning to the Figures, wherein like numerals denote like components throughout the several views, in FIG. 1 , a stain treatment receptacle, depicted as a resealable bag 10 , provides a barrier for enclosing a garment 12 bearing a stain 14 . The garment may be an item of clothing, bedding, or any other item in need of stain treatment. The bag 10 may include an inner cavity sized to receive the garment 12 . The size of the bag 10 and the inner cavity may vary based on the garment 12 intended to be treated. The bag 10 is configured to prevent transfer of the stain 14 to other garments and to contain a pre-treatment cleanser 16 . The cleanser 16 may include or comprise chemicals that prevent setting of the stain 14 into the fabric, such as detergents or surfactants that assist a detergent or water in removing a stain, any other suitable compounds or materials, and combinations thereof. The pre-treatment cleanser 16 may be placed in the bag 10 ; however, in the illustrated version a barrier 18 affixes the pre-treatment cleanser 16 to an interior surface of the bag 10 . The barrier 18 may be configured to release the pre-treatment cleanser 16 in response to a stimulus provided by the user, including but not limited to introducing water into the bag 10 , compressing the barrier 18 , or rupturing the barrier 18 . The barrier 18 may be porous for instances in which the pre-treatment cleanser 16 is initially in a solid form until dissolved by water passing through the barrier 18 . Alternatively, the barrier 18 may be initially impermeable, but be either frangible and subject to rupture under user compression or dissolved upon introduction of water to the bag 10 .
[0010] The bag 10 includes a resealable opening 20 , such as those commonly used in bags referred to as ZIPLOC™ bags (made and manufactured by S.C. Johnson & Son, Inc.), although any suitable type of closure may be used, including, but not limited to an adhesively held flap, a snap, a button, a zipper, or combinations thereof. Printed instructions 22 on the bag 10 may be included, such as the depicted:
1. Insert Garment; 2. Fill with water at indicated temperature and seal bag; 3. Remove garment for laundering when indicator has dissolved.
Of course, other phrasing, terminology or appropriate instructions, including but not limited to the amount of water, may be used instead of or in addition to the instructions depicted in FIG. 1 . In addition, the steps may be performed in any suitable order. By way of example only, the user may fill the bag 10 with water prior to inserting the garment 12 . The instructions may also include the additional step of releasing the pre-treatment cleanser 16 , which may occur before or after the garment 12 has been inserted and before or after the bag 10 has been filled with water. Thereby, contact of the garment 12 with other garments is prevented, which may avoid transfer of the stain and exposure of skin to the stain 14 and the water. In addition, this embodiment may minimize contact with the pre-treatment cleanser 16 or avoid such contact completely.
[0014] Advantageously, in the illustrated embodiment, the bag 10 further includes a thermochromatic label 24 depicted as having three temperature indicators, TOO COLD 26 , CORRECT 28 , and TOO HOT 30 . The temperature indicators 26 , 28 , 30 may be configured to respond to a particular temperature range corresponding to the optimum temperature for the pre-treatment cleanser 16 . Of course, the thermochromatic label 24 may include any suitable number of temperature indicators. The thermochromatic label 24 may be configured to respond to the temperature of the water in the bag 10 .
[0015] In this version, the bag 10 further includes a completion indicator 32 configured to respond to the presence of the pre-treatment cleanser 16 to indicate when sufficient exposure time has elapsed for effective stain removal. The completion indicator 32 may be a material that is dissolved at a rate comparable to stain material. This approach may compensate for differences in water quality, such as mineral content in the water (i.e. hardness or softness of the water), and temperature that may vary the time required for stain removal. Accordingly, in an alternate embodiment, the bag may comprise a completion indicator without a thermochromatic label 24 . The completion indicator may alternatively be a thin-film imprinted circuit with dissimilar metal electrodes that produce sufficient electrical current when exposed to the water and/or the pre-treatment cleanser to initiate a timer to indicate completion. Of course any other suitable material or device, or combinations thereof, may be used for the completion indicator.
[0016] Although FIG. 1 depicts one particular arrangement, it will be appreciated that the above described elements, including the pre-treatment cleanser 16 and barrier 18 , the printed instructions 22 , the thermochromatic label 24 , and the completion indicator 32 may be configured and placed in any suitable arrangement in or on one or more inner or outer surfaces of the bag 10 .
[0017] Turning to FIG. 2 , an alternative garment stain treatment receptacle is depicted as a transparent resealable bag 40 that advantageously incorporates multiple selective stain treatment regimens as appropriate for the type of stain. In this embodiment, bag 40 includes printed instructions 42 . Printed instructions 42 may be configured to direct the user to the appropriate regimen. As shown in FIG. 2 , printed instructions 42 include the following steps:
1. Select Stain Type; 2. Crush Corresponding Ampoule; 3. Insert Garment; 4. Fill with Water at Indicated Temperature and seal bag; 5. Remove garment for laundering when indicator has dissolved.
Of course, other phrasing, terminology or appropriate instructions, including but not limited to the amount of water, may be used instead of or in addition to the instructions depicted in FIG. 2 . In addition, the steps may be performed in any suitable order. By way of example only, the user may fill the bag 40 with water prior to inserting the garment or the garment may be inserted prior to crushing the appropriate ampoule.
[0023] In the illustrated version, the transparent resealable bag 40 encompasses four stain-specific treatment assemblies. Of course, a bag 40 may comprise any suitable number of stain-specific treatment assemblies. As shown in FIG. 2 , first, a protein stain-specific treatment assembly 44 includes a label 46 such as “PROTEIN”. Label 46 may include additional or alternative information to assist in identifying this category of stain. In this embodiment, a frangible ampoule 48 containing protein-specific pre-treatment cleanser 50 is adhered to the bag 40 . Ampoule 48 may be retained within a permeable barrier 52 configured to capture the ampoule 48 after ampoule 48 is crushed to release cleanser 50 . Alternatively, instead of a frangible ampoule, a resilient ampoule or pouch may be directly adhered to the interior surface of the bag 40 . The resilient ampoule or pouch may include a weakened or loosely adhered area or opening and be configured to readily release the cleanser 110 under compression. Bag 40 may also include a protein-specific thermochromatic indicator 54 configured to assist in filling bag 40 with water of an optimum temperature for the protein-specific pre-treatment cleanser 50 . In the illustrated embodiment, a protein-specific completion indicator 56 is attached to bag 40 . The completion indicator 56 may be configured to help the user determine when subsequent laundering is appropriate. Thermochromatic indicator 54 and completion indicator 56 may be configured and operate similarly to thermochromatic indicator 24 and completion indicator 32 described above.
[0024] Second, in the embodiment shown in FIG. 2 , an oil stain-specific treatment assembly 64 includes a label 66 such as “OIL BASED”. Label 66 may include additional or alternative information to assist in identifying this category of stain. As shown, a frangible ampoule 68 containing oil-specific pre-treatment cleanser 70 is adhered to the bag 40 . Ampoule 68 may be retained within a permeable barrier 72 configured to capture the ampoule 68 after ampoule 68 is crushed to release cleanser 70 . Alternatively, instead of a frangible ampoule, a resilient ampoule or pouch may be directly adhered to the interior surface of the bag 40 . The resilient ampoule or pouch may include a weakened or loosely adhered area or opening and be configured to readily release the cleanser 70 under compression. In the illustrated embodiment, bag 40 includes an oil-specific thermochromatic indicator 74 configured to assist a user in filling bag 40 with water of an optimum temperature for the oil-specific pre-treatment cleanser 70 . As shown, bag 40 further includes an oil-specific completion indicator 76 , which may be configured to help the user determine when subsequent laundering is appropriate. Thermochromatic indicator 74 and completion indicator 76 may be configured and operate similarly to thermochromatic indicator 24 and completion indicator 32 described above.
[0025] As shown in FIG. 2 , bag 40 includes a tannin stain-specific treatment assembly 84 , which comprises a label 86 such as “TANNIN”. Label 86 may include additional or alternative information to assist in identifying this category of stain. In this embodiment, a frangible ampoule 88 containing tannin-specific pre-treatment cleanser 90 is adhered to the bag 40 , perhaps retained within a permeable barrier 92 to capture ampoule 88 after crushing. Alternatively, instead of a frangible ampoule, a resilient ampoule or pouch may be directly adhered to the interior surface of the bag 40 . The resilient ampoule or pouch may include a weakened or loosely adhered area or opening and be configured to readily release the cleanser 90 under compression. Bag 40 may include a tannin-specific thermochromatic indicator 94 , as shown in FIG. 2 , configured to assist a user in filling bag 40 with water of an optimum temperature for the tannin-specific pre-treatment cleanser 90 . In the illustrated embodiment, bag 40 further includes a tannin-specific completion indicator 96 , which may be configured to help the user determine when subsequent laundering is appropriate. Thermochromatic indicator 94 and completion indicator 96 may be configured and operate similarly to thermochromatic indicator 24 and completion indicator 32 described above.
[0026] The embodiment shown in FIG. 2 includes a fourth stain-specific treatment assembly, namely a dye-ink stain-specific treatment assembly 104 , which includes a label 106 such as “DYE-INK”. Label 106 may include additional or alternative information to assist in identifying this category of stain. In the illustrated version, a frangible ampoule 108 containing dye-ink-specific pre-treatment cleanser 110 is adhered to the bag 40 , perhaps retained within a permeable barrier 112 to capture the ampoule 108 after crushing. Alternatively, instead of a frangible ampoule, a resilient ampoule or pouch may be directly adhered to the interior surface of the bag 40 . The resilient ampoule or pouch may include a weakened or loosely adhered area or opening and be configured to readily release the cleanser 110 under compression. In this example, the bag 40 includes a dye-ink-specific thermochromatic indicator 114 configured to assist a user in filling bag 40 with water of an optimum temperature for the tannin-specific pre-treatment cleanser 110 . As shown, the bag 40 includes a dye-ink-specific completion indicator 116 which may be configured to help the user determine when subsequent laundering is appropriate. Thermochromatic indicator 114 and completion indicator 116 may be configured and operate similarly to thermochromatic indicator 24 and completion indicator 32 described above.
[0027] The embodiment shown in FIG. 2 includes stain-specific treatment assemblies for protein based stains, tannin based stains, oil based stains and dye-ink based stains. Of course, an embodiment may include a stain-specific treatment assembly for any suitable type of stain. Additionally, the one or more stain-specific treatment assemblies may be positioned on the bag in any suitable configuration or arrangement.
[0028] While the present invention has been illustrated by description of several embodiments and while the illustrated embodiments have been described in considerable detail, it is not the intention of the applicant to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications may readily appear to those skilled in the art.
[0029] For example, while the illustrated embodiments depict a transparent bag, alternate embodiments consistent with the present invention may employ a translucent or opaque material, or some combination thereof, in order to provide privacy.
[0030] For another example, rather than having one bag containing a plurality of stain-specific treatment regimens, applications consistent with aspects of the invention may employ stain-specific bags, perhaps sold in an assortment, to reduce the cost of each bag or for users who tend to encounter the same type of stains repeatedly (e.g., a work environment liable to encounter oil stains).
[0031] As an additional example, it should be appreciated that some applications consistent with the present invention may require no addition of water to the bag in order to prevent a stain setting into the garment. For instance, a sufficient liquid quantity of the pre-treatment cleanser may be released to treat the stain.
[0032] It should be appreciated that any patent, publication, or other disclosure material, in whole or in part, that is said to be incorporated by reference herein is incorporated herein only to the extent that the incorporated material does not conflict with existing definitions, statements, or other disclosure material set forth in this disclosure. As such, and to the extent necessary, the disclosure as explicitly set forth herein supersedes any conflicting material incorporated herein by reference. Any material, or portion thereof, that is said to be incorporated by reference herein, but which conflicts with existing definitions, statements, or other disclosure material set forth herein will only be incorporated to the extent that no conflict arises between that incorporated material and the existing disclosure material. | A stain treatment apparatus uses a transparent plastic bag with a recloseable opening into which a stained garment is placed. A stain treatment compound is contained within the bag, such as within an ampoule or pouch that releases upon compression or that releases upon exposure to water added to the bag. A thermochromatic indicator assists in filling with water of an appropriate temperature. A completion indicator further assists in indicating completion of the stain treatment regimen. A plurality of stain-specific treatment assemblies may be included that are optimized for a category of stains (e.g., protein, tannin, oil, dye/ink). | 3 |
FIELD OF THE INVENTION
The present invention relates to a disk device such as a magnetic disk device or an optical disk device and, in particular, to a disk device which is started for spin up to an access speed or operational speed from a motionless idle mode in which the device medium is motionless, with a small start current according to a predetermined method of starting the same.
BACKGROUND OF THE INVENTION
Miniaturization of computers has proceeded from desk-top size computers through lap-top and note-book sizes and even to pocketbook sizes, recently. With such miniaturization, commercially available magnetic disk devices have been miniaturized from 3.5 inches, through 2.5 inches and 1.8 inches and even to 1.3 inches. This tendency is also true for optical disk devices. In the following description, the term "disk device" incudes both magnetic disk devices and optical disk devices.
With the miniaturization of the disk device and devices to be mounted thereon, it has been desired to reduce the power consumption thereof. An example of such prior art techniques for reducing the power consumption of a magnetic disk device is disclosed in U.S. Pat. No. 4,933,785 (corresponding to Japanese Patent Application Publication No. 3-503101). In this technique, the operation mode is divided into a sleep mode in which circuit functions other than a minimum interface function for an up-link connection necessary for restart of the CPU are stopped; an idle mode in which the CPU is operative and other functions of the spindle motor circuit, a servo circuit and a recording and reproducing circuit, etc., other than the up-link connection function are stopped; and another idle mode in which the servo function for a rotating spindle motor is operative and the data recording and reproducing circuit as well as the usual write and read seek mode are inoperative. Accordingly, there are specific power supply requirements for the respective modes, and the power supplied to circuit portions which are not needed to function in a specific mode is reduced. In this method, however, there is no provision made for the reduction of the power source current required to be provided for the start time of a disk device including during the initial portion of a start period of a spindle motor from a state wherein the disk is not spinning.
In another example, there is a method disclosed in Japanese Patent Application laid-open No. H4-205963, wherein power consumption during re-start of a spindle motor is reduced by reducing the rotation speed of the spindle to an extent that its rotation can be maintained in an idle mode in which write and read is not performed. Although this method is effective to reduce power consumption without increasing the required time for re-start, there is still no provision made for sufficiently reducing the power source current required during the start time of the disk device spin up during the initial portion of the start period for spin up of a spindle motor powered disk device from a motionless state of the disk.
On the other hand, in consideration of providing an alternative approach to meeting the low power and high speed start up requirements for miniaturized devices, initial start software, such as an OS (operating system) of a computer, has been expanded and diversified as can be seen in, for example, UNIX, so that a memory device can be provided that has large memory capacity, which is required for storing such software information. Although semiconductor memory devices are suitable for large capacity storage and short initial start times, a magnetic disk device is still preferred since there is a high cost per memory capacity of such semiconductor memories, compared with that of magnetic disk devices.
SUMMARY OF THE INVENTION
In general, with miniaturization of computer devices, the power source has a relatively small current supply capacity and is designed for minimum space requirements while economically providing the required power. Therefore, in a compact disk device that is mounted on or used with such a compact computer device, the start time and seek and access time are to be short and the maximum required power source current capacity is to be small. On the other hand, however, a high speed spindle motor is required in order to shorten the spin up rotation wait time, which is a source or an increase in the motor start current. Maximum current consumption of such compact disk devices occurs during a start time of the disk device including an initial start period of the spindle motor when spin up occurs from a motionless idle mode in which the device medium is not spinning or when a seek operation occurs. In general, the start time is very long compared with that of the seek time. Since, therefore, shortening of the start time is more important than shortening the seek and access time, the maximum current required for the starting of the disk device becomes the required power source current capacity of the disk device although the start operation is a temporary and transient operation compared with that of the write/read and seek operation, which is the main and usual operation of the disk device. Therefore, when the required maximum start current (maximum disk drive current) is increased to shorten the start time, the required power source current capacity must be increased, resulting in the necessity of a large power source device.
An object of the present invention is, therefore, to provide a disk device and a method of start up for the disk device that solves the above mentioned problems of the conventional techniques, that can shorten the start time for the disk device without increasing the required power source current capacity of the computer power supply and that can alternatively reduce the required power source current capacity of the computer power supply without increase of start time.
Another object of the present invention is to provide a disk device and a start method therefor that provides high performance, that has a short initial start time, and that is relatively inexpensive.
A further object of the present invention is to provide a disk device and a start method therefor by which an upper (host) device, etc., connected thereto selects the minimum start time for bringing the disk device up to speed in consideration of the available current from the power source.
In order to achieve the above objects according to the present invention, the disk device connects to an external power source and has a spindle motor drive circuit, and an auxiliary power source that is rechargeable from the external power source. Also, recharging means for the auxiliary power source and further current adding means are provided for adding a current from the external power source to a current from the auxiliary power source during a predetermined period. The period in which the current is added includes at least an initial period of start up of rotation of the spindle motor during which the spindle motor start current becomes maximum. Also included are means for supplying the added current to the spindle motor drive circuit during the predetermined period.
In particular, the disk device includes a charge state detector for detecting the charge state of a rechargeable auxiliary power source or recharging information holding means for holding information concerning the state of the recharging, a plurality of start control procedures including spindle motor start procedures having different required maximum start up currents for starting spin up of the disk device and means for selecting and executing one of the start control procedures. According to the invention, a relatively small start current is used, when the amount of charge of the auxiliary power source is judged to be smaller than a predetermined amount on the basis of the detection result of the charge state detector or the stored recharging information; and a relatively large start current is used when the amount of charge of the auxiliary power source is judged to be equal to or in excess of the predetermined amount.
In one embodiment of the invention, a portion or all of the auxiliary power source is provided externally of the disk device and electrical connection means are provided for electrically connecting the external auxiliary power source to the current adding means and the recharging means in the disk device.
The required current capacity of the external power source during the start time of the device is set to be equal to or not larger than the required current capacity of the external power source during a seek time.
In another embodiment of the invention, the whole of the auxiliary power source, the recharging means (circuit) and the charge state detector or the recharging information holding means are provided externally of the disk device and means is included for electrically connecting the external auxiliary power source to the current adding means within the disk device.
The device of the invention also includes an indicator for indicating that the auxiliary power source is to be replaced by a new auxiliary power source on the basis of the charging/discharging life of the auxiliary power source. Alternatively, an indicator or detector can be provided to report the charging/discharging life of the auxiliary power source to a host device or other monitoring device.
The housing or configuration of the auxiliary power source is a rectangular-parallelepiped casing, wherein two of the three outer dimensions of the casing have larger values than that of the remaining outer dimension and wherein these dimensions are substantially the same as those of two of the three outer dimensions of the disk device casing which also have larger values than that of the remaining dimension. The casing of the disk device and the casing of the auxiliary power source are therefore preferably assembled together to form a PCMCIA card sized device, according to one of the standard sizes. Accordingly, the casings are connected so that the areas defined by the two (larger) outer dimensions, respectively, are juxtaposed to provide a substantially rectangular-parallelepiped shape outer face. Since an external rectangular-parallelepiped configuration of the assembled casings of the auxiliary power source and the disk device is the same as the so-called form factor size (standard size) of the incorporated casing of the disk device, that is, the same as the standard size such as 3.5 inches, 2.5 inches, 1.8 inches, the handling is convenient.
Further, according to the invention, a plurality of the disk devices can be provided to commonly use a single rechargeable auxiliary power source means provided externally of the device. Such a plurality of disk devices may be configured in a well known disk array.
It is another object of the invention that the disk device stores procedures or data necessary for an initial start up of a computer device to which it is connected.
In accordance with another aspect of the invention, one of a plurality of spindle motor start control procedures is selected including at least a first spindle motor start control procedure and a second spindle motor start control procedure, wherein a required start power source current of the disk device during an execution of the first spindle motor start control procedure is set larger than that during the seek operation, and wherein a required start power source current of the disk device during an execution of the second spindle motor start control procedure is set substantially equal to or smaller than that of the seek operation. Additionally, the required time for the spin up of the spindle motor according to the first spindle motor start control procedure is set shorter than that of the second spindle motor start control procedure.
The invention is also directed to the operation of the disk device in that, according to the present invention, a current supplied from the external power source is added to the current supplied from the auxiliary power source, which is recharged for a long time with a relatively small current, during a transient period including an initial period of the start of the spindle motor. Specifically, the spindle motor start current that is provided to the spindle motor becomes maximum when the added current is supplied to the current from the external power source. Therefore, during the start time of the spindle motor which requires a large start current, a shortage in the supply current from the main external power source can be supplemented by the rechargeable auxiliary power source and thus it is possible to shorten the start time (spin up time) by using an external power source having a relatively small capacity. Preferably, also, any reverse current from the auxiliary power source that might tend to flow to the external power source is prevented by a reverse current blocking device.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a block diagram construction of a magnetic disk device according to a first embodiment of the present invention.
FIG. 2 is a flow chart showing the operation of a spindle motor according to the first embodiment of the invention.
FIG. 3 is a graph showing the current of an external main power source when charging is sufficient, according to the first embodiment.
FIG. 4 is a graph showing the spindle motor drive current when charging is sufficient, according to the first embodiment.
FIG. 5(a) shows a graph of the recharge circuit current when charging is sufficient, according to the first embodiment.
FIG. 5(b) shows a graph of a voice coil motor drive circuit when charging is sufficient, according to the first embodiment.
FIG. 5(c) shows a graph of the signal processing and other circuits when charging is sufficient, according to the first embodiment.
FIG. 6 is a graph showing the current of an external main power source when charging is insufficient, according to the first embodiment.
FIG. 7 is a graph showing the spindle motor drive current when charging is insufficient, according to the first embodiment.
FIG. 8(a) shows a graph of the recharged circuit current when charging is insufficient, according to the first embodiment.
FIG. 8(b) shows a graph of a voice coil motor drive circuit when charging is insufficient, according to the first embodiment.
FIG. 8(c) shows a graph of the signal processing and other circuits when charging is insufficient, according to the first embodiment.
FIG. 9 is a perspective view of a magnetic disk device with an auxiliary power source, according to the present invention.
FIG. 10 is a block diagram construction of a computer device with which the disk device of the present invention can be used according to an embodiment of the invention.
FIG. 11 shows a block diagram construction of a magnetic disk device according to a second embodiment of the present invention.
FIG. 12 is a graph showing the current of an external main power source when charging is sufficient, according to a second embodiment of the invention.
FIG. 13 is a graph showing the current of the external power source when the present invention is not employed.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a construction of a magnetic disk device according to a first embodiment of the present invention. A magnetic disk device 1, such as a hard disk, is connected to an external power source 2, a rechargeable auxiliary power source 3 and an upper (host) device 4. The external power source is a usual commercial power source, such as a battery, etc., which is also used by the host device and is essentially the main or only power source in use except for the auxiliary power source 3.
An external main power source current (I EX ) 2a supplied from the external power source 2 through an input connector 2b. Internally, current (I EX ) 2a is branched to an input current (I OT ) 5a for a signal processing system and other circuits, an input current (I VCM ) 6a and an input current I LIM 9a. Input current 6a drives a voice coil motor drive system which includes a voice coil motor 7 and a head 8 ganged therewith that is controlled by a voice coil motor drive system circuit 6. Input current (I LIM ) 9a, which passes through current limiting and reverse current blocking circuit 9, is supplied to a driver circuit 10 for controlling the spindle motor 11 and a disk 12. Circuit 9 controls an upper limit of the current and the reverse current blocking is achieved through a reverse current blocking diode, for example.
Since the auxiliary power source is rechargeable, an input current (I CH ) 13a is supplied to a recharging circuit 13 for recharging the power source 3. A charge state detection circuit 14 detects a charge state of the rechargeable auxiliary power source 3 on the basis of an output voltage thereof or a stored operational history (number of charging cycles, for example) of the recharging circuit 13 and reports it to a controller 16.
An output current (I SB ) 3a is supplied from the rechargeable auxiliary power source 3 through the connector 3b to the magnetic disk device 1 and is added to the current I SPM through a current adder switch 15 for supplying the spindle motor drive circuit 10. The host device (CPU) 4 is connected to a device controller 16 of the magnetic disk device 1 to exchange data and control information. The device controller 16 responds to the charge state of the auxiliary power source 3 to select an appropriate start control procedure. A spindle motor drive control portion 17 responds to an instruction from the device controller 16 to control the start of rotation from a motionless idle mode in which the disk is not spinning and normal rotation of the spindle motor 11 and the disk 12 through the spindle motor drive circuit 10 according to either a high speed start control procedure 17a or a low speed, low current start control procedure 17b. A required rotation start current and a required start time for the low speed, low current start control procedure 17b are set to be about 1/2 and about twice those for the high speed start control procedure 17a, respectively. A current limiting value in the current limiting/reverse current blocking circuit 9 is set to a value which is substantially equal to but not smaller than the maximum required current for the low speed, small current start control procedure 17b. A power source current of the spindle motor drive control portion 17 is a portion of the current (I OT ) 5a.
FIG. 2 is a flowchart showing a start operation of the spindle motor in the disk device (embodiment 1) shown in FIG. 1. The magnetic disk device 1 is triggered by a start of the power supply from the external main power source or a start instruction from the host device 4 according to a predetermined start mode for starting the operation of the spindle motor (step 18). Then, the charge state is detected (step 19).
In order to detect the charge state, a non-volatile memory is provided in the charge state detection circuit 14 (FIG. 1) in which a recharging completion flag is set, i.e. which becomes "1" when a recharging of the rechargeable auxiliary power source 3 is completed and is reset, i.e. becomes "0" when discharging of the auxiliary power source 3 is started. The status of the flag is stored in the memory device and can be accessed by the device controller 16. In step 19, the charge state is detected on the basis of this recharging completion flag and a terminal voltage of the auxiliary power source 3. When the auxiliary power source 3 is recharged enough, the current adder switch 15 is turned ON (step 20), the recharging completion flag in the non-volatile memory circuit is reset (step 21) and the high speed start control procedure 17a is selected (step 22). When the charge state detection flag is "1" (step 19) indicating that the auxiliary power source is not recharged enough, the current adder switch 15 is held in OFF state and the low speed, low current start control procedure 17b is selected (step 23). Then, according to the selected start control procedure, a start control of the spindle motor is executed (step 24). After the execution of the start control procedure terminates (step 25), the current adder switch 15 is turned OFF (step 26), recharging of the rechargeable auxiliary power source 3 is started (step 27) and the start operation of the spindle motor has been completed (step 28).
The recharging operation is stopped after a predetermined time lapses from the start of recharging or when an overcharge voltage is detected. Then, the recharging completion flag is set to "1", a recharge cycle counter (not shown) provided for the purpose of knowing the remainder of the life of the auxiliary power source (battery) by referencing the number of recharge cycles is updated (+1) and stored as recharge cycle data in a recharge history memory portion provided in the non-volatile memory, accessible on demand.
It is possible to provide, in the controller 16, means, such as a comparator, which judges the charge/discharge life of the auxiliary power source on the basis of this recharge cycle data and, when it is judged that a remaining life of the auxiliary power source is less than an acceptable minimum, displays or reports to the host device that the auxiliary power source is to be replaced by a new one.
FIGS. 3, 4, 5(a) to 5(c) are graphs showing variations of the external main power source current I EX , the spindle motor drive circuit current I SPM , the recharge circuit current I CH , the voice coil drive circuit current I VCM and the signal system and other circuit current I OT , respectively for the condition when the charge state of the auxiliary power source is deemed sufficient.
In these figures, t0 denotes a start time point at which the rotation of the spindle motor is started, t2 a time point at which the start of acceleration of the spindle motor rotation is ended, t3 a time point at which the current adding switch 15 is turned OFF, t4 a time point at which recharge is started, t6 a time point at which the recharge is ended and t5 a time point at which the drive of the voice coil motor is started. Further, I LIM is an input current to the recharge limiting and reverse current blocking circuit and I SB is an output current from the rechargeable auxiliary power source 3. The external main power source current (I EX ) 2a is represented as follows.
I.sub.EX =I.sub.LIM +I.sub.CH +I.sub.VCM +I.sub.OT
Therefore, the current I EX in FIG. 3 has a wave form which is a combination of wave forms of the currents shown in FIGS. 4 and 5(a) to 5(c). The input current (I SPM ) 10a of the spindle motor drive circuit is represented as follows.
I.sub.SPM =I.sub.LIM +I.sub.SB
In FIG. 3 or 5(b), a period (in the order of several ms to 10 ms) in which pulsed current flows indicates a seek period and the magnitude of these pulses depends upon the seek distance. A current between respective pulse currents of the current I VCM (from t5) is a read/write period.
In the start period T1 of the spindle motor rotation, the external main power source (I EX ) 2a is only about a half of the input current (I SPM ) 10a of the spindle motor drive circuit and is set such that it is smaller than the maximum required current (I EX ) of the external main power source during the seek period. It is clear that this is the effect obtained by utilizing the output current (I SB ) 3a of the auxiliary power source.
Similarly, FIGS. 6, 7 and 8(a) to 8(c) are graphs showing variations of magnitudes of the currents I EX , I SPM , I CH , I VCM and I OT when, in the first embodiment, the recharge of the auxiliary power source is insufficient.
Although the start time period T2 30 shown in FIG. 6 of the spindle motor rotation in this case is about twice the start time period T1 29 of the spindle motor rotation for the case shown in FIG. 3 where the charge of the auxiliary power source is sufficient, the required current (I EX ) from the external main power source is unchanged and, therefore, it is smaller than the required current (I EX ) from the external main power source during the seek period. This results from selecting the low speed, low current start control procedure 17b instead of the high speed start control procedure 17a.
If the present invention is not used and it is impossible to select the low speed, low current start control procedure 17b, the current (I EX ) 2a of the external main power source becomes as shown in FIG. 13 and, therefore, the maximum required current (I EX ) of the external main power source occurs not in the seek period but in the start period T3 31 of the spindle motor rotation. Therefore, a large power source large enough to supply the maximum current shown in this period T3 31 has to be used as the external main power source. Comparing this, since, according to the first embodiment, the current I EX of the external main power source which is required in the start time T1 or T2 does not exceed the maximum current during the seek period and so a small external main power source 1 can be used as shown in FIGS. 3 and 6.
FIG. 9 is a perspective view of the magnetic disk device according to the first embodiment of the present invention. The aspect ratio of a form factor (standard size) of a projection (shown by a hatching in FIG. 9) of a casing of a hard disk device of any size, for example of a 5.25 inch disk, a 3.5 inch disk, a 2.5 inch disk, a 1.8 inch disk and a 1.3 inch disk. This is the so-called golden section ratio and the aspect ratios for the 3.5 inch disk is obtained by dividing that for the 5.25 inch disk by 2, that for the 2.5 inch disk by dividing that for the 3.5 inch disk by 2, that for the 1.8 inch disk by dividing that for the 2.5 inch disk by 2 and that for the 1.3 inch disk by dividing that for the 2.5 inch disk by 2. The size (mm×mm) of the projection (longitudinal length×lateral length) is 101.6× 146 for the 3.5 inch disk, 73×101.6 for the 2.5 inch disk, 50.8×73 for the 1.8 inch disk and 36.5×50.8 for the 1.3 inch disk. The size of the projection (longitudinal length×lateral length) of the casing of the rechargeable external auxiliary power source is made equal to the projection of the casing of the disk device for, for example, the 5.25 (or 3.5) inch disk and the casing of the rechargeable external auxiliary power source and the casing of the disk device are fixed in a stacked arrangement as shown in FIG. 9 by suitable electrical coupling means. With this construction, it is possible to couple up to two disk devices each for the 3.5 inch disk (or 2.5 inch disk), up to 4 disk devices for the 2.5 (or 1.8 inch) disk, up to 8 disk devices for the 1.8 inch (or 1.3 inch) disk and up to 16 disk devices for the 1.3 inch disk for a single external auxiliary power source, respectively, as shown in FIG. 9.
FIG. 10 shows a construction of a computer device that uses the disk device according to the first embodiment. An initial start program of the computer device is stored in a memory region on a disk surface of the magnetic disk device and read out from the magnetic disk device to a CPU of the computer device at a start time of the computer device (at this time, the disk device has been started already and brought up to operational speed).
In the embodiment of the invention as shown in FIG. 1, a portion or the whole portion of the rechargeable auxiliary power source 3 may be provided within the magnetic disk device 1, instead of providing the whole portion thereof externally as shown. Further, the recharge circuit 13 and the charge state detection circuit 14 may be provided externally of the magnetic disk device 1, instead of providing it within the device as shown in FIG. 1. Also as shown in FIG. 1, one or more additional magnetic disk devices 1' may be connected to the external main power source and rechargeable auxiliary power source as well as the host computer for the purpose of establishing a redundant array of disks, for example.
FIG. 11 shows a construction of a magnetic disk device according to a second embodiment of the present invention. In contrast to the first embodiment shown in FIG. 1, there is no rechargeable auxiliary power source 3, connector 3b, current limiting and reverse current blocking circuit 9, recharge circuit 13, charge state detection circuit 14 and current adder switch 15, which are omitted or removed. The other components which are in common with the FIG. 1 embodiment operate in the manner as discussed with respect to the FIG. 1 embodiment.
FIG. 12 shows the required current of the external power source of the magnetic disk device according to the second embodiment of the present invention. The required current 32a of the external power source is shown when the high speed start control procedure is selected and the required current 32b of the external power source is shown when the low speed, low current start control procedure is selected. According to this embodiment, the low speed, low current start control procedure 32b is selected when an upper host device drives a liquid crystal display and other peripheral devices and consumes a large amount of the power for the upper device, which is provided by the external power source; and the high speed start control procedure 32a is selected when the above and other peripheral devices are inoperative and power consumption is small, so that the capacity of the upper power source can be made small.
Although, in the above mentioned embodiments, about half of the input current I SPM of the spindle drive circuit at the start time is supplemented by the current I EX of the external main power source and the output current I SB of the auxiliary power source, the ratio can be changed and, when the capacity of the auxiliary power source 3 is large, a half of the current I SPM or more can be supplemented by the current I SB .
As described in detail hereinabove, according to the present invention, the following effects are obtained.
(1) A current supplied from the external power source is added to a current supplied from the auxiliary power source during a transient period including an initial period of a start up of rotation of the spindle motor and the combined current is supplied to the spindle motor drive circuit. Therefore, it is possible to provide a disk device in which the start time is substantially shortened by the amount of supply current provided by the auxiliary power source for the start operation including the start of the spindle motor without increasing the maximum required power source current. That is, by making the start current supplied to the spindle motor N times, the time required for starting rotation can be made substantially 1/N. Further, it is possible to realize a disk device having a smaller required power source current capacity or a small required power source current capacity during the starting of the disk device without increasing the start time.
(2) It is possible to start a disk device without substantially increasing the required power source current capacity and without fault due to a shortage of power source current capacity, although requiring a longer start time, by executing a start control requiring a smaller current than usual even when the rechargeable auxiliary power source is insufficiently charged due to frequently starting the disk device, for example.
(3) It is also possible to obtain the same effects as those mentioned in the items (1) and (2) without providing a mounting space for a rechargeable auxiliary power source in the disk device. Further, it is possible to start a disk device without substantial increase of the required power source current capacity and without fault due to short of power source current capacity either when an external power source is mounted or when it is separated.
(4) When a user confirms compatibility between a disk device and a current specification of an external power source to be used therefor by means of a drawing design, experiment or test, etc., it is unnecessary to pay special attention to the power source current characteristics during a start time of the device, which have an initial and transient time.
(5) It is further possible to obtain the same effects as those mentioned in the items (1) and (2) without providing a mounting space for a rechargeable auxiliary power source in the disk device. Further, it is possible to start a disk device without substantial increase of the required power source current capacity and without fault due to a shortage of power source current capacity either when an external power source is mounted or when it is separated.
(6) It is still further possible to preliminarily avoid a loss of the effect (1) due to the performance of the rechargeable auxiliary power source being degraded beyond its charge/discharge life, by exchanging the auxiliary power source on the basis of a display of the time at which the auxiliary power source is to be exchanged according to the host device.
(7) The mounting of the disk device on an upper host device is convenient since the form factor size thereof is unchanged regardless of position of the external auxiliary power source with respect to the disk device. In particular, the auxiliary power supply and disk device combination of the invention can be designed to fit together so that their combined dimensions are the same as a standard PC card, which permits interchange versatility with a variety of different sized computers.
(8) It is also possible to reduce a required space for the external auxiliary power source.
(9) An initial start of the computer device is completed within a short time. If necessary, the difference in start times selected in accordance with the considerations set forth above are transmitted to the CPU or host device in order to prevent any conflicts that might result while waiting for a longer start time to elapse, for example. | A disk device, such as an optical disk or magnetic disk, for a computer is mounted on the computer or inserted in a slot in the computer. The computer or host device provides a power supply for the disk device that is used to drive the disk in rotation and power the seek operation for read and write. When the disk device is in an idle mode in which the disk media is not spinning, the disk(s) must first be driven to the access speed of rotation during a spin up or start of rotation time period. The current supplied by the external main power source for the computer provides the start current for the spindle motor that drives the disk(s) in rotation. An auxiliary power source provides an additional current that is added to the current provided by the main power source to decrease the time in which the start operation is executed or to ensure start up when only a limited amount of current is available from the main power source. The auxiliary power source is rechargeable from the main power source, and the additional current from the auxiliary power source is not provided unless the charge state of the auxiliary power source is determined to be sufficient. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims the priority of Chinese Application No. 201010606635.8, filed on Dec. 24, 2010. The contents of the application are hereby incorporated by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates to biotechnology, and particularly to a method for isolating and purifying recombinant human serum albumin (rHSA) from transgenic rice grain on a large scale.
BACKGROUND OF THE INVENTION
Human serum albumin (HSA) is a single chain, non-glycosylated protein consisting of 585 amino acids, having a molecular weight of 66.5 kD and an isoelectric point between 4.7˜4.9. It is the most abundant protein in human blood plasma, making up about 60% of the total plasma proteins. There is about 40 g of HSA in per liter of human blood. Besides being present in the plasma, HSA is also found in tissues and body secretions, skins and lymph cavities. Under normal physiological conditions, HSA has an effect of maintaining plasma colloid osmotic pressure, nourishing, accelerating concrescence of wounds, and as a carrier, participating in transportation of many hydrophobic biological molecules such as hormones, biological active substances and drugs in the blood. Therefore, HSA is an important medical protein that is mainly used clinically for treatment of hypoproteinemia caused by loss of blood, burn, scald, plastic surgery and brain lesion, as well as for treatment of liver cirrhosis, hydronephrosis and so on. At present, HSA for clinical use is mainly prepared by extracting and isolating from human plasma. However, this preparation approach has the following disadvantages: on one hand, the source of plasma is insufficient, i.e. the limited blood supply is unable to meet the demands of production of HSA and the relevant preparations thereof; on the other hand, blood itself may potentially be a risk factor, for example it may contain dangerous infectious pathogens such as hepatitis virus, human immunodeficiency virus (HIV) and so on, which causes enormously concerns about the application of HSA extracted from plasma. Therefore, it is urgent to develop an alternative process to produce HSA.
With the development of modern DNA recombinant and synthesis techniques, researchers take a profound interest in the production and application of recombinant human serum albumin (rHSA). So far, various expression systems have been experimentally used for mass production of rHSA. For example, prokaryotes such as colon bacillus (Latta, M. et al., Bio/Technology, 5:1309-1314, (1987)), bacillus subtilis (Saunders, C. W. et al, J. Bacteriol. 169: 2917-2925, (1987)), eukaryotes such as yeasts (WO 00/44772, EP0683233A2, U.S. Pat. No. 5,612,196) and also cultivation of animal cells have been used for the production of rHSA. However, such approaches supra are not suitable for industrialized production either due to low expression level or high production cost. Chinese patent application No. 200510019084.4 of the present inventors discloses a method for producing rHSA using rice endosperm cells as bioreactor, comprising: using promoters and signal peptides specifically expressed in rice endosperm to mediate the entry of rHSA into endomembrane system of the endosperm cells of rice and store rHSA in the protein bodies of the rice endosperm, thus allowing rHSA to accumulate extensively in the rice grain and reach a higher expression level finally. The expression level of the obtained rHSA is at least above 0.3% based on the weight of the rice grain. The method has the advantages of high expression level and low cost, thereby it provides the possibility to develop a novel strategy for the production of protein drugs. The rHSA produced by any expression system should be purified before entering market. The purification technique may affect the quality of the product as well as production cost. The cost of purification process makes up about 80˜90% of the total production cost. At present, there is no purification process for separating and purifying rHSA from rice grain. Therefore, it is technically difficult and economically risky to develop a simple and cost-effective purification process to purify rHSA from rice grain. At present, the techniques for extracting rHSA from yeast and plant suspension cells have been reported. For example, Chinese patent application CN101768206A disclosed a process for purifying rHSA expressed in Pichia pastoris , comprising: filtrating the fermentation broth of rHSA with a ceramic membrane, and sequentially subjecting the filtrate to cation exchange chromatography, hydrophobic chromatography and weak anion exchange chromatography to obtain purified rHSA. However, due to the substantial differences of the impurities among the rice grain, yeast and plant suspension cells, those prior art can not be directly used for separating and purifying rHSA from rice grain. Therefore, it is desirable to develop a simple and effective process for separating and purifying rHSA from rice grain to produce rHSA with high yield and high purity, which would provide a basis for future industrialized production.
SUMMARY OF THE INVENTION
The object of the present invention is to provide a method for separating and purifying recombinant human serum albumin (rHSA) from rice grain on a large scale.
To achieve the above object, the present invention provides the following technical solutions:
A method for separating and purifying recombinant human serum albumin from rice grain, sequentially comprising the steps of:
1) subjecting crude extract of recombinant human serum albumin to cation exchange chromatography to obtain primary product I; 2) subjecting the primary product I to anion exchange chromatography to obtain secondary product II; 3) subjecting the secondary product II to hydrophobic chromatography to obtain purified recombinant human serum albumin.
In step 1), the cation exchange chromatography may be performed on a strong cation chromatography resin as chromatography media, which is selected from the group consisting of UNO Sphere S, Nuvia. S, Capto MMC, MacroPrep-CM. UNO Sphere S or Capto MMC is preferred.
The cation exchange chromatography may employ pH gradient elution or NaCl concentration gradient elution. The pH gradient elution is preferred.
In an embodiment, elution buffer for cation exchange chromatography comprises acetate buffer, 0.25M sodium chloride, with a pH of 5.2.
In step 2), the anion exchange chromatography may be performed on a strong anion chromatography resin as chromatography media, which is selected from the group consisting of UNOsphere Q, Q Sepharose fast flow (FF), and DEAE sepharose FF. Q Sepharose FF is preferred.
In an embodiment, elution buffer for anion exchange chromatography comprises phosphate buffer, 0.2M sodium chloride, with a pH of 7.5.
In step 3), the hydrophobic chromatography may be performed on a chromatography media selected from the group consisting of Phenyl sepharose HP, Phenyl sepharose FF, macro-prep t-butyl and macro-prep methyl. Phenyl sepharose HP is preferred.
The eluate containing the target protein from hydrophobic chromatography column can be prepared into finished product by known techniques such as ultra-filtration concentration and freeze-drying.
Further, the method may comprise a step of subjecting the secondary product II to Macro-prep ceramic hydroxyapatite chromatography prior to the hydrophobic chromatography of said step 3). That is to say, in such an embodiment, the secondary product containing the target protein was subjected to Macro-prep ceramic hydroxyapatite chromatography as step 3) and then hydrophobic chromatography to obtain purified target protein as step 4).
The ceramic hydroxyapatite chromatography may be performed on a chromatography media selected from the group consisting of Macro-prep ceramic hydroxyapatite Type I and Macro-prep ceramic hydroxyapatite Type II. Macro-prep ceramic hydroxyapatite type I is preferred.
In an embodiment, the loading buffer employed in cation exchange chromatography comprises acetate buffer, with a pH below 5.0.
An elution buffer for eluting the target protein employed in cation exchange chromatography may comprise either acetate buffer and sodium chloride, or phosphate buffer and sodium chloride, with a pH of 5.0˜6.7. Preferably, the concentration of sodium chloride is 0.25M and the pH of the elution buffer is 5.2.
In one embodiment, the cation exchange chromatography is performed on UNO Sphere S or Capto MMC, and the elution buffer comprising acetate buffer, 0.25M sodium chloride, with a pH of 5.2 or 6.7 is employed.
In one embodiment, the cation exchange chromatography is performed on nuvia S as chromatography media, and an elution buffer comprising acetate buffer, 0.25M sodium chloride, with a pH of 5.0 or 5.2 is employed.
In one embodiment, the cation exchange chromatography is performed on Capto MMC as chromatography media, and a washing buffer comprising acetate buffer, 1M sodium chloride, with a pH of 4.7 is employed to remove impurities; and an elution buffer comprising phosphate buffer, 1M sodium chloride, with a pH of 6.7 is employed to elute the target protein.
In one embodiment, the cation exchange chromatography is performed on MacroPrep-CM as chromatography media, and a washing buffer comprising acetate buffer, 1M sodium chloride, with a pH of 4.7 is employed to remove impurities; and an elution buffer comprising phosphate buffer, 0.1M sodium chloride, with a pH of 6.5 is employed to elute the target protein.
In one embodiment, the anion exchange chromatography is performed on Q Sepharose FF as chromatography media, and an elution buffer comprising phosphate buffer, 0.25M sodium chloride with a pH of 6.0˜7.0 is employed.
In one embodiment, the anion exchange chromatography is performed on DEAE sepharose FF as chromatography media, and a washing buffer comprising phosphate buffer, 0.1 M sodium chloride with a pH of 6.0˜7.0 is employed to remove impurities; and an elution buffer comprising phosphate buffer, 0.25M sodium chloride with a pH of 6.0˜7.0 is employed to elute the target protein.
In one embodiment, the rHSA-containing fraction to be purified by hydrophobic chromatography may further comprise ammonia sulfate. The concentration of ammonia sulfate may be from 0.1M to 1M.
In one embodiment, the hydrophobic chromatography is performed on Phenyl sepharose HP as chromatography media, and the concentration of ammonia sulfate in the rHSA-containing fraction to be purified is 0.4M.
In one embodiment, the hydrophobic chromatography is performed on Phenyl sepharose FF as chromatography media, and the concentration of ammonia sulfate in the rHSA-containing fraction to be purified is 0.1M.
In one embodiment, the hydrophobic chromatography is performed on MacroPrep-t-Butyl as chromatography media, and the concentration of ammonia sulfate in the rHSA-containing fraction to be purified is from 0.6M to 1.0M.
In one embodiment, the Macro-prep ceramic hydroxyapatite chromatography employs an elution buffer comprising phosphate buffer with a pH of 7.0˜7.5 to elute the target protein.
Said rHSA of the present invention can be prepared using endosperm cells of rice as bioreactor, which is disclosed in Chinese patent application No. 200510019084.4 filed by the present applicant. The rHSA expressed in the transgenic rice can be extracted by the method disclosed in Chinese patent application No. 201010597544.2 filed by the present applicant, which preferably comprises the steps of:
i) mixing milled transgenic rice containing rHSA with an extraction buffer in w/v (kg/1) ratio of 1:5, followed by extracting for 1˜1.5 hours at 55˜60° C. to obtain a mixture I; the extraction buffer comprises 10˜30 mM phosphate buffer, 10˜20 mM sodium acetate, 15˜30 mM ammonia sulfate and 5˜20 mM sodium caprylate, with a pH of 6.5˜8; ii) adjusting pH of the mixture I of step i) to 4.0˜4.5 and precipitating it for 3˜12 hours to obtain mixture II; iii) filtrating the mixture II of step ii) to remove starches or non-target proteins, and then collecting the filtrate to obtain a crude extract containing high concentration of rHSA.
In one embodiment, said filtrating comprising steps of filtrating by pressure filtration with a filter cloth type plate-frame filter, then filtrating by micro-filtration with a polyethersulfone hollow fiber membrane. The hollow fiber membrane has a pore size of 0.20 μm˜45 μm, preferably 0.22 μm.
The technical solutions according to the present invention have the following advantages:
1. In respect to relatively high content of pigments and polysaccharides in rice grain, cation exchange chromatography is used as the first step in the present invention to effectively enhance the loading capacity for capturing or binding rHSA, which increases the chromatographic efficiency. In contrast, if anion exchange chromatography is used as the first step, the loading capacity for capturing rHSA is only about 20% of the theoretical capacity. Meanwhile, both UNO Sphere S and Capto-MMC have characters of excellent stability and a long lifetime even in sodium hydroxide, which extends the depreciation period of the chromatography media and simplifies the sanitization operation in the present invention, and finally reduces the cost of the target product.
2. Anion exchange chromatography is used as the second step in the present invention. After optimizing the elution conditions, above 80% of the non-target proteins in rice grain could be removed, thereby effectively eliminating the non-target proteins and recovering rHSA. Since the pigments and polysaccharides have been removed from the rice grain in the first step by cation exchange chromatography, their influence on loading capacity and purification efficiency in the anion exchange chromatography has been eliminated.
3. Macro-prep ceramic hydroxyapatite chromatography is used as the third step in the present invention to eliminate the dimer and polymers because of more dimers or polymers could cause allergenic when rHSA is used as injection medicine. This step improves markedly the purity, which meets the requirement of high purity for clinical application or more.
4. Hydrophobic chromatography is used as the final step in the present invention. After the three-step chromatographic procedure, the HPLC purity of the target product can reach about 99.0%.
DESCRIPTION OF DRAWINGS
FIG. 1 is an image of SDS-PAGE of fractions obtained from cation exchange chromatography performed on different chromatography media as primary purification, wherein A: UNOsphere S media, B: Nuvia S media, C: Capto MMC media and D: MacroPrep-CM media.
FIG. 2 shows a comparison diagram of the loading capacity (volume) for the rHSA extract between Nuvia S media and UNO Sphere S media at different flow rate (300 cm/h, 600 cm/h).
FIG. 3 is an image of SDS-PAGE of fractions obtained by anion exchange chromatography performed on different chromatography media as primary purification, wherein A: UNO Sphere Q media, B: Q Sepharose FF media.
FIG. 4 is a change chart showing the loading capacity for the rHSA extract of Q Sepharose FF media and the content of polysaccharides in the rHSA extract pre or after dialysis.
FIG. 5 is an image of SDS-PAGE of fractions obtained by anion exchange chromatography performed on different chromatography media as secondary purification, wherein A: Q Sepharose FFmedia, B: DEAE sepharose FF media.
FIG. 6 is an image of SDS-PAGE of fractions obtained by hydrophobic chromatography performed on different chromatography media as final purification, wherein A: Phenyl Sepharose HP media, B: Phenyl Sepharose FF media, C: Macro Prep-t-Butyl media.
FIG. 7 is an image of SDS-PAGE of eluate fractions obtained by sequentially subjecting crude rHSA extract to cation exchange chromatography, anion exchange chromatography and hydrophobic chromatography, performed on UNOsphere S(A), Q Sepharose FF(B) and Phenyl Sepharose HP(C) as chromatography media, respectively.
FIG. 8 is an HPLC chromatogram of the purified rHSA product (HPLC-SEC) obtained according to one embodiment of the present invention.
FIG. 9 is an image of SDS-PAGE of eluate fractions obtained by performing ceramic hydroxyapatite chromatography on Macro-prep Ceramic hydroxyapatite Type I media.
FIG. 10 is an HPLC chromatogram of the purified rHSA product obtained according to another embodiment of the present invention.
FIG. 11 is an image of SDS-PAGE of eluate fractions obtained by sequentially performing ceramic hydroxyapatite chromatography on Macro-prep Ceramic hydroxyapatite Type II media and hydrophobic chromatography on Phenyl Sepharose HP media.
FIG. 12 is an HPLC chromatogram of the purified rHSA product obtained according to another embodiment of the present invention.
In the above figures, S: loading sample, FT: transmission fluid, Elu: the rHSA-containing eluate, Elu 1: non-target protein eluate, Elu 2: rHSA eluate, CIP: cleaning-in-place fraction.
DETAILED DESCRIPTION OF THE INVENTION
The features and advantages of the present invention can be further understood from the following examples. The examples are illustrative only and should not to be construed as limiting the invention in any way.
Selection of Chromatography Media and Elution Conditions in Cation Exchange Chromatography
The present invention defines the chromatography media of a cation exchange resin as having a high working flow rate, including UNO Sphere S, Nuvia S, Capto MMC and etc. manufactured by Bio-RAD.
It is found by experiments that each of Capto MMC, Nuvia S and UNO Sphere S can be used for purification of rHSA. Capto MMC has the best effect on the protein purification, followed by UNO Sphere S and Nuvia S. There are no significant difference between the effects on protein purification of Nuvia S and UNO Sphere S. However, under the same working flow rate conditions, the loading capacity of UNO Sphere S is 1.5 times larger than that of Capto MMC; UNO Sphere S has a same working flow rate as Capto MMC; UNO Sphere S has excellent stability even in high concentration of sodium hydroxide and has better cleaning process, longer working lifetime and lower cost in comparison to Capto MMC.
Nuvia S and UNO Sphere S have similar properties but have difference in extention of ligands and matrix particle sizes. Under their respective optimal working flow rate, the loading capacity of Nuvia S is 1.4 times larger than that of UNO Sphere S; however, the working flow rate of Nuvia S is about a half smaller than that of UNO Sphere S. Instead, UNO Sphere S has larger loading capacity than Nuvia S at the same flow rate, and both of them have almost equivalent purification capability.
In view of the various factors, UNO Sphere S is preferably used as chromatography media for cation exchange chromatography.
The rHSA-containing extract is loaded on a column packing UNO Sphere S at a relatively low pH (pH=4.4) to ensure that rHSA can be completely absorbed on the media, and then eluted by pH gradient elution buffers and NaCl gradient elution buffers respectively to learn the basic elution conditions.
The results suggests that in pH gradient elution, the rHSA absorbed on the UNO Sphere S column is slightly desorbed when the pH of the elution buffer is above 5.5, indicating that the pH of loading buffer should not be higher than 5.5; when the pH of the elution buffer is 5.68, rHSA is completely desorbed from the column. Thus rHSA on the UNO Sphere S column is very sensitive to pH gradient elution.
In NaCl concentration gradient elution, the target protein rHSA is desorbed when the concentration gradient is from 35% to 60% 1M sodium chloride (NaCl), thus indicating that rHSA on the UNO Sphere S column is not sensitive to NaCl concentration gradient elution. The results demonstrate that both pH gradient and NaCl gradient can be used to elute the rHSA. Moreover, pH gradient elutes rHSA with more sensitivity and smaller volume of elution buffer. In contrast, NaCl gradient can not easily elute the rHSA, and requires high concentration of NaCl and larger volume of elution buffer.
Considering from purification efficiency and recovery rate, the preferred elution buffer is a phosphate buffer (pH 5.2) containing 0.25M NaCl.
Selection of Chromatography Media and Elution Conditions for Anion Exchange Chromatography
Like a cation exchange resin, an anion exchange resin can also be used for purification of rHSA. The present invention defines the chromatography media of an anion exchange resin as having a high flow rate and a high loading capacity, including UNOsphere Q, Q Sepharose FF, DEAE sepharose FF and etc.
It is found by experiments that each of UNOsphere Q, Q Sepharose FF and DEAE sepharose FF can be used for purification of rHSA. UNOsphere Q has a faster flow rate than Q Sepharose FF, but Q Sepharose FF has better purification efficiency than UNOsphere Q; while DEAE Sepharose FF has similar purification efficiency but a slower flow rate compared to Q Sepharose FF.
As described above, as a chromatography media for cation exchange chromatography, UNO-sphere S has a slightly poorer purification capability than Capto MMC. However, it is demonstrated by experiments that this adverse effect can be eliminated by the improvement of systematic purification capability. UNO-sphere S will not cause adverse effect on the subsequent anion exchange chromatography. In a preferred embodiment, Q sepharose FF is preferably used as the chromatography media for anion exchange chromatography and the elution buffer for eluting target protein comprises phosphate buffer and 0.2M NaCl, with a pH of 6.8.
Determination of the Order of Anion- and Cation-Exchange Chromatography
Both anion- and cation-exchange chromatography can be used as the primary purification of rHSA, however, it is found by experiments that when Q Sepharose FF anion exchange resin is used in the primary purification step, its loading capacity is far lower than the theoretical capacity. It may be associated with the soluble polysaccharides and nucleic acids largely present in rice grain. Because the soluble polysaccharides and nucleic acids contain negative charges may bind to Q Sepharose FF to reduce its loading capacity. It is demonstrated by experiments that the content of the soluble polysaccharides in rHSA extract can be reduced by dialysis, thereby increasing the loading capacity of Q Sepharose FF.
In contrast, cation exchange chromatography media such as UNO sphere S, Nuvia S and Capto MMC does not bind to the soluble polysaccharides or nucleic acids, avoid causing a decrease in the loading capacity. Therefore, cation exchange chromatography is determined as the primary purification and anion exchange chromatography is determined as the secondary purification in the present invention.
Selection of Chromatography Media for Hydrophobic Chromatography
The present invention employs various hydrophobic chromatography media with the similar properties for the purification step, including Phenyl sepharose HP, Phenyl sepharose FF (LS), macro-prep t-butyl and macro-prep methyl.
Phenyl sepharose HP has a strong hydrophobic property and excellent purification capability. The capability to remove the most non-target proteins and other impurities from the crude extract is critical to the purification efficiency; however, there is some inconvenience in the application of this chromatography media due to its fine particle size, low flow rate and special working mode.
Compared to Phenyl sepharose HP, Phenyl sepharose FF (LS) has the same ligand and matrix, but different diameter of the spherical matrix and different density of the ligand. The average particle size of the matrix of Phenyl sepharose FF (LS) is 3 times larger than that of Phenyl sepharose HP, and thus the former has a higher working flow rate. When used in the production of rHSA, it can shorten the production period. MacroPrep-Butyl has a weaker hydrophobicity than both Phenyl sepharose FF and Phenyl sepharose HP, while Macro-prep methyl has an even weaker hydrophobicity than MacroPrep-Butyl. Phenyl sepharose FF is performed experimentally at the same working mode as Phenyl sepharose HP to collect transmission fluid. In the selection of the concentration of salt in the loading sample, when the sample is loaded with an equilibration buffer (25 mM PB, 0.5M (NH 4 ) 2 SO 4 , pH 6.8) and eluted with 100% water, it is found that more than 50% of rHSA are retained on the column. As a result the salt concentration of the equilibration buffer should be reduced.
The samples filtrated by UNO sphere S and Q sepharose FF column are added with ammonia sulfate to adjust the concentration of ammonia sulfate to 0.2M and 0.1M, respectively prior to loading on a Phenyl sepharose FF (LS) column. The transmission fluid and pure water eluate are collected to perform SDS-PAGE detection. The results show that Phenyl sepharose FF (LS) has stronger hydrophobicity than Phenyl sepharose HP and has better effect to eliminate the non-target proteins in the sample even when the concentration of ammonia sulfate in the loading sample is as low as 0.1M. The product obtained by Phenyl sepharose FF (LS) has a purity of 93.5%. However, still 30% of rHSA is lost on the Phenyl sepharose FF(LS) column. The above experiment is performed using sodium chloride instead of ammonium sulphate, the similar results are obtained. Though the loss of rHSA on the column is reduced, the HPLC purity of the product is still about 93%.
The samples filtrated by UNO sphere S and Q sepharose FF column are added with ammonia sulfate to adjust the concentration of ammonia sulfate to 1M, 0.8M or 0.6M respectively, prior to loading on a macro-prep t-butyl and macro-prep methyl column. The transmission fluid and pure water eluate are collected to perform SDS-PAGE detection. The results show that macro-prep t-butyl and macro-prep methyl has poor hydrophobicity. Both of them have poor purification capability on rHSA, and the obtained rHSA has a purity of 90% by HPLC.
To select which Macro-prep ceramic hydroxyapatite Type I or Type II, we compared two types of Macro-prep ceramic hydroxyapatite from Bio Rad. We found the Macro-prep ceramic hydroxyapatite type I is much better than type II. After Macro-prep ceramic hydroxyapatite type I chromatography, the monomer content can reach up to 98.998%. As described above, though the other chromatography media has the advantage of fast working flow rate over Phenyl sepharose HP, they could not achieve the comparable purification efficiency to Phenyl sepharose HP. Phenyl sepharose HP has a relative low working rate, but can ensure that the target protein has a purity of more than 98%. Thus Phenyl sepharose HP is preferably used as the media for hydrophobic chromatography.
EXAMPLES
Materials and Instruments
Filter cloth type plate-frame filter press, type: XMS4/500-UB, manufactured by Shanghai Tianli Filter Press Co., Ltd (China); 0.20 μm hollow fiber column, available from Huzhou Kelu Membrane Technology Co., Ltd. (China);
UNO Sphere S, nuvia S, Capto MMC, MacroPrep-CM, MacroPrep-methyl, MacroPrep-Butyl media, available from BIO-RAD (US);
Q sepharose, Phenyl sepharose HP, Phenyl sepharose FF, DEAE-sepharose FF media, available from GE Healthcare (US);
C10/10, XK16/20 chromatography column, available from GE Healthcare (US) Biological 15/200 chromatography column, available from BIO-RAD (US)
Example 1
Extraction of rHSA from Transgenic Rice Grain
Transgenic rice could be prepared according to the method disclosed in Chinese patent application No. 200510019084 of the present inventors. The paddy rice was hulled to obtain half-polished rice and then grinded to obtain milled rice with a fineness of 80˜100 mesh. The milled rice was mixed with an extraction buffer in a ratio of 1:5 (w/v, kg/L) and extracted for 1.5 hours at 60° C. The extraction buffer comprises 25 mM phosphate buffer, 20 mM sodium acetate, 10 mM ammonium sulfate, 10 mM sodium caprylate, and has a pH of 7.5. The resultant mixture was adjusted to pH 4.5 with acetic acid and placed for at least 3 hours to precipitate non-target proteins. Then the resultant mixture was sequentially subjected to pressure filtration using a plate-frame press filter (filter cloth type) and micro-filtration by hollow fiber column with a pore size of 0.22 μm, to obtain supernatant containing rHSA. The concentration of rHSA was about 0.66 mg/mL.
Example 2
Cation Exchange Chromatography as Primary Purification
1. Cation Exchange Chromatography Performed on UNO Sphere S Media
A XK16/100 column was packed with about 8.7 ml of UNO Sphere S media and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid was added to adjust the pH to 4.5) at a flow rate of 300 cm/h until the pH of the effluent was stable. 250 ml of the rHSA extract sample obtained in example 1 was loaded on the column at a flow rate of 600 cm/h. The sample has a conductivity of 6.1 ms/cm and a pH of 4.53. After loading, the sample was eluted with an elution buffer (sodium acetate 2 g/L, acetic acid, pH 5.2, sodium chloride 14.61 g/L) at a flow rate of 300 cm/h. The eluate was collected and viewed by SDS-PAGE to obtain the fractions containing rHSA. The electrophoretogram was shown in FIG. 1A .
2. Cation Exchange Chromatography Performed on Nuvia S Media
A XK16/100 column was packed with about 9.3 ml of Nuvia S media and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid was added to adjust the pH to 4.5) at a flow rate of 300 cm/h until the pH of the effluent was stable. 250 ml of the rHSA extract sample obtained in example 1 was loaded on the column at a flow rate of 300 cm/h. The sample has a conductivity of 6.3 ms/cm and a pH of 4.56. After loading, the sample was eluted with an elution buffer (sodium acetate 2 g/L, acetic acid, pH 5.0, sodium chloride 14.61 g/L) at a flow rate of 300 cm/h. The eluate were collected and viewed by SDS-PAGE to obtain the fractions containing rHSA. The electrophoretogram was shown in FIG. 1B .
3. Cation Exchange Chromatography Performed on Capto MMC Media
A XK16/100 column was packed with about 15.1 ml of Capto MMC media and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid was added to adjust the pH to 4.5) at a flow rate of 300 cm/h until the pH of the effluent was 4.5 and stable. 250 ml of the rHSA extract sample obtained in example 1 was loaded on the column at a flow rate of 600 cm/h. The sample has a conductivity of 6.3 ms/cm and a pH of 4.56. After loading, the sample was eluted with elution buffer (sodium acetate 2 g/L, acetic acid, pH 4.7, sodium chloride 58.44 g/L) at a flow rate of 300 cm/h to remove impurities and then eluted with elution buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 58.44 g/L, pH 6.7) to obtain the rHSA-containing fractions. The electrophoretogram was shown in FIG. 1C .
4. Cation Exchange Chromatography Performed on Macroprep-CM Media
A XK16/100 column was packed with about 10 ml of MacroPrep-CM media and equilibrated with 300 ml of equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid was added to adjust the pH to 4.5) at a flow rate of 200 cm/h until the pH of the effluent was 4.5 and stable. 250 ml of the rHSA extract sample obtained in example 1 was loaded on the column at a flow rate of 300 cm/h. The sample has a conductivity of 6.3 ms/cm and a pH of 4.56. After loading, the sample was washed with washing buffer (sodium acetate 2 g/L, acetic acid, pH 4.7, sodium chloride 58.44 g/L) at a flow rate of 200 cm/h to remove impurities and then eluted with elution buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 5.84 g/L, pH 6.5) to obtain the rHSA-containing fractions. The electrophoretogram was shown in FIG. 1D .
5. Comparison of the Loading Capacity Between Nuvia S Media and UNO Sphere S Media
Two XK16/100 columns were packed with about 5 ml of Nuvia S and UNO Sphere S media respectively and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid was added to adjust the pH to 4.5) at a flow rate of 300 cm/h until the pH of the effluent was 4.5. The rHSA extract sample obtained in example 1 was loaded on the Nuvia S column and UNO Sphere S column at a flow rate of 300 cm/h, respectively. Absorption value of UV280 during the sample loading was recorded until the absorption value beyond plateau by 10%. The sample volume was recorded and the actual loading capacity per milliliter of Nuvia S or UNO Sphere S at a flow rate of 300 cm/h was calculated, respectively.
Further, the UNO Sphere S column was equilibrated with equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid was added to adjust the pH to 4.5) at a flow rate of 300 cm/h until the pH of the effluent was 4.5. The rHSA extract obtained in example 1 was loaded on the UNO Sphere S column at a flow rate of 600 cm/h and absorption value of UV280 during the sample loading was recorded until the absorption value beyond plateau by 10%. The sample volume was recorded and the actual loading capacity per milliliter of UNO Sphere S at a flow rate of 600 cm/h was calculated. The comparison of loading capacity was shown in FIG. 2 .
Example 3
Anion Exchange Chromatography as Primary Purification
1. Anion Exchange Chromatography Performed on UNO Sphere Q Media
A Biological 15/200 column was packed with a bout 10 ml of UNO Sphere Q media and equilibrated with 200 ml of equilibration buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium hydroxide or hydrochloric acid was added to adjust the pH to 7.5) at a flow rate of 300 cm/h until the pH of the effluent was 7.5. 250 ml of the rHSA extract sample obtained in example 1 was adjusted to pH 7.5 and diluted with the buffer until the conductivity was less than 10.0 ms, and then loaded on the UNO Sphere Q column at a flow rate of 300 cm/h. The sample was washed with washing buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 11.68 g/L) to remove impurities and then eluted with elution buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 23.36 g/L) to collect the rHSA-containing fractions. The electrophoretogram was shown in FIG. 3A .
2. Anion Exchange Chromatography Performed on Q Sepharose FF Media
A Biological 15/200 column was packed with about 10 ml of Q Sepharose FF media and equilibrated with 200 ml of equilibration buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium hydroxide or hydrochloric acid was added to adjust the pH to 7.0) at a flow rate of 300 cm/h until the pH of the effluent was 7.0. 250 ml of the rHSA extract sample obtained in example 1 was adjusted to pH 6.8 and diluted with the buffer until the conductivity was less than 10.0 ms/cm, and then loaded on the Q Sepharose FF column at a flow rate of 300 cm/h. The sample was eluted with elution buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 5.84 g/L) to collect the rHSA-containing fractions. The electrophoretogram was shown in FIG. 3B .
3. Testing for Actual Loading Capacity of Q Sepharose FF
A 10/100 column was packed with about 5 ml of Q Sepharose FF media and equilibrated with 200 ml of equilibration buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium hydroxide or hydrochloric acid was added to adjust the pH to 7.0) at a flow rate of 300 cm/h until the pH of the effluent was 7.0 and stable. 250 ml of the rHSA extract sample obtained in example 1 was adjusted to pH 7.5 and diluted with the buffer until the conductivity was less than 10.0 ms/cm and the total volume was 1000 ml. The sample was loaded on the Q Sepharose FF column at a flow rate of 300 cm/h. Absorption value of UV280 during the sample loading was recorded until the absorption value beyond plateau by 10%. The sample volume was recorded and the actual loading capacity per milliliter of Q Sepharose FF at a flow rate of 300 cm/h was calculated. Then the resin was regenerated.
The rHSA extract sample obtained in example 1 was adjusted to pH 7.0 and diluted with the buffer until the conductivity was less than 10.0 ms and then concentrated to 400 ml via GE 30 KD membrane cassette. Sulphuric acid-phenol method was used to determine the content of polysaccharides before and after dialysis. Then the sample was loaded on an equilibrated Q Sepharose FF column. Absorption value of UV280 during the sample loading was recorded until the absorption value beyond plateau by 10%. The sample volume was recorded and the actual loading capacity per milliliter of Q Sepharose FF at a flow rate of 300 cm/h was calculated. The change of loading capacity and the change of the content of polysaccharides were shown in FIG. 4 .
Example 4
Anion Exchange Chromatography as Secondary Purification
The rHSA-containing fraction obtained in example 2 was divided into two equal parts for use in the following experiments.
1. Anion Exchange Chromatography Performed on Q Sepharose FF Media
A 15/200 column was packed with about 7 ml of Q Sepharose FF and equilibrated with 200 ml of equilibtration buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium hydroxide or hydrochloric acid was added to adjust the pH to 7.0) at a flow rate of 300 cm/h until the pH of the effluent was 7.0. One part of the above fraction was adjusted to pH 7.0 and diluted with the buffer until the conductivity was less than 10.0 ms. The sample was loaded on the Q Sepharose FF column at a flow rate of 300 cm/h and then eluted with elution buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 11.68 g/L) to collect the rHSA-containing fractions. The electrophoretogram was shown in FIG. 5A .
2. Anion Exchange Chromatography Performed on DEAE Sepharose FF Media
A Biological15/200 column was packed with about 8 ml of DEAE Sepharose FF and equilibrated with 200 ml of equilibration buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, with sodium hydroxide or hydrochloric acid added to adjust the pH to 7.0) at a flow rate of 300 cm/h until the pH of the effluent was 7.0. Another part of the above fraction was adjusted to pH 7.5 and diluted with the buffer until the conductivity was less than 10.0 ms. The sample was loaded on to the DEAE Sepharose FF column at a flow rate of 300 cm/h and then eluted with elution buffer (sodium dihydrogen phosphate 0.3 g/L, disodium hydrogen phosphate 3.5 g/L, sodium chloride 11.68 g/L) to collect the rHSA-containing fractions. The electrophoretogram was shown in FIG. 5B .
Example 5
Hydrophobic Chromatography as Final Purification
1. Hydrophobic Chromatography Performed on Phenyl Sepharose Hp Media
A XK16/100 column was packed with about 8 ml of Phenyl sepharose HP and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2.32 g/L, sodium dihydrogen phosphate 2.81 g/L, ammonium sulfate 66 g/L) at a flow rate of 100 cm/h. 20 ml of the rHSA-containing fraction obtained in example 4 (Q Sepharose FF) was added with ammonium sulfate (0.4M) to make the conductivity be 80.0 ms. Then the sample was loaded on the column at a flow rate of 100 cm/h. The transmission fluid was collected to obtain the rHSA-containing fractions. The electrophoretogram was shown in FIG. 6A .
2. Hydrophobic Chromatography Performed on Phenyl Sepharose FF Media
A XK16/100 column was packed with about 10 ml of Phenyl sepharose FF and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2.32 g/L, sodium dihydrogen phosphate 2.81 g/L, ammonium sulfate 13.2 g/L) at a flow rate of 150 cm/h. 20 ml of the rHSA-containing fraction obtained in example 4 (Q Sepharose FF) was added with ammonium sulfate (0.1M) to make the conductivity be 80.0 ms. Then the sample was applied to the column at a flow rate of 150 cm/h. The transmission fluid was collected to obtain the rHSA-containing fractions. The electrophoretogram was shown in FIG. 6B .
3. Hydrophobic Chromatography Performed on Macroprep-T-Butyl Media
A 15/200 column was packed with about 6 ml of MacroPrep-t-Butyl and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2.32 g/L, sodium dihydrogen phosphate 2.81 g/L, ammonium sulfate 13.2 g/L) at a flow rate of 150 cm/h. 20 ml of the rHSA-containing fraction obtained in example 3 (Q Sepharose FF) was added with ammonium sulfate (1.0 M, 0.8 M, 0.6M, respectively) to make the conductivity be 130.0 ms, 90.0 ms, 70.0 ms, respectively. Then the samples were applied to the columns at a flow rate of 150 cm/h. The transmission fluid was collected to obtain the rHSA-containing fractions. The electrophoretogram was shown in FIG. 6C .
Example 6
Separation and Purification of rHSA from the rHSA-Containing Extract
Step 1): Cation Exchange Chromatography Performed on UNO Sphere S as Primary Purification
An XK16/20 column was packed with about 12 ml of UNO Sphere S media and equilibrated with 500 ml of equilibration buffer (anhydrous sodium acetate 2 g/L, acetic acid, pH 4.5) at a flow rate of 300 cm/h. 300 ml of the rHSA-containing extract sample obtained in example 1 was loaded on the column at a flow rate of 600 cm/h. The sample has a conductivity of 6.5 ms/cm and a pH of 4.5. After loading, the sample was eluted with elution buffer (sodium acetate 2 g/L, acetic acid, pH 5.0, sodium chloride 14.61 g/L) at a flow rate of 200 cm/h. The eluate were collected and observed by SDS-PAGE to obtain the fractions containing rHSA. The electrophoretogram was shown in FIG. 7A .
Step 2): Anion Exchange Chromatography Performed on Q Sepharose FF as Secondary Purification
An XK16/100 column was packed with about 13 ml of Q Sepharose FF media and equilibrated with 400 ml of equilibration buffer (anhydrous sodium acetate 6.51 g/L, sodium dihydrogen phosphate 0.72 g/L, pH 6.8) at a flow rate of 300 cm/h. The rHSA-containing fraction obtained in the previous step was diluted to about 200 ml with a conductivity of less than 10.0 ms and then loaded on the column at a flow rate of 300 cm/h. The sample had a conductivity of 8.3 ms/cm and a pH of 6.8. After loading, the sample was eluted with elution buffer (disodium hydrogen phosphate 6.51 g/L, sodium dihydrogen phosphate 0.72 g/L, sodium chloride 11.69 g/L) at a flow rate of 100 cm/h. The eluate were collected and observed by SDS-PAGE. The rHSA-containing fractions were collected. The electrophoretogram was shown in FIG. 7B .
Step 3): Hydrophobic Chromatography Performed on Phenyl Sepharose HP as Final Purification
An XK16/100 column was packed with about 12 ml of Phenyl sepharose HP and equilibrated with 200 ml of equilibration buffer (anhydrous sodium acetate 2.32 g/L, sodium dihydrogen phosphate 2.81 g/L, ammonium sulfate 66 g/L) at a flow rate of 100 cm/h. 20 ml of the rHSA-containing fraction obtained in the previous step was added with ammonium sulfate to make the conductivity be 90.0 ms. Then the sample was loaded on the column at a flow rate of 100 cm/h. The transmission fluid was collected to obtain the rHSA-containing fractions. The electrophoretogram was shown in FIG. 7C . The HPLC chromatogram of the purified rHSA product was shown in FIG. 8 . The rHSA has a purity of more than 99% (monomer plus dimer and polymer) by HPLC.
Example 7
Separation and Purification of rHSA from the rHSA-Containing Extract
This example employs a four-step method to separate and purify rHSA by sequentially subjecting crude rHSA extract from Example 1 to cation exchange chromatography, anion exchange chromatography, ceramic hydroxyapatite chromatography and hydrophobic chromatography, performed on UNOsphere S, Q Sepharose FF, Macro-prep Ceramic hydroxyapatite Type I and Phenyl Sepharose HP as chromatography media, respectively. The cation exchange chromatography and anion exchange chromatography herein are the same as that of Example 6.
A CHT column was packed with about 15 ml of Macro-prep ceramic hydroxyapatite type I media and equilibrated with 200 ml of equilibration buffer (20 mM sodium phosphate+50 mM sodium chloride, pH 7.5) at a flow rate of 100 cm/h. The rHSA-containing fraction obtained from anion exchange chromatography was directly loaded onto the column at a flow rate of 100 cm/h. The sample had a conductivity of 26 ms/cm and a pH of 7.4˜7.6. After loading, the sample was eluted with an elution buffer (500 mM sodium phosphate, pH 7.5). The transmission fluid was collected to obtain the rHSA-containing fraction. The rHSA purification capacity was estimated to be ≦30 mg/g CHT I and the recovery rate of rHSA was up to ≧80%. Lastly, the CHT ceramic hydroxyapatite column should be regenerated with 3˜5 column volume of 500 mM sodium ohosphate buffer at pH 7.0. The column can be sanitized in 1˜2N NaOH and stored in 0.1N NaOH if desired. The electrophoretogram was shown in FIG. 9 .
Then, the rHSA-containing fraction obtained above was subjected to hydrophobic chromatography according to the procedure similar to Example 6. The transmission fluid was collected to obtain the rHSA-containing fraction. The HPLC chromatogram of the purified rHSA product was shown in FIG. 10 . The rHSA has a purity of about 99% (only monomer) by HPLC.
Example 8
Separation and Purification of rHSA from the rHSA-Containing Extract
The example was carried out by the same method as Example 7 except that the ceramic hydroxyapatite chromatography was performed on Macro-prep Ceramic hydroxyapatite Type II as chromatography media.
A CHT column was packed with about 15 ml of Macro-prep ceramic hydroxyapatite type II media and equilibrated with 200 ml of equilibration buffer (20 mM sodium phosphate+50 mM sodium chloride, pH 7.0) at a flow rate of 100 cm/h. The rHSA-containing fraction obtained from anion exchange chromatography was directly loaded onto the column at a flow rate of 100 cm/h. The sample had a conductivity of 26 ms/cm and a pH of 7.4˜7.6. After loading, the sample was eluted with an elution buffer (500 mM sodium phosphate, pH 7.0). The transmission fluid was collected to obtain the rHSA-containing fraction. The rHSA purification capacity was estimated to be ≦25 mg/g CHT II and the recovery rate of rHSA was up to ≧85%. Lastly, the CHT ceramic hydroxyapatite column should be regenerated with 3˜5 column volume of 500 mM sodium ohosphate buffer at pH 7.0. The column can be sanitized in 1˜2N NaOH and stored in 0.1N NaOH if desired. Then, the rHSA-containing fraction obtained from the previous step was subjected to hydrophobic chromatography according to the procedure similar to Example 7. The transmission fluid was collected to obtain the rHSA-containing fraction. The electrophoretogram was shown in FIG. 11 . The HPLC chromatogram of the purified rHSA product was shown in FIG. 12 . The rHSA has a purity of about 99% (only monomer) by HPLC.
It can be seen from the results of Examples 6˜8 that the ceramic hydroxyapatite chromatography increases the monomer contents in final rHSA product effectively, allowing it to be up to about 99% purity. Further, the ceramic hydroxyapatite chromatography is simply operated because it used the flow-through way for further purified rHSA as the same as the way used in Phenyl sepharose HP step and the elutant solution is compatible without adjusting salt concentration and pH value. By ceramic hydroxyapatite chromatography, the purified rHSA can meet requirements for clinical application. | A method for separating and purifying recombinant human serum albumin (rHSA) from transgenic rice grain, sequentially comprising the steps of: 1) subjecting crude extract of rHSA to cation exchange chromatography to obtain primary product I; 2) subjecting the primary product I to anion exchange chromatography to obtain secondary product II; 3) subjecting the secondary product II to hydrophobic chromatography to obtain purified rHSA. The method may further comprise a step of ceramic hydroxyapatite chromatography prior to the hydrophobic chromatography. The method has the advantages of low cost and easy operation. The resultant rHSA has a purity of about 99% by HPLC. | 1 |
This invention relates to a testing apparatus for determining the resistance of surfaces of metals and the like to abrasion.
BACKGROUND OF THE INVENTION AND PRIOR ART
One well known conventional abrasion tester has an abrasion wheel the circumference of which is covered with an abrasive. The wheel is pressed onto the surface of a sample to be tested, which is supported on a sample support, at a specific pressure and is reciprocated back and forth over the surface of the sample. The abrasion wheel is turned 0.9° at every reciprocation by means of a ratchet and a pair of gear mechanisms connected to the abrasion wheel.
In this tester, the powder from the abrasive which is generated by the abrasion during the test falls onto and aheres to or remains on the surface of the sample being tested. This results in poor accuracy and reproducability of test results. Furthermore, because the means for driving the abrasion wheel is a complicated mechanism that executes reciprocating and fractional turning movements, it is difficult to make the surface of the sample and the surface of the abrasion wheel contact exactly parallel with each other. Therefore, the surface of the sample is liable to be only partly abraded, and the accuracy and reproducability of the test results is reduced even further.
Moreover, because a ratchet is used to turn the abrasion wheel through the predetermined angle at each reciprocation, and a pair of gears is used to transmit the turning movement, backlash which is inevitable in a gear mechanism, and which is caused by the reciprocating friction load due to the reciprocal movement of the abrasion wheel, badly affects the test results. Because the abrasion wheel tends to rotate back toward the former position at the end of every reciprocal movement due to the backlash, it is impossible to abrade the sample being tested perfectly evenly with a new abrasive surface on the next stroke of the abrasion wheel. These are all very serious drawbacks in the test apparatus.
OBJECTS AND BRIEF SUMMARY OF THE INVENTION
It is an object of the present invention to provide a testing apparatus for determining resistance to abrasion of surfaces of metals and the like, which overcomes the drawbacks of the prior art apparatus.
It is a further object of the invention to provide such a testing apparatus in which the powder from the abrasive generated by the abrasion during the test does not remain on the surface of the sample being tested.
It is still a further object of the invention to provide a testing apparatus in which reciprocating movements of the abrasion wheel are avoided, and the means for rotatably indexing the abrasion wheel at each stroke of the wheel relative to the sample being tested avoids any backlash.
These objects are achieved by providing a test apparatus in which the sample to be tested is placed with the surface to be tested facing downwardly, and the abrasion wheel is positioned beneath the sample. The means for supporting the sample to be tested is mounted for reciprocating movement in a direction parallel to the surface to be tested and a means is provided for reciprocating the sample supporting means relative to the abrasion wheel. The abrasion wheel is mounted for movement only upwardly and downwardly toward and away from the sample to be tested, and a balance lever with a weight thereon is provided for holding the abrasion wheel against the sample to be tested with a predetermined force. A stepping motor rather than a ratchet mechanism is connected through a gear means to the abrasion wheel to rotatably index it. Two pairs of gears are used to transmit the rotational movement of the stepping motor to the abrasion wheel, so that backlash is minimized or completely avoided.
By means of the apparatus of the present invention, the powder of the abrasive generated during the abrasion does not remain on the surface of the sample being tested, and the relative reciprocal movement of the sample being tested and the abrasion wheel is always parallel to the surface of the sample being tested, so that partial abrasion is avoided. The rotational indexing of the abrasion wheel is achieved without any backlash, so that excellent accuracy and reproducability of the test results can be achieved.
BRIEF DESCRIPTION OF THE FIGURES
The invention will now be described in connection with the accompanying drawings, showing a preferred embodiment of the invention, and in which:
FIG. 1 is a side elevation view, partly in section taken along line I--I of FIG. 2, showing a preferred embodiment of the present invention;
FIG. 2 is a top plan view of the apparatus shown in FIG. 1; and
FIG. 3 is an elevation view of the control panel for the apparatus of FIGS. 1 and 2.
DETAILED DESCRIPTION OF THE INVENTION
As shown in FIGS. 1 and 2, the apparatus of the present invention comprises a base B on which are upright support posts 6b supporting angle bars 6a extending transversely of the base B. Extending between the opposed ends of the angle bars 6a are two parallel guide rods 6, on which are slidably positioned two pairs of bearing blocks 5. Supported on the bearing blocks 5 is a sample support 4 having a central aperture 4a therein. Above the sample support 4 is positioned a top cover 14a and beneath the cover 14a and above the aperture 4a is a backing plate 3 which is spring loaded by coil springs 2 extending between the backing plate 3 and the top cover 14a and which bias the backing plate 3 toward the sample support 4.
The sample 1 to be tested is placed between the backing plate 3 and the support 4 over the aperture 4a so as to expose the surface to be tested downwardly through the aperture 4a.
Mounted substantially midway along the length of the angle bar 6a closer to the center of the base B is a sleeve 11, and slidably extending through the sleeve 11 is a connecting rod 10 having one end connected to the sample support 4. The other end of the connecting rod 10 has a link 9 pivotally connected thereto, and the other end of the link is pivotally connected to a crank 8 which in turn is rotated by a motor 7 supported on a motor mount 7a on the base B. It will be seen that rotation of the crank 8 by the motor 7 causes the connecting rod 10, and hence the sample support 4, to reciproate. Because the connecting rod 10 and the sleeve 11 are in a plane parallel to the plane of the surface sample support 4, the sample support 4 is reciprocated in the the plane of the surface thereof.
Positioned beneath the aperture 4a in the sample support 4 is an abrasion wheel 12 having a coating abrasion material 13 on the periphery thereof. The shaft 12b on which the abrasion wheel is mounted is supported in bearings on the sidewalls of an abrasion wheel support housing 14. The housing 14 is in turn mounted on a housing base 14b, and housing lift rods 17a project downwardly from the housing base 14b. The housing lift rods 17a are mounted on a triangular housing lift frame 17, to which is pivotally connected one end of a lever 19 which in turn is pivoted on a fulcrum 18, and which has an adjustable balance weight 20 on the opposite end thereof from the housing lift frame 17. The housing lift rods 17a are guided in guide sleeves 16 which in turn are mounted on a housing mount 15 supported on the base by supports posts 15b.
Thus, the housing 14 can be raised and lowered vertically in response to the balance weight 20, being guided in its vertical movement by the housing lift rods 17a sliding in the guide sleeves 16.
Within the housing 14 is a stepping motor 25 the output shaft of which is connected to the shaft 12b on which the abrasive wheel 12 is mounted by respective pairs of gears 26, 27 and 26' and 27'. The gear ratios of the gears and the rotational angle through which the stepping motor is rotated at each energization thereof is such as to index the abrasion wheel through 0.9°, or 400 indexing steps for one complete revolution of the abrasion wheel.
Pivotally mounted on a pivot support 22a on a pivot 22 is a pivotally reciprocating control rod 21, the upper end of which is connected to the connecting rod 10 by a pin and slot connection. At a point adjacent to the rear edge of the control rod 21 when the control rod is pivoted to an extreme position is a sensing device 24, such as a limit switch, which is connected to the energizing circuit for the stepping motor 25. At the end of each complete reciprocation of the connecting rod 10, and thus of the sample support 4, the sensing device 24 is actuated to energize the stepping motor 25 so as to index the abrasion wheel 12. Rigidly connected to the pivot 22 so as to be turned therewith during the pivoting movement of the reciprocating control rod 21 is a cam 23. In the dead center position of the reciprocating movement of the control rod 21 at which it actuates the sensing device 24, the cam 23 is positioned to engage the lever 19 to pivot it around the pivot 18 so as to move the housing base 14a downwardly, and hence disengage the abrasion wheel 12 from the sample 1 being tested. In the preferred embodiment, the reciprocating control rod 21 is positioned on the opposite side of the pivot 18 from the housing 14, the cam 23 is arranged to pivot the lever 19 counterclockwise as shown in FIG. 1. Obviously, the control rod 21 could be positioned on the opposite side of the pivot 22 and the cam 23 arranged to move the lever downwardly to pivot it in the same direction.
As shown in FIG. 3, the apparatus has a control panel with a power control switch 30 for energizing the power circuit connected to the apparatus, and a setting means 31 for setting the number of reciprocations which it is desired to have the sample support carry out relative to the abrasion wheel. An indicator 33 connected to the apparatus provides an indication of the actual number of reciprocations which have been carried out. A start button 32 for starting the operation of the motor 7 and a stop button 34 for stopping the operation thereof are also provided. These various elements are connected to the power supply circuit and the control circuits for the apparatus in a conventional manner, and need not be described further.
In operation, a sample 1 to be tested is placed between the backing plate 3 and the sample support 4 with the surface to be tested facing downwardly through the aperture 4a. The balance weight 20 is then adjusted so as to urge the abrasion wheel 12 against the surface of the sample 1 with the desired force.
Thereupon, the motor 7 is started and the crank 8 drives the connecting rod 10 through the link 9 so as to reciprocate the sample support 4 parallel to the plane of the surface of the sample 1, with the surface of the sample 1 being abraded by the abrasion coating 13 on the abrasion wheel 12 which is being pressed against the surface of the sample 1. At the end of each reciprocation, the reciprocatng control rod 21 actuates the sensing means 24 and simultaneously the cam 23 pivots the lever 19 so that the abrasion wheel 12 is moved out of contact with the sample 1. Simultaneously the energization of the circuit for the stepping motor 25 by the sensing means 24 rotationally indexes the abrasion wheel through 0.9° , so that a fresh portion of the abrasion coating is presented to the surface of the sample.
The use of the two sets of transmission gears between the stepping motor and the shaft of the abrasion wheel can, by proper design of the teeth of the gears, substantially eliminate any backlash. This is achieved by having the pair of gears 26 and 27 fixed to the respective shafts so that the leading surfaces of the gear teeth on the gear 26 are in firm contact with the trailing surfaces of the gear teeth on the gear 27. The gears 26' and 27' are fixed to the respective shafts so that the leading surfaces of the teeth on the gear 27' are tightly engaged with the trailing surfaces of the teeth on the gear 26'.
It will thus be seen that all of the drawbacks of the prior art apparatus have been overcome by the apparatus of the present invention. By placing the specimen unside down on the sample support, the powder which is generated during abrasion falls away from the surface, so that it does not affect the abrasion. The use of the connecting rod 10 extending through the sleeve 11 in a plane parallel to the plane of the surface of the sample support insures accurate reciprocating movement of the sample 1 and the surface thereof to test it. The use of the stepping motor and the relative positioning of the pairs of gears 26, 27 and 26', 27' eliminates the problem of backlash in the rotation of the abrasion wheel 12, so that a completely fresh abrasion material is presented to the sample after each indexing of the abrasion wheel.
Accordingly, the apparatus of the present invention can carry out abrasion testing with high accuracy and excellant reproducability of test results. | A test apparatus for determining the abrasion resistance of the surface of a sample to be tested. The sample is placed with the surface to be tested facing downwardly through an aperture in a sample support, an abrasion wheel is positioned beneath the sample and urged upwardly against the sample, the sample is reciprocated horizontally back and forth over the abrasion wheel, and at the end of each reciprocal movement, the abrasion wheel is moved away from the sample and rotationally indexed. | 6 |
RELATED PATENT APPLICATION
This application is a continuation-in-part of my prior copending U.S. Pat. Application Ser. No. 589,792, filed June 23, 1975, now abandoned.
BACKGROUND OF INVENTION
Much of the currently produced speech or musical sounds are recorded on magnetic tape. To produce a tape recording of speech or music, the sound is converted into corresponding electric signals by means of a microphone in conjunction with various amplification apparatus. These electric signals or voltage oscillations in turn produces variations in the strength of an existing magnetic field. The signals are thereby recorded on a magnetic tape which is magnetized along its length in accordance with the signals impressed on it.
In early tape recorders, steel wire or tape was used but has since been replaced by a plastic tape which is provided with a coating of powdered red iron oxide to provide a magnetic recording medium. The black oxide of iron is sometimes used for the same purpose. In any event, the oxide particles which are applied to the tape in a coating mixed with a binder substance, are strongly magnetizable and retain their magnetic properties almost indefinitely.
Sound is transmitted as pressure waves in the air. The lowest musical notes have a frequency of about 30 cycles per second. The highest notes of musical significance are about 4,000 cycles per second. The highest audible frequencies are in the 12,00 - 16,000 cycles per second range.
The tone color or timbre, however, consists of a complex mixture of frequencies, due to harmonies which may have as much as six times as high a frequency as that of the fundamental tone of the sound. All of these vibrations are picked up by the microphone, amplified and converted into variations in the magnetic field of an electromagnet in the recording head, whereby these variations are recorded on the magnetic tape.
To reproduce the sounds, the tape is passed over a similar head, called the reproducing head, at the same speed as that used in the recording. The magnetism stored in the tape induces voltage oscillations in the electromagnetic coil of the head and the electric signals thus produced are then used to energize a speaker.
The recording head consists of a coil wound about a core of magnetic iron which has a gap at the point where the tape moves across its surface. The current in the coil magnetizes the particles in the tape. During playback, the process is reversed. Thus, the recording head can be used as the reproducing head.
The faster the tape travels past the recording head, and subsequently past the reproducing head, the clearer will be the reproduction of the sound. This is for the reason that a higher tape speed provides more space for accommodating the highest frequencies on the tape. In order to record an overtone of, for example, 5,000 cycles per second, it is necessary to record 5,000 oscillations in the strength of the magnetic field on the tape during each second of its passage past the recording head. In ratio broadcasting, a tape speed of 15 inches per second is normally employed. Thus, each of the 5,000 oscillations has a space of 15/5,000 or 0.003 inches. Tape recorders for amateurs are usually operated at tape recording and playing speeds of 71/2 inches per second, 33/4 inches per second, or 17/8 inches per second. Most machines are provided, however, with means for providing any of these three speeds as is desired.
The widths of tape available for the recording of each oscillation of the overtone of 5,000 cycles per second are thus 0.0015 inches, 0.00075 inches, and 0.000375 inches, respectively. There is a progressive decline in recording and reproduction quality as the speed is lowered, since the width of the gap in the recording and reproduction head cannot be reduced indefinitely. Thus, each oscillation requires a certain minimum amount of space which is greater as the head and gap are of coarser construction. The greater the fineness and precision of the head, the more expensive is the tape recording equipment. To achieve high-fidelity recording and reproduction it is necessary to take many technical factors into account. Sound recorders for professional purposes generally include three motors, for example, one on the supply reel, one on the take-up reel, and a third motor drives the tape, Extreme care is taken to provide a smooth and uniform drive. Tape recorders for amateurs record generally on one-half of the 1/4 inch wide tape. Some machines are designed to record four or eight tracks on a 1/4 inch tape.
A great advantage of magnetic recording is that the recording can be erased and the tapes used over and over again. The erasure is done by the erasing head which produces a powerful and high alternating field that demagnetizes and thus erases the tape just before it passes the recording head.
This invention relates generally to eight-track tape cartridges and more particularly to a compact modular tape cartridge that fits inside a container, and can be used in an eight-track playing machine to perform the same functions of the larger eight-track tape cartridge. The eight-track tape cartridge assembly may be made of plastic by the injection molding procedure.
Eight-track tape cartridges contain a continuous loop of magnetic tape which is recorded in eight separate tracks. The tape travels through guides in the face of the cartridge with the recorded side of the tape facing the playback head in the eight-track playing machine. Depending on the type of playback head and depending on the number of tracks recorded on the tape to be read by the playback head, stereo, or quadraphonic sound may be played.
The music or message that is recorded on an eight-track tape continuously travels through the cartridge. The movement of the tape is due to the tape being pressed between a rotating pinch wheel built into the cartridge and the motorized capstan in the playing machine which moves the tape at a constant speed of 33/4 inches per second. The tape is spliced at the end of the recording with a conductive tape so that when the conductive tape passes in front of a switching device in the playing unit, the playing head physically moves to read a different set of tracks with a different song or message. The playback head may be designed to read two separate channels, or it may be designed to read four separately recorded tracks for quadraphonic sound, giving a total of two channels.
In the music industry, the average number of songs recorded on an eight-track stereo tape is three per channel. Though it is common knowledge in the music industry that one song per channel would provide the listener with immediate retrieval of a particular song, the cost of the conventional cartridge would still remain the same, and only a relatively small reduced cost of a shorter length of magnetic tape would be enjoyed.
SUMMARY OF THE INVENTION
This invention is for an improved tape cartridge adapted to be played in an eight-track playing machine. More particularly, there is provided a miniaturized tape cartridge which is designed to fit within a cartridge container of dimension allowing the container/cartridge assembly to be inserted into and played in a conventional-type eight-track player machine. The container is designed and provides for the insertion of the tape cartridge within either end of the container, and either end of the loaded container may be inserted into the eight-track playing machine. The container includes a pair of pinch wheels, one at each end thereof, whereas the pinch wheel of the tape cartridge is effectively eliminated. Within the tape cartridge is a continuous loop of magnetic tape. The tape cartridge is so constructed and arranged whereby it will record and play the same amount of material as the conventional eight-track tape musical album.
In one particularly ideal embodiment of the present invention, a more conveniently sized eight-track cartridge is provided which is adapted to produce and provide the same results as conventional eight-track cartridges twice the size. Thus, the cartridge of the present invention is half the size of conventional cartridges and is still capable of being played on existing eight-track player apparatus. Although half the size of conventional cartridges, the tape cartridge of the herein disclosed invention includes the same amount of magnetic tape as the larger conventional eight-track cartridge tape albums.
Another advantageous feature of the present invention, resides in the fact that unlike the conventional cartridges on the market today, the improved tape cartridge of the present invention does not include therein a pinch wheel. Thus, the resulting costs of providing a separate pinch wheel in each manufactured tape cartridge is avoided. This is provided herein by including the pinch wheel in the cartridge container rather than in the tape cartridge itself. The pinch wheel is removably mounted in the cartridge container and this fashion of mounting the pinch wheel provides easy access thereto for the purposes of cleaning and replacement. This removable mounting feature of the pinch wheel in the container for the tape cartridge has been otherwise unknown in the industry and provides an arrangement of a pinch wheel assembly that hitherto could not be replaced or readily cleaned.
In accordance with the present invention and by virtue of the reduced size of the herein disclosed tape cartridge, one is enabled to store twice as many cartridges in any given area. Thus, a standard glove compartment of an automobile is adapted to hold therein twice as many of the tape cartridges of the present invention than would be the case of the larger conventional eight-track cartridges presently available. It is also another advantageous feature of the reduced size of the tape cartridge disclosed herein that only half as much plastic material of construction will be required to manufacture the unit than is the case with the larger eight-track cartridges on the market today.
Accordingly, it is a feature of the present invention to provide a system whereby the cost per single song selection is reduced, and wherein the same amount of recording and playing time is provided as is the case with conventional eight-track cartridge albums.
It is also a feature of the present invention to provide a tape cartridge of reduced size when compared to the size of the conventional eight-track cartridges, and to therefore reduce the amount of storage space but at the same time retaining the length of playing time.
A further feature of the present invention is to provide a container which has an outer design similar to an eight-track tape cartridge. Inside the container there are provided two pinch wheels mounted on posts at both of its ends. The cartridge that is placed inside the container is designed without a pinch wheel and is designed to be placed into the container, utilizing the container pinch wheel. Therefore, the cost of a pinch wheel being placed in each cartridge is eliminated.
Another feature of the invention is that the cartridge is reduced in size to such an extent that two cartridges can be placed inside the container at either end, and either end of the containerized cartridge can be used in a conventional eight-track player. Therefore, the cost of plastic for the cartridge, on a song per channel basis, is reduced.
A still further feature of the present invention is that enough magnetic tape can be wound in a continuous loop on a spool (though the cartridge is still half the size of a conventional eight-track cartridge) to be of sufficient length to play the same amount of songs as a conventional eight-track cartridge.
Briefly stated, the invention provides an eight-track tape cartridge system that will provide the same uses as a conventional eight-track cartridge but at a reduced cost of manufacture per playing time in a more convenient size.
These and other features and advantages of the present invention will become apparent from the following detailed description, wherein reference is made to the figures in the accompanying drawings.
IN THE DRAWINGS
FIG. 1 is a view showing the container with one of the lids thereof open and exposing at one end thereof the miniaturized tape cartridge.
FIG. 2 is a pictorial representation of the article depicted in FIG. 1 wherein the mechanical features and configuration thereof is illustrated in greater detail and showing the switching mechanism and recording head of an eight-track playing machine.
FIG. 3 is a pictorial bottom view of the tape cartridge of the present invention and showing the cut-out feature of the cartridge which enables the cartridge to be placed over and received upon either one of the pinch wheels of the container.
FIG. 4 is a pictorial view of an embodiment of the present invention wherein there is provided means for blocking the switching mechanism of the eight-track player whereby the tape cartridge will play the same track or station over and over again.
FIG. 5 is a pictorial side view of the continuous loop spool that is provided in the tape cartridge depicted in FIG. 2.
FIG. 6 is an alternate embodiment in pictorial representation and illustrating mechanism therein for providing a speed change of the tape through the unit.
FIG. 7 is a pictorial side view of the speed change mechanism depicted in FIG. 6 and illustrating the pivoted relationship of the pinch wheel and capstan of the tape cartridge.
DETAILED DESCRIPTION
Referring now to the drawings, and more particularly to FIGS. 1 - 3, there will be seen the container 10 of the present invention and having one lid thereof open as seen in FIG. 1. A notch 12 is provided on both sides of the container and constitutes the locking device for holding container 10 in a conventional eight-track player. As will be apparent from FIG. 2, the container 10 includes therein a pair of pinch wheels 14. The magnetic tape 16 is seen to travel around guide post 20, past the switching mechanism 21, further toward and across the play-record head 22 of the eight-track playing machine, and then crosses the opening defined by cut-out 17. The tape thereupon travels across curved guide surface 24 and returns to the outer edge of the tape spool 18. The base plate of the axle 19 that supports the spool 18 is anchored to the floor of the cartridge. As seen in FIG. 3, the tape cartridge includes in its underside a circular cut-out 17 which allows the tape cartridge to be placed over and to be received upon either one of the pinch wheels 14 of the container.
Referring more particularly to FIG. 1, it will be seen that the tape cartridge unit is sized to fit within one half section of the container unit 10. Thus, container unit 10 is constructed to include a pair of lids with only one being shown in its raised position in FIG. 1. With lid 10 opened as shown, the small-sized tape cartridge may be easily removed from the container and a different tape cartridge re-inserted therein. By alternately opening and closing both lids of container 10, two tape cartridges may be removed or replaced. Obviously, the container 10 may be inserted into the eight-track player with only one tape cartridge therein. However, both ends of the container may contain a tape cartridge, in which case, one tape is played, and then the container is reversed to play the tape cartridge on the other end thereof. Thus, as clearly shown in FIG. 2, the container 10 includes a pinch wheel 14 at each end thereof for the reception of two tape cartridges, if desired, although as noted above, the container may be played while including only a single tape cartridge therein.
With reference now to FIG. 2, the head 22 and switch 21 are standard components of a conventional eight-track player and details thereof are familiar to those skilled in this area of the art. Needless to say, however, switch 21 monitors a metallic station changing strip placed on tape 16. Each time the metallic strip passes switch 21, the head 22 is caused to read another of the stations or tracks on the endless tape 16. Thus, tape 16 is seen to feed in an endless path from the interior of spool 18 and from the spool axle 19. The tape 16 then proceeds across the top of the spool 18 and is guided towards the switch 21 and head 22 by means of guide post 20 which is integral with the tape cartridge. The tape 16 thereupon passes across one side of the pinch wheel 14 as shown, which pinch wheel 14 supports the tape for engagement with the drive capstan of the eight-track playing machine. The drive capstan (not shown) turns the pinch wheel 14 with the tape 16 disposed therebetween, and hence the tape 16 is caused to travel in an endless path. Guide surface 24 thereupon directs the tape 16 again to the outside of spool 18 as it passes outside thereof. While FIG. 2 illustrates only a single tape cartridge received in the container unit at the upper end, obviously a second tape cartridge may be provided in the lower end thereof and in association with the lower pinch wheel 14. Thus, when the upper tape cartridge has finished playing, it is merely required to remove the container from the player and reverse the ends, thereby playing the tape on the lower tape cartridge.
As noted above, it is a feature of the present invention to provide for the easy replacement of the pinch wheel 14 and the cleaning thereof. This should be apparent from FIG. 2. Thus, as shown in the lower half thereof, the pinch wheel is totally accessible when the tape cartridge is removed from the container. The pinch wheel 14 is removably mounted in the container by conventional means such as a snug-fitted post, and may thereby be removed for cleaning thereof or replaced in its entirety by a new pinch wheel. This easy accessible feature is of importance since the pinch wheel must be cleaned from time to time in order to remove the graphite film that builds up thereupon from continued use over a long period of time. A simple swabbing of the pinch wheel with cotton soaked in alcohol has been found sufficient to remove this film which is deposited thereon by passage of the tape thereabout.
Since it is considered critical that the tape 16 leave the spool 18 in as smooth a fashion as possible, it has been found to be desirable to construct the spool axle 19 with guide surfaces which direct the tape upwardly therefrom. Thus, with reference to FIG. 5, there is shown the details of the spool wherein is seen the base member plate 30 which is preferably attached to the bottom of the tape cartridge. Extending upwardly of the base member 30 is the spool axle shown generally at 19. The axle 19 includes a pair of inverted and frusto-conical surfaces 32 and 34. The tape spool 18 is carried by the axle 19 with the tape 16 disposed generally within the confines of these surfaces. However, as the tape is fed from the interior of spool 18, these surfaces 32 and 34 function to smoothly guide the tape from the interior of spool 18 and upwardly therefrom for travel above the spool and toward guide post 20. The emergence of the tape smoothly from the axle 19 prevents any bending, kinking, or damage being imparted to the tape.
Referring now to FIG. 4, there may be seen a simplified pictorial representation of a modified version of the container depicted in FIG. 2. Thus, means are provided for effectively blocking the actuation of the switch mechanism 21. This will be seen to include an actuating button 40 located on one side of the container. Attached to the button 40 is a narrow strip of TEFLON or other non-conductive material that extends along one wall of the container. The container includes further a pair of guide surfaces 42 and 43 that direct the TEFLON strip 41 toward and between the tape and the switch 21. This disposition of the strip 41 between the tape and switch 21 blocks the action of the switch 21 from reading the metallic station or track changing strip on the tape 16. Thus, with button pushed upwardly, the tape cartridge will continue to play on the same station or track and will not shift tracks in the event that the metal strip passes switch 21. This mechanism is, of course, desirable where it is convenient to play the same track over and over again, and without the necessity of listening to other sounds on the other tracks or stations of the tape.
In many cases, it may be found that the speed of operation of the eight-track playing machine is different from the speed of recording of the tape cartridge to be played therein. In order to overcome this problem, the invention as depicted in FIGS. 6 and 7 provides a simple and convenient manner of bringing both speeds into alignment and equalization one with the other, whereby the tape cartridge may be played nevertheless. This system as depicted in FIGS. 6 and 7 contemplates a geared reduction system. Thus, there is shown the tape 16 and recording head 22 as depicted in FIG. 2, for example. A pinch wheel 14 is again provided, however, in this instance, the pinch wheel will be seen to include a flat gear 50 or pulley located at the bottom thereof. A second gear 52 is arranged to mesh with gear 50 and this second gear carried at its center an upstanding capstan 54. Both the geared pinch wheel 14 and the geared capstan 54 are mounted between a pair of plates 56 and 58. These plates 56 and 58 are in turn pivotally mounted as a unit to the bottom 60 of the tape cartridge at point 62. Thus, as viewed in FIG. 6, the geared unit will swing from right to left, and vice versa. As the unit swings left, the tape 16 will be placed between the capstan 54 and a second pinch roller 64. This movement of the unit occurs as a result of tab 70 being pushed to the left as the container is inserted into the playing machine and locked therein at notch 12. Since the capstan of the playing machine drives the geared pinch wheel 14, appropriate sizing of the gears 50 and 52 will result in the same speed being transmitted to the tape 16 at pinch roller 64. It should be apparent therefore, that if the playing machine capstan operates at 71/2 inches per second but that the tape to be played was recorded at only 33/4 inches per second, that appropriate sizing of the gears 50 and 52 will reduce the effective speed of the tape at pinch wheel 64 to its recorded speed of 33/4 inches per second. This simple system enables tapes of different recorded speeds to be played on playing machines where the recorded speed of the tape is not otherwise available.
It will be apparent that the foregoing structures provide another significant advantage. Since the purpose of the structure is to rotate the tape at one half of the speed of the recording machine the foregoing apparatus effectively doubles the capacity of the tape when used with conventional playing equipment.
It will be apparent from the foregoing that many other variations and modifications may be made in the structures and methods described herein without substantially departing from the essential concept of the present invention. Accordingly, it should be clearly understood that the forms of the invention described herein and depicted in the accompanying drawings, are exemplary only and are not intended as limitations in the scope of the present invention. | A miniaturized tape cartridge is provided and which is designed to fit within a cartridge container of dimension allowing the container/cartridge assembly to be inserted into and played in a conventional-type eight-track player machine. The container is designed and provides for the insertion of the tape cartridge within either end of the container, and either end of the loaded container may be inserted into the eight-track playing machine. The container includes a pair of pinch wheels, one at each end thereof, whereas the pinch wheel of the tape cartridge is effectively eliminated. Within the tape cartridge is a continuous loop of magnetic tape. The tape cartridge is so constructed and arranged whereby it will record and play the same amount of material as the conventional eight-track tape musical album. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a valve utilizing shape memory alloys and an anti-lock brake system with the valve, and more particularly to a valve utilizing electrically-controlled shape memory alloys and an anti-lock brake system provided with the valve.
2. Description of the Prior Art
A shape memory alloy denotes an alloy that preserves a shape deformed by an external force below a critical temperature, whereas a shape memory effect of the alloy is activated for recovering a memorized original shape by a shape recovering force after being heated up to the critical temperature. Shape memory alloys such as a titan-nickel alloy and an aluminum alloy are manufactured to have a predetermined shape at a high temperature. Such a shape memory alloy is utilized for valves of various types, and cooperates mechanically or electrically with the valve for moving elements of the valve to a predetermined direction to open/close ports of the valve.
There are methods for applying heat upon the shape memory alloys: one is to permit fluid to flow around the shape memory alloys to vary the temperature of the fluid, and another is to permit current to flow in the shape memory alloys to generate heat by an electrical resistance of the shape memory alloys.
FIG. 1 illustrates one example of a valve 10 for subjecting the shape memory alloys to heating by varying a temperature of fluid flowing around the shape memory alloys.
In FIG. 1, a spring 12 is in the shape of a coil spring which is manufactured by using a shape memory alloy. The fluid flows around spring 12. Once a temperature of the fluid is raised to reach a critical temperature of the shape memory alloy that initiates the shape memory effect, spring 12 is compressed by the shape recovery force to open valve 10. Meanwhile, when the temperature of the fluid is lowered, spring 12 is relaxed by a bias spring 14 to close valve 10.
However, the conventional valve 10 utilizing the above-described shape memory alloy spring 12 has drawbacks of difficulty in accurately controlling the opening range of valve 10 as well as a slow response speed of spring 12 with respect to the fluid temperature. Additionally, it involves a fastidious manufacturing process since the shape memory alloys must be shaped as the coil.
A valve for improving the above-stated problems is disclosed in U.S. Pat. No. 5,211,371 (issued to Coffee). Shape memory alloys utilized in the valve of Coffee are in the shape of a wire which is electrically-controlled by an electric circuit. The electric circuit is a closed circuit comprising a plurality of transistors and a plurality of capacitors, so that the shape memory alloys are actuated in conformity with a cycle by using operations of charging/discharging the capacitors and switching the transistors.
In the valve of Coffee, however, the valve should be continuously in the open state for maintaining a prescribed pressure. Furthermore, the shape memory alloys should be continuously supplied with current to maintain the open state of the valve. In this case, not only the power is significantly dissipated due to the continuous supply of the current, but also the control of the opening/closing operation of the valve by using the current supply is difficult while the shape memory characteristic is susceptible to be lost.
U.S. Pat. No. 5,092,901 (issued to Hunter et al.) describes shape memory alloy fibers with very short total contraction and relaxation time suitable for being employed as an electro-magnetic actuator. However, Hunter et al. do not specially disclose a valve utilizing the shape memory alloy fibers.
On the other hand, as is widely known, an anti-lock brake system (ABS) indicates a break system for preventing slipping along a road surface of wheels which are locked by the operation of the brake, and for improving a steering property. Especially, the anti-lock brake system affords an effective braking force and a steering capability in case of a sudden stop, braking on a curvy road, a wet road in the rain and an icy ground, and the like.
In the conventional anti-lock system as described above, pressure-regulating valve; of respective wheels are formed of two valves of a diaphragm pattern, i.e., a pressure-holding valve and an exit valve. The pressure-holding valve and exit valve are controlled by two solenoid valves. In a normal braking operation, operation fluid flows to a brake cylinder via the pressure-regulating valves to realize the braking operation. Meantime, if one of the wheels is too abruptly locked, an electronic control unit (ECU) of the anti-lock brake system operates two solenoid valves to control the pressure within the brake cylinder and repeats locking and unlocking of the wheel at a very high speed, so that the slipping of the wheels is prevented while enhancing the steering capability.
However, the solenoid valves utilized for the anti-lock brake system have a complicated structure to require a demanding job in designing and manufacturing process with the consequence of high cost. In connection with the aforesaid valve that utilizes the shape recovery force of the shape memory alloy attributed to the temperature variation of the fluid, the shape memory alloy having a slow response speed with respect to the fluid temperature cannot be employed for the anti-lock brake system which requires a high-speed operation. Moreover, the above valve of Coffee has a difficulty in controlling the opening/closing operation of the valve to be unsuitable for the anti-lock brake system. Further, even though the shape memory alloys of Hunter et al. having short contraction and relaxation time are employed in the anti-lock brake system, the continuous current supply as described above necessarily results in the risks of significant power dissipation and possible loss of shape memory characteristic.
SUMMARY OF THE INVENTION
Accordingly, it is a first object of the present invention to provide a valve utilizing shape memory alloys which are promptly operated, freely and accurately controlled in an open/close operation thereof, and have a simple structure to facilitate the designing and manufacturing thereof.
It is a second object of the present invention to provide an anti-lock brake system with a valve utilizing shape memory alloys capable of being promptly and accurately operated while having a simple structure.
To achieve the first object of the present invention, there is provided a valve including an electronic control unit for generating a first control current and a second control current. Here, the valve also has a housing that includes a first bore with a first inlet for introducing a fluid from a fluid supply and a first outlet for discharging the fluid at an upper portion thereof, and a compartment formed to a lower portion thereof. The first inlet is closed by a first valve spool on a first position of the first valve spool and is open on a second position thereof. A first means applies a biasing force to maintain the first valve spool on the first position of the first valve spool, and a first shape memory alloy member moves the first valve spool to the second position of the first valve spool while overcoming the biasing force of the first means when the first control current is supplied from the electronic control-unit. A second means maintains the first valve spool at the second position when the first valve spool moves to the second position of the first valve spool by the first shape memory alloy member. Furthermore, a third means releases the state of the first valve spool which maintains the second position by the second means when the second control current is supplied from the electronic control unit to permit the first valve spool to move to the first position of the first valve spool by the first means.
According to another embodiment of the present invention the valve further includes a second bore having a second inlet communicated with the first bore and a second outlet for discharging the fluid from the second inlet in the upper portion of the housing. The valve also has a second valve spool for closing the second outlet on a first position and opening the second outlet on a second position thereof. A fourth means is provided for applying a biasing force to maintain the second valve spool at the first position of the second valve spool, and a second shape memory alloy member moves the second valve spool to the second position of the second valve spool while overcoming the biasing force of the fourth means. Here, when the third control current is supplied from the electronic control unit to the second shape memory alloy member, the second valve spool is moved to the second position of the second valve spool by means of the second shape memory alloy member, and maintains its second position by means of the second means when the second control current is supplied from the electronic control unit to the third means, the second valve spool is released from the state that the second valve spool is maintained at the second position of the second valve spool by the third means. Therefore, the second valve spool is moved to the first position of the second valve spool by the fourth means.
Meanwhile, in order to achieve the second object of the present invention, an anti-lock brake system includes a master cylinder for generating a hydraulic pressure to a wheel brake attached to a wheel of a vehicle, a hydraulic regulating unit having a hydraulic pump for regulating the hydraulic pressure of the master cylinder and a hydraulic motor for driving the hydraulic pump. Furthermore, an accumulator is linked to the hydraulic pump for storing brake oil, a wheel-speed sensor is attached to the wheel for sensing a wheel speed to generate a wheel-speed signal, and a vehicle-speed sensor senses a vehicle speed to generate a vehicle-speed signal. An electronic control unit receives the vehicle-speed signal and wheel-speed signal, and calculates a difference between the vehicle-speed signal and wheel-speed signal to generate first control current, second control current and third control current. In addition to these elements, a valve driven by a plurality of shape memory alloy members and performing operations of pressurization, decompression and pressure maintenance is included thereto. The valve includes a housing having a first bore with a first inlet for introducing the brake oil from the master cylinder and a first outlet for discharging the brake oil to the wheel brake in an upper portion thereof, a second bore with a second inlet communicated with the first bore and a second outlet for discharging the brake oil received from the second inlet to the hydraulic pump-in the upper portion thereof, and a compartment formed to a lower portion thereof. The first inlet is closed by a first valve spool on a first position of the first valve spool and opened on a second position of the first valve spool. Also, a second valve spool closes the second outlet on a first position of the second valve spool and opens the second outlet at a second position thereof, a first means for applying a biasing force to maintain the first valve spool at the first position of the first valve spool, and maintain the second valve spool at the first position of the second valve spool. A first shape memory alloy member moves the first valve spool to the second position of the first valve spool while overcoming the biasing force of the first means when the first control current is supplied from the electronic control unit, and a second shape memory alloy member moves the second valve spool to the second position of the second valve spool while overcoming the biasing force of the first means when the second control current is supplied from the electronic control unit. Furthermore, a second means maintains the first valve spool to the second position thereof when the first valve spool is moved to the second position of the first valve spool by means of the first shape memory alloy member, and a third means releases the state that the first and second valve spools are maintained to the second position by the second means when receiving the third control current from the electronic control unit to move the first and second valve spools to the first position of the first and second valve spools by the first means.
According to the valve according to the present invention, the lowered state of the first valve spool which is lowered by the contraction of the first shape memory alloy member is maintained by the second means, so that the valve keeps the ON state. That is, the fluid flows from the first inlet to the first outlet. The first valve spool which maintains the lowered state by the second means is raised by the third and first means to close the first bore, thereby blocking the fluid from flowing to the first outlet. That is, the valve keeps the OFF state.
In the valve utilizing the shape memory alloys according to the present invention, the opening/closing operation of the valve ie controlled by using the Joule's effect by the current flowing in the shape memory alloys, so that the opening/closing operation of the valve is quickly and accurately controllable.
In conjunction with the anti-lock brake system according To the present invention, the first shape memory alloy member is activated by the first control current by stepping on the brake pedal to decelerate and/or stop the vehicle. Thus, the wheel brake is pressurized to decelerate the speed of the wheel. When the second control current is generated, the second shape memory member is activated to close the first inlet and the second outlet is opened to decompress the wheel brake. The pressure of the wheel brake is maintained by generating the third control current, in which the first and second valve spools are raided by the third means to close the first inlet and second outlet. By doing so, the pressurization, decompression and pressure maintenance of the wheel brake is repeated to decelerate the speed of the vehicle.
The anti-lock brake system according to the present invention is simple in its structure, easy to manufacture and low in price.
BRIEF DESCRIPTION OF THE DRAWINGS
The above objects and other advantages of the present invention will become more apparent by describing in detail a preferred embodiment thereof with reference to the attached drawings in which:
FIG. 1 is a schematic sectional view for showing a conventional valve utilizing shape memory alloy springs;
FIG. 2 is a schematic sectional view for showing a valve utilizing shape memory alloys according to one embodiment the present invention;
FIG. 3 is a detailed view for showing the state wherein the spool is locked by the plate in FIG. 2;
FIG. 4 is a construction view for showing an anti-lock brake system employing the valve of FIG. 2;
FIG. 5 is a schematic sectional view for showing the valve utilizing shape memory alloys according to a second embodiment of the present invention;
FIG. 6 is a block diagram for showing the electronic control unit applied to the anti-lock brake system shown in FIG. 4; and
FIG. 7 is a block diagram for showing the shape memory alloy driver employed to the electronic control unit of FIG. 6.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The preferred embodiments of the present invention will be described with reference to the accompanying drawings, in which the same reference numerals represent the same elements.
Embodiment 1
FIG. 2 is a sectional view for showing a schematic construction of a 3-position 3-way valve 100 according to a first embodiment of the present invention.
As shown in FIG. 2, a first bore 22 having a first inlet 22a communicated to a first outlet 22b, and a second bore 24 having a second inlet 24a communicated to first bore 22 and a second outlet 24b associated with second inlet 24a are formed in the upper portion of a housing 20. A compartment 28 is provided to the lower portion of housing 20.
A first valve spool 30 is movably installed in the up and down direction within first bore 22, and a second valve spool 32 is installed in second bore 24. As shown in FIG. 3, ratchets 30a and 32a of holding unit 60 are formed at the lower ends of first and second valve spools 30 and 32, respectively. First and second valve spools 30 and 32 respectively open and close first and second bores 22 and 24. A release spool 34 is placed onto the inner portion between first and second valve spools 30 and 32.
A first shape memory alloy member 40, a second shape memory alloy member 42 and a third shape memory alloy member 44 are respectively installed between the first and second valve spools 30 and 32, release spool 34 and the bottom surface of housing 20. Preferably, first, second and third shape memory alloy members 40, 42 and 44 are formed to have a linear wire. One end of first shape memory ally member 40 is connected to the lower end of first valve spool 30; one end of second shape memory alloy member 42 is to the lower end of second valve spool 32; and one end of third shape memory alloy member 44 as a release shape memory alloy member is to the lower end of release spool 34. The other ends of first, second and third shape memory alloy members 40, 42 and 44 are fixed to the bottom surface of housing 20 and then electrically connected to an electronic control unit (ECU) 70. First, second and third shape memory alloy members 40, 42 and 44 contract by the control of electronic control unit 70 to allow first and second valve spools 30 and 32 and release spool 34 to be lowered.
Within lower compartment 28 of housing 20, a holding unit 60 is disposed for maintaining a lowered state (the lowered position) of first and second valve spools 30 and 32 when first and second valve spools 30 and 32 are lowered (moves to the lowered position) by first and second shape memory alloy members 40 and 42. Holding unit 60 is further provided with a shaft 62, a plate 64 and a plate spring 66.
FIG. 3 illustrates the locked state of first vale spool by plate 64 shown in FIG. 2.
Shaft 62 is installed within compartment 28 of housing 20 in the transversal direction. Plate 64 is pivotally mounted about shaft 62. One end of plate spring 66 is fixed to the inner side wall of compartment 28 of housing 20, and the other end thereof is fixed to the lower surface portion of plate 64. Plate spring 66 elastically supports plate 64. When first valve spool 30 is lowered by the element, e.g., first shape memory alloy member 40 so that first valve spool 30 is positioned at the lowered position, ratchet 30a of first valve spool 30 is locked to the lower end of plate 64 as shown in FIG. 3 to maintain the lowered state of first valve spool 30.
A bias unit 50 is installed between first and second valve spools 30 and 32, release spool 34 and the bottom surface of housing 20. Bias unit 50 applies a biasing force on first and second valve spools 30 and 32 to maintain first and second valve spools 30 and 32 at a raised position thereof and includes a first bias spring 52 and a second bias spring 54. First bias spring 52 applies a biasing force on first valve spool 30 to maintain its original position when first valve spool 30 under the lowered state is unlocked from plate 64 of holding unit 60; while second bias spring 54 applies an upward biasing force to second valve spool 32 to maintain its original position when second valve spool 32 under the lowered state is unlocked from plate 64 of holding unit 60.
A releasing unit 31 includes a release spool 34, a third shape memory alloy member 44 and a third bias spring 56. Third bias spring 56 forces release spool 34 under the lowered state to move to its original position.
Hereinafter, pressurization, decompression and pressure maintenance operations associated with 3-position 3-way valve 100 shown in FIG. 2 according to the present embodiment of the present invention will be described.
At the state that first inlet 22a is closed by first valve spool 30 and second outlet 24b is closed by second valve spool 32, electronic control unit 70 supplies a first control current to first shape memory alloy member 40. As first shape memory alloy member 40 is heated to contract by the current supplied while overcoming the biasing force of first bias spring 52, first valve spool 30 is lowered to a lowered position. Upon lowering first valve spool 30, plate 64 pivots clockwise about shaft 62 by means of ratchet 30a, and plate spring 66 is compressed. After the end of ratchet 30a of first valve spool 30 passes lower end of plate 64, plate 64 pivots counter-clockwise by plate spring 66. Therefore, as shown in FIG. 3, first valve spool 30 is locked by ratchet 30a and plate 64 while maintaining the lowered state thereof.
At this time, first inlet 22a of housing 20 is opened to effuse an operation fluid to first outlet 22b through a flow passage consisting of first inlet 22a, first bore 22 and first outlet 22b. Therefore, a pressure of the side of the first outlet 22b is increased (pressurization).
In order to lower the pressure of first outlet 22b, electronic control unit 70 supplies a second control current to second shape memory alloy member 42. The contraction of second shape memory alloy member 42 caused by the supplied current overcomes the biasing force of second bias spring 54 so that second valve spool 32 lowers and then, plate 64 pivots clockwise by the lowering of second valve spool 32. First valve spool 30 having been locked to plate 64 is unlocked and second valve spool 32 is locked by plate 64 at the moment ratchet 32a of second valve spool 32 passes the lower end of plate 64. Thus, second valve spool 32 maintains the lowered state by plate 64, and first valve spool 30 is raised by first bias spring 52 to return to the original position.
At this time, first inlet 22a is closed while opening second outlet 24b to thereby form a new flow passage consisting of first outlet 22b, first bore 22, second inlet 24a, second bore 24 and second outlet 24b. As the result, the operation fluid that has been pressurized at first outlet 22b is discharged toward second outlet 24b along the newly-formed flow passage to lessen the pressure of first outlet 22b.
On the other hand, release spool 34 lowers when the current is supplied from electronic control unit 70 to third shape memory alloy member 44 to overcome the upward biasing force of third bias spring 56. Second valve spool 32 having been locked to plate 64 is unlocked (or released) by means of release spool 34. Second valve spool 32 then is raised by means of spring 54 to close second outlet 24b. Release spool 34 is raised to the original position by third bias spring 56.
Thus, both first inlet 22a and second outlet 24b are closed to constantly maintain the pressure of first outlet 22b (pressure maintenance).
The valve according the first embodiment of the present invention as described above performs pressurization, decompression and pressure maintenance operations. The operation of valve 100 does not necessarily proceed in the order from the pressurization, decompression to the pressure maintenance, and the operation order is changed by the control of electronic control unit 70 in accordance with situations. The above-described valve 100 according to the first embodiment of the present invention may be applied to an anti-lock brake system.
FIG. 4 shows a construction of an anti-lock brake system of a vehicle which employs the 3-position 3-way valve shown in FIG. 2 according to the first embodiment of the present invention. To implement the valve utilizing the shape memory alloys to the anti-lock brake system, the total contraction and relaxation time of the shape memory alloy members shall be below 100 milliseconds(ms), preferably within several tens to 100 ms and generates a maximum tension of 5 Kgf. For instance, the shape memory alloy disclosed in the above-mentioned U.S. Pat. No. 5,092,901 may be utilized. In order to satisfy the condition of 100 ms and 5 Kgf of shape memory alloy members, a single shape memory alloy fiber or a bundle of the shape memory alloy fibers which are commercially available, can be utilized to form the shape memory alloy members.
One side of a master cylinder 220 is linked to a brake pedal 210. By a driver's stepping on brake pedal 210, master cylinder 220 provides a hydraulic pressure to a wheel brake 254 attached to a wheel 250 of the vehicle.
A hydraulic regulator 240 has a hydraulic pump 242 for regulating the hydraulic pressure of master cylinder 220 and a hydraulic motor 244 for driving hydraulic pump 242. Hydraulic pump 242 of hydraulic regulator 240 is connected to master cylinder 220 via a first check valve 230. Hydraulic motor 244 regulates the hydraulic pressure to be constant and is automatically stopped when the pressure exceeds a predetermined value.
An accumulator 246 for storing brake oil is connected to hydraulic pump 242 of hydraulic regulator 240 via a second check valve 232.
3-position 3-way valve 100 according to the first embodiment of the present invention is used as an actuator in this embodiment. First inlet 22a of valve 100 is joined between master cylinder 220 and first check valve 230. Second outlet 24b is joined between second check valve 232 and accumulator 246. First outlet 22b is connected to wheel brake 254.
A wheel-speed sensor 252 is attached to wheel 250 to sense the speed of wheel 250, thereby generating a wheel-speed signal.
A vehicle-speed sensor 280 senses the speed of the vehicle to generate a vehicle-speed signal.
Electronic control unit 70 for controlling valve 100 and hydraulic regulator 240, as illustrated in FIG. 6, includes a filter 72, a microcomputer 74, a shape memory alloy driver 76 for actuating first, second and third shape memory alloy members 40, 42 and 44 and a motor driver 78 for driving hydraulic motor 244. Electronic control unit 70 is electrically-connected to wheel-speed sensor 252, vehicle-speed sensor 280, valve 100 and motor 244.
Filter 72 receives the wheel-speed signal from wheel-speed sensor 252 to filter the wheel-speed signal from wheel-speed sensor 252, and the filtered signals are then transmitted to microcomputer 74.
Microcomputer 74 calculates a difference between the received vehicle-speed signal and wheel-speed signal, and, in view of the difference, generates a current control signal that controls intensity of the current supplied to first, second and third shape memory alloy members 40, 42 and 44 and a timing signal that controls time taken for supplying the 40 current to first, second and third shape memory alloy members 40, 42 and 44. In addition, an hydraulic-pressure control signal is generated for controlling hydraulic motor 244 which drives hydraulic pump 242.
The current control signal comprises a first current control signal for controlling the intensity of the current supplied to first shape memory alloy member 40, a second current control signal for controlling the intensity of the current supplied to second shape memory alloy member 42, and a third current control signal for controlling the intensity of the current supplied to third shape memory alloy member 44. The timing signal comprises a first timing signal that controls the time for supplying the current to first shape memory alloy member 40, e second timing signal that controls the time for supplying the current to second shape memory alloy member 42 and a third timing signal that controls the time for supplying the current to third shape memory alloy member 44. The current control signal and timing signal are transmitted to shape memory alloy driver 76.
As illustrated in FIG. 7, shape memory alloy driver 76 has a digital/analog converter (hereinafter referred to D/A converter) 76a and a current controller 76b.
D/A converter 76a receives the first, second and third control signals from microcomputer 74 to convert the received signals to analog signals.
Current controller 76b receives the first, second and third timing signals from microcomputer 74, receives the first, second and third current control signals from D/A converter 76a and is supplied with power from a power supply (not shown), thereby supplying the current of a predetermined intensity to first, second and third shape memory alloy members 40, 42 and 44 for a predetermined time.
Motor driver 78 activates hydraulic motor 244 in accordance with the hydraulic-pressure control signal from microcomputer 74. When the pressure within the anti-lock brake system declines below the predetermined pressure, hydraulic motor 244 is driven again by motor driver 78.
The operation of the above-stated anti-lock brake system which employs valve 100 utilizing the shape memory alloys according to the first embodiment of the present invention will be described below.
When the driver steps on brake pedal 210 to decelerate and/or stop the vehicle, the hydraulic pressure is generated in master cylinder 220. At this time, microcomputer 74 of electronic control unit 70 receives the wheel-speed signal from wheel-speed sensor 252 and the vehicle-speed signal from vehicle-speed sensor 280 to compare the vehicle speed with wheel speed and obtain a difference between them. Then, in view of the difference, the first current control signal and first timing signal are generated. Shape memory alloy driver 76, in turn, supplies the current to first shape memory alloy member 40 in accordance with the first current control signal and first timing signal.
At this time, first shape memory alloy member 40 contracts to lower first valve spool 30 which is then locked to plate 64, so that first inlet 22a of first bore 22 is open. As the result, the brake oil flows to first outlet 22b through first inlet 22a and first bore 22 of valve 100 to increase the pressure of wheel brake 254 (pressurization). Hence, wheel brake 254 is operated to decrease the speed of wheel 250 (deceleration).
If wheel 250 becomes locked, i.e., if the difference between vehicle speed and wheel speed becomes the same as the vehicle speed, this situation adversely affects a braking distance and steering capability. Thus, the pressure of wheel brake 254 is required to be lowered so as not to lock wheel 250.
When the difference between the vehicle speed and wheel speed is smaller than a predetermined value, microcomputer 74 generates the second current control signal and second timing signal. In response to these signals, second valve spool 32 lowers, and first valve spool 30 is unlocked from plate 64. First valve spool 30 then is raised by first bias spring 50 to close first inlet 22a and open second outlet 24b.
As the result, the brake oil pressurizing wheel brake 254 flows to accumulator 246 via first outlet 22b, second inlet 24a, second bore 24 and second outlet 24b to decrease the pressure of wheel brake 254 (decompression). Accordingly, the speed of wheel 250 is increased again (acceleration).
If the wheel speed approaches the vehicle speed, i.e., if the difference between the vehicle speed and wheel speed is small, it is required to decelerate the vehicle. At this time, the pressure of wheel brake 254 is increased in the order of the deceleration process.
When the difference between the vehicle speed and wheel speed reaches the predetermined value, the pressure of wheel brake 254 needs to be maintained. For this purpose, microcomputer 74 produces the third current signal and third Liming signal. Thereafter, current controller 76b receives the third current control signal and third timing signal to supply the current to third shape memory alloy member 44 which, in turn, contracts to lower release spool 34, so that both first and second valve spools 30 and 32 are raised and first inlet 22a and second outlet 24b are closed. Thus, the pressure of wheel brake 254 is constantly maintained (pressure maintenance).
By the above-described operations, the pressurization, decompression and pressure maintaining of wheel brake 254 are repeatedly executed to decelerate the speed of the vehicle.
Embodiment 2
FIG. 5 is a sectional view for showing a schematic construction of a 2-position 2-way valve 300 according to a second embodiment of the present invention. As compared with 3-position 3-way valve 100 shown in FIG. 2, 2-position 2-way valve 300 has the same construction as valve 100 of FIG. 2 excepting the lack of second bore 24 having second inlet 24a and second outlet 24b, second valve spool 32, second shape memory alloy member 42 and second bias spring 52.
The operation of valve 300 according to the second embodiment of the present invention will be described.
Firstly, electronic control unit 70 supplies the current to first shape memory alloy member 40. Due to the supplied current, first valve spool 30 is lowered to be locked to plate 64. Therefore, first inlet 22a is open to allow the fluid to flow along first inlet 22a, first bore 22 and first outlet 22b (ON).
In order to block the fluid flowing to first outlet 22b, electronic control unit 70 supplies the current to third shape memory alloy member 44. Due to the supplied current, release spool 34 is lowered to unlock first valve spool 30 from plate 64. Unlocked first valve spool 30 is raised by first bias spring 52. Finally, first inlet 22a is closed to block the flow of the fluid to first outlet 22b (OFF).
As described above, 2-position 2-way valve 300 according to the second embodiment of the present invention is mainly used as an ON/OFF valve for managing the flow of the fluid. When employing two valves 300, however, the same operation and effect as of 3-position 3-way valve 100 according to the first embodiment of the present invention can be exerted.
In a valve utilizing shape memory alloys according to the present invention as described above, a Joule's effect by current passing through the shape memory alloys is utilized for controlling the opening/closing of the valve to enable a prompt and accurate control of the opening/closing operation of the valve,
Also, the open state can be continuously maintained by a holding unit without continuously supplying the current to the shape memory alloys, which not only prevents the loss of the shape memory characteristic of shape memory alloys but also economizes the electric power consumption while more accurately carrying out the opening/closing operation of the valve.
In addition to these, the valve utilizing the shape memory alloy wire according to the present invention is simple in its structure to facilitate the design and manufacturing thereof, thereby reducing manufacturing cost.
Furthermore, by utilizing the electrically-controlled shape memory alloys, there is provided an anti-lock brake system simple in its structure, easy to be manufactured and low in price. In the anti-lock brake system according to the present invention, the opening/closing operation of the valve can be accurately performed even without continuously supplying the current to the shape memory alloys to slightly consume the electric power and secure reliability during the operation thereof.
While the present invention has been particularly shown and described with reference to particular embodiment thereof, it will be understood by those skilled in the art that various changes in form and details may be effected therein without departing from the spirit and scope of the invention as defined by the appended claims. | A valve for performing pressurization, decompression and pressure maintenance includes linear shape memory alloys. An anti-lock brake system utilizes the valve. The valve has plural spools movable up and down within a housing having plural bores. The respective bores have inlets and outlets. A mechanism for holding a lowering state of the spools is installed to the lower portion of the housing, and the spools return to their original positions by bias springs. In the anti-lock brake system, a master cylinder, wheel brakes and a hydraulic pump are connected to the inlets and outlets of the valve, and an electronic control unit is connected to the shape memory alloys to actuate the shape memory alloys, thereby attaining pressurization, decompression and maintenance of brake pressure. | 8 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuous application of U.S. application Ser. No. 13/251,183, filed on Oct. 2, 2011, which claims the priority benefit of China application serial No. 201010529025.2, filed on Oct. 25, 2010. The entirety of the above-mentioned patent application is hereby incorporated by reference herein and made a part of specification.
FIELD OF THE INVENTION
[0002] The present invention relates to a filter, and in particular, to a filter circuit and a layout structure of the filter circuit fabricated by thin film technology.
BACKGROUND OF THE INVENTION
[0003] FIG. 1 is a schematic circuit diagram of a conventional bandpass filter 100 . The conventional bandpass filter 100 comprises a capacitor C 1 , a capacitor C 2 , a capacitor C 3 , an inductor L 1 and an inductor L 2 . One terminal of the capacitor C 1 , the capacitor C 3 and the inductor L 1 are electrically connected to a first I/O (input/output) terminal TA of the filter 100 . One terminal of the capacitor C 2 , the other terminal of the capacitor C 3 and one terminal of the inductor L 2 are electrically connected to a I/O terminal TB of the filter 100 , wherein if the I/O terminal TA is an input terminal, the I/O terminal TB is an output terminal, or vice versa. The other terminal of the capacitor C 1 , C 2 , L 1 and L 2 are connected to a ground voltage GND. The conventional bandpass filter 100 is fabricated by LTCC (Low Temperature Co-Fired Ceramics).
[0004] FIG. 2 is a frequency-response diagram of the circuit shown in FIG. 1 . The filter 100 has a resonant frequency f 0 in the center of the passband, and there is a notch on the left-side band of f 0 (which means the range smaller than f 0 ) at the position about 1.9 GHz. The notch means that the filter 100 will cause larger attenuation at the frequency herein. It can be seen clearly from FIG. 2 that the attenuation on the right-side band of f 0 (the range larger than f 0 ) is not as ideal as the attenuation on the left-side band of f 0 , but this frequency response is acceptable in some application conditions. However, due to some limitation of regulations, application environments or specification of products, the attenuation on the right-side band of the resonant frequency f 0 of the conventional bandpass filter 100 might not meet the requirement of them. For example, some regulations or specification of products require that the attenuation near a certain frequency (such as two times the resonant frequency, i.e. 2 f 0 ) on the right-side band of the resonant frequency f 0 should achieve a rated quantity (such as −35 dB), and it is thus very limited for the conventional bandpass filter 100 to apply.
SUMMARY OF THE INVENTION
[0005] An object of this invention is to provide a filter and a layout structure of the filter to make a notch on the right-side band of the resonant frequency f 0 of the frequency response.
[0006] One embodiment of the present invention provides a filter and a layout structure of the filter comprising a substrate, a first capacitor, a second capacitor, a third capacitor, a first inductor, a second inductor and a third inductor. The first, the second and the third capacitor and the first and the second inductor are disposed on the top surface of the substrate. A first electrode of the first capacitor and a first terminal of the first inductor are electrically connected to a first I/O terminal of the filter. A first electrode of the second capacitor and a first terminal of the second inductor are electrically connected to a second I/O terminal of the filter. The third capacitor is electrically connected between the first I/O terminal and the second I/O terminal of the filter. The third inductor is disposed on a first lateral surface of the substrate. A first terminal of the third inductor is electrically connected to second electrodes of the first and the second capacitors.
[0007] One embodiment of the present invention provides a filter comprising a first capacitor, a second capacitor, a third capacitor, a first inductor, a second inductor and a third inductor. A first electrode of the first capacitor and a first terminal of the first inductor are electrically connected to a first I/O terminal of the filter. A first electrode of the second capacitor and a first terminal of the second inductor are electrically connected to a second I/O terminal of the filter. The third capacitor is electrically connected between the first and the second I/O terminals of the filter. A first terminal of the third inductor is electrically connected to second electrodes of the first and the second capacitors, and a second terminal of the third inductor is electrically connected to a reference voltage.
[0008] Based on the above, thin film technology can be used to achieve the layout structure of the filter circuit according to the embodiment of the present invention so as to reduce costs. Moreover, the filter circuit provided according to the embodiment of the present invention has a notch on the right-side band of the resonant frequency f 0 of the frequency response.
[0009] The detailed technology and above preferred embodiments implemented for the present invention are described in the following paragraphs accompanying the appended drawings for people skilled in this field to well appreciate the features of the claimed invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The foregoing aspects and many of the accompanying advantages of this invention will become more readily appreciated as the same becomes better understood by reference to the following detailed description when taken in conjunction with the accompanying drawings, wherein:
[0011] FIG. 1 is a schematic circuit diagram of a conventional bandpass filter.
[0012] FIG. 2 is a frequency response diagram of the circuit shown in FIG. 1 .
[0013] FIG. 3 is a schematic circuit diagram of a filter according to one embodiment of the present invention.
[0014] FIG. 4 is a schematic circuit diagram of a filter according to another embodiment of the present invention.
[0015] FIG. 5 is a frequency response diagram of the circuit shown in FIG. 4 .
[0016] FIG. 6 is a top view of a layout structure of the filter shown in FIG. 4 according to the embodiment of the present invention.
[0017] FIG. 7 is a perspective view of the layout structure shown in FIG. 6 .
[0018] FIG. 8 is an explosion diagram of the layout structure shown in FIG. 7 .
[0019] FIG. 9 is an equivalent circuit diagram of the layout structure shown in FIG. 6 .
[0020] FIG. 10 is a perspective view of parts of the layout structure of the filter shown in FIG. 4 according to another embodiment of the present invention.
[0021] FIG. 11 is a block diagram of a communication system according to one embodiment of the present invention.
[0022] FIG. 12 is a frequency response diagram of the matching network shown in FIG. 11 .
[0023] FIG. 13 is a cross-sectional view of the filter shown in FIG. 6 according to the embodiment of the present invention.
[0024] FIG. 14 is a schematic circuit diagram of a filter according to yet another embodiment of the present invention.
[0025] FIG. 15 is a perspective view of the layout structure of the filter shown in FIG. 14 according to the embodiment of the present invention.
[0026] FIG. 16 is an explosion diagram of the layout structure shown in FIG. 15 .
DETAILED DESCRIPTION OF THE INVENTION
[0027] The detailed explanation of the present invention is described as following. The described preferred embodiments are presented for purposes of illustrations and descriptions, and they are not intended to limit the scope of the present invention.
[0028] FIG. 3 is a schematic diagram of a filter 300 according to one embodiment of the present invention. The filter 300 comprising a capacitor C 1 , a capacitor C 2 , a capacitor C 3 , a inductor L 1 , a inductor L 2 and a inductor LG 1 . An electrode 301 of the capacitor C 1 is electrically connected to an I/O terminal T 1 of the filter 300 . An electrode 303 of the capacitor C 2 is electrically connected to a I/O terminal T 2 of the filter 300 , wherein if the I/O terminal T 1 is an input terminal, the I/O terminal T 2 is an output terminal, or vice versa. An electrode 305 of the capacitor C 3 is electrically connected to the I/O terminal T 1 of the filter 300 and an electrode 306 of the capacitor C 3 is electrically connected to the I/O terminal T 2 of the filter 300 . A first terminal of the inductor LG 1 is electrically connected to a second electrode 302 of the capacitor C 1 and a second electrode 304 of the capacitor C 2 , and a second terminal of the inductor LG 1 is electrically connected to a first reference voltage (such as a ground voltage GND or other fixed voltages). A first terminal of the inductor L 1 is electrically connected to the I/O terminal T 1 of the filter 300 . A first terminal of the inductor L 2 is electrically connected to the I/O terminal T 2 of the filter 300 . Mutual inductance can be generated by interactive coupled magnetic field between the inductor L 1 and the inductor L 2 . Second terminals of the inductor L 1 and the inductor L 2 are connected to a second reference voltage (such as a ground voltage GND or other fixed voltages), wherein at least either the first reference voltage is a ground voltage or the second reference voltage is a ground voltage. The filter 300 can make a notch on the right-side band of the resonant frequency f 0 of the frequency response (such as the notch 502 in FIG. 5 ). The frequency of the notch 502 can be changed by modifying capacitance of the capacitors C 1 , C 2 and C 3 or modifying inductance of the inductor LG 1 . For example, inductance of the inductor LG 1 can be 0.01˜0.1 times inductance of the inductor L 1 or the inductor L 2 .
[0029] FIG. 4 is a schematic diagram of a filter 400 according to another embodiment of the present invention. A difference between the filter 300 and the filter 400 is that the filter 400 further comprises an inductor LG 2 . A first terminal of the inductor LG 2 is electrically connected to second terminals of the inductor L 1 and the inductor L 2 , and a second terminal of the inductor LG 2 is electrically connected to a third reference voltage (such as a ground voltage GND or other fixed voltages), wherein at least either the first reference voltage is a ground voltage or the third reference voltage is a ground voltage. The position of the notch 502 can also be changed by modifying an inductance of the inductor LG 2 . For example, an inductance of the inductor LG 2 can be 0.01˜0.1 times an inductance of the inductor L 1 or the inductor L 2 .
[0030] FIG. 5 is a characteristic-curve-of-frequency-response diagram of the filter 400 shown in FIG. 4 . The filter 400 has a resonant frequency f 0 in the center of the passband, and there are a first notch 501 and a second notch 502 on the left-side band (the range smaller than f 0 ) and the right-side band (the range larger than f 0 ) of f 0 respectively. A notch is a frequency at which it has larger attenuation in the filter 400 . For example, the resonant frequency f 0 is about 2.5 GHz; the frequency of the first notch 501 is about 1.8 GHz, and the attenuation herein is about −36 dB; the frequency of the second notch 502 is about 5 GHz, and the attenuation herein is about −54 dB.
[0031] Comparing to the conventional filter 100 , the filter 400 can make the second notch 502 on the right-side band of the resonant frequency f 0 of the frequency response. The frequency of the notch 502 can be changed by modifying capacitance of the capacitors C 1 , C 2 and C 3 or modifying the inductance of the inductors LG 1 and LG 2 . If the inductance of the inductor LG 1 or the inductor LG 2 is increased, the frequencies of the notch 501 and 502 will be close to (approach) the resonant frequency f 0 , and the attenuation at the notch 501 and 502 will decrease slightly (i.e. moving up along the Y axis in FIG. 5 ). Otherwise, if the inductance of the inductor LG 1 or the inductor LG 2 is decreased, the frequencies of the notch 501 and 502 will be far from (leave) the resonant frequency f 0 , and the attenuation at the notch 501 and 502 will increase slightly (i.e. moving down along the Y axis in FIG. 5 ). The frequency of the second notch 502 can be determined according to design requirements. For example, the filter 400 can make the frequency of the second notch 502 around a double resonant frequency (i.e. 2f 0 ) to meet the needs of the regulations or specification of products.
[0032] Those skilled in the art will readily realize the filter 300 and the filter 400 by any manufacturing process and any layout structure in light of the teaching of the foregoing embodiment. For example, FIG. 6 is a top view of the layout structure of the filter 400 shown in FIG. 4 . FIG. 7 is a perspective view of the layout structure shown in FIG. 6 , and FIG. 8 is an explosion diagram of the layout structure shown in FIG. 7 . The layout of the filter 400 comprising a substrate SUB, a capacitor C 1 , a capacitor C 2 , a capacitor C 3 , a inductor L 1 , a inductor L 2 , a inductor LG 1 , a inductor LG 2 and a soldering pad 601 . The capacitors C 1 , C 2 and C 3 and the inductors L 1 and L 2 are disposed on the top surface of the substrate SUB. The capacitor C 1 and the capacitor C 2 are symmetrically disposed on both sides of a central line CL, and the inductor L 1 and the inductor L 2 are symmetrically disposed on both sides of the central line CL as well. In this embodiment, the geometrical shape of the inductor L 1 and the inductor L 2 are both long-straight wires as shown in FIG. 6˜FIG . 8 , and inductance of the inductors L 1 and L 2 can be determined by changing the length and width of the wires.
[0033] FIG. 9 is an equivalent circuit diagram of the layout structure of the filter 400 shown in FIG. 6 . Please refer to FIG. 6˜FIG . 9 , the capacitor C 3 of the filter 400 is performed by a capacitor C 31 and a capacitor C 32 in series due to layout consideration. An electrode 305 of the capacitor C 31 is electrically connected to an I/O terminal T 1 of the filter 400 . An electrode 609 of the capacitor C 32 is electrically connected to an electrode 608 of the capacitor C 31 , and an electrode 306 of the capacitor C 32 is electrically connected to an I/O terminal T 2 of the filter 400 . The capacitor C 31 and the capacitor C 32 are symmetrically disposed on both sides of the central line CL.
[0034] A conducting wire 603 is disposed on a first edge of the top surface of the substrate SUB, wherein the first edge is adjacent to a first lateral surface of the substrate SUB, and the inductor LG 1 is disposed on the first lateral surface. In this embodiment, the geometrical shape of the inductor LG 1 is a vertical wire, and inductance of the inductor LG 1 can be determined by changing the width of the vertical wire. The central portion of the conducting wire 603 is connected to a terminal of the inductor LG 1 . Each end of the conducting wire 603 has an extending portion; and each extending portion is connected to an electrode 302 of the capacitor C 1 and an electrode 304 of the capacitor C 2 respectively. Therefore, the inductor LG 1 can be electrically connected to the electrode 302 of the capacitor C 1 and the electrode 304 of the capacitor C 2 through the conducting wire 603 . In a high-frequency application environment, the conducting wire 603 can be regarded as inductors LC 2 and LC 3 , and each of the extending portions of the conducting wire 603 can be regarded as inductors LC 1 and LC 4 respectively.
[0035] A conducting wire 602 is disposed on a second edge of the top surface of the substrate SUB, wherein the second edge is adjacent to a second lateral surface of the substrate SUB, and the inductor LG 2 is disposed on the second lateral surface. In this embodiment, the geometrical shape of the inductor LG 2 is a vertical wire, and inductance of the inductor LG 2 can be determined by changing the width of the vertical wire. The central portion of the conducting wire 602 is connected to a first terminal of the inductor LG 2 . A first terminal and a second terminal of the conducting wire 602 are connected to a second terminal of the inductor L 1 and a second terminal of the inductor L 2 respectively. In a high-frequency application environment, the conducting wire 602 can be regarded as inductors LL 2 and LL 3 .
[0036] A soldering pad 601 , a soldering pad 604 and a soldering pad 605 are disposed on the bottom surface of the substrate SUB. The soldering pad 604 is electrically connected to the I/O terminal T 1 of the filter 400 . The soldering pad 605 is electrically connected to the I/O terminal T 2 of the filter 400 . The soldering pad 601 is electrically connected to second terminals of the inductor LG 1 and the inductor LG 2 . The soldering pad 601 can be electrically connected to any reference voltage (such as a ground voltage GND or other fixed voltages) according to design requirements.
[0037] The process of fabricating the filter 400 is described as the following. Please refer to FIG. 8 , providing a substrate SUB first, which can be made of glass, ceramics, bakelite, plastics or other insulating materials, such as Aluminum oxide (Al 2 O 3 ). Then, form a first conducting layer M 1 on the substrate SUB and pattern it to form the electrode 301 of the capacitor C 1 , the electrode 305 of the capacitor C 31 , the electrode 306 of the capacitor C 32 , the electrode 303 of the capacitor C 2 , the conducting segment 603 a , the conducting segment 602 a , the I/O terminals T 1 and T 2 of the filter 400 . The material of the first conducting layer M 1 is mainly low-resistance material (e.g., Al, Cu, or Ag). The first conducting layer M 1 can be formed by conventional methods.
[0038] Next, form a first insulating layer DE 1 on the first conducting layer M 1 and pattern it to optionally form dielectric windows. The first insulating layer DE 1 can be made of organic, inorganic or hybrid materials, such as SiO 2 , SiNx, SiON, polyimide-based or acrylic-based (acrylic). The first insulating layer DE 1 can be formed by conventional methods, such as CVD (chemical vapor deposition), sputtering, spin coating or coating. Next, form a second conducting layer M 2 on the first insulating layer DE 1 and pattern it to form the electrode 302 of the capacitor C 1 , the electrode 608 of the capacitor C 31 , the electrode 609 of the capacitor C 32 , the electrode 304 of the capacitor C 2 , the conducting segment 603 b , the conducting segment 602 b , the inductor L 1 and the inductor L 2 , and form dielectric window vias in the dielectric windows of the first insulating layer DE 1 . The terminals of the inductor L 1 and the inductor L 2 can be electrically connected to the I/O terminal T 1 and the I/O terminal T 2 of the filter 400 through the dielectric window vias respectively. The material, thickness and manufacturing process of the second conducting layer M 2 can be the same as that of the first conducting layer M 1 .
[0039] Next, form a second insulating layer DE 2 on the second conducting layer M 2 and pattern it to optionally form dielectric windows. The material, thickness and manufacturing process of the second insulating layer DE 2 can be the same as that of the first insulating layer DE 1 . Then, form a third conducting layer M 3 on the second insulating layer DE 2 and pattern it to form the conducting segment 603 c , the conducting segment 602 c and interconnects, and form dielectric window vias in the dielectric windows of the second insulating layer DE 2 . The material, thickness and manufacturing process of the third conducting layer M 3 can be the same as that of the first conducting layer M 1 .
[0040] The conducting segments 603 a , 603 b , 603 c , 602 a , 602 b and 602 c of the conducting wire 603 and the conducting wire 602 on each conducting layer can be electrically connected through the dielectric window vias. The electrode 608 of the capacitor C 31 is electrically connected to the electrode 609 of the capacitor C 32 through the dielectric window vias and the interconnects. The conducting wire 603 is electrically connected to the electrode 302 of the capacitor C 1 and the electrode 304 of the capacitor C 2 through the dielectric window vias.
[0041] Next, form the inductor LG 1 on the first lateral surface of the substrate SUB, and form the inductor LG 2 on the second lateral surface of the substrate SUB. In this embodiment, the inductor LG 1 and the inductor LG 2 are symmetrical with respect to the central line CL. Sometimes, process error may induce misalignment based on the central line CL of the inductor LG 1 and the inductor LG 2 (i.e. the values of parasitic inductance LL 2 and LL 3 are not equal). To improve the forgoing problem of process error, the positions of the inductor LG 1 and the inductor LG 2 can not be adjacent to the edges of the substrate SUB. The following takes the inductor LG 2 for an example, by which the inductor LG 1 can be referred.
[0042] Those implementing this invention can moderately modify the layout structure shown in FIG. 8 according to the teaching of the foregoing embodiment or design requirements. In one example, dispose the electrode 608 of the capacitor C 31 and the electrode 609 of the capacitor C 32 in the third conducting layer M 3 . In another example, dispose the electrode 608 in the second conducting layer M 2 and dispose the electrode 609 in the third conducting layer M 3 . In yet another example, dispose the electrode 608 in the third conducting layer M 3 and dispose the electrode 609 in the second conducting layer M 2 .
[0043] In one example, dispose the electrode 302 of the capacitor C 1 and the electrode 304 of the capacitor C 2 in the third conducting layer M 3 . In another example, dispose the electrode 302 in the second conducting layer M 2 and dispose the electrode 304 in the third conducting layer M 3 . In yet another example, dispose the electrode 302 in the third conducting layer M 3 and dispose the electrode 304 in the second conducting layer M 2 .
[0044] In one example, dispose the inductor L 1 and the inductor L 2 in the third conducting layer M 3 . In another example, dispose the inductor L 1 in the second conducting layer M 2 and dispose the inductor L 2 in the third conducting layer M 3 . In yet another example, dispose the inductor L 1 in the third conducting layer M 3 and dispose the inductor L 2 in the second conducting layer M 2 . No matter in which layer the inductor L 1 and the inductor L 2 are disposed, the terminals of the inductor L 1 and the inductor L 2 can both be electrically connected to the first I/O and the second I/O terminals of the filter 400 through its dielectric window vias respectively.
[0045] FIG. 10 is a perspective view of portions of the layout structure of the filter 400 shown in FIG. 4 according to another embodiment of the present invention. What isn't shown and described in this embodiment can be referred by the description in FIG. 6˜FIG . 8 . The difference between this embodiment and the layout structure shown in FIG. 6˜FIG . 8 is that the second conducting wire 602 shown in FIG. 10 isn't adjacent to the edge of the substrate SUB. There is a small distance between the edge of the conducting wire 602 disposed on the top surface of the substrate SUB and the edge of the substrate SUB. A central portion of the conducting wire 602 has a central extending portion 1001 , which extends to the edge of the substrate SUB to connect to the inductor LG 2 . The inductor L 1 and the inductor L 2 are connected by the conducting wire 602 . Likewise, the first conducting wire 603 in this embodiment isn't adjacent to the edge of the substrate SUB, and there is a small distance between the edge of the conducting wire 603 and the edge of the substrate SUB. A central portion of the conducting wire 603 also has a central extending portion, which extends to a terminal of the inductor LG 1 . Each of the two ends of the conducting wire 603 has an extending portion to connect an electrode of the capacitor C 1 and an electrode of the capacitor C 2 respectively. Therefore, although there is misalignment with the central line CL of the inductor LG 2 (or the inductor LG 1 ) due to process error, the values of parasitic inductance LL 2 and LL 3 are still substantially equal, and the foregoing problem of process error can thus be effectively improved in this embodiment.
[0046] In the abovementioned description, the inductance of the inductor LG 1 and the inductor LG 2 is determined by design requirements. In one example, in the foregoing embodiment, total inductance of the inductor LG 1 and the central extending portion of the conducting wire 603 is 0.01˜0.1 times the inductance of the first inductor L 1 or the inductor L 2 . In another example, total inductance of the inductor LG 2 and the central extending portion 1001 of the conducting wire 602 is 0.01˜0.1 times the inductance of the inductor L 1 or the inductor L 2 .
[0047] Thin film technology can be used to perform the layout structure of the filter circuit described in the foregoing embodiments of this invention so that total manufacturing cost can be reduced. Furthermore, the filter circuit in the foregoing embodiments of this invention can make a notch on the right-side band of the resonant frequency f 0 of frequency response.
[0048] The abovementioned filter 300 and filter 400 can be applied in any system, for example, a communication system. FIG. 11 is a block diagram of a communication system 1100 according to one embodiment of the present invention. The communication system 1100 comprises an antenna 1110 , a matching network 1120 , a duplexer 1130 and a duplexer 1140 . The duplexer 1130 transmits signals to the antenna 1110 ; the duplexer 1140 receives the signals from the antenna 1110 . The matching network 1120 is also called impedance-matching circuit. The matching network 1120 can provide matching impedance, and improve the isolation of the foregoing transmitting and receiving of the signals. The foregoing filter circuit 300 and filter circuit 400 can be used as the matching network 1120 in the communication system 1100 . For example, connect the I/O terminal T 1 of the filter 400 to the antenna 1110 , and connect the I/O terminal T 2 of the filter 400 to the duplexer 1130 or the duplexer 1140 .
[0049] FIG. 12 is a frequency-response diagram of the matching network 1120 shown in FIG. 11 . The filter 400 is used in the matching network 1120 shown in FIG. 11 herein. By increasing inductance of the inductors LG 1 and LG 2 , the impedance of the matching network 1120 will increase, and the impedance band can be made narrower, as shown in the curve 1201 . On the contrary, by decreasing inductance of the inductors LG 1 and LG 2 , the impedance of the matching network 1120 will decrease, and the impedance band can be made broader, as shown in the curve 1202 .
[0050] In some application, the method or process of manufacturing the matching network 1120 may not be the same as that of the duplexers 1130 and 1140 . The matching network and the duplexers can be different package components, and a larger area of PCB (printed circuit board) may be occupied. The duplexers 1130 and 1140 can be stacked on the matching network 1120 (i.e. the filter 400 ), and the matching network and the duplexers can be in a single package component to save the area of PCB.
[0051] FIG. 13 is a cross-sectional view of the filter 400 shown in FIG. 6 . In some embodiment, those skilled in the art can further dispose a third insulating layer DE 3 on the third conducting layer M 3 according to design requirements and pattern it to form dielectric windows; and dispose a fourth conducting layer M 4 on the third insulating layer DE 3 and pattern it to form a die area, a soldering pad 606 and a soldering pad 607 . The soldering pad 606 is electrically connected to the I/O terminal T 1 of the filter 400 through the dielectric window vias; the soldering pad 607 is electrically connected to the I/O terminal T 2 of the filter 400 through the dielectric window vias. A die 1310 , such as a duplexer die, can be placed in the die area, and the duplexer 1130 or the duplexer 1140 , as shown in FIG. 11 , can be included in the duplexer die 1310 . The soldering pad 606 and the soldering pad 607 are electrically connected to the duplexer die 1310 by wire bonding. Therefore, by stacking the duplexers 1130 and 1140 on the matching network 1120 (i.e. the filter 400 ), the matching network and the duplexers made by different method (or process) can be in a single package component to reduce costs and save the area of PCB.
[0052] FIG. 14 is a schematic circuit diagram of a filter circuit 1400 according to yet another embodiment of the present invention. This embodiment illustrated in FIG. 14 can be easier to understand by referring to FIG. 4 . The difference between the filter 400 and the filter 1400 is that the filter 1400 further comprises a capacitor C 6 , an inductor L 3 , a capacitor C 4 and a capacitor C 5 . An electrode 1461 of the capacitor C 6 is electrically connected to a terminal of the inductor LG 1 . An electrode 1462 of the capacitor C 6 is electrically connected to a terminal 1431 of the inductor L 3 . A terminal 1432 of the inductor L 3 is electrically connected to a terminal of the inductor LG 2 . The electrode 301 of the capacitor C 1 , an electrode 1441 of the capacitor C 4 and a terminal 1411 of the inductor L 1 are electrically connected to an I/O terminal T 1 of the filter 1400 . The electrode 303 of the capacitor C 2 , a electrode 1451 of the capacitor C 5 and a terminal 1421 of the inductor L 2 are electrically connected to a I/O terminal T 2 of the filter 1400 , wherein if the I/O terminal T 1 is an input terminal, the I/O terminal T 2 is an output terminal, and vice versa. An electrode 1442 of the capacitor C 4 and an electrode 1452 of the capacitor C 5 are electrically connected to an electrode 1462 of the capacitor C 6 and a terminal 1431 of the inductor L 3 .
[0053] Comparing to the filter 300 , the filter 1400 , as illustrated in FIG. 14 , comprises not only the first capacitor-inductor pair (the capacitor C 1 and the inductor L 1 ) and the second capacitor-inductor pair (the capacitor C 2 and the inductor L 2 ) but also the third capacitor-inductor pair (the capacitor C 6 and the inductor L 3 ). Mutual inductance can be generated by interactive coupled magnetic field between the inductor L 1 , the inductor L 2 and the inductor L 3 .
[0054] Capacitance of the C 6 can be equal to capacitance of C 1 or C 2 ; capacitance of the C 4 or C 5 can be equal to capacitance of C 3 ; inductance of the inductor L 3 can be equal to inductance of the inductors L 1 and L 2 . Because the third capacitor-inductor pair (the capacitor C 6 and the inductor L 3 ) is added, the attenuation at the resonant frequency can be increased. Taking FIG. 5 for an example, the notch 501 and 502 can be pulled down.
[0055] Those skilled in the art will readily realize the filter 1400 by any manufacturing process and any layout structure in light of the teaching of the foregoing embodiment. For example, FIG. 15 is a perspective view of the layout structure of the filter 1400 shown in FIG. 14 , FIG. 16 is an explosion diagram of the layout structure shown in FIG. 15 . The layout of the filter 1400 can be easier to understand by referring to the description of the filter 300 and the filter 400 . The difference between the filter 1400 and the filter 400 is that the layout structure of the filter 1400 further comprises an inductor L 3 , a capacitor C 6 , a capacitor C 4 and a capacitor C 5 . The capacitors C 4 , C 5 , C 6 and L 3 are disposed on the top surface of the substrate SUB. The capacitor C 4 and the capacitor C 5 are symmetrically disposed on both sides of a central line CL, and the inductor L 3 is symmetrically disposed on the central line CL. In this embodiment, the geometrical shapes of the inductor L 1 , L 2 and L 3 are long-straight wires as shown in FIG. 15˜FIG . 16 , and inductance of the inductors L 1 , L 2 and L 3 can be determined by changing the length and width of the wires.
[0056] Please referring to FIG. 14˜FIG . 16 , the electrode 1441 of the capacitor C 4 is electrically connected to the I/O terminal T 1 of the filter 1400 . The electrode 1442 of the capacitor C 4 is electrically connected to the electrode 1462 of the capacitor C 6 , the electrode 1452 of the capacitor C 5 and the terminal 1431 of the inductor L 3 through the interconnects and the dielectric window vias.
[0057] Those implementing this invention can moderately modify the layout structure shown in FIG. 15 and FIG. 16 according to the teaching of the foregoing embodiments or design requirements. In one example, dispose the electrode 1442 of the capacitor C 4 , the electrode 1452 of the capacitor C 5 and the electrode 1462 of the capacitor C 6 in the second conducting layer M 2 . In another example, dispose the electrode 1442 , the electrode 1452 and the electrode 1462 in the third conducting layer M 3 . In yet another example, dispose the electrode 1442 , the electrode 1452 and the electrode 1462 in different layers, such as disposing the electrode 1442 and 1452 in the second conducting layer M 2 and disposing the electrode 1462 in the third conducting layer M 3 .
[0058] In one example, dispose the inductor L 3 in the second conducting layer M 2 . In another example, dispose the inductor L 3 in the third conducting layer M 3 . No matter in which layer the inductor L 3 is disposed, the terminal 1431 of the inductor L 3 can be electrically connected to the electrode 1442 , the electrode 1452 and the electrode 1462 through the dielectric window vias and the interconnects.
[0059] Those skilled in the art will readily observe that numerous modifications and alterations of the device and method may be made while retaining the teachings of the invention. Accordingly, the above disclosure should be construed as limited only by the metes and bounds of the appended claims. | A circuit structure is disclosed, wherein the circuit structure comprises: a substrate comprising a top surface, a bottom surface and lateral surfaces connecting the top surface and the bottom surface; a plurality of conductive layers disposed over the top surface of the substrate, wherein a dielectric layer is disposed between each two adjacent conductive layers, wherein at least one capacitor is formed by a first portion of the plurality of conductive layers with the dielectric layers therebetween, and wherein at least one first inductor is formed by a second portion of the plurality of conductive layers; and at least one conductive pattern layer disposed over at least one of the lateral surface to form at least one second inductor, wherein a third portion of the plurality of conductive layers electrically connects with said at least one capacitor, said at least one first inductor and said at least one second inductor. | 6 |
FIELD OF THE INVENTION
This invention relates to high-conductivity copper alloys with excellent workability and heat resistance suited for applications such as magnet wires and other very thin wires, lead wires for electronic components, lead members for tape automated bonding (TAB) and the like, and members for printed-circuit boards.
BACKGROUND OF THE INVENTION
Copper is a metal excellent in electric conductivity but inferior in mechanical strength. For the reason, in practical uses, it is a customary countermeasure to reinforce copper by the addition of some additive (an alloying element or elements). However, in the fields where conductivity is of prime importance (e.g., in the manufacture of very thin wires such as magnet wires, lead wires for electronic components, lead members such as TAB or others, and members for printed-circuit boards), pure copper (with purity on the order of 99.99%) is usually used to keep the outstanding conductivity of copper unimpaired.
A problem is that the higher the purity the softer copper becomes, with the increasing risk of breaking due to "stretching-to-break" during wire drawing or other similar working operation. In particular, it has been pointed out in the art that coating with urethane, polyimide, or the like, lessens seriously the mechanical strength of pure copper wires or members or parts, rendering it difficult for those to maintain their shapes, which causes "bending or turning", "over-elongation", "droop", or other troubles. Nevertheless, "high electric conductivity" has remained the most required of the properties of conductive materials for electric wires and other similar applications. Since conductivity is preferred to mechanical strength (which is intimately related to wire drawability and other working characteristics of the material), heat resistance, and other properties, pure copper has predominantly been obliged to be used.
Meanwhile, there have been intensified demands over the years for the miniaturization of electronic components, for thinner electric wires, and for efficient operation of the manufacturing processes. To keep up with the trend, requirements for copper materials are becoming more and more exacting. Materials not merely possessing excellent conductivity but, in addition, combining conductivity with greater mechanical strength, heat resistance, and other properties are in stronger demand than heretofore.
In view of these, the present applicant, in its attempts at meeting the above requirements, previously made some proposals as to "copper materials based on high-purity copper with the addition of minute amounts of In, Hf, Mg, Be, B, Zr, Y, Ag, Si, Ca, or/and a rare earth element or elements" (Patent Application Public Disclosure Nos. 127436/ 1987 and 127438/1987, and Patent Application No. 73152/1988).
The above copper materials proposed by the applicant exhibited better mechanical strength and heat resistance than conventional products while retaining the conductivity of the level of pure copper. Those favorable properties promised a high contribution of the materials to the qualitative improvement in electric and electronic components.
However, the prospects of ever escalating performance requirements are suggesting that there are still limits to such materials in the points of mechanical strength, heat resistance, and other properties.
OBJECT OF THE INVENTION
With the foregoing in view, the present invention has for its object to provide copper materials much improved in mechanical strength and heat resistance over the conventional products while retaining as high a level of conductivity as pure copper.
SUMMARY OF THE INVENTION
The present inventor has made intensive studies with numerous experiments to realize the above object. These efforts have led to the following unexpected discoveries:
(a) Among the elements in Group b of the Periodic Table, In, Ag, Cd, Sn, Sb, Pb, and Bi, and also the active elements Zr, Ti, and Hf of Group a of the Periodic Table can serve as very desirable alloying elements. Specifically, when they added only in very small amounts, they markedly improve the mechanical strength, heat resistance, etc. of copper with substantially no adverse effects upon the conductivity.
(b) The copper materials previously proposed by the applicant likewise is based on a copper with a purity of 5N (99.999%) to 6N (99.9999%) Cu and including partly similar elements. In spite of this fact, the reason why their improvements of mechanical strength and heat resistance were still insufficient has now become clear as follows: The evaluation with respect to purity of a rating "5N Cu" or "6N Cu" was done with the exclusion of C, O, N and H according to a customary manner. The final purity of such copper material containing these elements in its end use is actually dependent on its history (for example, melting, heat treatments in varied atmospheres, etc.). That is, these impurity elements, especially O, behave to hinder the desirable actions of the alloying elements (e.g., imparting improved mechanical strength and heat resistance). The presence of such impurity elements thus places limits on the effects of improving the mechanical strength and heat resistance which otherwise could have attained by "minor amount of addition of an alloying element enough to avoid an adverse influence upon the conductivity." For this reason, it is essential to more strictly control the contents of these impurities than in conventional definition. Other impurity elements which also behave unfavorably, besides O, are such gaseous constituents as C, N, and H, as noted above. It has now also been found that the presence of S is also of particular concern.
(c) It is therefore essential to restrict the contents of S and O, among all unavoidable impurities, within specific ranges, while also controlling the total content of the impurities. Under these conditions, when a copper alloy is prepared by allowing copper to contain one or two or more alloying elements chosen from among the group of In, Ag, Cd, Sn, Sb, Pb, Bi, Zr, Ti and Hf, in an amount or amounts minute enough to have practically no adverse effect upon the conductivity, a material can be obtained which combines outstanding conductivity well comparable to that of pure copper with markedly improved mechanical strength (which dictates the workability), heat resistance, and other properties. The present invention, predicated upon the foregoing discoveries, provides a high-conductivity copper alloy with excellent workability and heat resistance, characterized by that said copper alloy is consisted essentially of, by weight, at least one element selected from the group consisting of
______________________________________10-100 ppm In (indium), 10-1000 ppm Ag (silver),10-300 ppm Cd (cadmium), 10-50 ppm Sn (tin),10-50 ppm Sb (antimony), 3-30 ppm Pb (lead),3-30 ppm Bi (bismuth), 3-30 ppm Zr (zirconium),3-50 ppm Ti (titanium) and 3-30 ppm Hf (hafnium),______________________________________
and the balance copper, and that S (sulfur) and O (oxygen) as unavoidable impurities are controlled to amounts of
less than 3 ppm S and less than 5 ppm O, respectively, and other unavoidable impurities are controlled to less than 3 ppm in total amount.
DESCRIPTION OF THE DRAWINGS
FIG. 1 shows annealing curves of In-containing high-purity copper alloys;
FIG. 2 shows annealing curves of Ag-containing high-purity copper alloys;
FIG. 3 shows annealing curves of Zr-containing high-purity copper alloys;
FIG. 4 is a graph showing the relation between the In content and semisoftening temperature of In-containing copper alloys;
FIG. 5 is a graph showing the relation between the Ag content and semisoftening temperature of Ag-containing copper alloys; and
FIG. 6 is a graph showing the relation between the Zr content and semisoftening temperature of Zr-containing copper alloys.
DETAILED DESCRIPTION
The grounds on which the composition of the high-conductivity copper alloys of the invention is defined as above and the functions and effects of the individual constituents will be explained in detail.
The alloying elements In, Ag, Cd, Sn, Sb, Pb, Bi, Zr, Ti and Hf all act to form a solid solution with Cu to improve the mechanical strength of the resulting copper alloy and elevate its recrystallization temperature. Copper, therefore, is allowed to contain one such element, or two or more where necessary. Improvement in mechanical strength is effective in preventing breaking during wire drawing, resulting in better workability of the material and greater shape retention of the formed products. Elevated recrystallization temperature, of course, means enhanced heat resistance.
If the content of any such alloying element used is below the lower limit of the specified range, the desirable effect is not attained. Conversely if the content exceeds the upper limit, the effect upon the conductivity is so serious that the conductivity on the pure copper level is no longer secured. It is for these reasons that the content of In, Ag, Cd, Sn, Sb, Pb, Bi, Zr, Ti, and Hf is fixed within the range of: In 10-100 ppm; Ag 10-1000 ppm; Cd 10-300 ppm; Sn 10-50 ppm; Sb 10-50 ppm; Pb 3-30 ppm; Bi 3-30 ppm; Zr 3-30 ppm; Ti 3-50 ppm; and Hf 3-30 ppm.
Preferable ranges of these additives are as follows:
______________________________________30-80 ppm In, 100-800 ppm Ag,30-150 ppm Cd, 20-40 ppm Sn,20-40 ppm Sb, 10-25 ppm Pb,10-25 ppm Bi, 5-20 ppm Zr,5-30 ppm Ti and 5-20 ppm Hf______________________________________
Sulfur as an unavoidable impurity is an element which easily combines with other ingredients to form compounds, which in turn deteriorate the heat resistance, mechanical strength, workability (drawability) and the like of the resulting alloy. The S content must, therefore, be as low as possible. Importantly, for the copper alloys of the invention, an S content in excess of 3 ppm would strikingly reduce the property-improving actions of the alloying elements, rendering it impossible to improve the properties while securing the conductivity of pure copper. Hence the S content is specified to be less than 3 ppm, preferably less than 2 ppm, and more preferably less than 1.5 ppm.
Oxygen is another unavoidable impurity, the ingress of which into the alloy is inevitable. The O content too must be minimized because it readily forms compounds (oxides) with other constituents, thus reducing the heat resistance, mechanical strength, workability (drawability) etc. of the alloy. Oxygen easily finds an entrance from the surrounding atmosphere into metallic copper after the production of the alloy base, e.g., during the melting or hot processing such as heat treatment. It then combines with the alloying elements added to copper for property improvements, to form oxides in Cu, thereby reducing the amount of the alloying elements available for forming solid solutions. Consequently, it becomes difficult to ensure desired heat resistance, mechanical strength, etc. with amounts of alloying elements that are only just enough to maintain the conductivity on the pure copper level. Thus, while the O content is desired to be a minimum, its unfavorable effects as noted above may be reduced to generally allowable limits if the content is below 5 ppm. Hence the specified O content is less than 5 ppm, preferably less than 3-4 ppm. For the sake of balance between the manufacturing cost and performance of the alloy, an O content on the order of 1 to 2 ppm is more realistic.
Typical of the unavoidable impurities besides S and O include C, N, and H. The contents of these impure elements must also be minimized because of their undesirable influences upon the alloy properties required under the invention. The total content of these unavoidable impurities is specified to be less than 3 ppm, since it is the limit below which the impurities have adverse effects within permissible ranges.
The major advantageous effects offered by the copper alloys of the specified composition are as follows:
i) The high conductivity makes the alloys well suited for use as wire materials (for audiovisual and electronic wirings), and the conductivity plus excellent strength and heat resistance open up new markets for the alloys in the field of special electric wires.
ii) Because the amounts of the alloying elements added are small and the amounts of impure elements are limited to very minor amounts, the resulting alloys are free from large nonmetallic inclusions or voids. They therefore have sufficient bending fatigue resistance to withstand severe cold working (e.g., deep drawing and ultrafine-gage wire drawing). They also provide materials suited as materials for working into superfine wires or ultrathin foils.
iii) Little intergranular concentration of impurities makes the alloys practically non-brittle. This promises marketability for the alloys as materials to be hard cold worked (e.g., in heading or deep drawing).
iv) The resulting alloys are work-hardened only to a slight degree during cold working and still exhibit good heat resistance. They therefore undergo practically negligible changes in mechanical properties during working and while in use.
In manufacturing the alloys according to the present invention, it is desirable from the viewpoint of product quality and productivity to choose a continuous casting process whereby a high-purity copper rod or billet or the like satisfying can be produced efficiently and safely,
(a) high purity as a production alloy,
(b) extremely small amounts of internal faults such as foreign matter and pinholes,
(c) uniformity in quality throughout continuous length, with only limited segregation, and
(d) obtainment of unidirectionally solidified structure, or, where necessary, single crystalline structure.
Processes which can meet the above requirements are, for example, the two the applicant previously proposed, i.e.:
(A) A process for continuously casting a billet or the like through a mold with one end protruded into a molten copper bath and the other end being cooled; and
(B) A continuous casting process in which molten copper stored in a first vessel is drawn by suction into a second vessel, where it is vacuum refined; and a billet or the like is withdrawn through a mold with one end protruded into the molten copper bath in the first vessel and the other end cooled.
The process (B) is a particularly suitable means for the addition of active elements to copper and for the manufacture of a high-purity material.
The advantages of the invention will be further explained in the following examples.
EXAMPLES
Electrolytic copper of 6N(99.9999% Cu) purity was vacuum melted by high-frequency heating in a graphite crucible, an alloying element or elements were added, and each charge was continuously cast in an Ar atmosphere. In this way, 11 mm-dia. rods of the chemical compositions shown in Table 1 were obtained.
The rods then were cold drawn to 2 mm-dia. wires. The tensile strength and electric conductivity of the materials as drawn were measured.
Next, the 2 mm-dia. wires were held at varied temperatures for one hour to determine their semisoftening temperature limits and also the electric conductivity of the annealed materials.
The results are also given in Table 1.
As will be clear from Table 1, all the copper alloys that satisfy the conditions specified under the invention exhibited excellent strength (hence workability), heat resistance, and electric conductivity. It can be confirmed, on the other hand, that the materials of chemical compositions that fall to satisfy the conditions were inferior in at least one of strength (workability), heat resistance, or conductivity.
TABLE 1__________________________________________________________________________ Chemical Composition Electric (ppm) Semi- Conductivity Total Tensile softening (% IACS) amount of Strength Temper- AfterType of other (kg/ ature wire AfterMaterial In Ag Cd Sn Sb Pb Bi Zr Hf Ti S O impurities Cu mm.sup.2) (°C.) drawing annealing__________________________________________________________________________Alloys 1 30 -- -- -- -- -- -- -- -- -- 0.1 tr. <3 bal. 40.1 250 100.4 102.4of the 2 60 -- -- -- -- -- -- -- -- -- 0.5 2 <3 " 39.6 280 100.3 102.4Invention 3 100 -- -- -- -- -- -- -- -- -- 0.3 3 <3 " 38.2 320 100.2 102.3 4 -- 500 -- -- -- -- -- -- -- -- 1.1 3 <3 " 37.1 320 99.9 101.8 5 -- -- 100 -- -- -- -- -- -- -- 1.5 3 <3 " 42.8 300 99.6 101.6 6 -- -- -- 30 -- -- -- -- -- -- 0.5 2 <3 " 40.8 240 99.9 102.0 7 -- -- -- -- 30 -- -- -- -- -- 0.8 2 <3 " 41.2 230 99.8 101.9 8 -- -- -- -- -- 20 -- -- -- -- 0.5 2 <3 " 42.4 210 99.3 101.3 9 -- -- -- -- -- -- 20 -- -- -- 0.6 2 <3 " 42.2 220 99.2 101.310 -- -- -- -- -- -- -- 20 -- -- 0.2 tr. <3 " 41.5 350 100.0 102.111 -- -- -- -- -- -- -- -- 20 -- 0.4 tr. <3 " 40.3 330 100.1 102.212 -- -- -- -- -- -- -- -- -- 30 0.2 2 <3 " 40.9 330 99.5 101.613 20 -- -- -- -- -- -- 10 -- -- 0.5 3 <3 " 40.4 320 100.1 102.214 60 -- -- -- -- -- -- -- 10 -- 0.4 2 <3 " 42.3 340 100.3 102.315 60 -- -- -- -- -- -- -- -- 20 0.2 2 <3 " 42.5 330 100.0 102.016 -- 100 -- -- -- -- -- -- -- 20 0.8 4 <3 " 41.3 290 100.0 102.117 -- -- -- 20 -- -- -- 10 -- -- 0.3 2 <3 " 40.5 320 99.9 102.018 -- 200 -- -- -- -- -- 10 -- -- 0.5 3 <3 " 40.8 330 99.7 101.719 -- -- 50 -- -- -- -- -- 10 -- 0.6 2 <3 " 42.2 310 99.4 101.520 -- -- -- -- 20 -- -- -- -- 20 0.4 2 <3 " 41.7 300 99.6 101.721 -- -- -- -- -- 10 -- 10 -- -- 0.8 3 <3 " 40.1 290 100.3 102.422 -- -- -- -- -- -- 10 -- 10 -- 0.5 2 <3 " 40.4 300 99.7 101.8Compar-23 5 -- -- -- -- -- -- -- -- -- 0.2 2 bal. 40.7 120 100.5 102.5ative24 300 -- -- -- -- -- -- -- -- -- 1.3 3 " 37.3 350 98.2 101.1Alloys25 100 -- -- -- -- -- -- -- -- -- 6.0 12 " 40.3 190 98.9 101.526 -- -- 400 -- -- -- -- -- -- -- 0.6 3 " 37.6 320 96.8 99.327 -- -- -- 30 -- -- -- -- -- -- 0.5 10 " 43.2 180 99.7 101.928 -- -- -- -- 100 -- -- -- -- -- 0.7 2 " 38.4 300 97.9 100.529 -- 5 -- -- -- -- -- -- -- -- 0.8 2 " 40.8 120 100.1 102.430 -- -- -- -- -- 40 -- -- -- -- 0.7 3 " 43.5 240 98.6 101.231 -- -- -- -- -- -- -- 50 -- -- 1.0 3 " 40.6 450 98.3 100.832 -- -- -- -- -- -- -- -- 50 -- 0.6 3 " 40.2 430 98.6 101.133 -- -- -- -- -- -- -- -- -- 100 1.1 3 " 37.7 380 96.2 98.734 -- -- -- -- -- -- -- -- -- -- 0.1 2 <3 bal. 41.8 120 100.5 102.635 -- 12 -- -- -- -- -- -- -- -- 8.3 5 bal. 45.2 150 97.8 100.8__________________________________________________________________________ 34: 6N--Cu material. 35: Generalpurpose OFC material of 3N purity.
In addition, annealing curves were plotted for similarly produced high-purity copper of 6N-Cu grade and In-, Ag-, and Zr-containing copper alloys (each containing also 0.1 ppm S, 2 ppm O, and a total of less than 3 ppm impurities other than S and O). The results are given in FIGS. 1 to 3, which clearly show that the alloys of the present invention are extremely desirable materials which undergo little changes in mechanical properties through the period during which these materials are worked and used.
Next, in FIGS. 4 to 6, are compared the results of investigations on the "relation between alloying element content and semi-softening temperature" in In-, Ag-, and Zr-containing copper alloys which were based on three kinds of high-purity copper of 6N-Cu grade (containing 0.1 ppm S, 2 ppm O, and less than 3 ppm impurities other than S and O), tough pitch copper (containing 200-300 ppm O), and oxygen-free copper (containing 10 ppm or less O). FIGS. 4 to 6 also demonstrate the outstanding heat resistance of the alloys according to the present invention.
It will be understandable that a very excellent copper material can be produced by incorpolating an effective alloying element(s) in a specified amount under stricter control of impurities than has been employed before now.
ADVANTAGES OF THE INVENTION
As described above, the present invention provides high-conductivity copper alloys which combine the excellent conductivity of existing materials with good heat resistance, mechanical strength, workability, etc. The invention thus offers advantages of very great industrial significance, contributing, for example, to further improvements in performance of magnet wires, leads for electronic components, printed-circuit boards, and the like. | There is provided a high-conductivity copper alloy with excellent workability and heat resistance, characterized by the alloy consists essentially of, by weight, at least one element selected from the group consisting of
______________________________________
10-100 ppm In (indium), 10-1000 ppm Ag (silver),10-300 ppm Cd (cadmium), 10-50 ppm Sn (tin),10-50 ppm Sb (antimony), 3-30 ppm Pb (lead),3-30 ppm Bi (bismuth), 3-30 ppm Zr (zirconium),3-50 ppm Ti (titanium) and 3-30 ppm Hf (hafnium),______________________________________
and the balance copper. S (sulfur) and O (oxygen) as unavoidable impurities are controlled to amounts of less than 3 ppm S, and less than 5 ppm O, respectively. Other unavoidable impurities are controlled to less than 3 ppm in total amount. The alloy is very suitable for applications such as forming magnet wires and other very thin wires, lead wires for electronic components, lead members for tape automated bonding (TAB) and the like, and members for printed-circuit boards. | 2 |
FIELD OF THE INVENTION
The present invention relates to the field of hand tools and particularly to an apparatus for promoting router safety.
BACKGROUND OF THE INVENTION
For instance, United States Published Patent Application 2002/0043294 A1, entitled: Router, which is hereby incorporated by reference in its entirety, describes a device which permits rapid depth adjustment. While such a device provides the ability to adjust rapidly, rapid adjustment may result in injury to the user and/or damage to the router itself. For example, when an unwary user replaces the motor housing into the router base, such as after changing a bit, the motor housing and motor may drop upon utilizing a course adjustment device, if the motor housing is not grasped.
Furthermore, if a user is forced to support the motor housing, such as to prevent damage to the router when adjusting plunge depth, the user's grasping hand or fingers may be smashed and/or pinched, upon rapid depth adjustment, due to the weight of the router motor and housing.
Moreover, routers which include grasping apparatus for aiding in grasping the base or motor housing typically include a lip or rim for at least partially supporting the weight of the router during operation and transfer. A safety problem may occur if the motor housing and grasping apparatus interact to create a pinch point where a user's finger or hand may be easily caught.
Moreover, the router itself may become damaged, such as when an adjustment mechanism is released when the router is implemented with a router table. For instance, if a user actuates the course adjustment device, the router may drop suddenly.
Therefore, it would be desirable to provide an apparatus for promoting router safety.
SUMMARY OF THE INVENTION
Accordingly, the present invention is directed to an apparatus for promoting router safety when adjusting router depth. As will be appreciated by those of skill in the art, the apparatus of the present invention may be implemented in rotary cut-off tools, both standard and plunge routers, and the like.
In a first aspect of the present invention, a router includes a motor housing, a base, an adjustment mechanism and a hand grip attachment. The adjustment mechanism includes a shaft with a threaded portion and a thread engaging member. The shaft is attached to the motor housing and is received in the base wherein the engaging member may selectively engage the threaded portion. The hand grip includes a lip for at least partially supporting the router when grasped. The lip extends generally outward from the base to which it is attached. The lip may be disposed even with or below the end of the base adjacent to the motor housing so as to minimize potential user injury.
In an additional aspect of the invention, a router adjustment device includes a base, a motor housing, a frictional zone, and an adjustment mechanism including a shaft and threaded engaging member. The motor housing may adjustably secure within the base for permitting depth adjustment. The frictional zone may be disposed either on the base or motor housing. For instance, the frictional zone is disposed generally at the interface of the motor housing and base. The frictional zone at least partially resists the movement of the motor housing, such as when the thread engaging member is disengaged from the threaded shaft.
In a further aspect of the invention, an apparatus for controlling router adjustment includes a base, a motor housing, and an adjustment mechanism. The adjustment mechanism includes a shaft, a threaded engaging member and means for at least partially restraining the motor housing from moving with respect to the base. For instance, the adjustment mechanism contains a spring for generally biasing the shaft to prevent damage and/or injury.
In another aspect of the invention, a router adjustment device includes a base, a motor housing, an adjustment mechanism, and a brake element. The motor housing is adjustably secured in the base to permit longitudinal movement. The break element is disposed in the base substantially perpendicular to the motor housing. The break element may be activated to at least partially resist the movement of the motor housing, such as when a course adjust occurs.
It is to be understood that both the forgoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention as claimed. The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate an embodiment of the invention and together with the general description, serve to explain the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The numerous advantages of the present invention may be better understood by those killed in the art by reference to the accompanying figures in which:
FIG. 1 is an isometric view of a router including hand grip attachment with a support lip terminating generally even with the end of a base;
FIG. 2 is an exploded view of a router with a motor housing including an angled portion, for minimizing pinching, adjacent to a base;
FIG. 3 is an exploded view of a router adjustment device including a frictional zone for generally minimizing rapid course adjustment;
FIG. 4A is a cut-a-way view of an apparatus for controlling router adjustment including a compression spring for minimizing rapid adjustment;
FIG. 4B is a cut-a-way view of an apparatus for controlling router adjustment including a coiled spring with lever arm for minimizing rapid adjustment;
FIG. 4C is a cut-a-way view of an apparatus for controlling router adjustment including a gasket for minimizing rapid adjustment;
FIG. 4D is a cut-a-way view of an apparatus for controlling router adjustment including a frictional zone mounted to a thread engaging member for minimizing rapid adjustment;
FIG. 5A is cross sectional view of a router adjustment device including a biased breaking element;
FIG. 5B is cross sectional view of a router adjustment device including a biased breaking element capable of automatic actuation by a thread engaging member; and
FIG. 5C is cross sectional view of a router adjustment device including a thread engaging member with a contact zone for minimizing rapid course depth adjustment.
DETAILED DESCRIPTION OF THE INVENTION
Reference will now be made in detail to the presently preferred embodiments of the invention, examples of which are illustrated in the accompanying drawings.
Referring generally now to FIGS. 1 through 5C , exemplary embodiments of the present invention are shown.
Referring to FIG. 1 , a router 100 is shown. A base 102 and motor housing 104 are included in the router 100 . The base 104 is suitable for supporting the router 100 when the motor housing 104 is upwardly directed. The base 102 adjustably secures the motor housing 104 . For example, the motor housing is capable of being adjusted with respect to the base 102 , such that the router may achieve various cut depths when implemented with a router bit. Typically, bases include a furcation which may be drawn together by means of a clamping mechanism. In additional embodiments, a friction lock may be employed to secure the motor housing within the base. An adjustment mechanism 106 is further included in the router 100 .
The adjustment mechanism includes a shaft 108 , with a threaded portion, and a thread engaging member 110 . The engaging member 110 contains a lug or ridge for alternately engaging and releasing at least a portion of the threads included on the shaft 108 . The engaging member 110 may be biased, so the lug engages the shaft when unactuated. For instance, the engaging member 110 is biased by a spring so the motor housing is secured in a first orientation. When a user depresses the engaging member the lug and threads may disengage resulting in a second orientation being obtained. Additionally, fine depth adjustment may be achieved by rotating the shaft 108 .
A hand grip attachment 112 is connected to the exterior of the base 102 . The hand grip attachment 112 includes a lip 114 for at least partially supporting the router when grasped. The lip 114 extends generally outwardly from the exterior of the base. The portion of the lip 114 adjacent to the motor housing 104 of the present embodiment is either even with or less than the end of the base 102 . For example, the lip may be even with the base adjacent to the motor housing 104 . In a further embodiment, the top of the lip is below the end of the base. By orientating the top of the lip even with or below the end of the base a user is less likely to have their hand or fingers caught between the lip and the motor housing. For example, an unwary user's hand may be pinched between the motor housing and hand grip attachment during adjustment.
In further examples, the motor housing and/or the top of the lip generally opposing the housing may be angled away from the other so as to further minimize the pinch point. See generally FIG. 2 , wherein the motor housing is angled generally away from the base/lip to minimize pinching.
In an additional aspects, a motor housing is contoured for grasping by a user. For instance, the motor housing is shaped so a user may pinch the motor housing between their fingers and thumb when adjusting depth. Supporting the motor housing in the previous manner may prevent the motor housing from dropping suddenly while changing depth, while promoting safety. In additional embodiments, the motor housing includes a lip for at least partially supporting the motor housing when grasped. Moreover, the motor housing may include an elastomeric coating or formed at least partially of elastomeric material to promote user comfort and minimize muscle fatigue.
Referring to FIG. 3 , a router adjustment device 300 is shown. The adjustment device 300 includes a base 302 , a motor housing 304 , and an adjustment mechanism 306 . The adjustment mechanism includes a shaft 308 , with a threaded portion, and a thread engaging member 310 . The base 302 , motor housing 304 and adjustment mechanism 306 , including the shaft and engaging member 310 operate substantially as described with respect to FIGS. 1 and 2 . The router adjustment device 300 , of the present embodiment, includes a frictional zone 316 . A frictional zone is included to at least partially resist the movement of the motor housing 304 with respect to the base. The frictional zone 316 is disposed either on the portion of the motor housing 304 received in the base or is disposed in an interior recess of the base 302 .
A frictional zone permits course adjustment, via disengaging the engaging member 310 , and fine adjustment, via rotation of the shaft 308 . The frictional zone at least partially inhibits rapid course adjustment which would damage the device 300 or potentially injure a user.
Frictional zones may be formed of brass, ceramic material, polymeric materials, elastomeric materials and the like for increasing the coefficient of friction between the friction zone and the generally opposing surface, such as the base. The increase in the coefficient of friction is greater than the coefficient of friction provided by a router or device not containing at least one frictional zone. For instance, the static coefficient of friction between the zone and opposing surface is between 0.15μ and 0.58μ, so as to permit adjustment while offering resistance, and thus increased safety.
In additional examples, a second frictional zone is employed to generally oppose the first frictional zone 316 . In examples where two frictional zones are employed, the first and second frictional zones are disposed generally opposite with one zone disposed on the base and the other disposed on the motor housing.
Referring to FIGS. 4A , 4 B and 4 C an apparatus 400 for controlling router adjustment is discussed. The apparatus 400 includes a base 402 , a motor housing 404 and adjustment mechanism 406 , which operate substantially a previously described.
Referring to FIG. 4A , in a first example, a compression spring 418 is disposed in the base 402 so the shaft 408 is generally biased. For instance, when the shaft 408 included in the adjustment mechanism 406 is disengaged from the engaging member 410 the spring at least partially supports the shaft, and thus the motor housing, such as by contacting a shoulder included on the shaft 408 . By implementing the present apparatus when the engagement member 410 is disengaged from the shaft the spring acts to prevent rapid adjustment which may damage the apparatus or injure the user. The present apparatus retains the ability to permit a wrench to interact with a mechanical connection included on the shaft to permit base end adjustment. In additional examples, a washer may be disposed on the end of the spring 408 contacting the shaft for providing a suitable interface for the spring/shaft.
Referring to FIG. 4B , in a second example, a biased lever is disposed in the base 402 adjacent to the threaded portion of the shaft 408 . In the present example a coiled spring with a lever arm 420 is utilized. The lever 420 acts to at least partially restrain the longitudinal movement of the threaded shaft by alternately engaging and releasing the threads. For example, when the thread engaging member is disengaged from the shaft 408 , the lever 420 may permit gradual change.
Referring to FIG. 4C , in a further example, a gasket 422 formed of elastomeric or polymeric material is disposed in the base adjoining the shaft 408 , included in the apparatus 400 . For instance, the gasket 422 is formed of a semi-rigid plastic which couples to the shaft to at least partially restraining the shaft during longitudinal travel, such as when the shaft 408 is disengaged from the thread engaging member. Additionally, an inner ring formed of a metal such as brass, a ceramic and the like may be utilized to increase the durability of the gasket 422 . For instance, a gasket may include a washer with a metallic inner ring surrounded by an elastomeric material such that the inner ring contacts the shaft 408 .
Referring to FIG. 4D , in an additional example, a frictional zone 424 is attached to the thread engaging member 410 . The frictional zone 424 is disposed in the aperture generally opposite the lug or ridge for engaging the threads included on the shaft 408 . The frictional zone may contact the shaft 408 , thus retarding the longitudinal motion of the shaft, such as when the shaft is disengaged from the threaded engaging member 410 . For instance, when a user inadvertently releases the thread engaging member 410 the frictional zone may come in contact with the shaft, and resulting in a slower travel.
Referring now to FIG. 5A , a router adjustment device 500 is shown. The router device 500 includes a base 502 , a motor housing 504 and an adjustment mechanism 506 , including a shaft 508 and thread engaging member 510 . All of the above are substantially similar as discussed previously. The device 500 , of the present embodiment, further includes a brake element disposed in the base generally perpendicular to the axis motion for the motor housing 504 .
For example, the brake element is a biased pin 526 which is suitable for contacting the motor housing. Preferably, the pin 526 is biased in a disengaged orientation. For example, a user may wish to depress the pin 526 , and thus contact the motor housing and at least partially resist or inhibit motor housing motion, such as when performing a course adjustment. The pin 526 may be located so as to permit the user to utilize one hand to manipulate the pin 526 and the thread engaging member 510 .
In a further embodiment, the portion of the pin 526 contacting the motor housing may be formed of brass (e.g., a brass plug 527 ), ceramic material, plastic and the like for at least partially retarding the longitudinal motion of the motor housing without marring the motor housing 504 .
Referring to FIG. 5B , in an additional example, the biased pin includes an angled end directed towards a generally opposing angled surface included on the thread engagement member 510 . Employing the present arrangement, the pin 526 automatically engages when the engaging member 510 is actuated, thus resulting in the pin 526 being forced towards the motor housing 504 .
Referring now to FIG. 5C , in a further example, a contact zone 528 mounted to the thread engaging member 510 . For instance, the thread engaging member 510 includes an angled or curved protrusion, directed towards the motor housing, with a contact zone 528 for contacting the motor housing 504 when the engaging member 510 is pressed. The contact zone may be formed of brass, ceramic material, plastic and the like for at least partially resisting the longitudinal motion of the motor housing without marring the motor housing 504 .
It is believed that the apparatus of the present invention and many of its attendant advantages will be understood by the forgoing description. It is also believed that it will be apparent that various changes may be made in the form, construction and arrangement of the components thereof without departing from the scope and spirit of the invention or without sacrificing all of its material advantages. The form herein before described being merely an explanatory embodiment thereof. It is the intention of the following claims to encompass and include such changes. | The present invention is directed to a router depth adjustment mechanism for minimizing rapid course depth adjustment for standard and plunge routers. Routers with rapid or course adjustment mechanisms may permit a router motor housing to drop suddenly, if the user in inattentive. Sudden adjustments may result in damage to the router and even user injury. The mechanism of the present invention includes a threaded shaft and a biased thread engaging member which may be disengaged for rapid adjustment. A restraining device and/or a break may be included to minimize the rate of change. | 8 |
This application claims the benefit of U.S. Provisional Application No. 60/376,475, filed Apr. 30, 2002.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a training apparatus for use in connection with enhancing skill at pocket billiards. The training apparatus has particular utility in connection with simulating a racked set of balls on a pocket billiards table. More specifically, the training apparatus is used in a practice session to enhance the skill level of players wishing to improve their break shot.
2. Description of the Prior Art
Pocket billiards training apparatuses are desirable for enhancing the skill level of pocket billiards players. In fact, a variety of aids are available to help a player improve a variety of shots encountered in a pocket billiards game. However, the available aids do not allow a player to efficiently practice a break shot.
A break shot is the opening shot of a pocket billiards game, involving a cue ball and a plurality of object balls. To set up a break shot, the object balls are racked in a frame in the center of the table and arranged in a geometric angular pattern as called for in the rules of the game. During the break shot, the game commences with the cue ball being struck by the first contestant. The cue ball is directed toward the head object ball in such a manner that the impact of the cue ball causes the object balls to scatter over the area of the table. If one or more object balls enter a pocket during the break shot, the first contestant proceeds to attempt to shoot the remaining balls into the pocket under the rules of the game.
It has been universally agreed upon and demonstrated in the past that the break shot is of prime importance to the first contestant. If the break shot is executed with sufficient skill, the object balls will be efficiently scattered and the cue ball will be left in a favorable position. Frequently, a highly skilled contestant left with efficiently scattered object balls and a favorably positioned cue ball may win the game by shooting the entire range of object balls into the pockets. Thus, the faculty of making an excellent break shot is emphatic. Furthermore, there is a need for a pocket billiards training apparatus that enhances the skill level of players wishing to improve their break shot.
The use of pocket billiards training devices is known in the prior art. For example, U.S. Pat. No. 6,527,647 to Robert W. Ringeisen discloses a training device that assists the user in focusing upon the correct strike points on both the cue ball and the object ball. However, the Ringeisen '647 patent does not simulate a racked set of balls used during a break shot. The Ringeisen '647 patent has a further drawback of requiring the user to reposition the balls after each practice shot. In other words, the Ringeisen '647 device is inefficient because practice time is wasted setting up each shot.
U.S. Pat. No. 6,364,783 to Jack V. Kellogg discloses a practice billiard aiming system that is useful in teaching and practicing pocket billiards. However, the Kellogg '783 patent does not permit effective simulation of a break shot. Additionally, the Kellogg '783 invention utilizes balls with aiming line markings. This is a drawback because the marked balls prohibit training under regulation game conditions.
While the above-described devices fulfill their respective, particular objectives and requirements, the aforementioned patents do not describe a pocket billiards training apparatus that simulates a racked set of balls for use in a practice session to enhance the skill level of players wishing to improve their break shot. Neither the Ringeisen '647 nor the Kellogg '783 patent makes a provision for simulating the break shot setup. Moreover, neither patent discloses an invention that promotes efficient practice by automatically repositioning itself after each practice shot.
Therefore, a need exists for a new pocket billiards training apparatus that simulates a racked set of balls for use in a practice session to enhance the skill level of players wishing to improve their break shot. In this regard, the present invention substantially fulfills this need. In this respect, the pocket billiards break shot training apparatus according to the present invention substantially departs from the conventional concepts and designs of the prior art, and in doing so provides an apparatus primarily developed for the purpose of enhancing a players break shot.
SUMMARY OF THE INVENTION
In view of the foregoing disadvantages inherent in the known types of billiards training aids now present in the prior art, the present invention provides a new pocket billiards break shot training apparatus, and overcomes the above-mentioned disadvantages and drawbacks of the prior art. As such, the general purpose of the present invention, which will be described subsequently in greater detail, is to provide a new pocket billiards break shot training apparatus that has all the advantages of the prior art mentioned heretofore and many novel features that result in a pocket billiards training aid that is not anticipated, rendered obvious, suggested, or even implied by the prior art, either alone or in any combination thereof.
To attain this, the present invention essentially comprises a cross-shaped frame, an energy absorbing assembly, a plurality of balls, a bow restraint assembly, and a set of elastic restraint cords. The cross-shaped frame simulates a rack of pocket billiards balls that would be used in an actual game. Furthermore, the cross-shaped frame is moored in the center of the table to achieve the function of a training apparatus that can be used to enhance a player's break shot through repetitive practice.
To facilitate simulation of a break shot, the apparatus incorporates a head ball in the equivalent position to that of an actual rack of balls. The head ball is situated toward the player and carries a numeral “1” on the front view. Thus, in the same manner as in an actual pocket billiards game, the head ball becomes the player's aiming point In conjunction with the head ball, a set of side balls and a rear ball form the four ends of the cross-shaped frame. A center ball is positioned in the center of the frame for decorative purposes. Each ball is similar to a regulation billiards ball. Moreover, the side balls and rear ball are black.
In order to simulate a cue ball striking the head ball in an actual game of pocket billiards, the frame incorporates an energy absorbing assembly. The energy absorbing assembly comprises a bolt, an alignment cartridge, a spacer, and a cylindrical spring. The head ball is screwed to the metal bolt, which has a tapered socket head protruding to the rear. Furthermore, the metal bolt passes through a bronze alignment cartridge that has a tapered bore to allow the bolt to sag or deflect laterally when the head ball is struck off center. The bolt's tapered socket head mates with a corresponding seat in the alignment cartridge that realigns the bolt and the head ball to a central alignment after the impact of each shot.
The alignment cartridge has an external thread which mates with a corresponding internal thread in the cross-shaped frame's main shaft. Between the alignment cartridge and the head ball, the bolt passes through the cylindrical spring that may be constructed of metal or a solid elastomeric material. Furthermore, the bolt is threaded through a round metal spacer. After passing through the alignment cartridge and spacer, the bolt is threaded into the head ball. The bolt is tightened to a specific, preload torque setting, which compresses the spring between the alignment cartridge and the spacer. The alignment cartridge is then threaded into the main shaft.
In addition to the head ball energy absorbing assembly, the pocket billiards break shot training apparatus includes a bow restraint assembly. The bow restraint assembly is constructed of two fiberglass rods that are connected to a plastic joining rod by insertion into a set of hole sockets. The fiberglass rods are then bent to form an arc and positioned in the cavity below each side rail cushion and the end rail cushion of a pocket billiards table. This provides a point on each side of the pocket billiards table to anchor the elastic restraint cords. By adjusting the lengths of the fiberglass rods, the bow restraint assembly may be adapted to fit billiards tables of varying lengths and widths. Furthermore, by adjusting the tension of the restraint cords the training apparatus is moored into the center of the table. Thus, the entire assembly can be quickly installed for practice and conveniently removed to restore playing availability to the table.
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 attached.
Numerous objects, features and advantages of the present invention will be readily apparent to those of ordinary skill in the art upon a reading of the following detailed description of presently preferred, but nonetheless illustrative, embodiments of the present invention when taken in conjunction with the accompanying drawings. In this respect, before explaining the current 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.
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.
It is therefore an object of the present invention to provide a new pocket billiards break shot training apparatus that has all of the advantages of the prior art pocket billiards training aids and none of the disadvantages.
It is another object of the present invention to provide a new pocket billiards break shot training apparatus that may be easily and efficiently manufactured and marketed.
Still another object of the present invention is to provide a pocket billiards break shot training apparatus that simulates a racked set of balls on a pocket billiards table. This allows a player to participate in a practice session to enhance his or her break shot skill level.
Another object of the present invention is to provide a pocket billiards break shot training apparatus that permits a user to increase skill in controlling post break, cue ball positioning.
Lastly, it is an object of the present invention to provide a new pocket billiards break shot training apparatus that repositions itself after each shot. This permits a player to practice his or her break shot efficiently without continually gathering and re-racking the object balls.
These together with other objects of the invention, along with the various features of novelty that characterize the invention, are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its operating advantages and the specific objects attained by its uses, reference should be had to the accompanying drawings and descriptive matter in which there is illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be better understood and objects other than those set forth above will become apparent when consideration is given to the following detailed description thereof. Such description makes reference to the annexed drawings wherein:
FIG. 1 is a top plan view of the preferred embodiment of the pocket billiards break shot training apparatus constructed in accordance with the principles of the present invention.
FIG. 2 is a front perspective view (from above) of the training apparatus' cross-shaped frame.
FIG. 3A is an exploded view of the training apparatus' cross-shaped frame.
FIG. 3B is a left side view of the apparatus' alignment cartridge.
FIGS. 4A , 4 B, and 4 C are right side and front elevational views of the training apparatus' head, rear, and side balls, respectively.
FIG. 5 is a cross-sectional view of the training apparatus' cross-shaped frame.
FIG. 6 is a cross-sectional view of an alternative embodiment of the pocket billiards break shot training apparatus of the present invention. The same reference numerals refer to the same parts throughout the various figures.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, and particularly to FIGS. 1-6 , a preferred embodiment of the pocket billiards break shot training apparatus of the present invention is shown and generally designated by the reference numeral 10 . In FIG. 1 , a new pocket billiards break shot training apparatus 10 of the present invention for use in a practice session to simulate a break shot is illustrated and will be described. More particularly, the pocket billiards break shot training apparatus 10 has a cross-shaped frame 12 , a plurality of balls, an energy absorbing assembly 13 , a bow restraint assembly 14 , a first restraint cord 16 , and a second restraint cord 18 .
FIG. 2 further illustrates the apparatus' cross-shaped frame 12 . As shown in FIG. 2 , the cross-shaped frame comprises a main shaft 20 and a lateral shaft 94 . FIG. 3A better illustrates the intricacies of the main shaft 20 . The main shaft 20 is an elongated rod with a first end 30 and a second end 32 . The main shaft's first end 30 defines a first threaded receptacle 34 therein. Furthermore, the main shaft's second end 32 defines a second threaded receptacle 36 therein. Each bolt receptacle 34 , 36 is a bore in the end of the main shaft designed for threadable reception of a piece having external threads. A lateral bore 38 extends perpendicularly through the main shaft 20 . Moreover, the lateral bore 38 is located between the first threaded receptacle 34 and the second threaded receptacle 36 . The lateral shaft 94 is a threaded stud that has a first end 100 and a second end 102 . More specifically, the lateral shaft 94 is shaped and dimensioned for slidable insertion through the main shaft's lateral bore 38 .
In addition to the cross-shaped frame 12 , the pocket billiards break shot training apparatus 10 comprises a plurality of balls. The preferred embodiment has a head ball 22 , a rear ball 24 , a first side ball 26 , a second side ball 28 , and a center ball 120 . As illustrated in FIG. 4A , the head ball 22 has a generally spherical outer surface and defines a threaded bolt receptacle 40 therein. Similarly, the rear ball 24 has a generally spherical outer surface and defines a threaded stud receptacle 78 . Each bolt receptacle 40 , 78 is a bore in the ball designed for threadable reception of a piece having external threads.
FIG. 4C shows the first 26 and second 28 side balls. Each ball 26 , 28 has a generally spherical outer surface. The first side ball 26 defines a spacer receptacle 86 therein. Additionally, the first side ball 26 defines a bore 88 therethrough, extending from the spacer receptacle 86 to the outer surface at a point opposite the spacer receptacle 86 . Similarly, the second side ball 28 defines a spacer receptacle 90 therein. Moreover, the second side ball defines a bore 92 therethrough, extending from the spacer receptacle 90 to the outer surface at point opposite the spacer receptacle 90 . Each bolt receptacle 86 , 90 is a bore in the ball designed for threadable reception of a piece having external threads.
As shown in FIG. 4B , the center ball 120 has a generally spherical outer surface and defines a first bore 122 therethrough. Additionally, the center ball 120 defines a second bore 124 extending therethrough and aligned perpendicular to the first bore 122 . The first bore 122 is shaped and dimensioned for slidable reception of the main shaft 20 . On the other hand, the second bore 124 is shaped and dimensioned for slidable reception of the lateral shaft 94 .
In order to simulate a cue ball striking the head ball 22 in an actual game of pocket billiards, an energy absorbing assembly 13 is positioned between the cross-shaped frame 12 and the head ball 22 . FIG. 3A better illustrates the energy absorbing assembly 13 that connects the head ball 22 to the main shaft's first end 30 . The energy absorbing assembly 13 comprises a bolt 42 , an alignment cartridge 44 , a cylindrical spring 46 , and a spacer 48 . More specifically, the bolt 42 has a first end 50 and a second end 52 . The bolt's first end 50 is shaped and dimensioned for threadable insertion into the head ball's threaded bolt receptacle 40 . The bolt's second end 52 defines a tapered socket head 54 .
In addition to the bolt 42 , the alignment cartridge 44 shown in FIG. 3B is an integral part of the energy absorbing assembly 13 . The alignment cartridge 44 has a first end 56 and a second end 58 . Furthermore, the alignment cartridge defines a tapered bore 60 that extends from a first diameter 62 located at the first end 56 to a second diameter 64 located at the second end 58 . Moreover, the tapered bore 60 defines a third diameter 74 between the first 62 and second 64 diameters. The first diameter 62 is smaller than the second diameter 64 and the third diameter 74 is smaller than the first diameter 62 . Furthermore, the alignment cartridge's tapered bore 60 is shaped and dimensioned for slidable reception of the bolt's first end 50 . The alignment cartridge's second end 58 defines a set of external threads 66 . Moreover, the external threads 66 are shaped and dimensioned for threadable insertion into the main shaft's first threaded receptacle 34 .
The cylindrical spring 46 and spacer 48 interact with the bolt 42 and alignment cartridge 44 to form the energy absorbing assembly 13 . The cylindrical spring 46 defines a bore 66 extending therethrough. The cylindrical spring's bore 66 is shaped and dimensioned for slidable reception of the bolt's first end 50 . The spacer 48 has an exterior surface 70 and defines a threaded bore 72 therethrough. The spacer's threaded bore 72 is shaped and dimensioned for threadable reception of the bolt's first end 50 .
The head ball 22 connects to the bolt 42 by traversing the bolt's first end 50 through the alignment cartridge's tapered bore 60 from the cartridge's second end 58 to the cartridge's first end 56 , traversing the bolt's first end 50 through the cylindrical spring's bore 66 , threading the bolt's first end 50 through the spacer's threaded bore 72 , and threading the bolt's first end 50 into the head ball's threaded bolt receptacle 40 . After connecting the bolt 42 to the head ball 22 , the alignment cartridge's external threads 66 are threaded into the main shaft's first threaded receptacle 34 , securing the energy absorbing assembly 13 to the main shaft's first end 30 .
The rear ball is integrally attached to the main shaft 12 . FIG. 5 best illustrates the connection between the rear ball 24 and the main shaft's second end 32 . Generally, a threaded stud 80 connects the rear ball 24 to the main shaft's second end 32 . More specifically, the threaded stud 80 has a first end 82 that is shaped and dimensioned for threadable insertion into the rear ball's threaded stud receptacle 78 . Moreover, the threaded stud 80 has a second end 84 that is shaped and dimensioned for threadable insertion into the main shaft's second threaded receptacle 36 . Thus, the rear ball 24 and the main shaft's second end 32 are connected by threading the stud's first end 82 into the rear ball 24 and threading the stud's second end 84 into the main shaft's second end 32 .
The first 26 and second 28 side balls are attached to the lateral shaft 94 . FIG. 5 best illustrates the connection between the first 26 and the second 28 side balls and the lateral shaft 94 . The connection comprises a first spacer nut 96 , and a second spacer nut 98 . The first spacer nut 96 has a first end and a second end. Furthermore, the first spacer nut 96 defines a threaded shaft receptacle 108 therein. The first spacer nut's shaft receptacle 108 is shaped and dimensioned for threadable reception of the lateral shaft's first end 100 . The first spacer nut's second end defines a set of external threads 110 that are shaped and dimensioned for threadable insertion into the first side ball's spacer receptacle 86 . Thus, the first side ball 26 is attached to the lateral shaft's first end 100 by threading the first spacer nut's external threads 110 into the first side ball's spacer receptacle 86 and threading the lateral shaft's first end 100 into the first spacer nut's shaft receptacle 108 .
Similarly, the second spacer nut 98 has a first end 112 and a second end 114 . The second spacer nut 98 defines a threaded shaft receptacle 116 . The second spacer nut's shaft receptacle 116 is shaped and dimensioned for threadable reception of the lateral shaft's second end 102 . The second spacer nut's second end 114 defines a set of external threads 118 that are shaped and dimensioned for threadable insertion into the second side ball's spacer receptacle 90 . Thus, the second side ball 28 is attached to the lateral shaft's second end 102 by threading the second spacer nut's external threads 118 into the second side ball's spacer receptacle 90 and threading the lateral shaft's second end 102 into the second spacer nut's shaft receptacle 116 .
In the preferred embodiment, a center ball 120 is positioned between the first spacer nut 96 and the second spacer nut 98 . More particularly, the main shaft 20 passes through the center ball's first bore 122 . Additionally, the lateral shaft 94 passes through center ball's second bore 124 .
In addition to the cross-shaped frame 12 and energy absorbing assembly 13 , the pocket billiards break shot training apparatus 10 comprises a bow restraint assembly 14 . FIG. 1 best illustrates the bow restraint assembly 14 . The bow restraint assembly 14 further comprises a first rod 126 , a second rod 128 , and a joining rod 130 . Each rod 126 , 128 , and 130 is shaped and dimensioned to fit into the cavity between the rail cushion and surface of a pocket billiards table. Furthermore, the first rod 126 defines a bore therethrough. Similarly, the second rod 128 defines a bore therethrough. In the preferred embodiment, the first 126 and second rods 128 are constructed of a flexible, fiberglass-blended polymer.
The joining rod 130 has a first end 132 and a second end 134 . Moreover, the first end 132 defines a first rod receptacle 136 that is shaped and dimensioned for slidable reception of the first rod 126 . Similarly, the second end 134 defines a second rod receptacle 138 that is shaped and dimensioned for slidable reception of the second rod 128 . In the preferred embodiment, the joining rod is constructed of a durable, rigid plastic. Moreover the joining rod 130 may be constructed in different lengths to facilitate use on various table sizes. More particularly, use on seven foot, eight foot, or nine foot tables.
A flexible, fiberglass stabilizing tube 76 may be used to strengthen the stress points on the first 126 and second 128 rods. Each stabilizing tube 76 defines a bore therethrough that is shaped and dimensioned for slidable reception of either the first 126 or second 128 rod. In use, the first rod 126 is slid into a stabilizing tube 76 and then slid into the joining rod's first rod receptacle 136 . Similarly, the second rod 128 is slid into a stabilizing tube 76 and then slid into the joining rod's second receptacle 138 .
To facilitate use on different sized tables, the first 126 and second 128 rods are equipped with an adjustable extension assembly 206 . Each extension assembly 206 permits the length of either the first 126 or second 128 rod to be adjusted to fit any billiards table. The extension assembly 206 comprises an extension rod 208 and a fastening member 210 . The extension rod 208 is shaped and dimensioned for slidable insertion into and out of either the first 126 or second 128 rod's bore. When the fastening member 210 is loosened, the extension rod 208 may be repositioned by sliding it to a desired length. Tightening the fastening member 210 locks the extension rod 208 at the desired length.
The pocket billiards break shot training apparatus 10 further comprises a first restraint cord 16 and a second restraint cord 18 . The first restraint cord 16 has a first end 140 and a second end 142 . The first end 140 is removably attached to the first rod 126 opposite the joining rod 130 . As illustrated in FIG. 5 , the second end 142 extends through the first side ball's bore 88 and attaches to a lag bolt anchor 148 . Similarly, the second restraint cord 18 has a first end 144 and a second end 146 . The first end 144 is removably attached to the second rod 128 opposite the joining rod 130 . The second end 146 extends through the second side ball's bore 92 and attaches to a lag bolt anchor 150 .
While a preferred embodiment of the pocket billiards break shot training apparatus has been described in detail, it should be apparent that modifications and variations thereto are possible, all of which fall within the true spirit and scope of the invention. With respect to the above description then, it is to be realized that the optimum dimensional relationships for the parts of the invention, to include variations in size, materials, shape, form, function and manner of operation, assembly and use, are deemed readily apparent and obvious to one skilled in the art, and all equivalent relationships to those illustrated in the drawings and described in the specification are intended to be encompassed by the present invention.
For example, FIG. 6 illustrates an alternative embodiment of the cross-shaped frame 12 . Rather than attaching the balls by threading them to an adjacent piece, the alternative embodiment employs adhesive to connect the front 22 and rear 24 balls to the cross-shaped frame 12 . As shown in FIG. 6 , the alternative embodiment has a head nose piece 152 that connects to the head ball 22 . The head nose piece 152 has a first end 154 and a second end 156 . The first end 154 defines a barrel receptacle 158 therein. The barrel receptacle 158 is a bore in the head nose piece's first end 154 that is designed for slidable reception of a tube-shaped piece. Additionally, the head nose piece 152 defines a threaded bore 160 therethrough, extending from the first end 154 to the second end 156 . In order to receive the head nose piece 152 , the head ball 22 defines a nose piece receptacle 162 therein instead of a threaded bolt receptacle 40 as described in the previous embodiment. The nose piece receptacle 162 is shaped and dimensioned for slidable insertion of the head nose piece 152 . An adhesive 164 bonds the head nose piece 152 inside the nose piece receptacle 162 .
In this embodiment, the main shaft's second end 32 defines a rear nose piece 166 rather than a second threaded receptacle 36 . Furthermore, the rear ball 24 defines a nose piece receptacle 168 rather than a threaded stud receptacle 78 . The nose piece receptacle 168 is shaped and dimensioned for slidable reception of the rear nose piece 166 . An adhesive 170 bonds the rear nose piece 166 inside the nose piece receptacle 168 .
In addition to adhesively attaching the head 22 and rear 24 balls, the alternative embodiment utilizes tension to hold the first 26 and second 28 side balls in position. As shown in FIG. 6 , the alternative embodiment's lateral shaft 94 is an elongated tube 172 . The elongated tube 172 defines a bore 174 extending therethrough and is shaped and dimensioned for slidable insertion into the main shaft's lateral bore 38 . Furthermore, the elongated tube's bore 174 is shaped and dimensioned for slidable reception of a restraint cord 16 . In this embodiment, the first spacer nut 96 and the second spacer nut 98 are each replaced with a ball spacer 176 . Each ball spacer 176 is a washer-shaped piece defining an aperture therein.
To incorporate reception of the elongated tube 172 , the first side ball 26 defines a bore 178 therethrough rather than a spacer receptacle 86 . Similarly, the second side ball 28 defines a bore therethrough 180 rather than a spacer receptacle 90 . The side ball bores 178 , 180 are shaped and dimensioned for slidable reception of the elongated tube 172 . More particularly, the elongated tube 172 transverses the first side ball's bore 178 , transverses a spacer 176 , transverses the main shaft's lateral bore 38 , transverses a second spacer 176 , and transverses the second side ball's bore 180 . In use a restraint cord 16 attaches to the bow restraint assembly's first rod 126 , transverses the elongated tube 172 , and attaches to the bow restraint assembly's second rod 128 . A lag bolt anchor 148 located in the first side ball 26 and a lag bolt anchor 150 located in the second side ball 28 place a desired amount of tension on the restraint cord 16 to hold the side balls 26 , 28 and the spacers 176 in place.
In addition to the use of an adhesive and tension to replace the threaded ball connections, the alternative embodiment utilizes a solid elastomeric material to absorb the head ball's 22 energy rather than the cylindrical spring 46 . In this embodiment, the energy absorbing assembly comprises a barrel cartridge 182 , the head nose piece 152 , a barrel 194 , a first washer 196 , a second washer 198 , a set of three o-rings 200 , and a set of four backup rings 204 . The barrel cartridge 182 replaces the alignment cartridge 44 and the head nose piece 152 acts as the spacer 48 . The barrel cartridge 182 has a first end 184 and a second end 186 . The first end 184 defines a set of external threads 188 that are shaped and dimensioned for threadable insertion into the main shaft's first threaded receptacle 34 . The barrel cartridge's second end 186 defines a barrel receptacle 190 . Additionally, the barrel cartridge 182 defines a tapered bore 192 therethrough, extending from the first end 184 to the second end 186 . More particularly, the barrel cartridge's tapered bore 192 extends from a first diameter at the first end 184 to a second diameter at the barrel receptacle 190 . The first diameter is larger than the second diameter. Furthermore, the barrel cartridge's tapered bore 192 is shaped and dimensioned for slidable reception of the bolt's first end 50 .
The tube-shaped barrel 194 defines a bore extending therethrough. Moreover, the barrel 194 is shaped and dimensioned for slidable insertion into the head nose piece's barrel receptacle 158 and the barrel cartridge's barrel receptacle 190 . The first washer 196 is shaped and dimensioned for slidable reception of the bolt 42 and slidable insertion into the barrel cartridge's barrel receptacle 190 . Similarly, the second washer 198 is shaped and dimensioned for slidable reception of the bolt 42 and slidable insertion into the head nose piece's barrel receptacle 158 . The o-rings 200 are shaped and dimensioned to fit semi-loosely over the barrel 194 . Similarly, the backup rings 204 are shaped and dimensioned to fit semi-loosely over the barrel 194 . In use, the o-rings 200 and backup rings 204 are positioned on the barrel 194 in an alternating pattern. In other words, there is an o-ring 200 between each backup ring 204 .
The alternative embodiment of the energy absorbing portion connects together by placing the second washer 198 in the head nose piece's barrel receptacle 158 , placing the barrel 194 into the head nose piece's barrel receptacle 158 , sliding the o-rings 200 and backup rings 204 over the barrel 194 , sliding the first washer 196 into the barrel cartridge's barrel receptacle 190 , and sliding the exposed end of the barrel 194 into the barrel cartridge's barrel receptacle 190 . After positioning the barrel cartridge 182 , the assembly is completed by sliding the bolt's first end 50 through the barrel cartridge's bore 192 from the first end 184 to the second end 186 , sliding the bolt 42 through the first washer 196 , sliding the bolt 42 through the barrel's bore, sliding the bolt 42 through the second washer 198 , and threading the bolt 42 into the head nose piece's threaded bore 160 . Next, the barrel cartridge 182 is connected to the main shaft 20 by threading the barrel cartridge's external threads 188 into the main shaft's first threaded receptacle 34 .
Therefore, the foregoing is considered as illustrative only of the principles of the invention. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the invention to the exact construction and operation shown and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope of the invention. | A pocket billiards break shot training apparatus for improving the execution of a break shot. The training apparatus permits a user to make continuously repeated break shots without the time consuming necessity of gathering and re-racking the object balls after each shot. Moreover, the training apparatus permits a user to increase skill in controlling post break, cue ball positioning. The apparatus employs a head ball, rear ball, and two side balls oriented around cross-shaped frame to simulate a racked set of balls. Furthermore, the apparatus utilizes the compression of a spring element to sufficiently simulate the actual reaction of a set of racked balls to the impact of a cue ball. A bow restraint assembly interacts with a set of elastic cords to moor the frame in a desirable position on the table and reposition the frame after each shot. | 0 |
BACKGROUND OF THE INVENTION
1. Technical Field
The present invention relates to novel polyimidothioethers-inorganic nanoparticle hybrid material. More particularly, the present invention relates to polyimidothioethers-inorganic nanoparticle hybrid material, intermediate thereof and their preparation, wherein the hybrid material exhibits good surface planarity, thermal dimensional stability, tunable refractive index, and high optical transparency upon forming into films.
2. Description of Related Art
High refractive index polymers have been widely proposed in recent years for their potential in advanced optoelectronic applications. In addition to the basic parameter of the refractive index, the other ones such as birefringence, Abbe's number, optical transparency, proccessability, and thermal stability are often taken into consideration. Regarding the encapsulants for organic light-emitting diodes (OLEDs), commercial applications require materials with high refractive index, low birefringence, high optical transparency, and a long-term ultraviolet light and thermal stability. Therefore, to achieve a good combination of the above-mentioned parameters is a crucial and on-going issue (J. G. Liu and M. Ueda, J. Mater. Chem., 2009, 19, 8907). Recently, systematic work by Ueda revealed the influence of sulfur groups and related structures on the refractive index and optical dispersion of the resulted polyimides (C. A. Terraza, J. G. Liu, Y. Nakamura, Y. Shibasaki, S. Ando and M. Ueda, J. Polym. Sci., Part A: Polym. Chem., 2008, 46, 1510; N. H. You, Y. Suzuki, D. Yorifuji, S. Ando and M. Ueda, Macromolecules, 2008, 41, 6361; J. G. Liu, Y. Nakamura, Y. Shibasaki, S. Ando and M. Ueda, Macromolecules, 2007, 40, 4614; J. G. Liu, Y. Nakamura, Y. Suzuki, Y. Shibasaki, S. Ando and M. Ueda, Macromolecules, 2007, 40, 7902). The incorporation of sulfur atom into polymer systems could enhance the refractive index and optical transparency due to its large atomic refraction. It is also well known that the thermoset polyimides derived from bismaleimides (BMIs) exhibit excellent thermal and mechanical properties, thus made them extremely popular for advanced composites and electronics.
In addition, polymer-inorganic hybrid materials had recently attracted considerable interest owing to their enhanced mechanical, thermal, magnetic, optical, electronic, and optoelectronic properties when compared to the corresponding individual polymer or inorganic component. Chemical methods based on in-situ sol-gel hybridization approach made it possible to manipulate the organic/inorganic interfacial interactions at various molecular and nanometer length scales, resulting in homogeneous structures and thus overcoming the problem of nanoparticle agglomeration.
Based on the above mentioned industrial situation, the inventors of the present invention have investigated how to produce polyimides-inorganic nanoparticle hybrid material having optical transparency and thermoplasticity from BMI type monomer, and thus completed the present invention.
SUMMARY OF THE INVENTION
The present invention provides a polyimidothioethers-inorganic nanoparticle hybrid material, which comprises a polymer having repeat units represented by the following formula (I) and inorganic nanoparticles:
wherein, in the plurality of the repeat units, each X is the same or different and is at least one moiety selected from the group consisting of C 1-4 alkylene (preferably —CH 2 —), —S— and —SO 2 —; and in the plurality of the repeat units, in each repeat units is the same or different and is at least one moiety selected from the group consisting of C 1-4 alkylene, C 2-4 alkylene having at least one hydroxyl substituent, and a moiety of formula: -Ph-S-Ph- (wherein Ph represents phenylene), provided that in at least one repeat unit represents C 2-4 alkylene having at least one hydroxyl substituent; and n is a number of from 30 to 250, preferably from 40 to 180; wherein the inorganic nanoparticle is bonded to the polymer through the hydroxyl on , and the weight ratio of the polymer to the inorganic nanoparticle is from 95:5 to 40:60. In the above mentioned polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the C 2-4 alkylene having at least one hydroxyl substituent represented by is preferably a dihydroxybutylene group.
In the above mentioned polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the weight average molecular weight of the polymer part is from 16,200 to 312,800, preferably from 21,700 to 225,200.
In the above mentioned polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the polymer can be consisting of only one type of repeat unit or multiple types of repeat units each having different X and . For example, the polymer can consisting of a repeat unit in which X is C 1-4 alkylene and is C 2-4 alkylene having at least one hydroxyl substituent and a repeat unit in which X is —S— and is a group of formula -Ph-S-Ph- (wherein Ph represents phenylene); or consisting of a repeat unit in which X is C 1-4 alkylene and is C 2-4 alkylene having at least one hydroxyl substituent and a repeat unit in which X is —SO 2 — and is -Ph-S-Ph- (wherein Ph represents phenylene) simultaneously; or consisting of two or more types of repeat units in which each X and is defined as above, provided that in at least one repeat unit represents C 2-4 alkylene having at least one hydroxyl substituent. In other words, the polymer in the present polyimidothioethers-inorganic nanoparticle hybrid material can be consisting from the various repeat unit (I) as long as at least one group represents C 2-4 alkylene having at least one hydroxyl substituent
When the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention is formed into a film, in view of providing excellent dimension stability, the polymer not only comprises a repeat unit in which represents C 2-4 alkylene having at least one hydroxyl substituent, but also comprises the repeat units in which represents a group of formula -Ph-S-Ph- (wherein Ph represents phenylene).
In the above mentioned polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the inorganic nanoparticle is at least one oxide selected form the group consisting of titanium oxide, zirconium oxide, cerium oxide and silicon oxide.
In the above mentioned polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the hydroxyl group on the of the repeat units of formula (I) is to provide the bonding site with the inorganic nanoparticle.
According to the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, when producing into a film, the film has a refractive index of from 1.63 to 1.80 and a birefringence of from 0.0005 to 0.0034 of the polyimidothioethers, and transmittance of greater than 85% in the visible region (i.e. a range of wavelengths from 450 to 800 nm).
The present invention further relates to a method for preparing the present polyimidothioethers-inorganic nanoparticle hybrid material, comprising hydrolysis-condensing a polymer having the repeat units of formula (I) with an inorganic nanoparticle precursor through staged heating by using a sol-gel method under acidic conditions to obtain the polyimidothioethers-inorganic nanoparticle hybrid material. The term “staged heating” refers to the progress for curing the hybrid material at two or more temperatures each maintaining a certain period (for example, heating up to 150° C.). For example, the hybrid material is first pre-baked at 60° C. for 1 to 8 hours, and subsequently baked at 120° C. for 60 to 180 minutes. The resultant cured hybrid material is optionally further subjected to a hydrothermal process in 100° C. water, depending on the type of the inorganic nanoparticle precursor. Finally, the resultant material is dried at 100° C. for 5 to 8 hours in a vacuum oven.
In the method for preparing the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the inorganic nanoparticle precursor comprises alkoxide of titanium, zirconium, cerium and silicon, and the weight ratio of the polymer having the repeat unit of formula (I) to the inorganic nanoparticle precursor is from 95:5 to 40:60, preferably from 90:10 to 50:50.
In the method for preparing the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, the acidic condition which the hydrolysis-condensation carried out means a pH ranging from 4 to 7, which can be adjusted via adding acids, such as HCl.
In the method for preparing the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention, when the inorganic nanoparticle precursor is titanium alkoxide, the method further comprises a hydrothermal processing step for allowing the titanium oxide in the hybrid material to grow crystal into anatase type titanium oxide, which would increase the refreactive index of the hybrid material while imparting transparency without yellowing or discoloration. The term “hydrothermal processing step” refers to heating the hybrid material at 100° C. steam for several hours, preferably 8 to 12 hours, to allow the titanium oxide to grow crystal into anatase, resulting in increasing the refreactive index of the hybrid material. After hydrothermal processing step, the hybrid material is then dried at 100° C. in a vacuum oven.
The present invention further relates to a polyimidothioether intermediate, which comprises repeat units represented by the following formula (I):
wherein, in the plurality of the repeat units, each X is the same or different and is at least one moiety selected from the group consisting of C 1-4 alkylene (preferably —CH 2 —), —S— and —SO 2 —; and in each repeat units is the same or different and is at least one moiety selected from the group consisting of C 1-4 alkylene, C 2-4 alkylene having at least one hydroxyl substituent, and a moiety of formula: -Ph-S-Ph- (wherein Ph represents phenylene), provided that in at least one repeat unit represents C 2-4 alkylene having at least one hydroxyl substituent; and n is a number of from 30 to 250, preferably from 40 to 180.
The weight average molecular weight of polyimidothioether of the present invention is in a range of from 16,200 to 312,800, preferably from 21,700 to 225,200.
The polyimidothioether of the present invention is useful as an intermediate for synthesis the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention.
The present invention further relates to a method for preparing the present polyimidothioether intermediate, comprising: subjecting a bismaleimide of the following formula (II)
(wherein X is as defined above) to a Michael polyaddition reaction with a dithiol of the following formula (III):
(wherein {circle around (R)} is as defined above).
The above polyaddition reaction can be carried out in a solvent at room temperature in the presence of base as a catalyst.
In the above polyaddition reaction, the molar ratio of the bismaleimide of formula (II) to the dithiol of formula (III) is from 0.90:1.10 to 1.10:0.90, preferably from 0.95:1.05 to 1.05:0.95.
In the above polyaddition reaction, examples of the dithiol include (but is not limited to) 4,4′-thiobisbenzenethiol (DT-S), (2S,3R)-1,4-dimercapto-butane-2,3-diol (DT-OH), such dithiols can be used in one kind, or in a mixture of at least two kinds.
In the above polyaddition reaction, examples of the base catalyst include one or more selected from triethylamine, tri-n-propylamine, triisopropylamine, tri-n-butylamine and N,N,N′,N′-tetramethylethylenediamine. The solvent used in the reaction can be any type as long as it would not result in any adverse effects on the reaction, for example, a phenolic solvent including phenol, 4-methylphenol, m-cresol, etc., can be used as the solvent in the polyaddition reaction.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing the optical transmission spectra of polyimidothioether polymers prepared in Synthesis Examples 2 to 7.
FIG. 2 is a graph showing the transmittance UV-visible spectra of the polyimidothioether copolymer film prepared in Synthesis Example 5 and the hybrid material films (thickness: 15±3 μm) prepared in Examples 1 to 3.
FIG. 3 is a graph showing the variation of the refractive index of the polyimidothioether copolymer film prepared in Synthesis Example 5 and the hybrid material films prepared in Examples 1 to 3 with wavelength. The insert figure shows the variation of refractive index at 633 nm with titania content.
FIG. 4 is a graph showing XRD patterns of the polyimidothioether copolymer film prepared in Synthesis Example 5 and the hybrid material films prepared in Examples 1 to 3.
FIG. 5 is a TEM image of the hybrid material film prepared in Example 1, (a) top view, (b) cross-section.
FIG. 6 is a graph showing the variation of the reflectance with wavelength of the three-layer antireflection coating film prepared in Example 2.
DETAILED DESCRIPTION OF THE INVENTION
In the polyimidothioether having repeat units of formula (I) of the present invention, the C 1-4 alkylene represented by X in formula (I) means a straight chain or branched chain alkylene containing 1 to 4 carbon atoms, for example, methylene, ethylene, propylene, isopropylene, butylene, isobutylene, etc, preferably methylene (—CH 2 —).
Similarly, in the polyimidothioether having repeat units of formula (I) of the present invention, the C 1-4 alkylene represented by in formula (I) means a straight chain or branched chain alkylene containing 1 to 4 carbon atoms, for example, methylene, ethylene, propylene, isopropylene, n-butylene, isobutylene, etc, preferably n-butylene.
The C 2-4 alkylene having at least one hydroxyl substituent, represented by in formula (I) means a straight chain or branched chain containing 2 to 4 carbon atoms and having at least one, preferably at least two hydroxyl substituents, such as hydroxylethylene, 1,2-dihydroxylethylene, 1-hydroxylpropylene, 2-hydroxylpropylene, 1,2-dihydroxylpropylene, 1,3-dihydroxylpropylene, 1-hydroxyl-n-butylene, 2-hydroxyl-n-butylene, 1,2-dihydroxyl-n-butylene, 1,3-dihydroxyl-n-butylene, 2,3-dihydroxyl-n-butylene, etc.
EXAMPLES
The starting material of the present invention, bismaleimide, which is represented by formula (II), is synthesized by conventional methods. For example, it can be synthesized by reacting corresponding diaminodiphenylsulfide with maleic anhydride according to the method described in F. P. Glatz and R. Mulhaup, High Performance Polymers, 1993, 5, 213, or reacting diaminodiphenylsulfone with maleic anhydride according to the method described in B. S. Rao, R. Sireesha and A. R. Pasala, Polym. Int., 2005, 54, 1103. Specific examples will described in the following Synthesis Examples. Certain bismaleimide of formula (II) such as 4,4′-(diaminodiphenylmethane)bismaleimide (CH 2 -BMI) is commercially available.
Material
4,4′-(diaminodiphenylsulfide)bismaleimide (S-BMI) (corresponding to X representing —S— in the formula (II)) was synthesized by reacting 4,4′-diaminodiphenylsulfide with maleic anhydride according to the method described in F. P. Glatz and R. Mulhaup, High Performance Polymers, 1993, 5, 213, mp: 187° C. 4,4′-(diaminodiphenylsulfone)bismaleimide (SO 2 -BMI) (corresponding to X representing —SO 2 — in the formula (II)) was synthesized by reacting 4,4′-diaminodiphenylsulfone with maleic anhydride according to the method described in B. S. Rao, R. Sireesha and A. R. Pasala, Polym. Int., 2005, 54, 1103, mp: 252° C. 4,4′-(diamino-diphenylmethane)bismaleimide (CH 2 -BMI) (corresponding to X representing —CH 2 — in the formula (II)), (2S,3R)-1,4-dimercaptobutane-2,3-diol (DT-OH) and 4,4′-thiobisbenzenethiol (DT-S) were received from commercial sources and were used as received.
Synthesis Example 1
Synthesis of S-BMI and SO 2 -BMI
To a 250 ml three-neck round bottomed flask equipped with addition tube and purged with nitrogen gas, an acetone solution (100 ml) containing 9.44 g (96.28 mmol) of maleic anhydride was added. Then, an acetone solution (40 ml) containing 8.87 g (41.00 mmol) of compound 1 was slowly added dropwise into the three-neck round bottomed flask through the addition tube, and stirred at −5° C. to carry out reaction for 12 hours. After the reaction completed, the solid was filtered and washed with acetone to give 16.84 g (99.6% in yield) of light yellow solid product 2 after drying.
A 250 ml three-neck round bottomed flask was equipped with addition tube and purged with nitrogen gas, and then placed in oil bath. To the three-neck round bottomed flask, an acetone solution (180 ml) containing 16.84 g (40.83 mmol) of compound 2 and 3.75 g (45.72 mmol) of sodium acetate anhydrous were added. Then, 32.61 g (319.42 mmol) of acetic anhydride was slowly added dropwise into the three-neck round bottomed flask through the addition tube. The mixture was warmed to 80° C. slowly, refluxed and mixed for 10 hours. After washing and crystallization, 9.20 g of light yellow solid product 3 (60.0% in yield) was obtained. The flow chart of the aforementioned reaction is as follows (scheme 1):
Polymer Synthesis
Synthesis Example 2
Synthesis of 4,4′-(diaminodiphenylsulfide)bismaleimide-2,3-dihydroxylbutylenedithioether polymer (S—OH)
S-BMI (1.8819 g, 5 mmol) was dissolved in 12 ml of m-cresol, and (2S,3R)-1,4-dimercaptobutane-2,3-diol (DT-OH) (0.7712 mg, 5 mmol) was added into the mixture and stirred for 10 minutes. Then, 25 μl of triethylamine was slowly added to carry out Michael polyaddition reaction for 4 hours at room temperature. During the polyaddition reaction, the viscosity of the solution gradually increased. Then the resultant polymer solutions were added into 300 ml of acidic methanol to allow the polymer precipitated as white fibroid solid. The precipitates were collected by filtration and washed thoroughly with methanol and dried in vacuum at 100° C. For further purification, the precipitation from dimethyl acetamide (DMAc) to methanol was conducted twice. The obtained S—OH polymer (corresponding to polymer having the repeat units represented by the above formula (I), wherein X is —S— and {circle around (R)} is C 2-4 alkylene having at least one hydroxyl substituent) has a weight average molecular weight of 132,100. The flow chart of the aforementioned reaction is as follows (scheme 2):
Synthesis Example 3
Synthesis of 4,4′-(diaminodiphenylmethane)bismaleimide-2,3-dihydroxylbutylenedithioether polymer (CH 2 —OH)
CH 2 —OH polymer (corresponding to polymer having the repeat units represented by the above formula (I), wherein X is —CH 2 — and {circle around (R)} is C 2-4 alkylene having at least one hydroxyl substituent) was prepared by the same procedures described in Synthesis Example 2 except that S-BMI was instead of CH 2 -BMI. The obtained polymer has a weight average molecular weight of 133,700.
Synthesis Example 4
Synthesis of 4,4′-(diaminodiphenylsulfone)bismaleimide-2,3-dihydroxylbutylenedithioether polymer (SO 2 —OH)
SO 2 —OH polymer (corresponding to polymer having the repeat units represented by the above formula (I), wherein X is —SO 2 — and {circle around (R)} is C 2-4 alkylene having at least one hydroxyl substituent) was prepared by the same procedures described in Synthesis Example 2 except that S-BMI was instead of SO 2 -BMI. The obtained polymer has a weight average molecular weight of 103,700.
Synthesis Example 5
Synthesis of 4,4′-(diaminodiphenylsulfide)bismaleimide-2,3-dihydroxylbutylenedithioether-co-4,4′-(diaminodiphenylsulfide)bismaleimide-4,4′-thiodiphenylsulfide copolymer (S—OHS)
S-BMI (1.8819 g, 5 mmol) was dissolved in 12 ml of m-cresol, and 4,4′-thiobisbenzenethiol (DT-S) (0.6260 mg, 2.5 mmol) and (2S,3R)-1,4-dimercaptobutane-2,3-diol (DT-OH) (0.3856 mg, 2.5 mmol) were added into the mixture and stirred for 10 minutes. Then, 25 μl of triethylamine was slowly added to carry out Michael polyaddition reaction for 4 hours at room temperature. During the polyaddition reaction, the viscosity of the solution gradually increased. Then the resultant polymer solutions were added into 300 ml of acidic methanol to allow the polymer precipitated as white fibroid solid. The precipitates were collected by filtration and washed thoroughly with methanol and dried in vacuum at 100° C. For further purification, the precipitation from dimethyl acetamide (DMAc) to methanol was conducted twice. The obtained S—OHS polymer (corresponding to polymer having the repeat units represented by the above formula (I), wherein X is —S— and {circle around (R)} represents C 2-4 alkylene having at least one hydroxyl substituent and a formula: -Ph-S-Ph- (wherein Ph represents phenylene)) has a weight average molecular weight of 120,500. The flow chart of the aforementioned reaction is as follows (scheme 3):
The obtained S—OHS had inherent viscosities in the range of 0.33-1.25 dL/g (measured at a concentration of 0.5 g/dL in DMAc at 30° C. using Tamson TV-200 viscometer). IR (measured by Fourier Transform Infrared spectrometer (FTIR)) (KBr, ν cm −1 ): 3200-3700 (O—H stretch), 1781 (asymmetry C═O stretch), 1713 (symmetry C═O stretch), 1383 (C—N), 1082 (Ar—S—Ar stretch), 725 (imide ring deformation), respectively. Anal. Calcd. (%) for S—OHS (C 58 H 50 N 4 O 10 S 7 ) n (1187.49) n :C, 58.66; H, 4.24; N, 4.72; S, 18.90. Found: C, 56.65; H, 3.97; N, 4.69; S, 18.62.
Synthesis Example 6
Synthesis of 4,4′-(diaminodiphenylmethane)bismaleimide-2,3-dihydroxylbutylenedithioether-co-4,4′-(diaminodiphenylmethyl)bismaleimide-4,4′-thiodiphenylsulfide copolymer
CH 2 -BMI (1.7917 g, 5 mmol) was dissolved in 12 ml of m-cresol, and 4,4′-thiobisbenzenethiol (DT-S) (0.6260 mg, 2.5 mmol) and (2S,3R)-1,4-dimercaptobutane-2,3-diol (DT-OH) (0.3856 mg, 2.5 mmol) were added into the mixture and stirred for 10 minutes. Then, 25 μl of triethylamine was slowly added to carry out Michael polyaddition addition for 4 hours at room temperature. During the polyaddition addition, the viscosity of the solution gradually increased Then the resultant polymer solutions was added into 300 ml of acidic methanol to allow the polymer precipitated as white fibroid solid. The precipitates were collected by filtration and washed thoroughly with methanol and dried in vacuum at 100° C. For further purification, the precipitation from dimethyl acetamide (DMAc) to methanol was conducted twice. The obtained CH 2 —OHS polymer (corresponding to polymer having the repeat units represented by the above formula (I), wherein X is —CH 2 — and {circle around (R)} represents C 2-4 alkylene having at least one hydroxyl substituent and a formula: -Ph-S-Ph- (wherein Ph represents phenylene)) has a weight average molecular weight of 123,700.
Synthesis Example 7
Synthesis of 4,4′-(diaminodiphenylsulfone)bismaleimide-2,3-dihydroxylbutylenedithioether-co-4,4′-(diaminodiphenylsulfone)bismaleimide-4,4′-thiodiphenylsulfide copolymer
SO 2 -BMI (2.0419 g, 5 mmol) was dissolved in 12 ml of m-cresol, and then 4,4′-thiobisbenzenethiol (DT-S) (0.6260 mg, 2.5 mmol) and (2S,3R)-1,4-dimercaptobutane-2,3-diol (DT-OH) (0.3856 mg, 2.5 mmol) were added into the mixture and stirred for 10 minutes. Then, 25 μl of triethylamine was slowly added to carry out Michael polyaddition addition for 4 hours at room temperature. During the polyaddition reaction, the viscosity of the solution gradually increased. Then the resultant polymer solutions were added into 300 ml of acidic methanol to allow the polymer precipitated as white fibroid solid. The precipitates were collected by filtration and washed thoroughly with methanol and dried in vacuum at 100° C. For further purification, the precipitation from dimethyl acetamide (DMAc) to methanol was conducted twice. The obtained SO 2 —OHS polymer (corresponding to polymer having the repeat units represented by the above formula (I), wherein X is —SO 2 — and {circle around (R)} represents C 2-4 alkylene having at least one hydroxyl substituent and a formula: -Ph-S-Ph- (wherein Ph represents phenylene)) has a weight average molecular weight of 119,700.
Experimental Example 1
Preparation of Polyimidothioether Films
N-methyl-2-pyrrolidone (NMP) solution dissolving with the synthesized polyimidothioether copolymer of Synthesis Examples 2 to 7 (concentration ranged between 12.0 to 18.0 wt %) was drop-coated onto fused silica (amorphous SiO 2 ) or glass substrates and dried at 80° C. for 6 hours, and then at 150° C. for 8 hours under vacuum condition. Finally, polyimidothioether films with thicknesses of 20 μm were obtained and used for solubility tests, refractive index, transmittance, and thermal analyses. The results were shown in the following Table 1, where commercial optical film Kapton was used as a control. The optical transmission spectra of each film were shown in FIG. 1 . It can be seen from FIG. 1 that all the polymer films exhibited high transparency (>85%) in visible region (wavelengths: 450 to 800 nm).
TABLE 1
Properties of Polyimidothioethers
Thermal P roperties (° C.)
Optical Properties
Index
η inh (dL/g) a
T s b
T d c
ΔT d
λ 0 (nm) e
n f
Δn g
CH 2 —OH
1.25
80
301
221
310
1.637
0.0031
S—OH
1.01
85
303
218
327
1.660
0.0018
SO 2 —OH
0.35
92
267
175
312
1.648
0.0045
CH 2 —OHS
0.46
85
304
219
336
1.672
0.0005
S—OHS
0.50
103
317
214
338
1.692
0.0010
SO 2 —OHS
0.33
110
281
171
337
1.680
0.0022
Kapton
452
1.687
0.0770
a Measured at a polymer concentration of 0.5 g/dL in DMAc at 30° C.
b Softening temperature measured by TMA with a constant applied load of 10 mN at a heatingrate of 10° C. min −1 by penetration mode.
c Initial decomposition temperature recorded by TGA.
d The melting-process window (ΔT) was calculated as ΔT = T d − T s .
e The cutoff wavelength (λ 0 ) from the UV-vis transmission spectra of polymer films (thickness ~20 μm).
f Refractive index at 633 nm by ellipsometer.
g The in-plane/out-of-plane birefringence (Δn) was calculated as Δn = n TE − n TM were measured using a prism coupler.
From the above Table 1, these polyimidothioether films revealed the ultra-lowest birefringence values in the range of 0.0005 to 0.0034 and refractive indices about 1.63 to 1.69. Regarding optical transparency, as shown in Table 1, λ 0 value of the polyimidothioether films of the present invention was between 300 nm to 350 nm (outside of the range of visible wavelength), whereas λ 0 value of the commercial Kapton optical film was 452 nm (in the range of visible wavelength). Thus, the commercial Kapton optical film reveal color under visible light. In addition, as shown in Table 1, the polyimidothioether films of the present invention exhibited good thermal stability with insignificant weight loss up to 260° C. Accordingly, the polyimidothioether films of the present invention have excellent transparency in visible light region and low chromaticity, indicated their potential optical applications.
Example 1
0.117 g (0.10 mmol) of S—OHS solution of Synthesis Example 5 was dissolved in 5 ml of dimethylacetamide, then 0.498 g (1.46 mmol) of Ti(OBu) 4 was added drop-wise into the above solution by a syringe and stirred thoroughly. To the above mixture, 0.167 g (37 wt %) of HCl was added very slowly and further stirred at room temperature for 30 minutes to carry out hydrolysis condensation thus to obtain a precursor solution. The resulting precursor solution was filtered through a 0.45 mm PTFE filter and the filtered solution was then drained into film at room temperature for 6 hours under vacuum condition. The film was soft baked at 60° C. for 6 hours, baked at 120° C. for 150 minutes and then treated by hydrothermal process at 100° C. steam for 12 hours. Finally, the film was dried at 100° C. to obtain a hybrid film having 50 wt % of titanium oxide, called S—OHS50 for short, where the number 50 refers to the weight ratio of titanium oxide in the film.
Example 2
A hybrid film having 10 wt % of titanium oxide (called S—OHS 10 for short) was prepared by the same procedures described in Example 1 except that the weight ratio of S—OHS:Ti(OBu) 4 was changed to 90:10.
Example 3
A hybrid film having 30 wt % of titanium oxide (called S—OHS30 for short) was prepared by the same procedures described in Example 1 except that the weight ratio of S—OHS:Ti(OBu) 4 was changed to 70:30.
The flow chart of the aforementioned reaction is as follows (scheme 4):
X in S—OHSX of the above scheme refers to the weight percentage of titanium dioxide in the hybrid material.
The reactant composition, weight percentage of titanium dioxide in the hybrid films, and the thickness, toughness and refractive index of the polyimidothioether film prepared by the polymer of Synthesis Example 5 and the hybrid films of Examples 1 to 3 were shown in the following Table 2, and the optical and thermal properties were shown in the following Table 3, XRD patterns was shown in FIG. 4 . TEM image of the hybrid film of Example 1 was shown in FIG. 5 , (a) top view, (b) cross-section.
TABLE 2
Reaction composition and properties of the polyimidothioether film prepared by
the polymer of Synthesis Example 5 and the hybrid films of Examples 1 to 3
Reactant compostition (wt %)
Hybrid film TiO 2 conten (wt %)
Polmer
S-OHS
Ti(OBu) 4
Theoretical
Experimental a
h b /nm
R q c /nm
n d
S—OHS
100
0
0
0
253
2.035
1.69
S—OHS10
67.8
32.2
10
9.8
271
1.874
1.72
S—OHS30
35.4
64.6
30
28.3
284
1.263
1.77
S—OHS50
19.0
81.0
50
49.4
325
0.951
1.80
a Experimental titania content estimated from TGA curves.
b h: Film thickness.
c R q : The root mean square roughness.
d n: Refractive index at 633 nm by ellipsometer.
TABLE 3
Thermal Properties of the polyimidothioether film
prepared by the polymer of Synthesis Example 5
and the hybrid films of Examples 1 to 3
CTE
Td 5 /° C. c
Td 10 /° C. c
Polmer
Ts a
(ppm/K) b
N 2
Air
N 2
Air
R w800 (%) d
S—OHS
103
88
320
325
345
355
33
S—OHS10
172
72
380
405
450
470
61
S—OHS30
205
57
400
410
460
470
69
S—OHS50
231
45
390
390
450
450
76
a Softening temperature measured by TMA with a constant applied load of 10 mN at a heatingrate of 10° C. min −1 by penetration mode.
b The CTE data was determined over a 50-200° C. range by expansion mode.
c Temperature at which 5% and 10% weight loss occurred, respectively, recorded by TGA at a heating rate of 20° C. min −1 and a gas flow rate of 30 cm 3 min −1 .
d Residual weight percentages at 800° C. under nitrogen flow.
f Experimental titania content estimated from TGA curves.
As shown in FIG. 2 , the refractive index at 633 nm of the hybrid material film increased linearly with increasing titanium dioxide contents, suggesting that the Ti—OH groups of the hydrolyzed precursor condensed progressively to form the Ti—O—Ti structures and resulted in an enhanced refractive index. Furthermore, the refractive index of the hybrid film can be enhanced obviously owing to the TiO 2 in the hybrid film can be crystallized via hydrothermal treatment, and the transparency of the hybrid film can be maintained without yellowing. FIG. 4 revealed that the intensity of a titanina crystalline peak gradually increased with increasing titania content, suggesting that the titania clusters were well dispersed in polymers because of hydrolysis-condensation reactions occurred between Ti(OBu) 4 and pendent hydroxyl groups of the polyimidothioether polymer. The hybrid film shown in FIG. 5 exhibited the titania nanocrystallites with the average size of 3 to 5 nm and well dispersed in the hybrid material.
In Table 2, the ratio of surface roughness to film thickness (Rq/h) was less than 0.15% implying the excellent surface planarity of the hybrid film. In addition, as can be seen in Table 3, the softening temperature increased from 103° C. to 231° C. with the increasing titania content, and CTE of the hybrid films decreased with increasing the volume fractions of inorganic reinforcement.
Example 2
Preparation of Multilayer Antireflection Coating Films
Onto the glass substrate, SiO2, S—OHS30 prepared by Example 3 and S—OHS10 prepared by Example 2 were coated in sequence, the thickness and refractive index were 102 nm and 1.29; 151 nm and 1.79; 78 nm and 1.73, respectively. The glass substrate usually revealed a refractive index (n=1.52) higher than air (n=1.0) and had an average reflectance of about 4.5% in the visible range. As shown in FIG. 6 , the reflectance of prepared anti-reflection coatings was less than 0.7% in the visible range (400 nm to 700 nm), which was significantly smaller than that of the glass with 4.5%. Thus, it suggested the potential application of the prepared hybrid films in optical devices.
According to the present invention, a series of thermoplastic polyimidothioethers are readily prepared from a variety of bismaleimides and dithiols through the Michael polyaddition, then the bonding between organic and inorganic materials is provided by utilizing the hydroxyl group on the polyimidothioethers, and hence hydrolytic condensation with an inorganic oxide precursor occurs to obtain a hybrid material of polyimidothioethers-inorganic nanoparticles where inorganic nanoparticles are fully dispersed in the polyimidothioether polymer. Furthermore, according to the method of the present invention, it is easy to control the proportion of inorganic nanoparticles in the film of the hybrid material and hence the desired optical properties. In addition, a considerably high amount of titanium oxide may be added thereto and a refractive index up to 1.80 may be achieved, so it has potential for use in optical applications.
Moreover, due to its good solubility in organic solvents, the polyimidothioethers-inorganic nanoparticle hybrid material of the present invention is suitable for solution-casting, spin-coating, inkjet-printing or injection-molding processes for optical practical applications. | The present invention relates to novel polyimidothioethers-inorganic nanoparticle hybrid material, which exhibit good surface planarity, thermal dimensional stability, tunable refractive index, and high optical transparency upon forming into films. The present invention also relates to polyimidothioethers which is an intermediate for preparing the present hybrid material, and their preparation. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the chemical arts. More particularly, this invention relates to the recovery of sulfur from a gas stream rich in hydrogen sulfide using the Claus process.
2. Discussion of the Related Art
It is known in the prior art to recover elemental sulfur from hydrogen sulfide (H 2 S) containing acid gas streams as is set forth in the article “Fundamentals of Sulfur Recovery by the Claus Process” by B. Gene Goar, published in the 1977 Gas Conditioning Conference Report. The Claus reaction is represented by the following equation:
4H 2 S+2SO 2 →3S 2 +4H 2 O
Claus sulfur recovery units (SRU's) are widely utilized to recover sulfur from acid gas streams produced in natural gas purification and in petroleum refineries, primarily from amine sweetening. In refineries, the H 2 S is in crude oil and is contained in hydrocarbon desulphurization unit off gases and fluidized catalytic cracker unit off gases. Oftentimes, the acid gas stream produced from the amine unit is quite rich in H2S, particularly in petroleum refineries, where it may be 80–95 mol % H 2 S. Also in many refineries, the Claus plant units are either fully loaded or subject to becoming fully loaded (capacity limited) due to the processing of heavy crude oils, which contain relatively large amounts of sulfur compounds. With the dwindling known reserves of refinable hydrocarbons and crude oils, less attractive known oil reserves are now being processed, which less attractive oil reserves typically have high sulfur contents. The trend in refining such high sulfur containing feedstocks will increase in the future. Additionally, the requirements to produce lower sulfur fuels will result in more acid gases containing H 2 S. Therefore, it is a desideratum to increase the capacity of Claus plants to process sulfur.
In conventional Claus sulfur recovery systems, the feed pressure of the acid gas feed stream is only about 12 psig. This low pressure level does not provide enough driving force to allow a significant increase in the amount of acid gas feed that can be passed through the many items of equipment that constitute a typical Claus SRU. As Claus SRU feed rates are increased above capacity, several problems develop. At increased flow, the pressure drop through the Claus plant and tail gas cleanup unit increases, and the back pressure increase requires H 2 S and air feed inlet pressures beyond what is available from the amine regenerator that supplies the acid gas feed and the air blower that provides feed air. The increased flow also decreases the residence times and increases the space velocity in the reaction furnace and the catalytic reactor stages, which reduces conversion to sulfur and increases emissions to the tail gas cleanup unit. The increased flow also results in overloading some or all of the heat exchangers in the SRU, which may reduce conversion of H 2 S to sulfur and also increases sulfur vapor carryover to the tail gas unit. The increased flow to the tail gas cleanup unit increases its pressure drop and further lowers tail gas sulfur recovery, which ultimately leads to increased and usually unacceptable sulfur emissions. The increased back pressures may in some Claus plants pose the risk of blowing the liquid sulfur drain seals, which would release process gas containing highly toxic H 2 S into the atmosphere. While booster blowers for the H 2 S and air feeds, and higher pressure sulfur liquid drain seals can provide some increase in capacity, these measures will not overcome problems associated with undersized heat exchange equipment, reduced sulfur conversion, or increased sulfur emissions.
It is also known to use oxygen enrichment in the operation of a Claus sulfur plant in order to increase the capacity of H 2 S handled as well as the total throughput of the plant as set forth in the article “Oxygen Use in Claus Sulfur Plants” by M. R. Gray and W. Y. Svrcek published in the 1981 Gas Conditioning Conference Report. In that article, it was disclosed that oxygen can be added in the air feed to the burner of a Claus reaction furnace in order to increase the amount of H 2 S which is combusted to sulfur dioxide (SO 2 ) for later catalytic conversion, with additional H 2 S to the elemental liquid sulfur product of the Claus process. The combustion reaction of H 2 S with oxygen (whether pure oxygen or air) can be represented by the following equation:
2H 2 S+3O 2 2SO 2 +2H 2 O (Equation 2)
The Gray and Svrcek article recites that the pressure drop through the plant and the reactor space velocities determine the maximum capacity increase which can be achieved with oxygen enrichment. Consequently, it is a desideratum to improve efficiency by reducing the amount of air, thereby maximizing the amount of oxygen available to react with the H 2 S.
However, a further limitation set forth in the Gray and Svrcek article is that for a given plant stream, temperatures and sulfur condenser capacity may limit the potential capacity increase using oxygen enrichment. Specifically, stream temperatures in the reaction furnace and in the converter beds may increase due to oxygen enrichment and, in fact, such increase from oxygen enrichment reaches the maximum tolerable temperature of the materials used in such a furnace, namely the refractory lining. Similarly, in the 1983 publication by Linde of Union Carbide entitled “Claus Plant Oxygen Enrichment,” it is noted that oxygen-enrichment limitations exist for H 2 S rich streams due to temperature limits in the furnace or waste heat boiler of a Claus plant. Therefore, it is also a desideratum to moderate the temperature in the Claus reaction furnace.
It is also known in the prior art to recycle effluent gases back into the Claus reaction furnace. For example, U.S. Pat. No. 3,681,024 discloses the addition of oxygen and a recycle gas to a Claus reaction furnace. Combustion gases from a reactor unit are first sent to a water scrubber to reduce the water content of the effluent, and a sufficient amount of the scrubber off gases are then recycled to dilute the oxygen feed so that furnace conditions are essentially equivalent to operation with air.
U.S. Pat. No. 3,822,341 describes a Claus plant using oxygen enrichment in which water is removed from the combustion gases, first in a liquid vapor contractor and then in an SO 2 stripper, before the reaction gases are recycled to a waste heat boiler.
U.S. Pat. No. 4,756,900 discloses a process for splitting the effluent from the waste heat boiler of a Claus reaction furnace and recycling a portion thereof using a separate sulfur condenser and a mechanical blower to moderate the high furnace temperatures induced by oxygen-enrichment.
U.S. Pat. No. 4,552,747 describes a process for moderating the high temperatures in a Claus reaction furnace induced by oxygen-enrichment by passing reaction gases through a sulfur condenser and then using a mechanical blower to recycle the resulting effluent stream back to the Claus reaction furnace. U.S. Pat. No. 6,508,998 describes a process for moderating the high temperatures in a Claus reaction furnace induced by oxygen-enrichment by passing reaction gases through a sulfur condenser and then using an eductor to recycle the resulting effluent stream back to the Claus reaction furnace.
There remains a definite need for a simple and effective system and process for recovering elemental sulfur from H 2 S containing gas streams that minimizes the amount of air required in a Claus reaction furnace. There remains a further definite need for such a system and process that allows the processing of more acid gas through the system. There remains a still further definite need for such a system and process that moderates the temperature in the Claus reaction furnace. The present invention satisfies these and other needs, and provides further related advantages.
SUMMARY OF THE INVENTION
Now in accordance with the invention there has been found a simple and effective system and process employing steam to minimize the amount of air required in a Claus reaction furnace, to maximize the feed rate of the acid gas stream, and to moderate the temperature in the furnace. The method includes partially combusting a feed gas stream rich in hydrogen sulfide with an oxygen-enriched gas in a Claus reaction furnace to produce to a combustion reaction product stream containing sulfur. In some embodiments, one or more feed gas streams rich in hydrogen sulfide, air, and supplemental oxygen are introduced into the Claus reaction furnace to form a mixture including the feed gas stream rich in hydrogen sulfide which is then partially combusted. The resulting combustion reaction product stream is split into a recycle stream and a treatment stream. The recycle stream is then directed back into the Claus reaction furnace, without first condensing sulfur out of the stream; while the treatment stream is directed into a condenser to condense out sulfur.
In some embodiments, the recycle stream is passed through a pressure booster, such as a blower or an eductor before the stream enters the Clause reaction furnace. And in some embodiments the pressure of the recycle stream as it leaves the pressure booster is from about 20 to about 30 psia, preferably from 23 to about 27 psia.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a flow diagram of a Claus reactor system in accordance with the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Particular embodiments of the invention are described below in considerable detail for the purpose of illustrating its principles and operation. However, various modifications may be made, and the scope of the invention is not limited to the exemplary embodiments described below. For example, in the embodiments described below, there is described a reaction furnace that includes both a burner and a reaction chamber and the reactants are introduced into the burner. However, one skilled in the art will understand that the reactants can be introduced directly into a reaction chamber. Similarly, in the embodiments described below, only one acid gas feed stream is shown. One skilled in the art will understand that the acid gas can be supplied in one or more streams.
Shown in FIG. 1 is a Claus reactor system in accordance with the invention. An acid gas feed stream rich in H 2 S is introduced from an acid gas source, such as the acid gas produced by a petroleum refining plant (not shown), through at least one acid gas feed line 10 into a Claus reaction furnace 21 . In the embodiment shown in FIG. 1 , the Claus reaction furnace includes a burner 20 and a reaction chamber 22 , such that the reactants are partially combusted in burner 20 and evolved into the reaction furnace 22 .
Typically, the H 2 S content of such feed streams is from about 50 to about 95 mol %. The feed stream is introduced into the reaction furnace 21 at a temperature generally of from about 350° to about 650° F., preferably from about 400° to about 600° F., and more preferably from about 450° to about 550° F., and at a pressure generally of from about 20 to about 30 psia, preferably from about 22 to about 28 psia, and more preferably from about 23 to about 27 psia. An oxygen stream, such as a stream of commercially pure oxygen or oxygen-enriched air, is provided to the reaction furnace 21 through an oxygen supply line 12 . In the embodiment shown in FIG. 1 , a stream of commercially pure oxygen is provided by the oxygen supply line, while an air stream is separately provided through air supply line 14 at an elevated pressure, typically of from about 20 to about 30 psia, preferably from about 22 to about 28 psia, and more preferably from about 23 to about 27 psia, from compressor 16 .
The concentration of oxygen contained in the sum of oxygen stream 12 and air stream 14 entering the Claus reaction furnace 21 is typically from about 25 mol % to about 100 mol %, preferably from about 35 mol % to about 95 mol %. It is a significant advantage in accordance with the invention that the oxygen concentration in the Claus reaction furnace can be increased above the levels of those employed in conventional Claus recovery systems. In turn, the capacity of the Claus plant is increased due to the increased oxygen concentration, which backs out air flow.
The resulting reactant mixture is combusted in burner 20 and evolved into reaction chamber 22 , of the reaction furnace 21 , where the reactions of the oxygen-enhanced Claus process occur. The operating temperature in the reaction chamber is preferable at a temperature greater than about 2400° F., and more preferably greater than about 2600° F.
As illustrated in the combustion reaction (Equation 2), oxygen contained in the air and/or oxygen streams reacts with some of the H 2 S in the acid gas feed stream to produce SO 2 and H 2 O. It can be see from the stoichiometry of the Claus reaction (Equation 1), that the combustion reaction consumes about one-third of the H 2 S initially contained in the acid gas feed stream. The SO 2 produced in accordance with the combustion reaction then reacts with some of the remaining H 2 S in accordance with Equation 1 to produce S 2 and more H 2 O.
The resulting combustion reaction product stream is then passed through a circuitous heat exchange zone or waste heat boiler 24 wherein the effluents are cooled against boiler feed water in line 26 , which then produces steam in line 28 . Typically, the temperature of the cooled effluents are from about 450° F. to about 750° F., preferably from about 550° F. to about 650° F. In the waste heat boiler 24 , the sulfur is converted from one form of sulfur species to other forms according to the following equations:
3S 2 →S 6 (Equation 3)
4S 2 →S 8 (Equation 4)
The cooled stream is carried out of the waste heat boiler in a line 29 at a pressure of from about 20 to about 26 psia, preferably from about 22 to about 24 psia. A portion of the combustion reaction product stream is split into line 44 as a recycle stream taken immediately downstream from the waste heat boiler 24 . This portion is recycled, in some embodiments, after passing through a pressure booster, such a mechanical blower or, as shown in FIG. 1 , as a suction fluid through eductor 46 . A motive fluid selected from high pressure steam, air, nitrogen, carbon dioxide, sulfur or other compatible gas, powers the eductor. In the embodiment shown in FIG. 1 , the recycle stream is fed in line 18 into the acid gas feed line 10 in order to moderate the temperature in burner 20 . Alternatively, the recycle stream can be introduced into burner 20 , oxygen supply line 12 or air supply line 14 . The pressure of the recycle stream as it leaves line 18 is preferably from about 20 to about 30 psia, and more preferably from about 23 to about 27 psia. Typically, the recycle stream is from about 10 to about 50 mol % of the combustion reaction stream, preferably from about 15 to abut 40 mol % The remaining portion of the combustion reaction product stream, a treatment stream, is directed through line 30 and introduced into a first liquid sulfur condenser 32 . The treatment stream is again heat exchanged to further cool the effluents against boiler feed water in line 34 , which produces steam in line 36 . The resulting liquid sulfur is condensed out in line 38 . The elemental sulfur remaining in the treatment stream constitutes from about 40% to about 75% of the sulfur in the original acid gas feed.
Because the recycle stream is removed, before the treatment stream enters the first liquid sulfur condenser 32 , the first condenser is removed from the recycle loop. Thus, it is an advantage of the inventive process that the thermal and hydraulic load on the first condenser is reduced.
Additionally, since the pressure drop from the first condenser is not included in the recycle loop, less differential pressure is required from the pressure booster.
The treatment stream is removed from the first liquid sulfur condenser in line 42 at a temperature of from about 330° F. to about 390° F., preferably from about 350° F. to about 370° F. and at a pressure generally of from about 19 to about 25 psia, preferably from about 21 to about 23 psia.
Those effluents that still remain in the treatment stream are carried through line 42 to be reheated in a first reheater heat exchanger 48 with process steam. The treatment stream, now in line 50 , has a temperature of from about 400° F. to about 500° F., preferably from about 440° F. to about 460° F., and is then introduced into a first catalytic converter reactor 52 wherein residual H 2 S and SO 2 are reacted to produce sulfur species and water according to the following equations:
12H 2 S+6SO 2 →3S 6 +6H 2 O (Equation 5)
16H 2 S+8SO 2 →3S 8 +16H 2 O (Equation 6)
The thus reacted treatment stream, now in line 54 , is introduced into a second sulfur condenser 56 , which again cools the effluents with boiler feed water in line 58 to produce additional steam in line 60 . This additional elemental sulfur is recovered in line 62 . The amount of elemental sulfur remaining in the treatment stream constitutes from about 18% to about 50% of the sulfur in the original acid gas feed.
The further condensed treatment stream is carried from the second condenser through line 64 at a temperature of from about 310° F. to about 370° F., preferably from about 330° F. to about 350° F., and at a pressure generally of from about 18 to about 24 psia, preferably from about 20 to about 22 psia, into a second reheater, heat exchanger 66 , where the treatment stream is heated with high pressure steam to a temperature of from about 400° F. to about 460° F., preferably from about 420° F. to about 440° F. The thus reheated stream is then carried through line 68 and introduced into a second catalytic converter reactor 70 , wherein the catalytic reaction between hydrogen sulfide and SO 2 represented in Equations 5 and 6, again occur. The thus reacted treatment stream, now in line 72 , goes to a third sulfur condenser 74 which is cooled with boiler feed water 76 to produce steam in line 78 . The resulting liquid sulfur is removed in line 80 . The amount of elemental sulfur in the treatment stream constitutes from about 5% to about 15% of the sulfur in the original acid gas feed. Some units only include two stages and are complete at this point. Most have the additional processing steps, as follows below.
As is understood in the art, in some SRU's the sulfur recovery is substantially compete after two stages, i.e., once the treatment stream passes through the second catalytic converter 70 and then the third sulfur condenser 74 . In the embodiment shown in FIG. 1 , the treatment stream, now in line 82 , at a temperature of from about 300° F. to about 350° F., preferably from about 315° F. to about 335° F. and at a pressure of from about 17 to about 22 psia, preferably from about 18 to about 21 psia, is again reheated in a third reheater heat exchanger 84 . The treatment stream is heated with process steam to a temperature of from about 370° F. to about 420° F., preferably from about 390° F. to about 410° F. The thus reheated stream is then carried through line 86 and introduced into a third catalytic converter reactor 88 . In the third catalytic converter reactor, substantially all or most of the remaining H 2 S and SO 2 are reacted c to produce sulfur species as represented in equations 5 and 6, which are then removed in line 90 . The treatment stream is introduced into a fourth condenser 92 cooled by boiler feed water in line 94 producing steam in line 96 . Further elemental sulfur in liquid form is removed in line 98 constituting from about 1% to about 6% of the sulfur in the original acid gas feed.
The treatment stream now in line 100 is at a temperature of from about 255° F. to about 330° F., preferably from about 265° F. to about 320° F. and at a pressure of from about 15 to about 20 psia, preferably from about 17 to about 19 psia.
The resulting treatment stream comprises predominantly steam, nitrogen, carbon dioxide, and hydrogen, as well as residual H 2 S and other sulfur compounds. The stream is carried in line 100 into a tail gas coalescer 102 wherein additional residual liquid sulfur compounds are removed in line 104 . The residual stream now in line 106 is then introduced into a tail gas cleanup unit 116 , where the bulk of the residual sulfur compounds are recovered to meet sulfur emission environmental standards typically by conversion to H 2 S. The H 2 S, is recovered and returned to the acid gas feed line 10 , while the effluent is sent to an incinerator burner 112 .
Alternately, the tail gas in line 106 is sent to an incinerator burner 112 that is fired with natural gas in line 108 and air in line 110 . The materials are then vented in stack 114 , at an acceptable sulfur content level, as an effluent to the atmosphere.
The present invention has been described with regard to preferred embodiments, but those skilled in the art will be capable of contemplating other variants, which are deemed to be within the scope of the invention, which scope should be ascertained from the claims, which follow. | Disclosed is a method for treating a feed gas stream rich in hydrogen sulfide by partially combusting the feed gas stream rich in hydrogen sulfide with an oxygen-enriched gas in a Claus reaction furnace to produce to a combustion reaction product stream containing sulfur. The combustion reaction product stream is split into a recycle stream and a treatment stream and the recycle stream directed back into the Claus reaction furnace, without first condensing sulfur out of the recycle stream, while the treatment stream is directed into a condenser to condense sulfur out of the treatment stream. | 2 |
BACKGROUND OF THE INVENTION
This invention relates broadly to the chemical modification of wool by reacting it simultaneously with a halogenated acid anhydride and an isocyanate. In particular, the invention concerns and has as its prime object the provision of processes wherein the reaction of wool with the above reagents is conducted in the presence of cresol, whereby to facilitate and promote the reaction. The unqualified term "cresol" used herein includes o-cresol, m-cresol, p-cresol, or any mixture of these isomers. Further objects and advantages of the invention will be apparent from the following description wherein parts and percentages are by weight, unless otherwise specified.
Although wool is a very useful fiber, it is often desirable to improve its properties for particular applications by chemically modifying it. Previously, wool has been shrinkproofed with isocyanates, but the product is not flameproof. Furthermore, wool has been flameproofed with halogenated acid anhydrides, but the product does not meet consumer requirements for shrinkproofing.
Wool which is both shrinkproof and flameproof has also been prepared. However, a two-step process is required-- the wool is first shrinkproofed and then flameproofed. The two-step process has the disadvantage of being less efficient and economical than a one-step process.
SUMMARY OF THE INVENTION
The invention described herein obviates the above problem. In accordance with the present invention, wool is reacted simultaneously with a halogenated acid anhydride and an isocyanate in the presence of cresol. The latter compound catalyzes the actual chemical combination of the wool and the other reactants. As a consequence, one is enabled to readily prepare wools containing substantial proportions of combined acid anhydride and isocyanate with correspondingly improved properties.
It should be noted that the success of the simultaneous feature of the instant invention is a quite unexpected result. The reaction of wool with certain acid anhydrides in cresol is known, having been described by Koenig, U.S. Pat. No. 3,332,733, July 25, 1967. However, the inclusion of another chemical modifying agent in the process of the above-mentioned patent would be expected only to either inhibit or prevent the intended reaction. Surprisingly, however, when the above reactants are combined in cresol and reacted simultaneously with wool, substantial modification of the wool results due to the actual chemical combination of the wool with both the acid anhydride and the isocyanate. The result is a flameproofed and shrinkproofed product, and the effectiveness of the combined treatment is much greater than if either reagent is used alone.
One advantage of the instant process is that it is efficient and economical. A one-step process is less expensive to carry out than a two-step process.
A further advantage of the invention is that the modified wool retains its improved properties even after aqueous launderings. It should be noted further that the wool modified in accordance with the invention also retains its improved properties when subjected to normal dry-cleaning.
DETAILED DESCRIPTION OF THE INVENTION
Carrying out the process of the invention essentially involves contacting wool with a halogenated acid anhydride and an isocyanate in the presence of cresol. The reaction conditions such as specific acid anhydride and isocyanate used, proportion of reagents, time, temperature, etc., are not critical but may be varied to suit individual circumstances without changing the basic nature of the invention. The proportion of cresol may be varied widely and may be as low as 0.3-0.5 parts per part of wool. Usually, it is preferred to use a larger proportion of cresol, i.e., about 2 to 6 parts per part of wool, to attain an increased catalytic effect.
The temperature of reaction may be about from 50° to 200° C. The reaction rate is increased with increasing temperature and a suitable temperature range to expedite the reaction without damage to the wool is 100°-120° C. In commercial practice shorter reaction times are possible by employing temperatures up to 200° C., provided the time of contact between the wool and the solvent is such that damage to the fiber is avoided.
It is preferred to carry out the reaction under anhydrous conditions, thereby to ensure reaction between the wool, acid anhydride, and isocyanate but the reaction can also be applied to wool in its normal undried condition (containing about 12-14% water). The degree of modification of the wool is related to the proportion of reactants taken up by the fiber, that is, the higher the uptake of acid anhydride and isocyanate, the greater will be the flameproof and shrinkproof nature of the wool. In general, about 0.1 to 0.5 parts of each reactant is used per part of wool. The time of reaction will vary depending on the temperature of reaction, reactivity of the reagents, proportion of cresol, and the degree of modification desired. In general, the reaction may take anywhere from a few minutes to several hours.
The process in accordance with the invention may be carried out in various ways. For example, the wool may be directly contacted with a mixture of acid anhydride, isocyanate and cresol, and the reaction mixture preferably heated as indicated above to cause the reagents to react with the wool. In the alternative, the wool may be pretreated (padded) with either hot or cold cresol. The wool can then be brought in contact with a mixture of acid anhydride and isocyanate and heated to complete the reaction.
After reaction of the wool with the reagents, the chemically modified wool is preferably treated to remove excess reactants, reaction by-products, and cresol. Thus, the wool may be treated as by wringing, passage through squeeze-rolls, centrifugation, or the like, to remove the excess materials. In place of such mechanical action, or following it, the product may be extracted with an inert, volatile solvent such as trichloroethylene, benzene, acetone, carbon tetrachloride, alcohol, etc. Successive extractions with different solvents may be used to ensure complete removal of all unreacted materials. The treated wool is then dried in the usual way.
By treating wool with an acid anhydride and an isocyanate as herein described, the wool is chemically modified because there is a chemical reaction between the above reactants and the protein molecules of the wool fibers.
Although the properties of the modified wool indicate beyond question that actual chemical combination between the wool and the reactants has taken place, it is not known for certain how the wool and these reactants are joined. It is believed, however, that the reagents react with some of the sites on the wool molecule where there are reactive hydrogen atoms, e.g., amino, guanidino, hydroxyl, and phenolic groups. A possible explanation for the effectiveness of the combined treatment is that acylation of the wool by the acid anhydride forms carboxyl groups that swell the wool structure and provide additional sites of reaction for the isocyanate. This effect cannot operate when wool is treated with either agent alone. It may be, however, that other reactions occur and it is not intended to limit the invention to any theoretical basis.
When the reaction is carried out with a diisocyanate, for example, tolylene-2,4-diisocyanate, combination with the wool may establish cross-links between protein molecules that may increase the resistance of the wool to attack by chemicals, carpet beetles, moths, and the like. The presence of halogen introduced by the halogenated acid anhydride may also be beneficial in improving resistance to attack by insects.
The tendency of wool to shrink when subjected to washing in aqueous media has long been a deterrent to the more widespread use of wool. An important advantage of the invention is that it yields modified wools which have a decreased tendency to shrink when subjected to washing with conventional soap and water or detergent and water formulations.
Although wool does not ignite readily, flames will propagate in wool once ignition has occurred. A need, therefore, exists to flameproof wool for many uses such as airplane upholstery, carpeting, blankets, sleepwear, and the like. The invention described herein fulfills this need.
Another advantage of the invention is that the improvement is essentially permanent, unlike some surface treatments. The treated materials do not lose their new properties after long use or wear, but retain these properties for the life of the material.
It is to be noted that the reaction in accordance with the invention does not impair the wool fiber for its intended purpose, that is, for producing woven or knitted textiles, garments, etc. The process of the invention may be applied to wool in the form of fibers, as such, or in the form of threads, yarns, slivers, rovings, knitted or woven goods, felts, etc. The wool textiles may be white or dyed goods and may be of all-wool composition or blends of wool with other textile fibers, such as cotton, regenerated cellulose, animal hair, etc.
Acid anhydrides to be used in the process of the invention must be chosen for their ability to flameproof the treated material. Various halogenated acid anhydrides may be employed, such as tetrachlorophthalic anhydride, tetrabromophthalic anhydride, chlorendic anhydride, chloroacetic anhydride, dichloroacetic anhydride, dichlorosuccinic anhydride, tetrachlorosuccinic anhydride, dichloromaleic anhydride, and the like.
Isocyanates which may be used in accordance with the invention to produce a shrinkproof product include tolylene diisocyanate, xylylene diisocyanate, phenylene diisocyanate, cyclohexyl diisocyanate, 4,4'-diphenylmethane diisocyanate, 4,4'-dicyclohexylmethane diisocyanate, dianisidine diisocyanate, hexamethylene diisocyanate, phenyl isocyanate, chlorophenyl isocyanate, dichlorophenyl isocyanate, bromophenyl isocyanate, tetrabromophenyl isocyanate, octadecyl isocyanate, isophorone diisocyanate, 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethylcyclohexane, dimer oleic acid diisocyanate, etc.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The invention is further demonstrated by the following illustrative examples.
The wool used in the experiments set forth below was undyed wool flannel, 6.5 oz./square yd., cut into circles (8 cm. in diameter) or swatches (5× 10 in.). These samples were exhaustively extracted with trichloroethylene followed by ethanol, then oven-dried and weighed. All weight increases are given on a dry wool basis.
Flame tests were carried out according to a modified AATCC 34-1969 procedure published in AATCC Technical Manual, Vol. 48, pages 201-202 (1972). Specimens (2.5× 9.5 in.), conditioned at 70° F., 65% RH, were exposed to a flame for 12 seconds. Treatment is considered effective when the average char length is less than 7 inches, and the after-flame persists less than 12 seconds on the average after removal of the source.
Shrinkage tests were conducted on the circles of fabric as follows: Measured fabric samples, including an untreated wool control, were violently agitated in an "Accelerotor" at 1,780 rpm for 2 minutes at 39°-40° C. with 200 ml. of 0.5% aqueous sodium oleate solution. After this laundering operation, the samples were remeasured to determine area shrinkage.
The swatches were measured after conditioning, and household aqueous laundering tests were conducted in a reversing, agitator-type, household washing machine, using a 3-lb. load, a water temperature of 105° F., and a low-sudsing detergent in a concentration of 0.1 percent in the wash liquor. The wash cycle itself was for 75 minutes, followed by the usual rinses and spin-drying. The damp material was press-dried, conditioned, and re-measured to determine the extent of shrinkage.
EXAMPLE 1
Run A: Circular samples of dried wool fabric (1.2 g.), tetrabromophthalic anhydride (TBPA, 0.5 g.) tolylene-2,4-diisocyanate (TDI, 0.3 ml.), and m-cresol (3.0 ml.) were placed in a Petri dish and heated in an oven at 120° C. for 20 minutes.
The treated wool was extracted with hot ethanol to remove unreacted reagents and then was dried. The weight increase was determined and shrinkage tests were conducted in an "Accelerotor."
The above procedure was repeated on other samples of dried wool fabric with the following changes in the reaction parameters:
Run B: temperature, 180° C.; time, 5 minutes.
Run C: temperature, 180° C.; time, 5 minutes; amount of TBPA, 0.4 g.; amount of TDI, 0.1 ml.
For purposes of comparison the following changes were made in the procedure described for Run C:
Run D: TBPA was omitted.
Run E: TDI was omitted.
As a Control, untreated wool was examined. It should be obvious that Runs D and E are not illustrative of the invention.
The results of all the experiments are tabulated below:
______________________________________ Area Temp- Weight shrin- erature Time TBPA TDI increase kageRun (° C.) (min.) (g.) (ml.) (%) (%)______________________________________A 120 20 0.5 0.3 24 0B 180 5 0.5 0.3 23 0C 180 5 0.4 0.1 18 4D 180 5 0 0.1 1 36E 180 5 0.4 0 14 15Control Untreated wool 42______________________________________
A comparison of Runs C, D, and E indicates that the process of the invention (Run C) yields greater shrinkproofing than the individual use of the agents as evidenced in Runs D and E.
EXAMPLE 2
A dry wool swatch, TBPA (2.0 g.), TDI (0.5 ml.), and m-cresol (15.0 ml.) were placed in an enameled tray. The sample was heated in an oven at 180° C. for 15 min. The modified wool was extracted with hot ethanol and then dried.
The so-treated sample (A) was treated to determine the extent of shrinkage after laundering in a household washing machine. An untreated wool sample was examined as a control. The results are summarized below:
______________________________________ Weight increase Area shrinkageSample Reactants (%) (%)______________________________________A TBPA and TDI 24 0Control None None 43______________________________________
EXAMPLE 3
A sample (B) of wool modified in accordance with the procedure outlined in Example 2 was tested for flame resistance subsequent to laundering as described in Example 2. Untreated wool was examined as a control. The results are summarized below:
______________________________________ After flame Char lengthSample Reactants (sec.) (in.)______________________________________B TBPA and TDI 0.9 3.6Control None 26.7 Totally burned______________________________________ | Wool is flameproofed and shrinkproofed by a process wherein the wool is reacted simultaneously with a halogenated acid anhydride and an isocyanate in the presence of cresol. The flameproofing treatment is durable to both aqueous laundering and drycleaning. | 3 |
BACKGROUND OF THE INVENTION
The present invention is directed to a printing apparatus adapted to print information on a print media in a simple and efficient manner. The device is engineered for inexpensive manufacture in order to render the printing apparatus available for use by small proprietors and businesses. The printing apparatus is constructed for use with specialty print media, such as lottery cards, wherein it is important that the integrity of the print media not be damaged when identification information is printed thereon.
The printing industry has become increasingly pervasive in modern times, yet there remains a need for small automated printing units that are economical in construction giving individuals and small business entities the ability to purchase such device for use in low volume printing tasks. Although some printing devices have been developed in the past which are fairly small and compact, there apparently is no wide spread use of these devices in small business applications. An example of such a hand operated printing device is shown in U.S. Pat. No. 835,903 issued Nov. 13, 1906 to W. C. Grant. The device according to this patent includes a hand driven platen roller and an upper print roller carrying printing elements. The print roller is secured to a pair of upright supports by means of a spring biased mechanism pressing the printing elements against the platen roller. Inking rollers distribute a print fluid onto the printing elements.
Another apparatus is shown in U.S. Pat. No. 872,302 issued Nov. 26, 1907 to M. McMahon. In the McMahon patent, a print roller is formed of a half cylinder and is mounted between a pair of upright supports. The print roller carries a printing element that contacts an inking roller which coats the printing element with printing fluids as the print roller is rotated by a hand crank. A platen roller is upwardly biased between a pair of vertical supports so that it may contact the printing element as it is rotated.
Despite the structure shown in the prior art, a need has arisen for a printing apparatus that is specifically adapted to print identification information on lottery tickets. This need has resulted from the institution by several state governments of state controlled lotteries as a method of raising revenue. Such lotteries typically take the form of small tickets that may be purchased by a player; each ticket carries prize information hidden by an opaque material that is readily removed from the ticket by scratching the ticket with a coin or other rigid object. Sellers of these tickets are often required to stamp an identification number on the back of each ticket so that the state may monitor the sales of the winning lottery tickets as well as for other identification purposes.
The problem that has confronted many businesses, such as grocery stores, filling stations and the like, is that they must hand stamp a large number of these lottery tickets. Hand stamping the tickets is time consuming and expensive where a business must pay an employee to perform this simple task. Some businesses have tried various printing devices to automatically print an identification number on each ticket, but two significant problems have been confronted. First, since the lottery tickets are normally connected in a long sequential series, a problem has arisen in the lack of ability for the identification number to be stamped at a precise location on each consecutive ticket. A second, and more significant problem, is that conventional printing apparatus often removes portions of the opaque masking material so that a portion of the hidden prize information is exposed. Naturally, this ruins the tickets so that they must be returned and destroyed resulting in a financial loss and in an increase in administrative time for the lottery.
Accordingly, a need has recently arisen for a printing apparatus that is simple in construction so that it may be inexpensive in manufacture, thus allowing small businesses to purchase the printing apparatus. A need has also arisen for a simply constructed printing apparatus that can print identification information on a delicate print media, such as lottery tickets at a precise location and without marring the print media.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a novel and useful printing apparatus that is simple in construction and economical in manufacture.
It is another object of the present invention to provide a printing apparatus adapted to precisely print information on a stream of print media without damaging the integrity of the print media.
Yet another object of the present invention is to provide a printing apparatus especially adapted to print business identififying information on a consecutive stream of lottery tickets without damaging opaque masking material located on those tickets.
Still a further object of the present invention is to provide a printing apparatus wherein a freely floating platen roller is adjustably biased against a print roller so as to accomodate different thickness in the print media as it is passed between the rollers.
It is still a further object of the present invention to provide a printing apparatus for printing an accordian array of cards, such as a set of lottery tickets, wherein the printing rollers interact with a feed rack, a feed table and a take-up rack so that the accordian array of cards is unstacked, printed and restacked automatically.
To accomplish these objects, the preferred embodiment of the present invention includes a print roller that is rotatably journaled between a pair of upright supports with the print roller being driven by an electric motor. The print roller carries printing elements that may be contacted by an inking roller that is pivotally movable into and out of vertical abutment with the print roller. A freely floating platen roller is rotatably journaled between a pair of movable supports that are preferably supported by elongated lever arms that are pivotally secured to a fulcrum element. Adjustable springs pivot the platen roller into contact with the print roller and these rollers are movable into and out of abutment with one another either manually or through a manual cam arrangement. Interlocking gears connect the platen roller to the print roller so that the platen roller is positively driven by the motor through these gear elements.
Where the print media is in the form of an accordian array of cards, the printing apparatus includes a feed rack supporting an unprinted array of cards that is upstream of the print and platen rollers a distance greater than the length of one card. A feed table is mounted between the print and platen rollers and the feed rack so that it supports a print media card immediately prior to introduction to the printing operation. A take-up rack is located a distance downstream of the print and platen rollers that is slightly less than the length of a card, and an inclined stop helps stack the printed cards into an accordian array in the take-up rack. An indexing hub is located on the print roller axle so as to permit easy alignment of the printing element or elements such that they will precisely print identifying information at selected locations on the print media. The motor is switched both by a constant action switch or by an intermitent switch to allow an operator to manually pulse the printing apparatus when the constant switch is in the "off" position. The printing apparatus is preferably mounted on a series of hinged surfaces that may be folded together in a box-like configuration that includes a handle so that the apparatus is readily stored in a compact form and is easily transportable.
These and other objects and advantages of the present invention will become apparent to those skilled in the art after considering the following detailed specification which discloses the preferred embodiments thereof in conjunction with the accompanying drawings, wherein:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of the printing apparatus according to the preferred embodiment of the present invention;
FIG. 2 is a rear elevational view in partial cross-section showing the printing roller assembly according to the preferred embodiment of the present invention;
FIG. 3 is a left end elevational view taken in partial cross-section about line 3--3 of FIG. 2;
FIG. 4 is an end view in elevation showing the support structure and printing apparatus of the preferred embodiment of the present invention folded into a compact storage mode;
FIG. 5 is an end view in elevation of the feed rack, feed table and take-up tray according to the preferred embodiment of the present invention;
FIG. 6 is a right end elevational view of a first alternate embodiment of the printing roller assembly and feed table according to an alternate embodiment of the present invention;
FIG. 7 is a side view in elevation of a second alternate embodiment of the printing apparatus according to the present invention;
FIG. 8 is an end view in elevation of the printing apparatus shown in FIG. 7; and
FIG. 9 is a cross-sectional view taken about line 9--9 of FIG. 8.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention relates to a printing apparatus that is adapted for printing information on a stream of print media such as that found in an accordian array of print cards which correspond to lottery tickets used by some states. In the preferred form of the present invention, the printing apparatus includes a novel print roller assembly mounted on a foldable support surface which also supports a feed rack, a feed table, a take-up rack and guide structure. The print roller assembly is driven preferably by an electric motor that includes an intermitent activation switch as well as a normal on/off switch.
As is shown in FIG. 1, printing apparatus 10 includes a printing assembly 12 mounted on a support surface 14. Support surface 14 is defined by a bottom support element 15, a first side support element 20, and a second side support element 26. Bottom support element 15 also mounts a drive motor 16 which is mechanically connected to printing assembly 12, and a feed table 18 is mounted to support element 15 and is located immediately upstream of printing assembly 12.
A first side support element 20 is pivotally connected to bottom support element 15 by means of a piano hinge 22. First side support element 20 mounts a feed rack 24 that is aligned with feed table 18 when support elements 15 and 20 are coplanar. A second side support element 26 is pivotally connected to support element 15 by means of piano hinge 28. Second side support element 26 mounts a take-up tray 30 and a guide fin 32 that are each aligned with feed rack 24 and feed table 18 when support elements 15, 20 and 26 are coplanar. Second side support element 26 also mounts a switch assembly 34 that includes a constant on/off switch 36 and an intermediate or pulse switch 38 that are electrically connected to motor 16. A top wall support element 40 is rigidly connected perpendicularly to second support element 26.
As is shown in FIG. 4, the foldable construction of printing apparatus 10 about hinges 22 and 26 allow printing apparatus 10 to be conveniently folded into a stored or transport position. To this end, as is shown in FIG. 4, first side support element 20 and top support element 40 are provided with latching members 42 and 44 which allow support elements 20 and 40 to be releaseably secured to one another thereby defining a boxlike configuration. Support element 40 also mounts a handle 46 to permit ready manual transport of printing assembly 10.
Printing assembly 12 is shown in greater detail in FIGS. 2 and 3 and primarily includes a print roller 50, a platen roller 52 and an inking roller 54 that cooperate with one another as described below. Print roller 50 is rotatably journaled between a pair of vertical upright support members 56, and print roller 50 carries printing elements 58 in a recessed portion formed at one end thereof. Thus, print roller 50 is mounted upon a rotatable axle 60 that extends between supports 56 and is coupled, at one end, to a gear box 62 by means of coupling 64. Gear box 62 is mounted to support surface 14 by means of housing 64 and includes a drive shaft 66 that is connected to motor 16. Motor 16 thus rotatably drives roller 50.
Inking roller 54 is rotatably journaled between a pair of parallel ink roller supports or armatures 68. One end of each armature 68 is connected to ink roller axle 70 which rotatably mounts ink roller 54, while the other end of each armature 68 is rigidly connected to pivot axle 72 that is rotatably journaled between supports 56. To this end, each support 56 includes a laterally projecting shoulder 74 at an upper end thereof with pivot axle 72 extending between shoulders 74, as is shown in FIG. 3. Ink roller 54 is thus movable into and out of vertical abutment with print roller 50 by rotating pivot axle 72 to pivot ink roller 54 into and away from print roller 50 as is shown in phantom in FIG. 3. To this end, a locking hub 74 is secured to pivot axle 72. A pivot handle 76 having a shaft 78 and an enlarged head 80 is secured to pivot hub 74 so that an operator may manually rotate pivot axle 72 thereby pivoting inking roller away from and into abutment with print roller 50.
Platen roller 52 is freely floating on an axis of rotation defined by platen axle 82 that is not connected to supports 56. As is seen in FIGS. 2 and 3, axle 82 is rotatably journaled between bearing ends 84 of a lever arm 86. Each lever arm 86 is supported at its mid portion by means of a fulcrum element 88 that is attached by screws 90 to support surface 14. Each lever arm 86 terminates at a leverage end 92 opposite bearing end 84 with leverage ends 92 being formed as flat, plate-like elements in planes generally parallel to surface 14. Thus, it should be appreciated that, as leverage ends 92 are raised and lowered, bearing ends 84 are lowered and raised to move axle 82 and thus platen roller 52 into and out of abutment with print roller 50.
To accomplish the pivoting of each lever arm 86 about is fulcrum element 88, an adjustable bias means and cam assembly are provided at each leverage end 92. As is shown in FIG. 3, a threaded bolt 94 is rigidly affixed to support surface 14 and extends through a bore 96 in leverage end 92. An adjustable thumb screw 98 is threaded on the free end of bolt 94 so that it may be moved upwardly and downwardly along bolt 94, and a spring 100 is positioned between thumbscrew 98 and washer 102 which abuts leverage end 92. Thus, spring 100 urges leverage end 92 downwardly so as to bias bearing end 84 upwardly. This urges platen roller 52 (shown in phanton) into abutment with print roller 50.
In order to disengage platen roller from print roller 50, a cam element 104 is mounted underneath each leverage end 92 by means of a transverse axle 106 that rotatably extends between a pair of brackets 108 that are mounted by screws 110 to support surface 14. Axle 106 may be partially rotated in brackets 108 by means of a manual handle 112 that has a shaft 114 formed as a right-angle extension of axle 106 and which terminates in an enlarged head 116. As is shown in phantom in FIG. 3, handle 112 may be pivoted through 90 degrees of motion to cause cams 104 to bear upwardly against leverage ends 92, thus compressing springs 100.
It should therefore be appreciated that platen roller 52 moves into and out of abutment with print roller 50 depending upon the position of cams 104. This movement also causes platen roller 52 to become positively driven by drive motor 16. Specifically, as is seen in FIGS. 2 and 3, drive motor 16 is coupled through drive shaft 66 to axle 60 in order to cause rotation of print roller 50. A print gear 118 is attached to axle 60 for common rotation therewith so that gear 118 is driven by drive motor 16. A mating platen gear 120 is attached to platen axle 82 for common rotation therewith and is movbale into and out of engagement with gear 118 by the pivotal action of lever arm 86. Thus, as is shown in FIG. 2, when platen roller 52 is moved into abutment with print roller 50, gear 120 is moved into engagement with gear 118. When drive motor 16 then turns print roller 50, gear 118 positively drives gear 120 so that platen roller 52 is positively driven. This prevents relative slippage of the print roller and platen roller with respect to one another so as to more precisely print information on the print media.
Gears 118 and 120 are shown disengaged in FIG. 4, where it should be appreciated that handle 112 has been pivoted to cause cams 104 to elevate leverage end 92 of each lever arm 86. To permit the vertical movement of platen roller 52 caused by the pivoting action of arm 86, an elongated opening 122 is provided at a lower end portion of each vertical support 56, as is shown in FIG. 3. It should be appreciated that gear 120 has been omitted in this figure so that slot 122 is more apparent.
In order to more efficiently handle a print media comprising of an accordian array of cards, various racks and trays are relatively positioned on support surface support 14. This structure can best be seen in FIG. 5 where a stack of print media 130 as shown positioned in feed rack 24. Each card has a length "L" measured in a direction that corresponds to the stream of cards through printing assembly 12. Each print card is also hinged by perforations to each of its adjacent cards so that it may be folded in a vertical stack in an accordian-like manner.
Feed rack 24 includes an upstanding rear rib or wall 140 and a pair of parallel upstanding ribs or sidewalls 142 extending perpendicularly from end wall 140 in a direction corresponding to the stream of material through printing assembly 12. Sidewalls 142 are spaced apart a distance slightly greater than a width of a print card measured transversely to the full stream of the print media so that stacks 130 can conveniently nest in feed rack 24 with a downstream edge abutting rear wall 140.
A feed table 18 is supported from surface 14 by means of a support bracket 144 at a height "H" that equals the height of the contact line between the printer roller 50 and platen roller 52 when they abut one another. Feed table 18 includes a pair of upturned flanges or sidewalls 146 located either side of the bottom wall 148 and is positioned between rollers 50, 52 and rear wall 140 of feed rack 24. A forward edge of bottom wall 148 is protected by a plastic channel 150 so that the print media is protected as it slides onto feed table 18. Rear wall 140 of feed rack 24 is located upstream of the plane P, that is defined by the rotational axes of print of rollers 50 and 52, a distance A that is greater than length L of a print card. Such is important to keep the print cards from jamming and they are consecutively pulled off stack 130 during the printing operation.
The ratio of the distance A to the length L of a print card, or A/L, has been found to be critical within a given range where the apparatus is used to print lottery tickets. The acceptable range for this ratio has been determined to be 1.4 to 1.7. Should the ratio be less than 1.4, the stacked array of cards will not unfold properly during the printing operation. Should the ratio exceed 1.7, the stream of cards may sag, thus allowing the edges of the apparatus to scrape the cards. This in turn may cause unwanted removal of the opaque masking material on the lottery cards.
A take-up assembly for the printed cards is located downstream of plane P and includes a take-up tray 30 that includes a bottom wall 160 mounted at an acute angle with respect to support surface 14. Bottom wall 160 has a forward edge 162 which is located adjacent support surface 14 and includes a pair of upstanding flanges or sidewalls 164 that are generally in line with sidewalls 142 and sidewalls 146 of feed rack 24 and table 18, respectively. The upper edge 166 of take-up tray 30 is elevated above print surface 14 by means of a vertical support bracket 168 that is mounted to support surface 14 and in a convenient manner.
As is shown in FIG. 5, a printed stack 170 of cards is received by take-up tray 130 during the printing operation. To this end, it should be appreciated that the distance between edge 162 of take-up rack 30 and the line of contact between roller 50 and 52 in plane P is slightly greater than length L. Further, to aid in the take-up of the printed card a guide fin 172 is mounted on support surface 14 forwardly of edge 162 and downstream of printing assembly 12. Drive fin 172 has an angled upper edge 174 and terminates at a rearward end 176 located downstream a distance B from plane P that is less than length L. To this end, distance B should approximately equal L sin θ, where θ is the angle between plane P and the plane containing edge 162 and the contact line between rollers 50 and 52. Support bracket 168 lies in a plane O that is parallel to plane P and that is spaced a distance M from plane P. A stack point S for the downstream edge of cards 170 is located adjacent plane Q so that it is also spaced a distance M from plane P. Again, it has been found that a perferred range M/L exists so that proper stacking occurs. Preferably, M/L is in the range of 1.9 to 2.2.
Operation of printing apparatus 10 can now be more fully appreciated for the foregoing in mind. When a user desires to print information on print media, such as an array of print cards, the apparatus is unfolded from the figuration shown in FIG. 4 so that it lays flat with panels 15, 20 and 26 oriented in a common plane to define a support surface 14. This assembly may be set on a counter or table top, and motor 16 may be plugged into a conveniently located electrical outlet. Ink roller 54 is pivoted away from print roller 50, and cams 104 are pivoted to disengage gears 118 and 120 and thus bring platen roller 52 out of contact with print roller 50. Ink is then applied to ink roller 56, and print roller 50 is manually turned by means of index hub 61 so that pointer 63 is pointing straight upward. Since pointed 63 denotes a position of the upper printing element 50, this provides for an alignment of the printing elements for purposes of printing information at a precise location on the print media.
Once ink roller 54 has been sufficiently soaked with a print fluid, it is pivoted back so that it will be in contact with printing elements 58 on print roller 50. It should be appreciated from FIG. 2 that ink roller 54 includes some axial space to allow for expansion of an absorbent ink pad that forms a typical construction of an ink roller. An array of cards may then be placed in feed rack 24 and the cards extended downstream across feed table 8 until the leading edge of the first card is aligned with plane P. At this point, cams 104 are rotated to allow engagement gears 118, 120 and abutment of print roller 50 and platen roller 52 so that the rollers slightly grip the edge of the first card therebetween. The tension by platen roller 52 may then be adjusted by turning by thumb screws 98, and the device is ready for operation. Preferably, the tension is adjusted up to five pounds, with best operation occurring at a pressure of four pounds.
The operator may then intermitently feed the cards through the printing assembly 12 by manually pushing button 38. Once it has been established that the printed information is located at a precise, desired location on the print cards, switch 36 may be initiated to constantly operate the print apparatus until all the cards in stack 130 are printed.
While the above description is directed to the preferred embodiment of the invention, it is possible to change the structure without departing from the scope of the invention. Two such departures are shown in FIG. 6 which eliminates cam 104, cam axle 106 and handle 112, and alters the ink roller support structure. Here, an extension 190 is provided on each lever arm 86 with extension 190 extending through plane P on an opposite side of fulcrum elements 88. The cam elements are omitted and engaged and disengagement of gears 118, 120 and the movement roller 52 out of abutment with print roller 50 is simply accomplished by manually pushing down on extensions 190.
FIG. 6 also discloses an alternative assembly for biasing an ink roller against print roller 50. Here, ink roller 254 is mounted on an axle 270 which is rotatably journaled between a pair of slide brackets 260. Each slide bracket 260 is slidely mounted to a respective vertical support 56 by means of a pair of bolts 262 at an upper edge of each bracket 56. Bolts 262 pass through holes 264 formed in cross arm 266 of slide bracket 260, and a pair of springs 268 are mounted on each blot 262 above cross arm 266. Springs 268 are retained on these threaded bolts by means of nuts 272 so that downward tension may be applied on axle 270, thus adjustably maintaining ink roller 254 in abutment with print roller 50. Further adjustment of the position of axle 270 is provided by a slide adjustment element 280 which is mounted to support 56 by means of a locking screw 284 which passes through a vertical slot 282 formed in adjustment element 280. This element can be adjusted upwardly to abut nub 286 provided on bracket 260 so that it can provide a lower stop limit for slide bracket 260.
A second alternate embodiment of the present invention is shown in FIGS. 7, 8, and 9. This embodiment is a simplified, hand-crank unit that has been found to suitably print lottery tickets. As is shown in FIGS. 7 and 8, printing apparatus 300 includes a base support 302 to which is mounted a pair of vertical upright supports 304 and 306. Supports 304 and 306 mount a platen roller 308, a print roller 310, and an inking roller 312.
Each of supports 304 and 306 has a first slot 314 and a second slot 316 which mount axles 318 and 320 of rollers 308 and 312 respectively. Axle 318 is rotatably supported at each end by a guide bearing, such as bearing 322, which is slideably positioned in slot 314. Similarly, axle 320 is slideably positioned in slot 316 and held in position by clips 324. Print roller 310 has an axle 326 that is mounted between a pair of bearings, such as bearing 328 which is mounted in an opening, such as hole 330 formed in respective support 304, 306.
It should thus be appreciated that platen roller 308 has a freely floating axle 318 while axle 326 of print roller 310 is immovable with respect to upright supports 304 and 306. In order to tension platen roller 308 against print roller 310, a tensioning spring is provided in each of supports 304 and 306. As is shown in FIG. 9, support 304 includes a longitudinal bore 331 which intersects slot 314 at its lower edge. A tensioning spring 332 is mounted in bore 330 and has one end abuting guide bearing 322 with the other end held in position by means of a set screw 334. As noted with respect to the prefered embodiment, the pressure applied by platen roller 308 against print roller 310 is important. To this end, each set screw 334 is tightened so that platen roller 308 bears against print roller 310 with a force of between three and five pounds. Preferably, this force is set at approximately four pounds.
Ink roller 312 is mounted between supports 304 and 306 in a manner similarly to that described with respect to the platen roller 308. Each of supports 304 and 306 are provided with longitudinal bores, such as bore 336, and a spring 338 is mounted in each bore 336 with one end abutting axle 320 and the other end held in position by means of a set screw 340. Tension is applied by springs 338 sufficient to bear ink roller 312 against print roller 310. The force of this pressure, though, is not as critical as that with respect to the pressure between platen roller 308 and platen roller 310, due to the construction of ink roller 312.
Roller 312 is constructed of a soft, spongy material 342 flanked on either side by means of rigid plates 344 which bear against the cylindrical surface of print roller 310. Since print rollers 308 and 310 are constructed out of anodized aluminum, and since plates 344 are constructed as rigid metallic disks, it is necessary the sufficient force be applied to springs 338 to maintain plates 344 in contact with roller 310. Hence, roller 312 is rotated when roller 310 is driven, for example, by handcrank 346 which is secured to axle 326. The danger of overtensioning ink roller 312 against roller 310 is reduced since sponge material 342 is thus protected.
Print roller 310 is provided with a recessed portion 348 having a smaller diameter than the diameter of the main portion of roller 310. A printing element 350 extends circumferentially around reduced diameter portion 340, and it should be understood that the combined diameter of reduced portion 348 and printing element 350 is slightly larger than the diameter of roller 310 so that printing element 350 will contact spongy material 342. Thus, printing element 350 will continually receive printing fluid.
As noted with respect to the preferred embodiment, the present apparatus is designed for use in printing accordian-like arrays of cards that are hinged together at adjacent edges. Further, as noted above, the distance between the downstream edge of the unprinted stack of cards and plane P defined by axles 318, 320, and 326 can be as important. Likewise, the distance between plane P and the downstream point or edge of the restacked printed cards can be important so that proper feeding and take-up of the stream of cards is accomplished. To this end, as is shown in FIGS. 7 and 9, a stack of cards 360 is made up of individual cards 362, all of which have a length L. Cards 362 are pulled off of stack 360 and fed between rollers 308 and 310 and are restacked as a printed stack 364. To provide a downstream stop for stack 360 of cards 362, base 302 extends laterally of plane P to terminate at an edge 366 that is located a distance A from plane P. A support bar 368 extends across edge 366 underneath base 302 and cooperates with edge 366 in providing the downstream stop 436 for the stack of cards 360. Support bar 368 may be defined by a soft strip of material that may also act as a cushion for base 302. A similar support bar 370 may be provided at an edge 372 of base 302 opposite edge 366 so that base 302 will be supported in a parallel manner with respect to a horizontal support surface.
To provide a take-up stack 364 of printed cards 362, a narrow, elongated take-up arm 380 is releasably secured at one end 382 to base 302. Arm 380 terminates at its free end in an upturned finger 384 downstream of card stacks 364. Finger 384 acts as a limit stop for the printed cards as they are fed off of rollers 308 and 310, a finger 384 is spaced a distance M from plane P.
The operation of the device shown in FIGS. 7, 8, and 9 is similar to that with respect to the preferred embodiment. After proper tensioning has been set up for rollers 308 and 310, a stack 360 of cards to be printed are placed in abutting relationship to edge 366 of base 302. A leading edge of one card 362 is then fed between rollers 308 and 310, and drive handle 346 is manually turned to advance the cards therethrough. As handle 346 is turned, consecutive cards 362 are pulled off of stack 360 and printed with the desired information located on printing element 350. As this takes place, the leading edge of a card 362 abuts finger 384 and the printed cards are restacked on arm 380. As noted above, the ratio A/L has been found to preferably be in the range of 1.4 to 1.7 and the ratio M/L is preferably in the range of 1.9 to 2.2.
Embodiments of the present invention have been shown and described above with a degree of particularity to enable a complete understanding of those embodiments. However, it should be understood that the present invention involves inventive concepts defined in the appended claims, and these inventive concepts are not intended to be limited except insofar as the prior art requires. This printing apparatus may take other forms and is susceptible to various changes in detail without departing from the principles of this invention. | A printing apparatus includes a print roller, a platen roller and an ink roller mounted between a pair of upright supports secured to a support surface. The platen roller is resiliently biased against the print roller, and is preferably supported independently of the upright supports by a spring-biased lever and cam assembly. The printing apparatus is especially constructed for printing accordian arrays of cards, having delicate masking material thereon, and includes a feed tray with a feed stop and a take-up tray with a take-up stop each located at a position within a defined ratio with respect to the length of a single card in the array. The platen roller is preferably biased within a selected range to prevent damage to the masking material. A drive mechanism rotates the print roller which, in turn, drives the platen roller either by direct pressure or through gears. | 1 |
BACKGROUND OF INVENTION
This invention relates to a plane element to be used as a facing panel on the exterior surface in buildings.
Previously known is a facing panel (2) with a body of corrosion resistant sheet metal. By means of punching tools tiling guides have been made in the sheet which are tongues extracted from the sheet with the tool and bent off the sheet in the direction of the tiling. Guided by the tongues, the tiles are laid and jointed.
To be transportable and mountable, such a facing panel needs extra support. The back sheet must be stiff if used to provide handling strength to the panel. The panel will then be heavy and have a thickness of many millimeters. Known panels of this kind are, as matter of fact, facing panels with insulation, frame and inwall lining. Accordingly, on using thin sheet the panel requires a separate supporting framework. Examples of such frameworks are constructions a.o. in U.S. Pat. No. 4,334,394, in the Finnish application No. 884288 and in the publication print No. FI-58810. The panels are as thick as the whole wall and have a thin back plate for fixing of tiles, concrete or casting material.
SUMMARY OF THE INVENTION
The object of this invention is to bring forth a facing panel sufficiently rigid upon handling and mounting and onto which especially tiles, e.g. lining bricks are easily fastened. The panel is fixed on a wall as a lining. This object is reached by a means of facing panel according to the invention, characterized in what is presented in the patent claims.
A facing panel according to the invention is made sufficiently rigid by means of a lattice structure, the vertical profiles of which are made of thin sheet metal. The whole profile construction, which functions as the panel back plate, is formed from sheet metal material. With a framework of profiles according to the invention the facing panel needs no other bearing frame and can therefore be handled and mounted independently as a facing panel on a wall. For laving the tiles or lining bricks and distribution of jointing compound there are necessary guides in the profiles for the tiles and bearing surfaces for jointing compound.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
In the following the invention is disclosed with reference to the enclosed drawing, where
FIG. 1 is a front view of the facing panel.
FIG. 2 is a vertical view of the facing panel.
FIG. 3 is a horizontal view of the facing panel.
FIG. 4 is a joint of tile and horizontal profile.
FIG. 5 is another joint of tile and horizontal profile.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows the facing panel framed by a L-profile 6. Inside the frame a lattice of vertical and horizontal profiles is formed. The vertical profiles 2 are fixed at a pitch of half of the tile length from each other. The horizontal profiles 3 are fixed at a pitch of half of the tile width from each other. Most suitably the profiles are shaped of corrosion resistant thin metal sheet. The profiles are fixed together as a lattice for instance by spot welding in the intersections. Profiles 2 and 3 are then at different levels and, most advantageously, the vertical profiles are undermost. The vertical profiles 2 have tile guide brackets 5 in every second space between the horizontal profiles 3. Most advantageously the tile guides 5 are made punching them partly off profile with a tool to form tongues sticking out from the profile. The tile pattern shown in the figure is produced with tile guides 5 in every second space in the vertical profiles 2. The purpose of tile guides 5 is to function as tiling guides and bearing surfaces for the jointing compound.
As tiling guide and bearing surface for the jointing compound the surface of horizontal profile 3 can have an unbroken profile shape 4 similar to the bracket shown in FIG. 1. Naturally, on the surface of this profile 3 there can also be brackets partially punched out with a tool at a distance from each other.
The profiles of the lattice can be fixed together also with a punching tool by percussing them partly through both profiles in the intersections and thus producing a joint locking the profiles together. Other know jointing methods are also possible.
FIG. 2 shows a vertical section of the facing panel, whereat a cross-section of horizontal profile 3 becomes visible. There are folds in the edges of profile 3 by means of which the profile can be easily connected, in different ways, to the criss-cross profile 2 underneath. Further, profile 3 has a protruding shape 4 hitting the joint space between the tiles. The width of the joint space is determined by profile 3 when the tiles are arranged as shown in FIG. 2, i.e. the tile edges are placed on the skirts of the edges of profile 3.
FIG. 3 shows a horizontal section of the facing panel, whereat a cross-section of vertical profile 2 becomes visible. In this embodiment the vertical profile is a U channel, on the one side of which the horizontal profiles are fixed. On the same side the tiles guides 5a are also made. Depending on the tiles, the thickness of tiling varies for instance from 8 to 30 mm and the width of the profile is for instance 30 mm. Accordingly, the width of the facing panel amounts only to appr. 60 mm. The outer dimensions of a typical facing panel are 1 m×2,7 m.
FIG. 4 shows another embodiment of this invention, where there is a groove 7 in the tile 1 edge. Further, the shape of the edge of vertical profile 2 differs from the shape in FIG. 2 because it is bent inward. For the jointing compound a nest is formed because of the vertical profile 2 and the groove in tile 1. The next has the effect to bind tile 1 to the profiles if it has been made sure during jointing that the nest is filled with jointing compound. The next can be on one side of the profile 3 and have an uninterruped shape or it is produced in form of pits pressed in profile 3 at a certain distance from each other. In the tiles 1 as per the figures, the grooves 7 are, for instance, on the long sides of the tiles.
The next can be also formed between tile 1 with groove 7 and a vertical profile 2 as shown in FIG. 2 so that there is on one side of the vertical profile holes made at distance from each other, which hit the groove 7, whereby the jointing compound extrudes through the holes partly to the inside of profile 3. In this manner a corresponding locking effect is reached.
The groove in the edge of tile 1 can be replaced by pits or with a uninterrupted or interrupted bulge.
Further, a tile guide 5 is partly punched off from profile 3 is also illustrated in FIG. 4. Such tile guides 5 are used at a distance from each other to function as bearing surface for the jointing compound.
FIG. 5 shows tiles 1 furnished with still deeper grooves 9 and a horizontal profile 8 still comprising bracket shapes in both directions designed so that the bracket wings hit grooves 9 in tile 1 to keep the tiles mechanically fastened by profiles 8 even without any jointing compound. Also in this embodiment the intention is to add also jointing compound between the tiles. This construction is of such a kind that the tiles and the next horizontal profile 8 are laid and mounted in turns. A solution may also be pushing the tiles sidewards to their place if the horizontal profiles 8 are mounted in the vertical profiles. Guides (5) have to be bent up later in this case.
The lattice offers sufficient rigidity and most characteristically it is made of steel sheet band with a thickness of 0,5 mm. The shape of profile is made most advantageously by rolling the sheet band. The use of material corresponds to the material used in a compact back board.
The facing panel can be easily made more rigid and fixing of tiles improved by spraying adhesive onto the back of the facing panel, for instance glass fibre resin together with or without reinforcing fibres. Fixing means close to the corners with counter parts on the wall, are sufficient for mounting the panel on a wall. It is possible to make various facing panel shapes needed due to deviations caused by window and door openings. Likewise, as a corner element a facing panel can be used with its sides in a 90° angel to each other.
For each facing panel size the latice shall be built with proper spaces between profiles so that guides and bonds fall in the joint space. Tiling is most advantageously carried out with a facing panel in vertical position while jointing is carried out simultaneously.
The body material of profiles can be aluminum, polymer plastic or even carbon fibre in addition to corrosion protected sheet metal profile. The facing panel is well applicable also to fences, for instance shielding fences alongside roads, inwalls and floor levels. | A wall element for a building, especially a lining element used as a facing panel, the front of which is formed of brick, ceramic or similar tiles (1), the joints of which are most advantageously filled with jointing compound. The panel body comprises vertical profiles (2) at a distance from each other and horizontal profiles (3, 8) at a distance from each other, forming a lattice when fixed together, and profiles (2, 3) furnished with guides (4, 5) to facilitate laying of tiles (1) on said profiles. | 4 |
FIELD OF THE INVENTION
[0001] This invention relates generally to decoding codewords of an error-correcting code, and more particularly to optimally decoding codewords using linear programming.
BACKGROUND OF THE INVENTION
[0002] Data communication systems often use binary linear codes to offset the effect of noise. The ideal goal is to reach the Shannon limit of a communication channel. The Shannon limit is the highest rate of error-free transmission possible over a communication channel.
[0003] One class of codes that exhibit very good performance is low-density parity-check (LDPC) codes. Conventional decoders for LDPC codes are based on iterative belief-propagation (BP) decoding. An alternate decoding method is based on linear programming (LP), J. Feldman, M. J. Wainwright, and D. Karger, “Using linear programming to decoding binary linear codes,” IEEE Trans. Inform, Theory, 51:954-972, March 2005, incorporated herein by reference.
[0004] LP decoding has some attractive features. An LP decoder deterministically converges, and when the decoder converges to an integer solution, one knows that the optimal maximum likelihood (ML) codeword has been found. When LP decoding converses to a non-integer solution, a well-defined non-integer “pseudo codeword” has been found. Unfortunately, LP decoding is more complex than BP decoding. In the formulations originally described by Feldman et al., the number of constraints in the LP decoding problem grows exponentially with the maximum check node degree, and the resulting computational load can be prohibitive.
[0005] The very large computational burden of LP decoding has motivated the introduction of adaptive linear programming (ALP) decoding, M. H. Taghavi N. and P. H. Siegel, “Adaptive linear programming decoding,” In Proc. Int. Symp. Inform. Theory, pages 1374-1378, July 2006, incorporated herein by reference. Instead of starting with all of the LP constraints, they first solve for the LP optimum of a problem where the values of the binary codeword symbols are only constrained to be greater than zero and less than one. At the resulting optimum, for each check node, they determine the local constraints that are violated. Adding the violated constraints back into the problem, they then solve the resulting LP. They iterate this process until no local constraints are violated. The result is guaranteed to exactly match the solution to the original LP, even though only a small fraction of the original constraints are used. They observe that the number of constraints used for linear codes is only a small multiple (1.1-1.5) of the number m of parity-checks, even for codes with high check degree, and that ALP decoding is significantly, sometimes several orders of magnitude, more efficient, than standard LP decoding.
[0006] Details of Linear Programming and Adaptive Linear Programming Decoders
[0007] Suppose that the code that must be decoded is a length-n binary linear code C. Assume that a binary codeword x ∈ C is transmitted from a source to a destination, over a memory-less communication channel. The destination receives a codeword y, which is a version of the codeword x that has been distorted by the channel. Pr[{circumflex over (x)}|y] is the probability that: a particular codeword {circumflex over (x)} ∈ C was sent, given, that y is received. If all the codewords are equally likely to be sent, then the ML decoding problem reduces to the following problem:
[0000]
Minimize
∑
i
γ
i
x
^
i
(
1
)
subject
to
the
constraint
x
^
∈
C
,
where
γ
i
is
the
i
th
negative
log
-
likelihood
ratio
defined
as
(
2
)
γ
i
=
log
(
Pr
[
y
i
|
x
i
=
0
]
Pr
[
y
i
|
x
i
=
1
]
)
.
(
3
)
[0008] Here {circumflex over (x)} i is the ith symbol of the candidate codeword {circumflex over (x)}, y i is the ith symbol of the received sequence y, and x i is the ith symbol of the transmitted codeword x. For example, if the channel is a binary symmetric channel (BSC) with bit-flip probability p, then γ i =log(p/(1−p)) if the received bit y i =1, and γ i =log((1−p)/p) if the received bit y i =0. The appropriate negative log-likelihood ratios γ i can be calculated for other channels as well.
[0009] The constraints ( 2 ) for the minimization problem ( 1 ) are binary. Feldman et al. introduced the idea of solving a relaxed version of this minimization problem in which the binary constraints of ( 2 ) are replaced by more tractable constraints over continuous variables. Specifically, the symbols {circumflex over (x)} i are allowed to take any value between and including 0 and 1. This relaxed version of the minimization problem is a linear program.
[0010] Each parity check in the code C implies a number of local linear constraints that codewords of that code must satisfy. The intersection of these constraints defines a “polytope” over which a linear programming (LP) decoder operates. The polytope has both integer and non-integer vertices. An integer vertex is one in which for all i, {circumflex over (x)} i is 0 or 1, while a non-integer vertex is one that includes {circumflex over (x)} i values that are greater than 0 and less than 1.
[0011] The integer vertices of the polytope correspond to codeword in C. When the LP optimum is at an integer vertex. Equation (2) is satisfied and the ML solution is found, even though only a relaxed version of the minimization problem was solved. However, when the LP optimum is at a non-integer vertex. Equation (2) is not satisfied and the LP solution is not the ML codeword. Such non-integer solutions are termed “pseudo codewords.”
[0012] The precise form of the parity check constraints that define the polytope used by Taghavi, et al. is as follows. First, for all bits i, {circumflex over (x)} i is continuous-valued and satisfies the inequalities
[0000] 0≦{circumflex over (x)} i ≦1. (4)
[0013] Then, for every check j=1, . . . , m, every configuration of the set of neighboring variables N(j) ⊂{1, 2, . . . , n} must satisfy the following parity-check inequality constraint: for all subsets Ω ⊂ N(j) such that |Ω| is odd,
[0000]
∑
i
∈
Ω
x
^
i
-
∑
i
∈
M
(
j
)
/
Ω
x
^
i
≤
Ω
-
1.
(
5
)
[0014] Taghavi et al. define a violated constraint as a “cut.” The iterative ALP decoding method starts with the vertex obtained by solving a simple initial problem that only includes a small number of all the LP constraints, and iteratively adds violated constraints and re-solves until no constraints are violated. Taghavi et al. show that violated constraints can be sorted and found efficiently.
[0015] The simple initial problem consists of using only the constraints
[0000] 0 23 {circumflex over (x)} i if γ i >0,
[0000] {circumflex over (x)} i ≦1 if γ i <0. (6)
[0016] The optimum solution of this simple initial problem is immediately found by hard-decision decoding.
[0017] As shown in FIG. 5 , the conventional ALP method operates as follows;
[0018] Initialize 510 the initial problem using the constraints in Equation (6);
[0019] Perform 520 LP decoding;
[0020] Find 530 all violated constraints of the current solution;
[0021] If one or more violated constraints are found, then add 540 the violated constraints to the problem constraints, and go to step 2 if true); and
[0022] Otherwise, if false, then the current solution, is an estimate of the final ALP codeword 541 .
[0023] The ALP decoding method obtains the same codewords or pseudo codewords as standard LP decoders, the only difference is that ALP decoders consume less time.
[0024] When the solution of LP or ALP decoder is non-integer, the ML codeword has not been found, and one is motivated to find a tightening of the original LP relaxation.
[0025] One method of tightening the original LP relaxation is to introduce additional linear constraints that result from redundant parity-check equations. That approach is described by Feldman et al., “Using linear programming to decoding binary linear codes,” and Taghavi et al., “Adaptive linear programming decoding.” Not all redundant parity-check equations improve performance. Therefore, one must search for useful redundant parity-check equations. The computational load of that search, and the quality of the search results, have a large impact on the usefulness of the resulting algorithm. So far, those approaches have not yielded a useable ML decoder.
[0026] Another method enforces a set of integer constraints. That approach is described by Feldman et al, “Using linear programming to decoding binary linear codes,” and by K. Yang, J. Feldman, and X. Wang, “Nonlinear programming approaches to decoding low-density parity-check codes, IEEE J. Select, Areas Commun. 24; 1603-1613, August 2006. A mixed-integer LP solver is used, but complexity constraints keep the applicability of that method to short block-lengths. Feldman et al. only describes decoding results for a block-length, up to 60 bits, and word error rates down to only 10 −4 .
[0027] Another related method is the augmented BP approach, N. Varnica, M. Fossorier, and A. Kavcic, “Augmented belief-propagation decoding of low-density parity check codes,” IEEE Trans. Commun, Volume 54, Issue 10, pages 1896-1896, October 2006. They start with BP, and progressively fix the least certain bits. However, because that method uses BP, the decoder may not succeed in returning a codeword in a reasonable amount of time, and if it does return a codeword, it is not guaranteed to be the optimal ML codeword.
[0028] None of the prior-art decoding methods have provided a decoding method capable of performing optimal ML decoding of LDPC codes with long block-lengths (e.g., block-lengths greater than 100) in a reasonable amount of time, e.g., to be able to produce ML decoding results for word error rates down to 10 −6 or less. Such a decoding method is strongly desired.
SUMMARY OF THE INVENTION
[0029] The embodiments of the invention provide an optimal maximum-likelihood (ML) decoder that uses an adaptive LP decoder as a component. Whenever the adaptive LP decoder returns a pseudo codeword rather than a codeword, an integer constraint is added to the least certain symbol of the pseudo codeword. More generally a set of integer constraints can be added.
[0030] For some codes, and especially in the high-SNR error floor regime, only a few integer constraints are required to force the resultant mixed-integer LP to the ML solution. For example, the invention can efficiently and optimally decode, throughout the entire noise regime of practical interest, a (155, 64) LDPC code. The (155, 64) LDPC code has 2 64 codewords, which is clearly far too great a number to search using any conventional method.
[0031] In contrast to some prior art decoders, which focus on adding redundant parity-checks to LP decoders, the present method adds a small number of integer constraints to the decoding problem. Also in contrast to some prior art that add integer constraints, the method integrates selected integer constraints into an adaptive linear programming decoder.
[0032] The methodology for selecting each binary constraint is as follows. The “least certain” symbols of the optimum pseudo codeword are selected. In very many cases, only a few integer constraints are needed to force the decoder to the ML solution.
[0033] The unexpected effect of the present methodology is particularly striking in the low-noise regime. For example for the (155, 64) LDPC code, the error-rate is decreased by a factor of about a million times compared to both conventional LP decoding and the conventional belief propagation (BP) decoding. What is most unexpected is that in this low noise regime, the increase in decoding time required by the ML method according to the embodiments of the invention, as compared to the conventional LP decoding, is negligible. Therefore, the invention makes ML decoding practical for much longer block-lengths, even when implemented on conventional general-purpose processors.
BRIEF DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 is a graph comparing the word error rate as a function of bit flips of conventional LP decoding, and the ML decoding according to an embodiment of the invention;
[0035] FIG. 2 is a graph comparing the word error rate as a function of crossover probability of conventional LP decoding, conventional BP decoding, and the ML decoding according to an embodiment of the invention;
[0036] FIG. 3 is a table of statistics on the computation time requirements of the ML decoder according to an embodiment of the invention as a function of the number of bit flips;
[0037] FIG. 4 is a graph of the number of binary constraints as a function of the number of bit flips according to an embodiment of the invention;
[0038] FIG. 5 is a flow diagram of a prior art adaptive linear programming decoding; and
[0039] FIG. 6 is a flow diagram of a maximum likelihood decoding using adaptive linear programming decoding according to an embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0040] Method Overview
[0041] FIG. 6 shows a method for decoding a sequence of symbols 607 received via a channel 601 to a codeword 605 of an error-correcting code 604 according to out invention. We begin with a sequence of symbols received via a channel 601 . We presume that the channel can corrupt the symbols because of noise and other factors. Therefore, we use the error correcting code.
[0042] From the sequence of symbols we determine 602 log-likelihood ratios 603 . We use the log-likelihood ratios to initialize 610 a set of constraints 620 for use in our adaptive linear programming decoder. The ALP decoder includes a number of procedures: a LP decoder 630 and a procedure for applying the current solution to the code 604 to find all violated constraints. If violated constraints are found 650 , then the corresponding additional constraints 660 are used to update 670 the constraint set 620 .
[0043] When no further violated constraints are found 650 , then the result is an estimated ALP codeword. If this estimate codeword is not integral 680 , then integer constraints I* are identified 690 . The integer constraints are used to update 670 the constraint set 620 . Otherwise, if the ALP solution is integral, the decoding has converged to the ML solution. In this case, the current ALP solution is the final estimated codeword 605 .
[0044] We now describe our decoding method in greater detail.
[0045] Optimal ML Decoding Via Mixed Integer Adaptive LP Decoding
[0046] When an adaptive linear programming (ALP) decoder fails, it returns a “pseudo codeword,” Recall that pseudo codewords are non-integer vertices of the feasible polytope. If the ALP decoder converges to such a vertex, then we know that the ML codeword has not been found. Therefore, we therefore add additional integer constraints.
[0047] If the ALP decoder fails to find the ML solution, then we add 670 an integer constraint 660 . We identity the symbol {circumflex over (x)} i whose value is closest to 0.5, as a least certain symbol. The index i*, of the symbol {circumflex over (x)} i is
[0000] i* =arg i min|{circumflex over ( x )} i −0.5|. (7)
[0048] Then, we add the constraint {circumflex over (x)} i , ∈{0.1} to the problem, which is now a mixed integer-LP problem and repeat the ALP decoding. If the LP solver 630 does not accommodate integer constraints, then the integer constraint can still be added as follows, solve the LP problem separately for each of the two possible values of x i , and then select the more likely solution.
[0049] After solving the problem including the integer constraint, our solution may still be a pseudo codeword, in which case another integer constraint 680 is added 670 , again for the least-certain symbol of the pseudo-codeword solution.
[0050] The complexity of a mixed-integer linear program grows exponentially with the number of enforced integer constraints. Therefore, our method will succeed in decoding in a reasonable time if and only if the required number of added integer constraints is relatively small. Fortunately for some codes, notably LDPC codes in low-noise applications, a relatively small number of integer constraints are required. Thus, we can obtain a practical and optimal ML decoder, even though the general ML decoding problem is NP-hard.
[0051] Overview of Results
[0052] We describe results of using our mixed-integer ALP method on a (N=155, k=64, d=20) LDPC code as described by R. M. Tanner, D. Sridhara, and T. Fuja, “A class of group-structured LDPC codes.” In Proc. ICSTA, Ambleside, UK, 2001, incorporated herein by reference. This LDPC code has an excellent minimum distance for its dimension and block-length. However, the code has pseudo codewords that greatly impair the performance of a BP or LP decoder. Our method, in contrast with prior-art methods such as “augmented BP,” results in a ML decoder, which provably gives optimal performance and avoids the negative effects of the pseudo codewords.
[0053] FIG. 2 summarized the performance improvement of our approach for a binary-symmetric channel. We compare the word-error rate (WER) of LP decoding 201 using “conventional” ALP decoding, i.e., the ALP relaxation of Equations (6) and (7) without any additional integer constraints, to conventional BP decoding, and to ML decoding 203 obtained using our mixed-integer ALP decoder as shown in FIG. 6 . We categorize the noise levels as low-noise (small cross-over probability) 211 , medium-noise 212 , and high-noise (large cross-over probability) 213 .
[0054] The improvement in WER of ML decoding compared to LP or BP is about 10 5 in the middle of the low-noise level. In the low; end of the low-noise regime the improvement can be a factor of a million or better. In the middle and high-noise levels the improvement is 10 3 and 10, respectively. What is even more startling is that these improvements can be obtained by negligible increase in computational complexity incurred by our method. It should also be noted in contrast with the prior art, that our method does not fail at higher crossover probabilities.
[0055] FIG. 3 summarized the decoding time statistics versus the number of bit flips. The rows listed in column 301 indicate the type of statistic, and columns 302 the result for that statistic categorized by the number of bit flips. For 12, 14 , and 16 bit flips, the average decoding times of LP decoding are 0.12, 0.15, and 0,23 seconds respectively. For our method of ML decoding via mixed-integer ALP, the corresponding average decoding times are 0.14, 0,22, 0.87 seconds. With our method, five to six orders magnitude in improvements in WER require very little increase in the average decoding time.
[0056] Details of Experimental Results
[0057] We also describe the number of ALP iterations needed to obtain to the ML solution, the number of binary constraints required, and provide statistics on the computation time requirements of our ML decoder.
[0058] While we simulate code performance for the binary-symmetric channel, we note that our decoder also works on other channels, such as an additive-white Gaussian noise (AWGN) channel. The minimum distance of the (155, 64) LDPC code is 20 . Therefore, the ML decoder is guaranteed to succeed if nine or fewer bits are flipped. When ten or more bits are flipped, the ML decoder may fail because another codeword is more likely than the transmitted codeword. We find that the number of required integer constraints and ALP decoding iterations grows with the number of bit flips, but is manageable for all bit flips up to 23. We employ a cap of 200 ALP decoding iterations (defined as the overall number of linear programs solved—pure linear programs or mixed-integer LPs) before giving up on a particular received word as taking too long to decode.
[0059] The rate of the (155, 64) code is 0.4129. If we could operate near capacity, then we could only expect to correct about 22 bit flips. To simplify our analysis as shown in FIG. 2 , we estimate the error rate at a number of noise levels, each corresponding to a fixed number of bit flips. We simulate up to 23 bit flips and simply assume decoding will fail, with probability 1 for the very high noise regime of more than 23 bit flips. This is slightly pessimistic given that the ML word-error rate (WER) is about “only” 0.73 for 23 bit flips but is also realistic given that for 24 or more bit flips the decoder runs very slowly. We perform decoding experiments at each number of bit-flips from 23 down, to 12, until we accumulated 200 ML decoding errors at each bit-flip level. The WERs resulting from these experiments are shown in FIG. 1 .
[0060] For 10 and 11 bit flips, the ML decoder performs very well. However, it is difficult to obtain enough failures through simulation. At 11 bit flips, we accrued only 79 ML decoding errors. Therefore, we estimate the performance as follows. We start by noting that, e.g., in a 12-bit flip failure, at least 10 of the flips must overlap another codeword, or else the ML decoder would decode to the codeword that was transmitted. Empirically, nearly all failures are produced when exactly 10 bits overlap; 11 bit and 12 bit overlaps are much less likely. In such a case, we start with a 12 bit failure pattern and reduce by one the number of bit flips. Then, the probability that we take away one of the two (non-overlapping) bits so that we would still have a failure is (2/12). The resulting estimated error probability of 8.3×10 −7 =(2/12) 5.9×10 −6 for 11 bit flips is in rough agreement with our experimental observation of 1.1×10 −6 based on only 79 decoding failures. We use the same idea to estimate the WER at 10 bit flips to be (1/11)th of the estimated WER at 11 bit flips.
[0061] To generate FIG. 2 , we need to estimate the ML WER for a range of crossover probabilities. To make these estimates, we again note that the WER is zero for nine or fewer bit flips and assume that the WER equals one for 24 or more bit flips. We then calculate the probability of realizing each number of bit flips for a particular crossover probability and average the empirical WERs at fixed number of bit flips by the appropriate binomial coefficient. The combination of knowing that no ML errors occur for nine or fewer bit flips, and the error statistics for larger number of bit flips, allows us to estimate ML performance down to much lower WERs than, would be possible if we generated the number of bit flips stochastically.
[0062] Another quantity of interest is the time requirement of our mixed-integer ALP decoding. FIG. 3 shows a table of statistics on decoding time to produce our results. The first row indicates the number of bit flips, and subsequent rows indicate average and median decoding times for all simulations, correct decoding and erroneous decodings, respectively.
[0063] We also collect statistics on the number of integer constraints required to decode. Integer constraints slow the LP solver considerably as compared to regular linear constraints. FIG. 4 shows the number of integer constraints as a function of the number of bit flips. The top line 401 is the worst case number of iterations, the next line 402 depicts the 95 th percentile—95% of the simulations at each bit flip level took at most the indicated number of integer constraints to find the ML codeword. We also indicate the 90 th percentile 403 and the 50 th percentile 404 (the median). Note that the worst case is much worse than even the 95 th percentile. These numbers combine all decodings (successes and failures). Recall that we imposed a cap of 200 ALP decoding iterations on our decoder. This cap is reached only very rarely and only at the highest bit flip levels. In our simulations, the cap is reached at least once only at 20, 22, and 23 bit flips. For all other numbers of bit flips, the cap is never reached.
[0064] By comparing FIG. 4 and the table in FIG. 3 , one can see that the number of integer constraints has a large impact on the decoding time. FIG. 4 shows that the median case for 12, 14 and 16 bit flips is zero integer constraints. This means that the median case is performing ALP decoding without integer constraints.
[0065] Turning to the table of FIG. 3 , this means that the corresponding median decoding times—0.12, 0.15, 0.23 seconds—tell us the decoding time requirements of ALP decoding without integer constraints. In contrast, the corresponding average decoding times—0.14, 0.22, 0.87 seconds—tell us the average decoding time requirement of ML decoding via mixed-integer ALP decoding. Thus, a 10 3 to 10 5 improvement in error rate requires only a small increase in average decoding time.
[0066] For higher noise levels, e.g., when there are 18 or 20 bit flips, the median case uses a positive number of integer constraints. The corresponding median decoding times increases sharply, to 1.33 and 20.6 seconds, respectively.
EFFECT OF THE INVENTION
[0067] We describe a method for adding integer constraints to an ALP decoder to find the ML codeword. We exploit the computational efficiency of adaptive LP decoding to speed up our method. We apply the decoder to a (155, 64) LDPC code, which is a surprisingly long code for which to obtain ML decoding performance.
[0068] Although the invention has been described by way of examples of preferred embodiments, it is to be understood that various other adaptations and modifications can be made within the spirit and scope of the invention. Therefore, it is the object of the appended claims to cover all such variations and modifications as come within the true spirit and scope of the invention. | A method and system decodes a sequence of symbols received via a channel to a codeword of an error-correcting code. Log-likelihood ratios are determined from a sequence of symbols received via a channel. A set of constraints is initialized according to the log-likelihood ratios. An adaptive linear programming decoder is applied to the set of constraints and the log-likelihood ratios according to an error-correcting code to produce an estimate of the codeword and an updated set of constraints. If the estimate of the codeword is a non-integer pseudo codeword, further update the set of updated constraints with a set of integer constraints if the estimate of the codeword is the non-integer pseudo codeword, and proceeding with the applying step, and otherwise producing the estimate of the codeword as the final codeword. | 7 |
This is a divisional application of Ser. No. 07/239,288, filed Sept. 1, 1988 which is a continuation-in-part of U.S. application Ser. No. 07/176,144 filed Mar. 31, 1988.
BACKGROUND OF THE INVENTION
This invention relates to a method of manufacturing superconducting patterns.
Along with efforts to make integrated circuits more dense, high operational speeds are required. The fine structures of electric circuits give rise to problems of decrease in operational speed and in reliability at exothermic parts of integrated circuits. Because of this, if semiconductor devices are driven at the boiling point of liquid nitrogen, the mobilities of electron and hole become 3-4 times as faster as those at room temperature and as a result the frequency characteristics can be improved.
The Josephson devices such as a memory which functions based on the Josephson effect are known as superconductive electronical devices. In this device, switching operation assciated with the Josephson effect is performed. A schematic view of an example of such a device is shown in FIG. 1. The device comprising a superconducting film 24 adjoined to a superconducting region formed within a substrate 21 with a barrier film 23 therebetween. The advantege of the device is operability at a very high frequency. However, the oxygen proportion contained in the superconducting ceramics of this type tend to be reduced.
SUMMARY OF THE INVENTION
It is therefore an object of the invention to provide a method of effectively manufacturing superconducting patterns.
It is another object of the present invention to provide a method of manufacturing superconducting patterns at high production yield.
In order to accomplish the above and other objects and advantages, non-superconducting regions are formed within ceramic superconductors by adding an element which fuctions to spoil the superconducting structure of the ceramics and insulating the same. The non-superconducting region is thermal annealed or fired. When a superconducting film is formed on a surface, the (a,b) plane in the crystalline film is aligned parallel to the underlying surface because current can flow along that plane 100 time as dense as along the normal direction thereto.
Preferred examples of the elements to be added to superconducting ceramics for the purpose of converting the superconducting structure to insulating non-superconducting structure are Si, Ge, B, Ga, P, Ta, Mg, Be, Al, Fe, Co, Ni, Cr, Ti, Mn and Zr. Preferred examples of the superconducting ceramic materials used in accordance with the present invention are represented by the stoichiometric formula, (A 1-x B x ) y Cu z O w , where A is one or more elements of Group IIIa of the Priodic Table, e.g., the rare earth elements or lantanoides, B is one or more alkaline earth metals, i.e. Ba, Sr and Ca, and x=0-1; y=2.0-4.0, preferably 2.5-3.5; z=1.0-4.0, preferably 1.5-3.5; and w=4.0-10.0, preferably 6.0-8.0. When added to superconducting ceramics of this type, the spoiled non-superconducting ceramics are represented by the stoichiometric formula, referred to "non-superconducting ceramics" hereinafter, [(A' p A" 1-p ) 1-x (B' q B" 1-q ) x ] y (Cu r X 1-r ) z O w , where A' is one or more elements of Group IIIa of the Priodic Table, e.g., the rare earth elements or lantanoides, B' is one or more alkaline earth metals, i.e. Ba, Sr and Ca, A", B" and X are selected from a group consisting of Mg, Be, Al, Fe, Co, Ni, Cr, Ti, Mn and Zr, and x=0.1-1; y=2.0-4.0, preferably 2.5-3.5; z=1.0-4.0, preferably 1.5-3.5; and w=4.0-10.0, preferably 6.0-8.0. The numbers p, q and r are chosen to be 0.99 to 0.8 so that the total proportion of A", B" and X is 1-25 atom % in the ceramic material, particularly in case of Mg and Al, the proportion may be 1-10 atom %, e.g. 5-10 atom %. The total density of the spoiling elements in a non-superconducting ceramic is about 5×10 18 to 6×10 21 cm -3 . Since the superconducting properties of superconducting ceramics are sensitive to proportion of thier constituents, the spoiling element can be selected from among the constituents of themselves. When superconducting constituents are employed as the spoiling element, the total density of the additional elements is 5×10 19 to 5×10 22 cm -3 .
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic view showing a prior art superconducting device.
FIGS. 2(A), 2(B), and 2(C) are cross sectional views showing first, second and third embodiments in accordance with the present invention.
FIG. 3 is a graphical diagram showing the current voltage characteristic of devices in accordance with the present invention.
FIGS. 4(A), 4(B), and 4(C) are cross sectional views showing first, second and third embodiments in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIGS. 2(A) to 2(C), superconducting devices in accordance withthe present invention is illustrated.
The device shown in FIG. 2(A) comprises a substrate 1 having a non-conductive upper surface such as a substrate of YSZ(yttria stabilized zircon), a pair of superconducting regions 3 and 5, an intervening barrierfilm 4 between the regions 3 and 5, insulating films 20 positioned at the opposed ends of the superconducting regions 3 and 5, an overlying passivation film 11 formed with openings 11-1 and 11-2 at the regions 3 and 5 and electrodes 8 and 9 electrically contacting the superconducting regions 3 and 5.
An exemplary method of manufacturing the device will be described. First, aceramic oxide film of composition in agreement with the composition of a superconducting material as specifically stated in the last portion of this description is formed on the substrate 1 by screen printing, sputtering, MBE (Molecular Beam Epitaxial), CVD and the other methods. At the same time or thereafter, the ceramic oxide is thermally annealed at 600°-950° C. for 5-20 hours followed by gradually cooling. In accordance with experimental, the critical temperature was measured to be 91K for example.
The barrier film 4 is formed after or before the annealing by adding a spoiling element such as alminium or magnesium by ion implantation to 5×10 8 -6×10 21 cm -3 , e.g. 2×10 20 cm -3 . This ion implantation is performed at an accelation voltage of 50-2000 V with a photoresist mask covering the superconducting regions 3 and 5 so that the barrier film 4 and the insulating films 20 become "non-superconducting." The barrier film 4 is no wider than 1000 Å in the lateral direction in order to permit tunnel current thereacross.
The passivation film 11 of an insulating ceramic having similar compositionas the underlying superconducting ceramic film is formed over the structure, followed by oxidation in an oxidizing atmosphere at 300°-950° C., e.g. 700° C. for the purpose of fittingthe films of the structure together and compensating the oxygen proportion at the surface area. The passivation film 11 is spoiled in the same manneror formed by making use of a spoiled composition. The spoiling element is oxidized during this oxidation process. Then, after forming the openings 11-1 and 11-2, the lead electrodes 8 and 9 is formed in ohmic contact withthe superconducting regions 3 and 5 respectively. The electrodes 8 and 9 may be formed of superconducting ceramics. In that case, the formation of the electrodes is preferably carried out before the annealing. FIG. 3 is an example of the voltage-current characteristic of the devices in accordance with the present invention.
In the previous example, the densities of the spoiling elememt in the barrier film 4 and the insulating films 20 are same. However, by separately effecting ion implantation, the films 4 and 20 can be formed sothat the density of the barrier film is 0.1 to 20 atom % which is 1/10-1/5,e.g. 1/5, of the density of the insulating films.
Referring to FIG. 2(B), a second embodiment of the present invention is illustrated. This embodiment is approximately same as the previous embodiment except for a control electrode 10 formed over the barrier film 4 with the insulating film 11 therebetween. The current passing through the barrier film 4 is controlled by the applied voltage by the control electrode 10. In this embodiment, the barrier film 4 may be superconducting. In that case, the operation temperature of the device should be selected so that the superconducting barrier film 4 is in an intermediate state between superconducting state and non-superconducting state. Namely, the temperature is selected within the range from Tc onset and Tco. The action of the device is described in our commonly assigned U.S. patent application Ser. No. 167,987 filed on Mar. 14, 1988, now abandoned.
Referring to FIG. 2(C), a third embodiment is illustrated. This device is approximately same as the second embodiment except for provision of an underlying control electrode 10'. The barrier film 4 is sandwitched by theoverlying control film 10 and the underlying control film 10'.
FIGS. 4(A) to 4(C) are modifications of the preceding embodiments shown in FIGS. 2(A) to 2(C) respectively. These embodiments are constructed in substantially same manner with the exception specified as below.
FIG. 4(A) is a cross section view showing a fourth embodiment of the present invention. The substrate 1" is a proportion of a silicon semiconductor substrate within which an integrated circuit is formed. The upper surface of the substrate 1" is made non-conductive by covering a ceramic oxide film 1'. After forming the superconducting regions 3 and 5, the barrier film 4 and the insulating films 20 on the substrate in the same manner, a superconducting, ceramic oxide film 40 is formed and partlymade non-superconducting by adding a spoiling element thereto except for connection portions 8' and 9'. Further, a superconducting ceramic film 50 is formed on the structure of the film followed by spoiling the superconducting structure except for the electrodes 8 and 9. Although the fabricating process substantially corresponds to that of preceding embodiments, the electrodes 8 and/or 9 which may be connected with the integrated circuit have not to be given thermal treatment at no lower than400° C. in order to avoid oxidation of the silicon semiconductor by the oxygen content of the superconducting electrodes 8 and 9.
Referring to FIG. 4(B), a fifth embodiment of the present invention is illustrated. This embodiment is approximately same as the fourth embodiment except for a control electrode 10 made of a superconducting ceramic formed over the barrier film 4 with the insulating film 11 therebetween. The current passing through the barrier film 4 is controlledby the applied voltage by the control electrode 10. In this embodiment, thebarrier film 4 may be superconducting. The operation temperature of the device should be selected so that the superconducting barrier film 4 is inan intermediate state between superconducting state and non-superconductingstate. Namely, the temperature is selected within the range from Tc onset and Tco.
Referring to FIG. 4(C), a sixth embodiment is illustrated. This device is approximately same as the fifth embodiment except for provision of an underlying control electrode 10'. The barrier film 4 is sandwitched by theoverlying control film 10 and the underlying control film 10'.
Superconducting ceramics for use in accordance with the present invention also may be prepared in consistence with the stoichiometric formulae (A 1-x B x ) y Cu z O w , where A is one or more elements of Group IIIa of the Periodic Table, e.g., the rare earth elements, B is one or more elements of Group IIa of the Periodic Table, e.g., the alkaline earth metals including beryllium and magnesium, and x=0-1; y=2.0-4.0, preferably 2.5-3.5; z=1.0-4.0, preferably 1.5-3.5; and w=4.0-10.0, preferably 6.0-8.0. Also, superconducting ceramics for use in accordance with the present invention may be prepared consistent with the stoichiometric formulae (A 1-x B x ) y Cu z O w , where A is one or more elements of Group Vb of the Periodic Table such as Bi, Sband As, B is one or more elements of Group IIa of the Periodic Table, e.g.,the alkaline earth metals including beryllium and magnesium, and x=0.3-1; y=2.0-4.0, preferably 2.5-3.5; z= 1.0-4.0, preferably 1.5-3.5; and w=4.0-10.0, preferably 6.0-8.0. Examples of this general formula are BiSrCaCuCu 2 O x and Bi 4 Sr 3 Ca 3 Cu 4 O x . Tc onset and Tco samples confirmed consistent with the formula Bi 4 Sr y Ca 3 Cu 4 O x (y is around 1.5) were measured to be 40°-60° K., which is not so high. Relatively high critical temperatures were obtained with samples conforming to the stoichiometric formulae Bi 4 Sr 4 Ca 2 Cu 4 O x and Bi 2 Sr 3 Ca 2 Cu 2 O x . FIGS. 7 and 8 are graphical diagrams showing therelationship between the resistivity and the temperature for both samples. The number x denoting the oxygen proportion is 6-10, e.g. around 8.1. Suchsuperconducting materials can be formed by screen press printing, vacuum evaporation or CVD.
While a description has been made for several embodiments, the present invention should be limited only by the appended claims and should not be limited by the particular examples. For example, the present invetnion canbe applied for SQUIDs, VLSIs or ULSIs. The superconducting ceramics in accordance with the present invention may have single crystalline or polycrystalline structures. | A manufacturing method of Josephson devices is described. A superconducting ceramic film is deposited on a non-conductive surface and partly spoiled in order to form a barrier film by which two superconducting regions is separated. The spoiling is performed by adding a spoiling element into the ceramic film by ion implantation. | 8 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Pursuant to 35 U.S.C. §119(a), this application claims the benefit of earlier filing date and right of priority to Korean Application No. 10-2009-008220, filed on Sep. 1, 2009, the contents of which is hereby incorporated by reference herein in its entirety.
FIELD OF THE INVENTION
[0002] The present invention relates to a method and an apparatus for transmitting and receiving a media signal using different wireless communication techniques.
DISCUSSION OF THE RELATED ART
[0003] A display device includes a receiving unit that receives a media signal including video and audio from a broadcasting system, a cable system, and other external apparatuses (VCR, DVD, etc.) and processes and outputs the received media signal on a display of the display device. Further, the receiving unit may be physically separated from the display device. In recent years, a wireless type display system has been provided, which transmits a media signal received using an additional receiver to the display device through wireless communication and displays the transmitted media signal on the display.
SUMMARY OF THE INVENTION
[0004] Accordingly, one object of the present invention is to provide a method and an apparatus for efficiently transmitting and receiving a media signal using wireless communication.
[0005] To achieve these and other advantages and in accordance with the purpose of the present invention, as embodied and broadly described herein, the present invention provides in one aspect a method of controlling devices, and which includes converting, via a transmitting apparatus, a signal including at least one of the video/audio and data into a first definition wireless signal, transmitting, via the transmitting apparatus, the converted first definition wireless signal to a receiving apparatus, receiving, via the receiving apparatus, the first definition wireless signal, extracting, via the receiving apparatus, said at least one of the video/audio and data included in the first definition wireless signal, outputting said at least one of the video/audio and data included in the first definition wireless signal on the receiving apparatus, detecting, via a detector on the receiving apparatus, a quality of the received first definition wireless signal, and comparing, via a processor on the receiving apparatus, the detected quality of the received first definition wireless signal with a predetermined value, and transmitting a first command to the transmitting apparatus to transmit a second definition wireless signal including said at least one of the video/audio and data to the receiving apparatus, when the detected quality of the received first definition wireless signal is lower than the predetermined value, the first and second definition wireless signals using different wireless communication standards. A corresponding system for controlling devices is also provided.
[0006] In still another aspect, the present invention provides a television including a receiver configured to receive a first definition wireless signal including at least one of video/audio and data from an external device, a processor configured to extract said at least one of the video/audio and data included in the first definition wireless signal, and an output device configured to output said at least one of the video/audio and data included in the first definition wireless signal. Further, the processor is further configured to detect a quality of the received first definition wireless signal, to compare the detected quality of the received first definition wireless signal with a predetermined value, and to transmit a first command to a second transmitting apparatus associated with the external device to transmit a second definition wireless signal including said at least one of the video/audio and data to the television, when the detected quality of the received first definition signal is lower than the predetermined value, said first and second definition wireless signals using different wireless communication standards. A method of controlling a television is also provided.
[0007] Further scope of applicability of the present invention will become apparent from the detailed description given hereinafter. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The above and other aspects, features, and advantages of the present invention will become more apparent upon consideration of the following description of preferred embodiments, taken in conjunction with the accompanying drawing figures.
[0009] FIG. 1 is a block diagram illustrating a signal transmitting/receiving system according to an embodiment of the present invention;
[0010] FIG. 2 is a block diagram illustrating a transmitting apparatus according to an embodiment of the present invention;
[0011] FIG. 3 is a block diagram illustrating a receiving apparatus according to an embodiment of the present invention;
[0012] FIG. 4 is a flowchart illustrating a method for receiving a signal according to a first embodiment of the present invention;
[0013] FIG. 5 is a flowchart illustrating a method for receiving a signal according to a second embodiment of the present invention;
[0014] FIG. 6 is a flowchart illustrating a method for receiving a signal according to a third embodiment of the present invention; and
[0015] FIGS. 7 and 8 are block diagrams illustrating a signal transmitting/receiving system according to still other embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0016] Hereinafter, a method for receiving a signal, a transmitting/receiving apparatus and a display apparatus thereof according to embodiments of the present invention will be described in detail with reference to the accompanying drawings.
[0017] FIG. 1 is a block diagram illustrating a signal transmitting/receiving system according to an embodiment of the present invention. As shown, the transmitting/receiving system includes a transmitting apparatus 100 and a receiving apparatus 200 . In more detail, the transmitting apparatus 100 receives a media signal from a broadcasting system, a cable system, or external apparatuses, converts the received media signal into data of a wireless transmittable format and then wirelessly transmits the data.
[0018] In addition, the receiving apparatus 200 receives and processes the media signal wirelessly transmitted from the transmitting apparatus 100 . To perform this operation, one or more wireless communication standards for wirelessly transmitting and receiving the media signal can be previously established between the transmitting apparatus 100 and the receiving apparatus 200 . Also, the transmitting apparatus 100 includes various input terminals such as a high-definition multimedia interface (HDMI) terminal connected with an antenna or external apparatuses, a universal serial bus (USB) terminal, a component terminal, an external input terminal, an RGB terminal, an antenna cable terminal, etc. and can receive the media signal using the input terminals. For example, the broadcasting signal may include a media signal received using the antenna, a cable, or the like or video and audio signals received from connected external devices in the transmitting apparatus 100 .
[0019] In addition, the transmitting apparatus 100 may be a set-top box (STB) that receives the media signal using a wired or wireless network, and converts and wireless transmits the received media signal to the receiving apparatus 200 . However, the transmitting apparatus 100 is not limited to the set-top box (STB) and can include all types of devices that can receive the media signal transmitted from the outside and wirelessly transmit the received media signal to the receiving apparatus 200 . For example, the transmitting apparatus 100 can be implemented by being provided in a computer or a portal terminal such as a cellular phone, etc.
[0020] Further, the receiving apparatus 200 receives and processes the signal wirelessly transmitted from the transmitting apparatus 100 , and thereafter can transmit the data to an external apparatus that outputs the video or audio included in the signal. For example, the receiving apparatus 200 can convert the media signal wirelessly transmitted from the transmitting apparatus 100 into a displayable format and output the video signal on a display device. More specifically, when the media signal wirelessly transmitted from the transmitting apparatus 100 is encoded by a coding scheme such as an MPEG, etc., the receiving apparatus 200 decodes the received video signal and outputs the decoded video signal to the display device.
[0021] Also, according to embodiments of the present invention, the transmitting apparatus 100 and the receiving apparatus 200 can transmit and receive the media signal using various wireless communication standards, for example, wireless communication standards such as wireless HD (WiHD), wireless home digital interface (WHDi), wireless Lan (WiFi), etc. In more detail, the WiHD uses a frequency band of approximately 60 GHz and can transmit and receive data at transmission rate of approximately 4 Gbps to thereby transmit HD video data of 1080p (1902×1080) without compression. However, WiHD uses a high frequency band of 60 GHz such that a data transmitting/receiving distance is approximately 10 m and the transmission/reception quality can be easily influenced by obstacles in the vicinity of an installation space.
[0022] In addition, WHDi can transmit and receive the data at a transmission rate of approximately 1.8 Gbps using a frequency band of approximately 5 GHz. Further, the WHDi uses a comparatively low frequency band of 5 GHz such that the data transmitting/receiving distance is approximately 30 m and the transmission/reception quality is not significantly influenced by the obstacles in the vicinity of the installation space. Meanwhile, when the HD video data of 1080p (1920×1080) is transmitted using WHDi at the transmission rate of approximately 1.8 Gbps, the transmitting apparatus 100 partially compresses and transmits the HD video data.
[0023] Further, WiFi can transmit and receive the data at a transmission rate of approximately 54 Mbps using a frequency band of approximately 2.4 GHz. WiFi uses a comparatively low frequency band of 2.4 GHz such that the data transmitting/receiving distance is approximately 50 to 200 m and the transmission/reception quality is almost not at all influenced by the obstacles in the vicinity of the installation space. Meanwhile, when the HD video data of 1080p (1920×1080) is transmitted using WiFi at the low transmission rate of approximately 54 Mbps, the transmitting apparatus 100 can compress and transmit the HD video data and as a result, the image quality of the video signal received from the receiving apparatus 200 is generally not deteriorated.
[0024] In addition, the transmitting apparatus 100 and the receiving apparatus 200 can wirelessly transmit and receive the media signal using various short-range wireless communication standards, for example, communication standards such as Bluetooth, ZigBee, or binary code division multiple access (CDMA), etc. in addition to the above-mentioned wireless communication standards. Further, the transmitting apparatus 100 and the receiving apparatus 200 can transmit and receive video and audio data using a plurality of wireless communication standards of various wireless communication standards. That is, the transmitting apparatus 100 can support two or more communication standards, and convert the same media signal received from the outside into two or more signals and wirelessly transmits the signals in accordance with the wireless communication standards.
[0025] Further, the receiving apparatus 200 can also support the two or more wireless communication standards and can receive two or more signals wirelessly transmitted using different wireless communication standards from the transmitting apparatus 100 . The receiving apparatus 200 can also select any one of two or more signals in accordance with different wireless communication standards, and convert the selected signal into a displayable format and output the converted signal. For example, the receiving apparatus 200 can select and process a signal depending on a wireless communication scheme to provide an optimum signal transmission/reception performance in accordance with a current transmission environment, and more specifically, a distance between the transmitting and receiving apparatuses 100 and 200 , an installation space, or the resolution of the transmission image.
[0026] Next, FIG. 2 is a block diagram illustrating the transmitting apparatus 100 according to an embodiment of the present invention. As shown, the transmitting apparatus 100 includes a baseband unit 110 and an RF transmitting unit 120 . Further, the baseband unit 110 includes a media access control (MAC) layer 113 and a physical (PHY) layer 114 . In addition, the signal processing unit 111 can process the media signal received from the outside and output the processed media signal to the control unit 112 . For example, the signal processing unit 111 may include a frame buffer, store the video signal received from the outside in the frame buffer and output the video signal in accordance with a predetermined format.
[0027] The control unit 112 also controls an overall operation of the transmitting apparatus 100 , for example, controls the signals output from the signal processing unit 111 to be converted into a wirelessly transmittable format in accordance with a predetermined wireless communication standard through the media access control (MAC) layer 113 and the physical (PHY) layer 114 and wirelessly transmitted through the RF transmitting unit 120 . In addition, the media access control (MAC) layer 113 may include a plurality of media access control (MAC) layers corresponding to different communication schemes, respectively so that the transmitting apparatus 100 supports a plurality of different communication schemes.
[0028] That is, the media access control (MAC) layer 113 may include a first media access control (MAC) layer corresponding to a first wireless communication scheme and a second media access control (MAC) layer corresponding to a second wireless communication scheme different from the first wireless communication scheme. In addition, in one embodiment of the present invention, the transmitting apparatus 100 can support WiHD and WHDi, and to perform this function, the baseband 110 of the transmitting apparatus 100 includes a WiHD media access control (MAC) layer and a WHDi media access control (MAC) layer.
[0029] Hereinafter, the situation in which the transmitting apparatus 100 can support WiHD and WHDi will be given as an example, and an operation of the transmitting apparatus 100 will be described according to an embodiment of the present invention. In particular, the control unit 112 outputs the signal output from the signal processing unit 111 to each of the WiHD media access control (MAC) layer and the WHDi media access control (MAC) layer. The WiHD media access control (MAC) layer then converts the media signal into wirelessly transmittable data in accordance with a WiHD wireless communication standard, and the WHDi media access control (MAC) layer converts the media signal into wirelessly transmittable data in accordance with a WHDi wireless communication standard.
[0030] As described above, the signals converted in accordance with the WiHD and WHDi wireless communication standards can be transmitted to the RF transmitting unit 120 through the physical (PHY) layer 114 , and the RF transmitting unit 120 can wirelessly transmit the first signal converted in accordance with WiHD and the second signal converted in accordance with WHDi. For example, the RF transmitting unit 120 can receive the first and second signals converted in accordance with WiHD and WHDi, respectively from the baseband 110 and wirelessly transmit the first and second signals using different frequency bands, that is, a frequency band of approximately 60 GHz for WiHD and a frequency band of approximately 5 GHz for WHDi. To do this operation, the RF transmitting unit 120 includes a wideband antenna and a converter corresponding to each of the frequency bands.
[0031] In addition, the RF transmitting unit 120 includes an up-converter and a down-converter corresponding to the frequency bands, respectively to transmit the signal and wirelessly receive the signal from the outside. Further, in the above description, the transmitting apparatus 100 can support WiHD and WHDi, for example, but this is just one embodiment of the present invention. That is, the transmitting apparatus 100 can support two or three or more wireless communication schemes among various wireless communication schemes. For example, as another embodiment of the present invention, the transmitting apparatus 100 can support WiHD and WiFi. To perform this operation, the baseband unit 110 of the transmitting apparatus 100 includes the WiHD media access control (MAC) layer and a WiFi media access control (MAC) layer.
[0032] Next, FIG. 3 is a block diagram illustrating the receiving apparatus 200 according to an embodiment of the present invention. As shown, the receiving apparatus 200 includes a baseband unit 210 and an RF receiving unit 220 . Further, the RF receiving unit 220 can receive video and audio signals transmitted form the transmitting apparatus 100 , and the received signal can be input into a signal processing unit 211 through a physical (PHY) layer 214 and a media access control (MAC) layer 213 . For example, the signal processing unit 111 may include a frame buffer, store the received video signal in the frame buffer and output the video signal to execute the corresponding application.
[0033] In addition, the control unit 212 controls an overall operation of the receiving apparatus 200 , for example, allows the video signal received through the RF receiving unit 220 to be converted into a displayable format through the physical (PHY) layer 214 and the media access control (MAC) layer 213 by the corresponding application. The media access control (MAC) layer 213 can also include a plurality of media access control (MAC) layers corresponding to different communication schemes, respectively so that the transmitting apparatus 200 supports a plurality of different communication schemes. Further, the receiving apparatus 200 can support WiHD and WHDi by including a WiHD media access control (MAC) layer and a WHDi media access control (MAC) layer.
[0034] Hereinafter, the situation in which the receiving apparatus 200 supports WiHD and WHDi will be given as an example, and an operation of the receiving apparatus 200 will be described in detail according to an embodiment of the present invention. In more detail, the RF receiving unit 220 can receive a first signal wirelessly transmitted using WiHD and a second signal wirelessly transmitted using WHDi. For example, the RF receiving unit 220 can receive the first and second signals transmitted from the transmitting apparatus 100 using different frequency bands, that is, a frequency band of approximately 60 GHz for WiHD and a frequency band of approximately 5 GHz for WHDi. To do this, the RF receiving unit 220 includes a wideband antenna and converters corresponding to the frequency bands.
[0035] In addition, the RF receiving unit 220 includes down-converters and up-converters corresponding to the frequency bands, respectively and can receive the signal and wirelessly transmit the signal to the outside as described above. The control unit 212 can also select any one signal of the received first signal depending on WiHD and the received second signal depending on WHDi. For example, the control unit 212 can select a signal of the first and second signals corresponding to the wireless communication scheme and provide the selected signal to the signal processing unit 211 by selecting a wireless communication scheme to provide an optimum signal transmission/reception performance in accordance with a current data transmission/reception environment between the transmitting and receiving apparatuses 100 and 200 .
[0036] Further, the wireless communication scheme to provide the optimum transmission/reception performance may be input by a user through a user input unit provided in the transmitting apparatus 100 or the receiving apparatus 200 . Alternatively, the control unit 212 can measure reception signal sensitivities of the received first and second signals, and select a signal having the high measured reception sensitivity of the first and second signals and provide the signal to the signal processing unit 211 . Also, the data transmission/reception performance between the transmitting apparatus 100 and the receiving apparatus 200 that wirelessly transmit and receive data, that is a signal reception sensitivity in which the signal transmitted from the transmitting apparatus 100 is received in the receiving apparatus 200 may be influenced by a distance between the transmitting apparatus 100 and the receiving apparatus 200 , existence of an adjacent obstacle, etc.
[0037] In particular, when transmitting and receiving the data between the transmitting apparatus 100 and the receiving apparatus 200 using WiHD having a high frequency band of dozens of GHzs, for example, a frequency band of approximately 60 GHz, a data transmission/reception distance is short at approximately 10 m and the signal reception sensitivity may be influenced depending on the adjacent obstacle by high linearity. Further, when the signal reception sensitivity decreases as described above, the data between the transmitting apparatus 100 and the receiving apparatus 200 may be lost, thereby deteriorating the quality of an image displayed when received through the receiving apparatus 200 .
[0038] As described above, WiHD is fast in transmission speed to transmit HD image data through non-compression, but the transmission/reception distance is short (e.g., approximately 10 m) and transmission/reception quality may easily be influenced by the adjacent obstacles of an installation space, while WHDi is slower in transmission speed to transmit the HD image data through compression, but the transmission/reception distance is long (e.g., approximately 30 m) and the transmission/reception quality may not be influenced by adjacent obstacles of the installation space.
[0039] Therefore, when the distance between the transmitting apparatus 100 and the receiving apparatus 200 is long, for example, when the distance is 10 m or more, the control unit 212 of the receiving apparatus 200 selects the second signal of the first and second signals, which is transmitted via WHDi. Further, when obstacles exist between the transmitting apparatus 100 and the receiving apparatus 200 , the transmitting apparatus 100 and the receiving apparatus 200 are installed in different spaces divided by a wall, etc., the control unit 212 of the receiving apparatus 200 selects the second signal of the first and second signals, which is transmitted via WHDi.
[0040] Further, the control unit 212 can measure or detect a distance between the transmitting apparatus 200 and the receiving apparatus using a laser, for example, or other detection mechanism. The control unit 212 can also determine if there are any obstacles placed between the transmitting apparatus 200 and the receiving apparatus 100 . The control unit 212 can then select the best wireless transmission method. The quality of the received signal or the bit error rate can also be used to select the best wireless transmission method as discussed above.
[0041] Meanwhile, when the HD image data is transmitted from the transmitting apparatus 100 , the control unit 212 selects the first signal of the first and second signals, which is transmitted via WiHD. Thus, it is possible to prevent the quality of an image from being deteriorated due to compression by selecting and via WiHD. However, even in this instance, the distance between the transmitting apparatus 100 and the receiving apparatus 200 and whether or not obstacles exist are preferably considered as described above. Further, the user can previously set any one of WiHD and the WHDi to a wireless communication scheme of the transmitting and receiving apparatuses 100 and 200 by considering the distance between the transmitting and receiving apparatuses 100 and 200 that are currently installed, the installation space, or the resolution of the transmitted image.
[0042] In the above description, the receiving apparatus 200 can support WiHD and WHDi, for example, and this is just one embodiment of the present invention. That is, the receiving apparatus 200 can support two or three or more wireless communication schemes among various wireless communication schemes. For example, as another embodiment of the present invention, the receiving apparatus 200 can support WiHD and WiFi by including the WiHD media access control (MAC) layer and the WiFi media access control (MAC) layer.
[0043] In addition, WiFi is slower at approximately 54 Mbps, but the transmission/reception distance is longer (e.g., approximately 50 to 200 m) and the transmission/reception quality is not significantly influenced by the adjacent obstacles of the installation space such that when the distance between the transmitting apparatus 100 and the receiving apparatus 200 is long such as 10 m or more or obstacles exist between the transmitting apparatus 100 and the receiving apparatus 200 as described above, the control unit 212 of the receiving apparatus 200 selects the signal transmitted via WiFi among the received signals.
[0044] Hereinafter, embodiments of a method for receiving a signal in the receiving apparatus 200 according to the present invention will be described in more detail with reference to FIGS. 4 and 5 . In particular, FIG. 4 is a flowchart illustrating a method for receiving a signal according to a first embodiment of the present invention. FIG. 3 will also be referred to throughout the description of the present invention.
[0045] Referring to FIG. 4 , the RF receiving unit 220 receives the first and second signals transmitted from the transmitting apparatus 100 in different wireless communication schemes (step 300 ). As one embodiment of the present invention, the transmitting apparatus 100 can transmit the first signal using WiHD, and transmit the second signal using WHDi. Meanwhile, the first and second signals include the same video and audio depending on the media signal which the transmitting apparatus 100 receives and are signals converted in a wirelessly transmittable format in accordance with different wireless communication schemes.
[0046] Further, the received first and second signals may be the media signal including the video and the audio or a pilot which is a signal for measuring the reception sensitivity. The control unit 212 also measures the signal reception sensitivity of each of the received first and second signals (step 310 ). For example, the control unit 212 can measure a received signal strength indicator (RSSI) and a packet error rate (PER) of each of the first and second signals. Thereafter, the control unit 212 determines a signal having the higher reception sensitivity of the first and second signals by using the measured signal reception sensitivity (step 320 ).
[0047] For example, a signal having the high received signal strength indicator (RSSI) of the first and second signals may be a signal having the high reception sensitivity, and a signal having the low packet error rate (PER) of the first and second signals may be a signal having the high reception sensitivity. When the first signal of the first and second signals has the higher reception sensitivity, the control unit 212 acquires the first signal from the media access control (MAC) layer 213 (step 330 ). Also, the received first signal is provided to the corresponding application and the application is executed such that the first signal is processed (step 340 ).
[0048] For example, when the first signal is the signal transmitted via WiHD, the control unit 212 can receive and output the signal of the WiHD media access control (MAC) layer to the signal processing unit 211 , and the signal processing unit 211 can process the signal by executing a WiHD application to process the signal. Meanwhile, when the second signal of the first and second signals has the higher reception sensitivity, the control unit 212 acquires the second signal from the media access control (MAC) layer 213 (step 350 ). The received second signal is then provided to the corresponding application and the application is executed such that the second signal is processed (step 360 ). For example, when the second signal is the signal transmitted via WHDi, the control unit 212 can receive and output the signal of the WHDi media access control (MAC) layer to the signal processing unit 211 and the signal processing unit 211 can process the signal by executing a WHDi application to process the signal.
[0049] Next, FIG. 5 is a flowchart illustrating a method for receiving a signal according to a second embodiment of the present invention. Referring to FIG. 5 , a wireless communication scheme to receive the media signal is first input from the user, that is, a wireless communication scheme for transmitting/receiving the data between the transmitting apparatus 100 and the receiving apparatus 200 (step 400 ). To perform this operation as discussed above, the transmitting apparatus 100 or the receiving apparatus 200 includes a user input unit. The RF receiving unit 220 then receives the first and second signals transmitted from the transmitting apparatus 100 in first and second schemes which are different wireless communication schemes (step 410 ). For example, the first and second schemes may be WiHD and WHDi, respectively.
[0050] The control unit 212 then verifies the wireless communication scheme input from the user at step 400 (step 420 ). When the wireless communication scheme input from the user is the first scheme, the control unit 212 acquires the first signal transmitted in the first scheme of the first and second signals from the media access control (MAC) layer 213 (step 430 ). The received first signal is also provided to the corresponding application and the application is executed such that the first signal is processed (step 440 ). For example, when the first scheme input by the user is WiHD, the control unit 212 can receive and output the signal of the WiHD media access control (MAC) layer to the signal processing unit 211 , and the signal processing unit 211 can process the signal by executing a WiHD application to process the signal.
[0051] In addition, when the wireless communication scheme input from the user is the second scheme, the control unit 212 acquires the second signal transmitted in the second scheme of the first and second signals from the media access control (MAC) layer 213 (step 450 ). The received second signal is then provided to the corresponding application and the application is executed such that the second signal is processed (step 460 ). For example, when the second scheme input by the user is WHDi, the control unit 212 can receive and output the signal of the WHDi media access control (MAC) layer to the signal processing unit 211 , and the signal processing unit 211 can process the signal by executing a WHDi application to process the signal.
[0052] Next, FIG. 6 is a flowchart illustrating a method for receiving a signal according to a third embodiment of the present invention. Referring to FIG. 6 , the RF receiving unit 220 receives the first signal transmitted from the transmitting apparatus 100 in the first wireless communication scheme (step 500 ). For example, the first wireless communication scheme may be WiHD, and therefore the RF receiving unit 220 can receive the first signal depending on the WiHD from the transmitting apparatus 100 . The control unit 212 also measures the signal reception sensitivity of the received first signal (step 510 ). For example, the control unit 212 can measure a received signal strength indicator (RSSI) and a packet error rate (PER) of the first signal.
[0053] Thereafter, the control unit 212 verifies whether the measured reception sensitivity of the first signal is equal to or more than a predetermined reference value “a” (step 520 ). For example, the control unit 212 can verify whether the received signal strength indicator (RSSI) of the first signal is equal to or more than a predetermined reference strength or the packet error rate (PER) of the first signal is equal to or more than a reference error rate. According to the comparison result, when the reception sensitivity of the first signal is equal to or more than the reference value “a”, the control unit 212 can control the RF receiving unit 220 by continuously receiving the first signal transmitted in the first wireless communication scheme.
[0054] In addition, when the reception sensitivity of the first signal is less than the reference value “a” (No in step 520 ), the control unit 212 switches the wireless communication scheme into the second wireless communication scheme (step 530 ) such that the RF receiving unit 220 receives the second signal from the transmitting apparatus 100 in accordance with the second wireless communication scheme (step 540 ). For example, the second wireless communication scheme may be WHDi. In this instance, information on the second wireless communication scheme which is the switched wireless communication scheme may be transmitted to the transmitting apparatus 100 such that the transmitting apparatus 100 can transmit the second signal to the receiving apparatus 200 in accordance with the switched second wireless communication scheme.
[0055] In addition, the control unit 212 can control the information on the switched second wireless communication scheme to be displayed on the screen to be transmitted to the user, while the information on the second wireless communication scheme may be displayed by using a display unit provided in the receiving apparatus 200 or an external display apparatus. For example, when the wireless communication scheme is switched from WiHD into WHDi in accordance with the method for receiving the signal, a warning message indicating that the resolution of the image may decrease can be displayed to the user.
[0056] Further, the user can select whether or not the wireless communication scheme is to be switched into the WHDi, and when the user does not want to switch the wireless communication scheme into WHDi, the receiving apparatus 200 continuously receives and processes the first signal transmitted via WiHD. The received second signal is then provided to the application corresponding to the second wireless communication scheme, and the received second signal is processed in accordance with the second wireless communication scheme corresponding to the second signal as the application is executed.
[0057] Also, as discussed above, the receiving apparatus 200 can detect or measure a distance between the receiving apparatus 200 and the transmitting apparatus 100 , detect whether there are obstacles blocking or interfering with the communication, and then use this information in selecting the best wireless communication standard to use. Similarly, the transmitting apparatus 100 can measure the distance from the receiving apparatus 100 , whether obstacles exist therebetween, etc.
[0058] Next, FIG. 7 is a block diagram illustrating another signal transmitting/receiving system according to another embodiment of the present invention. As shown, the transmitting/receiving system includes the transmitting apparatus 100 and a plurality of receiving apparatuses 200 , 210 , and 220 . Further, the transmitting apparatus 100 may be connected with the plurality of receiving apparatuses 200 , 210 , and 220 through a wireless network. That is, the transmitting apparatus 100 converts the media signal received from the outside into wirelessly transmittable data, and thereafter wirelessly transmits the data to at least one of the plurality of receiving apparatuses 200 , 210 , and 220 .
[0059] For example, the transmitting apparatus 100 may select one or more receiving apparatuses that will receive the media signal among the plurality of receiving apparatuses 200 , 210 , and 220 from the user and wirelessly transmit the media signal received from the outside to the receiving apparatus selected by the user. To perform this operation, the transmitting apparatus 100 includes a plurality of wireless transmitting units corresponding to the plurality of receiving apparatuses 200 , 210 , and 220 configured to wirelessly transmit the video and audio data to the receiving apparatuses corresponding thereto.
[0060] Further, the wireless communication standards for data transmission/reception may be the same as or different from each other in the plurality of receiving apparatuses 200 , 210 , and 220 . For example, in accordance with the performance or installation position of each of the plurality of receiving apparatuses 200 , 210 , and 220 , the wireless communication standards for the plurality of receiving apparatuses 200 , 210 , and 220 to receive data may be established to be different from each other. In addition, the transmitting apparatus 100 may include a number smaller than the number of the plurality of receiving apparatuses 200 , 210 , and 220 , for example, one wireless transmitting unit and in this instance, the transmitting apparatus 100 can wirelessly transmit the data using a plurality of channels corresponding to the plurality of receiving apparatuses 200 , 210 , and 220 , that is, using multi-channel communication.
[0061] Next, FIG. 8 is a block diagram illustrating a signal transmitting/receiving system according to yet another embodiment of the present invention. As shown in FIG. 8 , a display device 600 includes the receiving apparatus 200 having the above-mentioned configuration and a display module 610 . That is, the transmitting apparatus 100 receives the media signal from the outside and wirelessly transmits the received media signal to the receiving apparatus 200 , and the receiving apparatus 200 provided in the display apparatus 600 processes the wirelessly transmitted data into a video signal of a displayable format and outputs the processed data to the display module 610 .
[0062] And, the receiving apparatus 200 is detachable to the display device 600 .
[0063] In addition, the display module 610 may display a video using the video signal input from the receiving apparatus 200 . To perform this operation, the display module 610 may include display panels of various display types such as a liquid crystal display (LCD), a plasma display panel (PDP), an electro luminescent display (ELD), a vacuum fluorescent display (VFD), etc. Also, the receiving apparatus 200 can automatically select the best wireless communication method for the particular scenario involved. Thus, the signals can be switched without user intervention.
[0064] Further, in another embodiment, the user can set the predetermined reference value “a” in FIG. 6 . For example, the receiving apparatus 200 (or a remote control associated with the receiving apparatus 200 ) can include a dial that the user can rotate to change the value. This is particularly advantageous, because the user can set the reference value based on how many people are in the room, for example, which may affect the reception of the signal. For example, during a sporting event, the user may have many guests, so the user can adjust the sensitivity in real time to provide the best reception method. In addition, the receiving device 200 can be a television connected to the transmitting device 100 .
[0065] Further, the signal receiving method according to embodiments of the present invention may be stored in a computer-readable recording medium by being produced as a program to be executed in a computer. An example of the computer-readable recording medium includes a ROM, a RAM, a CD-ROM, a magnetic tape, a floppy disk, an optical data storage, etc. and in addition also includes Internet transmissions. In addition, the computer-readable recording media are distributed on computer systems connected through a network, and thus a computer-readable code may be stored and executed by a distribution scheme. Also, a functional program, a code, and code segments for implementing the signal receiving method will be easily interred by programmers skilled in the art.
[0066] According to embodiments of the present invention, a transmitting apparatus and a receiving apparatus that transmits and receives video and audio signals using wireless communication, respectively can provide the optimum signal transmission/reception performance depending on a distance between the transmitting and receiving apparatuses, an installation space, or the resolution of an image by supporting a plurality of wireless communication schemes, thereby improving the quality of a displayed image.
[0067] The present invention encompasses various modifications to each of the examples and embodiments discussed herein. According to the invention, one or more features described above in one embodiment or example can be equally applied to another embodiment or example described above. The features of one or more embodiments or examples described above can be combined into each of the embodiments or examples described above. Any full or partial combination of one or more embodiment or examples of the invention is also part of the invention.
[0068] As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, unless otherwise specified, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the metes and bounds of the claims, or equivalence of such metes and bounds are therefore intended to be embraced by the appended claims. | A method of controlling devices, and which includes converting, via a transmitting apparatus, a signal including at least one of the video/audio and data into a first definition wireless signal, transmitting, via the transmitting apparatus, the converted first definition wireless signal to a receiving apparatus, receiving, via the receiving apparatus, the first definition wireless signal, extracting, via the receiving apparatus, the at least one of the video/audio and data included in the first definition wireless signal, detecting, via a detector on the receiving apparatus, a quality of the received first definition wireless signal, and comparing, via a processor on the receiving apparatus, the detected quality of the received first definition wireless signal with a predetermined value, and transmitting a first command to the transmitting apparatus to transmit a second definition wireless signal including the at least one of the video/audio and data to the receiving apparatus, when the detected quality of the received first definition wireless signal is lower than the predetermined value, the first and second definition wireless signals using different wireless communication standards. | 7 |
BACKGROUND OF THE INVENTION
The invention relates generally to tools and systems for measuring the performance of mass storage systems, and more particularly, to methods and apparatus for developing, measuring, analyzing, and displaying the performance statistics of a plurality of disk drive elements controlled through a disk drive controller connected to a plurality of host computers.
As the size and complexity of computer systems increase, including the number of host computers and the number of disk drive elements, it becomes increasingly important to measure and understand the functions and parameters which affect the performance of the system. The performance of the system can be typically measured in terms of input/output (I/O) response times, that is, the time it takes for a read or write command to be acted upon, as far as the host computer is concerned, by the disk drive controller system.
It is well known, in the field, to measure, usually using a single parameter, the instantaneous or average response time of the system. Typically, a host computer outputs one or more I/O requests to the disk drive controller, and then measures the time for a response to be received from the disk drive controller. This time duration, while representative of the response of a specific read or write command to the disk drive system, is most often not representative of the actual performance which can be obtained from the system.
A similar distortion, not representative of system performance, can occur when average response time values are determined. For example, a disk controller, using a cache memory in its write process, can have substantially different write time responses depending upon the availability of cache memory. An average response (the average of, for example, a write where cache was available and one where cache was not available) would be misleading and meaningless.
The performance of a large storage system is particularly difficult to measure since more than one of the host computers, which connect to be disk drive controller(s), can operate at the same time, in a serial or in a parallel fashion. As a result, a plurality of disk drive elements, usually arranged in a disk drive array, operating in either an independent fashion, a RAID configuration, or a mirrored configuration, for example, can have a significant yet undetectable bandwidth or operational problem which cannot be addressed, or discovered, when commands are sent only from a single host computer.
In U.S. Pat. No. 5,953,689, issued Sep. 14, 1999, assigned to the assignee of this application, an improved method of time synchronizing a plurality of hosts operating in a variety of different configurations, and of issuing commands according to a prescribed sequence, was described. The method described in the above-identified patent features sending test requests, for the mass storage system, from a “main” host computer to each of a plurality of client host computers, executing at each host computer a test request sequence by sending commands to the mass storage system, accumulating at each host computer data regarding performance of the mass storage system, the data being in response to the requests or commands sent by each particular host computer, and sending, from each host computer to a master host computer, data regarding the performance of the mass storage system in response to the host generated commands. Significant data reduction techniques control and organize the data for later analysis.
While this system worked well, it had, at the time the application for the system was filed, specific limitations with regard to creating the test configurations and with regard to the flexibility of the analysis and processing once the statistics had been collected.
SUMMARY OF THE INVENTION
The invention relates to an improved method for measuring the system performance of a mass storage system having a plurality of disk drive storage elements controlled by a disk drive controller. Typically the disk drive controller has a cache memory. The controller receives commands and data from, and returns at least data to, typically, a plurality of host computers.
The method relates to presenting system performance to a user in a mass storage system. The storage system has a plurality of disk drive storage elements controlled by a disk drive controller, and the controller receives commands and data from and returns at least data to a plurality of host computers. The method features executing, at at least one host computer, a test request by sending commands to the mass storage system; accumulating, at at least the executing host computer, data regarding performance of the mass storage system in response to the requests sent by the host computer, and presenting the accumulated data in a graphical plot format, for enabling the visualization of trends in the performance of the mass storage system as a function of at least one selected parameter, in response to the host generated commands.
In particular aspects of the invention, the selected parameter is time; the accumulating step accumulates the data in a plurality of databases; and the method further features selecting one of the databases for test and viewing.
In yet other aspects of the invention, the method features the presenting step in which it either prints and/or displays on a cathode ray tube the data in the graphical plot format. Further, the method features selecting at least one test phase for viewing in the graphical plot format, as selected by the user. The method can also display, in association with the graphical plot format, parameters relating to the graph. The parameters can include one or more of, for example, the nature of the test, the size of data blocks which have been used, and the number of data ports.
Advantageously, therefore, the system easily, and in large part automatically, develops, measures, generates and analyzes statistics describing the dynamic performance of the mass storage system, from the host computers to the disk drive elements, wherein individual operations as well as sequences of operations can easily be set up, with selected initial conditions, and accurately and automatically tested according to desired criteria using graphical user interfaces. The method and apparatus of the invention further advantageously enable the user to easily configure, set, and determine read/write sequencing and a relative mix of read and write commands, as well as enabling the dynamic performance of the system to be repeatedly enabled and tested for consistency, accuracy, and effectiveness.
DESCRIPTION OF DRAWINGS
Other features and advantages of the invention will be apparent from the following description, taken together with the drawings, in which:
FIG. 1 shows a typical system in which the invention is useful;
FIG. 2 shows, in more detail, a particular controller system in which the invention finds particular use;
FIG. 3 is a flow chart showing overall operation of the setup/analysis portion of the 30 system;
FIG. 4 is a map to the table represented by FIG. 4A and FIG. 4B .
FIG. 4A is the first part of a table used to show the arguments used in the testing.
FIG. 4B is the second part of a table used to show the arguments used in the testing.
FIG. 5 shows a more detailed flow chart in accordance with the operation of the system;
FIG. 6 shows the operational subsystems of the system;
FIG. 7 shows data reduction sequential flow;
FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , 8 C 1 – 8 C 4 , 8 D 1 – 8 D 4 show examples of trends data presentation;
FIG. 9 shows screen shots of the graphical user interface of the system for post test data processing;
FIGS. 9A–9O show screen shots of the graphical user interface system;
FIG. 10 shows a flow chart illustrating post processing;
FIGS. 10A–10B show screen shots of the post processing presentation;
FIG. 11 is a map to the table represented by FIG. 11A and FIG. 11B .
FIGS. 11A and 11B are two parts of a single table that illustrate various system database files; and
FIG. 12 shows a screen shot of the trends analysis presentation.
DETAILED DESCRIPTION
Referring to FIG. 1 , the invention relates to a computer system wherein a plurality of host computers or processors 12 a , 12 b , . . . , 12 n , connect to a storage controller system 14 , such as the EMC Symmetrix® storage system. The controller acts as an intelligent interface between the host computers and a plurality of mass storage devices, such as, for example, disk drive elements 16 a , 16 b , . . . , 16 k . Data written by the host or read from the disk drive elements passes through the memory controller system which acts as a two way communications path with substantial capabilities. The disk drive elements can have any of, or a combination of, a plurality of configurations. For example, in some systems, the data from a host is uniformly striped across all of the disk storage devices; and in other systems, the data from a host is stored on the disk drives 16 according to a RAID protocol or an n-way mirrored protocol. In yet other embodiments of the invention, all of the data from a particular host may be stored in a logical volume on a single disk drive or allocated to different logical volumes of the same or different disk drives, depending upon the nature and the source of the data and host. A host computer can also read data from one or more of the disk drive units to generate a single host logical volume.
To determine the limits of performance in the system, the hosts can, according to the invention, be operated to exercise and test the memory controller and the disk drive elements. Thus potential problems which can create a bottleneck on those communication lines connected from the disk drive controller to either the disk drive elements or the hosts can be identified, as can cache memory loading issues in the drive controller.
Referring to FIG. 2 , in a particular embodiment according to the invention, the disk controller has a plurality of host adaptors (also referred to as channel directors, FA's or SA's) 30 connecting to a global memory 32 through which, in this embodiment, all data and commands flow. The global memory 32 is connected to a plurality of disk adaptors (also referred to as DA's or disk directors) 34 which connect the disk drives 16 to storage 32 through drive ports 35 of the adaptors 34 over lines 39 . In accordance with this particular embodiment of the invention, each host adaptor has a SCSI adaptor embedded therein which communicates with the global memory 32 . In the illustrated embodiment, the read and write operations pass through each SCSI adaptor unit 34 and to the disk adaptors to the disk drive elements. Each host adaptor connects to one or more host computers over buses 36 at host processor ports 37 of the host adaptors. The host processors also can communicate with each other, for example over an Ethernet based bus 50 ( FIG. 1 ).
Referring now to FIG. 3 , in general operation, a series of arguments or parameters describing the tests or test to be performed within the mass storage system is entered into a master host processor (step 60 ). The parameters, represented by the data entered into the master host processor, will define and effectively control the operations by which the hosts gather statistics describing performance of the mass storage system. The arguments or parameter data are entered into a main control program (step 62 ). Once the parameters are set in the main control program, operation transfers to a main driver program, running on the master host computer. The driver program controls operation not only of the master host computer, but of all of the other (client) host computers as well.
The driver program effects time synchronization of the host computers and causes the next lower level controller programs (the programs which control the commands and data sent to and received from the disk controller), to operate in time synchronization (step 64 ). In order to achieve both time synchronization of the host computers, and accurate and timely operation of the mass storage system, the driver program may first cause each of the client host computers to synchronize its clock with the master host computer. Further, in response to a communication from the master computer, all host computers begin to issue commands to the controller of the mass storage system, based upon the arguments or parameters previously stored in their memories.
After the necessary test-defining parameters are stored in the memory of each respective host computer, the test is ready to proceed. The next lower level controller program in each of the host computers, designated the scripting program, causes each of the host computers to command the controller in accordance with the command information provided to it by the master host computer driver program (step 66 ). (Note that the master host computer itself also “receives” such information from the driver program.)
Depending upon the particular disk controller system, one of two possible methods of operation can proceed. If the controller is a “simple” controller, each host computer will itself measure and collect statistics (the raw data) identifying, for example, the response time for each command which it sends to the controller. These response times are collected in a manner which allows the host computer to identify to which command the response time corresponds. Alternatively, for a controller such as the EMC Symmetrix® controller, the controller itself can provide or supplement the raw data for each of the commands which it receives from the hosts. Under this latter circumstance, the controller will return not only the data requested by the command, but in addition, in response to special host requests, the statistics describing the response times for the commands which are being received. That information is provided to the particular host which requested the operation.
Each host computer, then, analyzes the response time data which it either has received or generated itself (step 68 ). In the illustrated embodiment of the invention, this raw data, which can amount to several gigabytes of information, is analyzed preferably, at each host computer. The analysis is basically a data reduction analysis whereby each host computer, rather than maintaining the full raw data set, operates to reduce the received response times to a smaller set of data. In a first particular embodiment, the data is placed into “buckets”, each bucket representing, for example, 0.25 seconds. (In other embodiments, differently sized buckets can be employed). The buckets, however, collectively represent a non-overlapping, continuous sequence of time durations.
In another embodiment of the invention, the response times can be accumulated for a period of time, so that the data returned to the master host computer will represent the cumulative response times for all commands issued during each of a plurality of non-overlapping contiguous larger durations of time, for example 5 or 10 seconds. That is, for each of the contiguous time periods, the response times for each command initiated in the period will be accumulated. This is particularly useful where the tests can run for several hours and in which tens of gigabytes of data will be produced for each of the host computers.
No matter what method is used to collect and/or reduce the data, the master host computer collects the resulting data from each other host computer (step 70 ). The master host computer, at the driver program level, then can further analyze the reduced data, as described below, to obtain and present statistics to the user (step 72 ). These additional statistics can provide further insight and understanding into the performance and operation of portions of or the entire of computer/memory system.
Referring now to the operation of the computer system in more detail, and referring to FIGS. 4A and 4B , at the main program level, in the master host computer, a number of parameters or arguments are entered and recorded using a graphic user interface. These are illustrated in the table of FIGS. 4A and 4B . Turning to the table, the initial parameters include the number of logical disks to be tested, the number of “child” processes to start (as that term is used in the Unix operating system), the number of processes that capture response times, the number of response times to collect, the buffer size requested, and the offset size, in bytes, rounded down from a randomly generated number (this supports seeks on random reads and writes to even boundaries of stripes). Other required arguments include the maximum range in megabytes to span the device, the time in seconds to effect read or write operations or the amount of data in actual bytes to read and write, and the percent of operations which will be read operations (with the remainder being write operations). Other optional arguments, in the illustrated embodiment, include identification of the devices to test, identification of which host will be the master host computer and whether the I/O operations will be sequential or random. Other optional arguments include the number of sequential I/O operations to perform, once the system has “seeked” to the correct offset for a random operation, and the displacement in bytes back from that particular offset. In this particular embodiment of the invention, there are the yet further optional arguments which include the amount of time to delay between I/O commands, the initial byte offset to start sequential read or write commands, the method in which response start times will be collected (for example the use of buckets), a parameter identifying a percent hit rate to be implemented in connection with Integrated Cache Disk Arrays (ICDA's), including Intelligent Storage. Systems, with controller cache to read or write a specific number of megabytes of data, and a random range multiplier (for devices larger than the scope of the random number generator).
Referring now to FIG. 5 , the operation of the system, in accordance with the invention, can be viewed as a series of nested loops, the outer most loop being the main program, the next loop being the driver program, and the inner loop being the scripting 10 program. In the outer loop, the system receives the arguments or parameters which control or set up the operation of the test program. Those parameters or arguments have been described above in connection with the table of FIGS. 4A and 4B . Referring to FIG. 5 , the main program receives (at step 100 ) and enters (at step 102 ) the various arguments in its data files. In a preferred embodiment of the invention, each test is performed typically three times (tested at step 104 ) to ensure a statistical averaging which creates both confidence and accuracy, thereby avoiding variability and statistical anomalies. A test may also be performed once for verification purposes (and with less data).
Once the arguments have been stored in the data files on that host computer, which is designated as the master computer, the main program invokes the driver program, running on the master computer, to set up all of the hosts. This is indicated at step 106 . The driver program, in response to the arguments provided, will initialize the cache memory, if necessary, and will initialize as well, all of the host computers, including the master host computer. The driver program, at 108 , causes all of the host computers to be time synchronized. (If time synchronized, it may perform this function by sending to each of the client host computers over channel 50 , the clock time of the master host computer.) Each client host computer now runs the scripting program in response to initialization by the driver program and communications from that program over communications channel 50 , linking all of the host computers. (Thus all of the client host computer clocks may then be set in some embodiments of the invention, with the result that all of the host computers participating in the test are operating with time synchronized clocks.)
The driver program then transfers to each of the client host computers the necessary configuration and parameter files with which the scripting program, at the client host computers and at the master host computer, will operate to test the mass storage system. This is indicated at step 110 .
Next, the driver program initiates testing of the mass storage system by communicating to each host computer, directly from the master host computer and over the interconnecting communications channel 50 . As a result, each host computer begins sending commands and data to and receives at least data from the mass storage system at the same time. At this point, it is the configuration and parameter input to the master host computer, as delivered to the client computers, which controls the actions of each of the client host computers. Thus, the provided information and arguments can cause, for example, only a subset of the host computers to communicate and issue commands to the mass storage system, and/or only a specific set of logical units at the mass storage level may be exercised in a specific configuration dictated by the arguments input at step 100 .
The scripting program, when a test is complete, as tested at 114 , then reduces the data which it has collected (step 116 ). As noted above, the data reduction process, if one is used, can use either a bucket compression or an accumulation compression approach. (The approach can be dynamically changed during the test sequence by, for example, a user command to the master host computer.) Alternatively, the initial raw data may be maintained in its original form. The raw data can include, for example, the response times to read and/or write operations, which have been commanded in accordance with the input parameters. (In accordance with the invention, when there is a mix of read and write commands, the system first issues a block of one set of the commands and then a block of the other set of commands. For example, when there are to be 40% read commands, the system can issue three write commands, followed by two read commands, followed by three write commands, etc. In this manner, the associated statistical data which is collected can be directly correlated to a particular read or write command.)
Once the data is in its final (and most likely, reduced) form at the client host computers, it is transferred over channel 50 to the master host computer. This is indicated at step 118 . Thereafter the master host computer can effect a more comprehensive data analysis, at step 120 , to determine the performance of the mass storage system, for example, the number of I/O's, and in particular, the number of writes, as a function of time. The driver program then determines whether another test is to be performed, at step 104 , and if not, the driver checks to determine whether further analysis of the data is to be performed (at step 122 ). If further analysis data is to be collected using a new configuration, the new configuration is generated at step 124 , and the process begins again starting with step 110 . If no further analysis data is needed, the system returns to the beginning of the process as indicated by loop 126 . In this manner, the three nested loops of this preferred particular embodiment, loops represented by the main program, the driver program, and the scripting program, can provide effective and dynamic testing of the storage system to determine its performance under a large variety of situations.
Referring to FIG. 6 , in accordance with the operation of the system, there are provided, generally, six operational subsystems. These are designated administrative 200 , data transfer 210 , processing of raw data 220 , post processing of raw data 230 , reporting 240 , and database and trend analysis 250 . These elements of operation are initiated, by the user, in a sequential manner as noted in FIG. 7 , after the system for collecting the raw data (on the disk controller) is initiated at 260 .
The data reduction workbench system of the invention begins with a “project tab” which creates or opens a directory structure to allow for management of the project data. This function organizes the data reduction workbench and allows creation and management of new, or the opening of existing, projects and test phases, and further insures consistent naming of all of the components within a project. It also logs all operations performed at both a project and a test phase level. At the test phase level, the system creates or opens the folders for a particular test phase which will hold all of the test data and informational data regarding that particular test. Each test is identified, at 290 , and the organization process to effect data transfer begins. Next, in the data transfer phase, at 300 , a file transfer protocol is incorporated for transferring the data from the test environment (either the host computers or the disk controller system, such as the EMC Symmetrix® controller system). This mechanism provides the directory structure of all test data and information data for the particular test (benchmark) which has been run.
Once the data has been transferred and is ready to be processed, the system processes the raw data, at 310 , by reading the test files and creating summaries and error files for the test. The processing of raw data further creates statistical analysis program files, for example, for further processing and a cache ratio report to ensure that the actual cache ratio is within an acceptable margin of the targeted cache ratio for the characterization workload test. The data is also checked for errors at this stage and those errors are reported, and in some instances, corrected. The coalesced data is then formatted for input to the post processing stage at 320 . The coalesced data results from processing the raw data, by automatically processing characterization and database simulation benchmark data, as well as controller generated internal data, and coalescing, according to the test, test iteration, and test configuration, the data collected by each host operating in the test. The coalesced data is thus provided in a single data file for the following post processing.
The post processing phase 320 provides an interface to the statistical analysis data processing program, and to other analysis tools such as the Write Analysis Tool described in U.S. application Ser. No. 09/542,463 entitled BENCHMARK TOOL WRITE ANAYSIS FOR A MASS STORAGE SYSTEM, and filed Apr. 4, 2000, and incorporated herein in its entirety by reference, and allows for plot generation, data summarization, and the importing of the test and information data for a particular test, using a graphical user interface. As a result, formal plot presentations can be automatically loaded into an electronic document, for presentation in a standardized format.
Once post processing has been completed, the system provides interfaces to other presentation formats to generate spreadsheets from the statistical analysis program summary files created during post processing to enable charts and tables to be created in, for example, a standardized word processing report. This enables the development of performance reports. This is indicated at 330 . In addition to the reports, this system also automatically loads the benchmark statistical analysis summary data into a database (at 340 ). With the data thus available, a trend analysis can be created and displayed according to the test types and system configurations. This is indicated at 350 . This enables the comparison of performance behaviors across multiple projects (that is, as a function of time) and test phases (for example as a result of different operating software for the same configuration of equipment) in order to determine visually, at first impression, trends which may affect the analysis of system performance.
Post Processing
Once the data is collected, according to the invention, the system organizes, validates, checks, and presents the data as noted below. In the raw data post processing and correction stage, the validity checks can include checking individual data points for errors and applying predetermined decision criteria to either correct, ignore, or delete erroneous data. In addition, an overall validity comparison of the actual (and corrected) results with expected results based on the I/O configuration profile can be effected. The user of pre-established criteria to decide whether to correct, ignore or use the erroneous data is implemented in accordance with one embodiment of the invention by flagging any inconsistencies based on expected results of a particular input/output type and storing such flagged data in a system data files. Once the corrections have been effected, the revised data can be put into any of a number of industry standard templates.
Referring to FIG. 9 , a post processing “tab” enables the user to first start a statistical analysis program by clicking on button 900 . The user can then bring up the statistical analysis program window to watch, on screen, for errors and to use it during any update-objects-routine which may follow. The user then selects the number of graphs per page as indicated at 902 (in FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , . . . one graph per page has been selected) and thereafter can select processing of the data as described above.
Accordingly, during the post processing phase of operation, in a preferred embodiment of the invention, referring to FIGS. 9 , 10 A, and 10 B, the system first checks individual data points against predetermined criteria to determine if any errors have occurred. Any error data are then, in accordance with the settings by a user in the graphical user interface, either corrected, ignored, or deleted. This is indicated at 1002 . The results are then compared with the expected results for this particular I/O configuration profile. This is indicated at 1004 . Any deviations from standard expectations are flagged at 1006 . The results then are placed into a data files in a format for later presentation and operation.
The various data files are summarized in FIG. 11 . These data files are typically statistical analysis program related files and can be used to create database simulation objects as well as being placed into the correct report format as noted above.
Trends Analysis
The trend analysis referred to above, taking place as indicated at 350 , provides a series of graphs, such as those illustrated in FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , 8 C 1 – 8 C 4 , 8 D 1 – 8 D 4 . These graphs provide a display of the collected data in a format easily viewable by the user so as to enable the user to understand and recognize trends in the data as a function of changes in one or more parameters. Thus, changes which result over time can be plotted to clearly enable the user to see and analyze, for example, the number of I/O's per second as a result of changes in the parameter, or the number of megabits per second throughput by the controller. The illustrative presentations of FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , . . . enable such presentations to be made effectively, and preferably in color.
Referring more particularly to FIG. 12 , which is a screen shot useful in connection with the trends analysis, a user can browse the available databases by selecting the “Select DB” button 1200 and selecting a database of interest. Thereafter, the system will load the database information into the form ( FIG. 12 ) creating a selection tree 1202 on the left side, as shown, and all of the default test types and configurations will be provided in the drop down boxes.
If the chart selection was “on-line”, the analysis generates the chart on the display screen. The chart can also, as an alternative, for example, be placed in a word processing document by selecting “test type” or “view all”, for example, at the chart selection 1204 .
The user selects the test phases which are to be graphed together. By default, the project and one test phase will be selected, however, all test phases for a project can be selected by clicking, for example, on the project. Alternatively, specific desired test phases can be selected (or deselected) as needed. As noted above, the graphs can be generated and viewed online, or printed, and can be shown according to test type or types as required. The system also, by pressing the “scale” selection 1206 , will calculate the minimum and maximum values for the data and use those values to scale the graph. A percent scale is also available where the largest value of the chart is considered at 100% and all of the values are displayed accordingly.
The various specific information is shown in the characterization frame 1208 and is selected by the user and viewed as a chart online or report.
During the input process, the user selects, using the graphical user interface, the parameters which enable the graphs of FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , . . . to be generated. The data corresponding to the graphs have been previously created in the database of the system. When the graphs are presented, as illustrated in FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , . . . , the presentation identifies the parameters relating to the graph including the ports of the controller which have been used, the nature of the tests, such as a random delayed fast write, the size of the blocks which have been used, and other test parameters as indicated in the FIGS. 8 A 1 – 8 A 4 , 8 B 1 – 8 B 4 , 8 C 1 – 8 C 4 , 8 D 1 – 8 D 4 . By plotting this information in a graphical format, the user is enabled to spot trends in the data as a result of changes over time, or other parameters. This data is also available for viewing on screen.
By plotting this information in a graphical format, the user is enabled to spot trends in the data as a result of changes over time, or other parameters. This data is also available for viewing on screen.
Graphical User Interface
The system provides for a graphical user interface which enables operational parameters of the system to be created quickly, with repeatability, reliability, and use by a much broader audience. The graphic user interface is essentially a front-end device for the invention which automatically operates to generate and/or work on three types of files: configuration rule data, workload data, and benchmark data. It allows the selection of various test types based upon the user inputs which are provided in a “point and click” manner. The graphic user interface of the invention is substantially more reliable for the user and enables the user to quickly and easily define the system tests which are to be performed.
The typical graphic user interface is presented, in accordance with the invention, in FIGS. 9A , 9 B, . . . In accordance with these Figures, and referring to the nomenclature either well known in the art or noted above in connection with various adaptor elements of a system, the various elements of the interface are indicated and described therein.
The user is thus enabled to form this presentation using the graphical user interface.
Additions, subtractions, and other modifications of the illustrated embodiment of the invention will be apparent to those practicing in this field and are within the scope of the following claims. | A method for measuring mass storage system performance in which the mass storage system has a plurality of disk drive storage elements controlled by a disk drive controller, the controller typically having a cache memory, and the controller receiving commands and data from and returning at least data to a plurality of host computers, provides the flexibility of issuing commands to the controller in a variety of different configurations from a plurality of hosts in a time synchronized and organized fashion. Some significant data reduction techniques control and organize the data for later analysis according to the invention. Effective presentation of collected data can be effected using a novel trends analysis presentation approach. | 6 |
This is a division of application Ser. No. 073,051 filed Sept. 6, 1979, now U.S. Pat. No. 4,247,710, which in turn is a divisional of U.S. Patent Application Ser. No. 875,966, filed Feb. 8, 1978, now U.S. Pat. No. 4,202,978 issued May 13, 1980.
DESCRIPTION OF THE INVENTION
The present invention relates to binary α,β-Adrenergic Blocking Agents of the formula ##STR7## wherein R 1 is selected from the group consisting of lower alkyl; R 8 is selected from the group consisting of --O--(CH 2 ) n --wherein n is 2 to 20, ##STR8## and ##STR9## and R 6 is selected from the group consisting of hydrogen or lower alkoxy, and ##STR10## wherein R 1 is selected from the group consisting of lower alkyl; R 8 is selected from the group consisting of --O--(CH 2 ) n -- wherein n is 2 to 20, ##STR11## and ##STR12## and R 6 is selected from the group consisting of hydrogen or lower alkoxy and the racemates thereof.
The presently disclosed and claimed compounds exhibit both α and β-adrenergic blocking activities which are essential to their use as antihypertensive agents. They provide competitive and reversible blockade of both α and β adrenoreceptors and have the unexpected property of being cardioselective, having low activity at one site (β 2 ) and good activity at the β 1 site. This selectivity has important consequences when selecting an antihypertensive agent. Further the compounds have exhibited anti-secretory, i.e. spasmolytic activity.
By the term "lower alkyl" is meant straight or branched chains of C 1 to C 10 length with branched chains of C 3 to C 4 as preferred, e.g., isopropyl or tertiary butyl.
By the term "lower alkoxy" is meant straight or branched chain saturated hydrocarbonoxy groups containing from 1 to 7 carbon atoms, preferably 1 to 4 carbon atoms such as methoxy, ethoxy, propoxy and the like.
The term "halo" or "halogen" refers to all four forms thereof, i.e., bromine, chlorine, fluorine or iodine with bromine and chlorine as preferred.
It should be noted that the racemates of the above compounds are also novel and exhibit activities similar to the preferred (S) isomers although not as quantitatively active. The racemates may also be resolved into the desired isomers when desired.
The following reaction schemes represent the methods of synthesis available to produce the novel end compounds of the present invention: ##STR13## wherein R 1 is lower alkyl,R 2 and R 3 are selected from the group consisting of hydrogen, mesyl, tosyl, brosyl or benzenesulfonyl and R 4 is selected from the group consisting of halo, mesyloxy or tosyloxy. ##STR14## wherein R 5 is halo. ##STR15## wherein R 1 and R 3 are as above, R 6 is hydrogen or lower alkoxy, n is 2 to 20 and X is halo. ##STR16## wherein R 1 and R 6 are as above and n is 2 to 20. ##STR17## wherein R 1 and R 6 are as above and n is 2 to 20. ##STR18## wherein R 1 and n are as above and R 7 is halo. ##STR19## wherein R 1 , R 6 and n are as above. ##STR20## wherein R 1 and R 6 are as above. ##STR21## wherein R 1 , R 6 and n are as above.
D-Mannitol→I
The compound of formula I which is a known compound is produced by utilizing an acid catalyzed ketal exchange reaction. The reaction is carried out utilizing a strong mineral acid, such as, sulfuric acid or p-toluenesulfonic acid or a cation exchange resin. The reaction is carried out at a temperature range of about 0° C. to 100° C. with room temperature as preferred. The time of the reaction to completion will vary from 1 to 16 hours depending on the reaction temperature selected.
I→II→V
The two step reaction to produce the compound of formula V is a known reaction, see, for example, J. Lecocq and C. E. Ballou, Biochemistry, 3, 976, (1964).
V→VI
The compound of formula VI is produced by reaction of the primary alcohol (V) with a lower alkyl or aryl sulfonyl halide in the presence of a tertiary amine base. Examples of lower alkyl or aryl sulfonyl halides which may be used are mesyl, tosyl, brosyl or benzylsulfonyl chlorides or bromides. Examples of tertiary amine bases include pyridine or trialkylamines, e.g. tri-n-butyl or triethylamines. An inert solvent may be utilized to facilitate the reaction such as methylene chloride or tetrahydrofuran or pyridine. The latter functions as both reactant and solvent. The reaction temperature may vary from about -25° C. to 15° C. with -10° C. to 15° C. as preferable and 0° C. to 15° C. as optimum. The reaction time may range from 30 minutes to 1 hour depending on the reaction temperature chosen.
VI→IV
The compound of formula IV is thereafter produced by displacement of the leaving group (the alkyl or arylsulfonyloxy group) using a primary amine such as a methyl, ethyl, isopropyl or tertiary butyl amine. The reaction can be performed with or without an inert solvent (benzene, lower alcohols or ethers may be employed). In the case of lower boiling amines, e.g. isopropylamine, the reaction should be run in a pressurized vessel. The reaction temperature may vary from room temperature to about 150° C. with approximately 100° C. as the preferred temperature.
I→II→III→IV
A multistep sequence may also be utilized to produce a compound of formula IV in which the intermediates II and III are not isolated. The compound of formula I is oxidized to II utilizing lead tetraacetate in an inert aromatic hydrocarbon solvent, such as, benzene, toluene or xylene. The reaction temperature should be kept at room temperature or below, e.g., 0° C. After one side product, Pb(0Ac) 2 , has been removed by filtration, the acetic acid which has been generated in the reaction is neutralized by the addition of an alkali metal (Na,K,etc.) carbonate or oxide, e.g., BaO.
The aldehyde (II) is thereafter reacted with a large excess of a primary amine, e.g. methyl, ethyl, isopropyl, etc. amine to form the imine (III). The reaction temperature should be at about 25° C. or less and a desiccant, e.g. K 2 CO 3 , should be used to remove any water formed and drive the reaction to completion.
Thereafter the imine (III) is hydrogenated to the secondary amine (IV) by the use of a catalyst such as noble metals (Platinum, Palladium, Ruthenium, etc.) on carbon or Raney Nickel/H 2 under pressure. This reaction may be carried out at 20° C.-50° C. with room temperature as preferred. The reaction may be run at 1 to 10 atmospheres depending on the catalyst chosen.
IV→VII
The amine (IV) is thereafter reacted with an alkyl or aryl sulfonyl halide such as a mesyl, tosyl, brosyl or benzylsulfonyl chloride or bromide in an inert aprotic solvent such as high boiling ethers, e.g., dioxane, tetrahydrofuran or methylene chloride in the presence of a tertiary amine base, e.g., triethyl or trimethylamine. The reaction is carried out at a temperature range of about -50° C. to 25° C. with about -10° C. to 5° C. as preferred.
VII→VIII
The compound of formula VII thereafter undergoes an acid catalyzed hydrolysis of the ketal protecting group. To effect this catalysis, strong mineral acids are utilized, e.g., HCl, H 2 SO 4 or p-toluenesulfonic acid or a strongly acidic ion exchange resin (H + form). The reaction solvent may be water and a miscible co-solvent, such as, a lower alcohol (methanol, ethanol, propanol, etc.) and ethers such as tetrahydrofuran or dioxane. The reaction temperature range is from about room temperature to 80° C. with about 60° C. to 80° C. as preferred. The reaction time may range from 1 hour to 2 days depending on the temperature selected.
VIII→IX
The diol of the formula VIII is thereafter reacted with an alkyl or aryl sulfonyl halide (as previously disclosed in step V→VI) in the presence of a tertiary amine base (also disclosed in V→VI) wherein the primary hydroxyl group is selectively converted into an alkyl or aryl sulfoxy group. As disclosed previously in step V→VI pyridine may serve as the base and solvent or other previously disclosed solvents may be utilized (V→VI). The reaction temperature ranges (depending on what sulfonyloxy group) is desired may vary from about -45° C. to -50° C. (mesyl) to -5° C. to 5° C. (tosyl). When R 4 of formula IX is to be halo the reaction will differ from above. The compound of formula VIII undergoes an acid catalyzed exchange reaction with a trialkylorthoacetate, e.g., trimethyl, triethyl, etc. to give the cyclic orthoacetate of the formula ##STR22## and alkanol. The alkanol is distilled from the reaction mixture as formed to facilitate reaction completion. No solvents are necessary for the reaction. The reaction temperature ranges from about 60° C. to 100° C. with 80° C. as preferred. The time of the reaction varies from 30 minutes to 1 hour depending on the reaction temperature. The cyclic orthoacetate is thereafter reacted with trimethylhalosilane in an inert, aprotic solvent, such as, methylene chloride, giving rise to the intermediate of the formula ##STR23## which on attack by the halide ion gives the haloacetate. As solvents for this step, inert aprotic solvents such as high boiling ethers and halogenated hydrocarbons, e.g., methylene chloride, are best. The reaction may be run from about room temperature to reflux temperature for about 30 minutes. A reaction temperature of 40° is preferred. Thereafter the haloacetate is reacted in an acid catalyzed hydrolysis. To carry out the reaction a solution of the substrate in a hydrolytic solvent such as alcohols, e.g., methanol, ethanol, propanol etc. or aqueous alcohol mixtures containing a catalytic amount of a mineral acid such as HCl, H 2 SO 4 or an acidic ion exchange resin are utilized. The reaction temperature may be varied from 0° C. to reflux temperature (solvent dependent) for 30 minutes to 16 hours. Room temperature is preferred.
I→II→V
This procedure is carried out as disclosed previously by a prior art method.
V→XI
The hydroxyl group of the compound of formula V is protected as its benzyl ether by producing the compound of the formula XI. The reaction is one of the alcohol (V) with an alkali metal hydride, e.g., Na, Li, K, etc., to form the alkoxide which then is reacted with an alkylating agent, i.e. a benzyl halide (Cl or Br) to give the benzyl ether (XI). Solvents suitable for such a reaction include anhydrous dimethylformamide, dimethylsulfoxide and high boiling ethers such as tetrahydrofuran or dioxane. The reaction temperature may range from about room temperature to 100° C. with about room temperature as preferred.
XI→XII
The compound of formula XII is thereafter produced by an acid catalyzed hydrolysis of the ketal protecting group. Reagents and reaction parameters are the same as in previously disclosed step VII→VIII.
XII→XIII→XIV
The diol of formula XII is converted into the haloacetate of formula XIV via the compound of formula XIII and the intermediate of the formula ##STR24## by following the steps and utilizing the reactants and reaction parameters disclosed previously in step VIII→IX. This series of reactions are performed because selective alkyl or aryl sulfonyloxy of the primary hydroxyl group in XII is difficult due to the similar reactivity of both of the hydroxyl groups in XII.
XIV→XV
The compound of formula XIV thereafter undergoes a two step reaction wherein the acetate (XIV) is saponified to give the intermediate halohydrin of the formula ##STR25## which is then converted under basic conditions into the epoxide of formula XV. The reaction is carried out utilizing an alkali metal, e.g., Na or K, hydroxide in a solvent of H 2 O plus an inert water miscible co-solvent such as a lower alcohol, e.g., methanol, ethanol, propanol, etc. The reaction temperature may vary from about -10° C. to 25° C. with a range of about 0° C. to 10° C. as preferred. It should be noted that the above reactions preserve the stereochemistry of the asymmetric carbon atom throughout.
XVI→XVII
This reaction is a two step sequence wherein a compound of the formula IX under basic reaction conditions is converted into the epoxide of the formula ##STR26## wherein R 1 and R 3 are as above.
This compound acts as the alkylating agent in the ensuing reaction with the phenol (XVI) under basic catalysis conditions to form the ether (XVI). The base utilized in the reaction is an alkali metal hydroxide, e.g., NaOH or KOH and the reaction temperature ranges from about room temperature to 100° C. The reaction time may vary from about 2 hours to several days depending on the reaction temperature chosen. The solvents utilized may be dimethylsulfoxide, tetrahydrofuran and lower alcohol/water mixtures.
HYDROXYPHENOL→XVII
This reaction is similar to XVI→XVII except a large excess of hydroxyphenol is utilized to minimize any dialkylation which might occur. As in XVI→XVII the effective alkylating agent is the epoxide (see above). The reagents and reaction parameters are as above (XVI→XVII).
XVII→XVIII
The compound of formula XVII thereafter undergoes hydrogenolysis to a compound of formula XVIII. Catalysts for the reaction may be noble metals such as Platinum, Palladium, Rhodium or Ruthenium on carbon. Suitable solvents include lower alcohols (methanol, ethanol, etc.), esters (ethyl or butyl acetate) and ethers (dioxane or tetrahydrofuran). The reaction temperature may be varied from about 0° C. to 100° C. with room temperature preferred.
XVI→XIX
This reaction consists of the O-alkylation of the phenol of formula XVI with a compound of the formula ##STR27## wherein X is a leaving group selected from the group consisting of halogen, tosyloxy and mesyloxy, R 6 is hydrogen or alkoxy and n is 2 to 20, utilizing an alkali metal hydroxide (NaOH, KOH, etc.) in an inert water miscible solvent, e.g., a dimethylsulfoxide/H 2 O mixture. The reaction temperature may vary from about room temperature to 60° C. with 60° C. as preferred with a reaction time from 1-2 hours to several days depending on the reaction temperature. Alternate O-alkylation systems which may be utilized in conjunction with the phenylpiperazine include alkali metal alkoxides in lower alcohols e.g., sodium methoxide in methanol or potassium carbonate in acetone.
XVIII→XXIII
The compound of formula XVIII is reacted with a compound of the formula
Y(CH.sub.2).sub.n X
wherein X and Y are the same or different leaving groups with X as above and Y selected from the same leaving groups as X.
The reaction which is an O-alkylation of a phenol (XVIII) with an α,ω-dihaloalkane (for example) is carried out utilizing an alkali metal carbonate, such as, potassium or sodium carbonate in, as preferred, refluxing acetone. The reaction temperature may vary from room temperature to reflux with reflux as preferred.
XVIII→XXIV
This reaction follows the same reaction parameters and utilizes the same reagents as previously disclosed in step XVI→XIX.
XVIII→XX
The compound of formula XVIII is thereafter reacted with a compound of the formula ##STR28## wherein X is as above and R is lower alkyl.
This O-alkylation of the phenol (XVIII) with the alkyl ω-haloalkanoate, for example, ethyl-6-bromohexanoate or ethyl bromoacetate, using as a base an alkali metal alkoxide, such as, potassium tert-butoxide, methoxide or ethoxide in a lower alcohol, e.g., methanol, ethanol, etc., at a temperature range of about 0° C. to 100° C. with 60° C. to 80° C. as preferred. The product is subsequently saponified to give the acid (XX). The saponification is usually carried out at between room temperature to 65° C. for a period of 3 to 40 hours.
XVIII→XXII
The compound of the formula XVIII is reacted with an alkylating agent of the formula ##STR29## wherein X, n and R 6 are as before, such as, 1-(ω-haloalkanoyl)-4-phenylpiperazine, in an alcohol/water mixture or tetrahydrofuran or dimethylsulfoxide/water mixture containing an alkali metal hydroxide, e.g., NaOH or KOH. The reaction is carried out at from about room temperature to 100° C. with 75° C.-80° C. as preferred.
XIX→XXI→XXIV
The compound of formula XIX undergoes hydrogenolysis of the benzyl ether portion by utilizing a noble metal catalyst, e.g., Palladium, Platinum, Rhodium, etc. on carbon. The solvent for such a reaction may be an alcohol (methanol, ethanol, etc.) or acetic acid containing a small amount of mineral acid such as HCl or H 2 SO 4 . The reaction temperature may vary from about 0° C.-100° C. with room temperature as preferred. The compound of formula XXI thereafter undergoes an O-alkylation using an alkylating agent (IX) in the presence of an alkali metal hydroxide as a base. The reagents and reaction parameters for this reaction are as previously disclosed for step XVI→XVII.
XX→XXII
The acid of the formula XX is converted to the activated intermediate ##STR30## wherein R 1 , R 3 and n are as above on treatment with ethyl chloroformate under anhydrous conditions in an aprotic solvent, e.g. tetrahydrofuran or dioxane, at a low temperature e.g., about 0° C. to 5° C. in the presence of a tertiary amine base, e.g. trialkylamine. This mixed anhydride is treated in situ with a phenylpiperazine of the general formula ##STR31## wherein R 6 is as above to give the tertiary amide. This reaction is carried out at between about 10° C. to 25° C.
XXIV→XXV
The compound of formula XXIV undergoes a reductive cleavage of the --R 3 protecting group utilizing as the reducing agent a 60-70% solution of sodium bis-methoxyethoxy aluminum hydride in an inert aromatic hydrocarbon solvent such as benzene or toluene. Inert aprotic solvents such as tetrahydrofuran or dioxane may also be utilized. The reaction may be carried out at from about room temperature to 100° C. with a range of about 80° C. to 100° C. as preferred.
XXII→XXV
The compound of formula XXII undergoes a reductive cleavage of the --R 3 protecting group with a concommitant reduction of the amide function to an amino group. The reagents and reaction parameters for this reaction are as previously disclosed in step XXIV→XXV with the exception that a proportionately greater amount of the hydride reducing agent is employed.
XV→XXX
Suitably protected the optically active 2,3-epoxypropanol (XV) is thereafter reacted with a substituted phenol of the formula XVI in an O-alkylation using an alkali metal alkoxide, e.g., sodium or potassium methoxide or ethoxide, as the base in a lower alcohol solvent (methanol, ethanol, etc.). Also useful as a base in the above reaction would be an alkali metal hydroxide, e.g., NaOH or KOH in an aqueous alcohol, tetrahydrofuran, dioxane or dimethylsulfoxide solvent. The reaction temperature may range from room temperature to reflux for the chosen solvent with 60° C.-80° C. as preferred.
XXX→XXXI
The benzyl ethers of the formula XXX thereafter undergo a hydrogenolysis utilizing a catalyst of a noble metal such as Palladium, Platinum, Ruthenium etc. on carbon. Suitable solvents include alcohols (methanol, ethanol, propanol, etc.) or acetic acid containing a small amount of a mineral acid such as H 2 SO 4 or HCl. The reaction temperature may range from about 0° C. to 100° C. with room temperature as preferred. The hydrogenolysis may also be run under pressure up to 10 atmospheres if a catalyst such as H 2 /Raney Nickel is chosen.
XXXI→XXXII→XXXIII
The reagents and reaction parameters for this step have been previously disclosed in step XII→XIII→XIV.
XXXIII→XXXIV
The acetate (XXXIII) thereafter undergoes an acid catalysed hydrolysis wherein the acetate reacts in a hydrolytic solvent, such as, alcohols, e.g., methanol, ethanol, etc. or alcohol/water mixtures which contain a catalytic amount of a mineral acid such as H 2 SO 4 or HCl or an acidic ion exchange resin. The reaction may be carried out at from about 0° C. to reflux of the chosen solvent with a range of about room temperature to 60° C. as preferred.
XXXIV→XXXV
The halohydrin (XXXIV) is therefore reacted with a phenylpiperazine of the formula ##STR32## wherein X is halo.
This reaction involves two separate and unrelated base-induced transformations, i.e., (1) conversion of the halohydrin into an epoxide and (2) the O-alkylation of the phenol with the selected phenylpiperazine. The reaction is carried out under basic conditions utilizing an alkali metal hydroxide, e.g., NaOH or KOH in an aqueous dimethylsulfoxide, tetrahydrofuran or alcohol (methanol, ethanol, etc.) solvent. The reaction is carried out from about 0° C. to 40° C. with higher temperatures, e.g., 40° C. as preferred.
XXXV→XXV
The epoxide of formula XXXV is reacted with a monoalkylamine such as isopropyl, t-butyl, etc. amine to produce the amino alcohol. Solvents for such a reaction are alcohols (C 1 -C 4 ) with methanol preferred or ethers, such as, tetrahydrofuran or dioxane. The reaction may be run from about 0° C. to 100° C. with about 65° C. as preferred.
XVII→XXXVI
The compound of formula XVII undergoes a reductive cleavage of the N-protected amine to give the secondary amine. Reagents and reaction parameters for this reaction have been previously disclosed for step XXIV→XXV.
XXXVI→XXXVII
The benzyl ether of formula XXXVI thereafter undergoes hydrogenolysis in a catalyzed reaction. Suitable catalysts include noble metals (as previously disclosed) on carbon in a solvent such as lower alcohols (C 1 to C 4 ) e.g., methanol or ethanol at a temperature range of from about 0° C. to 100° C. If H 2 /Raney Nickel is chosen as the catalyst, the reaction should be run under pressure, e.g., up to 10 atmospheres.
XXXVII→XXV
The phenol (XXXVII) undergoes a base induced O-alkylation with a phenylpiperazine of the formula ##STR33## wherein n and R 6 are as above in an aqueous dimethylsulfoxide, tetrahydrofuran or dioxane solvent. Suitable bases include alkali metal hydroxides, such as, NaOH or KOH. The reaction temperature ranges from about 0° C. to 100° C. with about 60° C. as preferred.
XLII→XLIII
The compound of the formula XLII is reacted with a compound of the formula ##STR34## to produce the compound of the formula XLIII. The reactants and reaction parameters have been previously disclosed in step XV→XXX.
XLIII→XLIV
The compound of formula XLIII thereafter undergoes a hydrogenolysis as previously disclosed and with the same reagents and reaction parameters as step XXX→XXXI.
XLIV→XLV→XLVI
The compound of formula XLIV is converted to a compound of formula XLVI utilizing the same reagents and reaction parameters as previously disclosed in step XII→XIII→XIV.
XLVI→XLVII
The compound of formula XLVI undergoes a three step reaction under basic conditions as follows:
(A) saponification of the methyl ester
(B) saponification of the acetate to give the halohydrin and
(C) conversion of the intermediate halohydrin into the epoxide (XLVII).
As the base, an alkali metal hydroxide, e.g., NaOH or KOH, in a solvent of water plus an inert water miscible co-solvent such as a lower alcohol (C 1 to C 4 ) e.g., methanol or tetrahydrofuran or dioxane. The reaction is carried out from about 0° C. to 30° C. with a preferred temperature range of about 10° C. to 25° C.
XLVII→XLVIII
The activated ester of formula XLVIII is produced by treatment of the acid (XLVII) with an excess of a haloacetonitrile (Halo-CH 2 C.tbd.N) in the presence of a tertiary amine base, such as, trialkylamine, e.g., triethyl-or trimethylamine. The reaction temperature may range from about 0° C. to 70° C. with a range of about 25° C.-70° C. as preferred. The activated ester may be utilized to undergo condensation reactions, such as reactions with amines to form amides at a much faster rate than the ordinary methyl or ethyl esters.
XLVIII→XLIX
The ester of formula XLVIII is thereafter condensed with a primary amine of the formula ##STR35## to form the amide (XLIX). An inert solvent, such as, tetrahydrofuran or dioxane, may be utilized at a temperature range of about 0° C. to 100° C. with room temperature as preferred.
XLIX→L
The epoxide of formula XLIX is thereafter reacted with a primary amine e.g., an amine of the formula
NH.sub.2 --R.sub.1
wherein R 1 is as above in a solvent, such as, C 1 to C 4 alcohols or ethers, e.g., tetrahydrofuran or dioxane, to form the amino alcohol (L). The reaction may be run at from about 0° C. to reflux temperature with room temperature to 65° C. as preferred.
LI→LII
The alkene portion of the formula LI* compound is reacted with a hypohalous acid (generated in situ from an N-Halosuccinimide in aqueous acetone containing a catalytic amount of HCLO 4 ) to give a mixture of halohydrins, i.e., LII and the compound of the formula ##STR36##
LII→LIII
The bromohydrins (LII and LII') are thereafter converted under basic conditions to the epoxide (LIII). As a base, an alkali metal (Na, K, etc.) hydroxide may be utilized. Suitable solvents for the reaction include ethers, such as, dioxane or tetrahydrofuran and alcohols (C 1 to C 4 ) e.g., methanol, ethanol, etc. The reaction can be run at from about 0° C. to 40° C. with room temperature as preferred.
LI→LIV
The acid portion of the compound of formula LI is esterified by treatment of LI with an excess of an alkylating agent, CH 3 -Halo, e.g., CH 3 I, CH 3 Br, in the presence of an alkali metal (Na, K) carbonate in a solvent, such as, acetone, dimethylformamide, dimethylsulfoxide or hexamethylphosphoramide to give the ester of formula LIV. The reaction temperature is not critical but about room temperature is preferred for its ease.
LIII→LV
The acid portion of the epoxide (LIII) may also be esterified by using diazomethane in the presence of a solvent such as ethers (tetrahydrofuran) or a C 1 to C 4 alcohol. As above, this reaction is preferably run at room temperature.
LIV→LV
The alkene portion of the compound of formula LIV is thereafter reacted with an aromatic or aliphatic peracid, such as, m-chloroperbenzoic acid, peracetic acid, performic acid, trifluoroperacetic acid, permaleic acid, perbenzoic acid, monoperphthalic acid, o-sulfoperbenzoic acid or p-nitroperbenzoic acid. The reaction utilizes as a solvent any inert halogenated aliphatic hydrocarbon, such as, methylene chloride or chloroform. The reaction temperature may range from about 0° C. to reflux with room temperature as preferred.
LV→LVI
The epoxide portion of the compound of formula LV is thereafter reacted with a primary amine of the formula NH 2 R 1 , wherein R 1 is as above, in a suitable solvent, such as, C 1 to C 4 alcohols or ethers, such as, dioxane or tetrahydrofuran. The reaction temperature may vary from about 0° C. to room temperature with room temperature as preferred.
LVI→LVII
The ester portion of LVI is thereafter condensed with a primary amine of the formula ##STR37## wherein n and R 6 are as above, to form the amide. No solvent is necessary for this step. The reaction temperature may be from about 100° C. to 150° C. with a preferred range of from about 140° C. to 145° C.
XVI→LXII
The phenol portion of XVI undergoes an O-alkylation with an epihalohydrin, e.g., epichlorohydrin, using as a base, an alkali metal hydroxide, e.g. KOH or NaOH in a mixture of H 2 O and dioxane, tetrahydrofuran or dimethylsulfoxide. The reaction may be carried out from about 0° C. to 100° C. with about room temperature as preferred.
LXII→LXIII
The epoxide portion of LXII is thereafter reacted with an amine of the formula
NH.sub.2 R.sub.1
wherein R 1 is as above, in an solvent, such as, a C 1 to C 4 alcohol, or an ether, such as, tetrahydrofuran or dioxane. The reaction temperature may range from about 0° C. to reflux with a range of about room temperature to 65° C. as preferred.
LXIII→LXIV
The benzyloxy portion of the compound of formula LXIII is converted to the phenol function by utilizing the reagents and reaction parameters previously disclosed for the isomer, see, step XXXVI→XXXVII.
LXIV→XXV'
The phenol portion of LXIV is reacted with a phenylpiperazine as previously disclosed in step XXXVII→XXV along with the reagents and reaction parameters.
4-(2-bromoethoxy)phenol *→LVIII
The phenol portion of the bromoethoxy phenol undergoes an O-alkylation with an alkylating agent, such as, allyl halide, e.g. chloride or bromide, in the presence of an alkali metal (Na,K) carbonate in refluxing solvent, such as, acetone. The reaction temperature should be about or at reflux of the solvent.
LVIII→LIX and LIX'
The alkene portion of the compound of formula LVIII is thereafter converted to the halohydrins of formulas LIX and LIX' by utilizing the reagents and reaction parameters set forth in step LI→LII.
LIX and LIX'→LX
The halohydrins (LIX and LIX') are thereafter converted to the epoxide of formula LX by utilizing the reagents and reaction parameters set forth in step LII→LIII. LX→LXI
The epoxide (LX) is thereafter reacted with a primary amine of the formula NH 2 -R 1 wherein R 1 is as above, to give the amino-alcohol (LXI). Suitable solvents include C 1 to C 4 alcohols, ethers such as tetrahydrofuran or dimethylsulfoxide or dimethylformamide. The reaction may be carried out from about room temperature to 60° C. with a range of about room temperature to 55° C. as preferred.
LXI→XXV'
The halogen portion of LXI is thereafter displaced with a secondary amine of the formula ##STR38## wherein R 6 is as above to produce a compound of formula XXV'. Solvents suitable for this reaction include C 1 to C 4 alcohols and ethers, such as, dioxane and tetrahydrofuran. The reaction may be carried out at from about 0° C. to 100° C. with 80° C. to 100° C. as preferred.
LXV*→LXVI
A compound of the formula LXV is reacted with an appropriately substituted amine of the formula ##STR39## wherein R 6 is as above in a C 1 to C 4 alcohol. The temperature of the reaction may be varied from room temperature to the boiling point of the selected alcohol. A preferred alcohol is ethanol and the preferred reaction temperature is its boiling point.
LXVI→LXVII
The compound of formula LXVI is thereafter converted to a compound of formula LXVII by treatment with a base such as an alkali or alkaline earth metal hydroxide (NaOH, KOH, Ba(OH 2 ) in a solvent such as water, C 1 to C 4 alcohols or dimethylformamide or alkali metal (K,Na) salts of lower alcohols in solvents such as dimethylformamide or C 1 to C 4 alcohols. To this reaction mixture containing the salt of LXVI is added epihalohydrin to generate LXVII.
LXVII→LXVIII
The compound of formula LXVII is treated with an amine of the formula
R.sub.1 NH.sub.2
wherein R 1 is as above in a suitable solvent, e.g., C 1 to C 4 alcohols. The reaction may be carried out at from about room temperature to reflux with about reflux as preferred. A preferred solvent would be methanol. If faster reaction rates are desired, the reaction mixture can be heated above its boiling point in a pressurized vessel.
LXIX→LXVIII→LXX
The compound of formula LXVIII can alternatively be prepared from LXIX by treatment with a propenoyl halide in an inert solvent e.g., dioxane, dimethylsulfoxide, etc. at from about 0° C. to 50° C. The intermediate is treated in situ with an appropriately substituted amine of the formula ##STR40## wherein R 6 is as above The reaction conditions are as in step LXV→LXVI above. The compound of formula LXX is generated by mixing maleic acid with LXVIII in an inert solvent.
LXXI→LXXII
The haloalkanoyl halide of formula LXXI is reacted with 4-aminophenol in the presence of excess 4-aminophenol or an equivalent of a tertiary amine, such as, pyridine, triethylamine or the like in an inert solvent, such as, an ether, e.g., tetrahyrofuran or dioxane or a polyhalogenated hydrocarbon, e.g., methylene chloride at a temperature of from about 0° C. to 100° C. A preferred reaction system for this conversion is dioxane in the presence of excess 4-aminophenol at room temperature.
LXXII→LXXIII
The compound of formula LXXII is reacted with an appropriately substituted amine of the formula ##STR41## wherein R 6 is as above in the presence of a hydrogen halide scavenger, such as excess reagent or a less reactive amine such as triethylamine or pyridine in an inert solvent e.g., C 1 to C 4 alcohol. The reaction temperature may vary from about room temperature to 100° C.
LXXIII→LXIV→LXXV
Conversion of the compound of formula LXXIII into that of formula LXXV is the same for reagents and reaction parameters as previously disclosed in steps LXVI→LXVII→LXVIII→LXX
The end compounds of the subject invention may be converted to their pharmaceutically acceptable salts which exhibit comparable pharmacological activity. The end products have three amine functions, but only two of these groups are sufficiently basic to form stable salts. Accordingly they form diacid salts with various organic and inorganic acids. Some of the useful organic or inorganic acids include maleic acid, fumaric acid, tartaric acid, citric acid, hydrochloric acid, hydrobromic acid and sulfuric acid. A typical preparation of one of these salts entails the mixture of a solution of the base end product, for example, XXV in a C 1 to C 4 alcohol with a solution of a pharmaceutically acceptable acid as outlined above, also in a C 1 to C 4 alcohol. The salt thus formed crystallizes spontaneously from solution or does so on the addition of a suitable co-solvent, for example, ethyl acetate, ether, acetone, or halogenated hydrocarbons, such as, chloroform, 1,2-dichloroethane, etc.
An alternative method which may be useful in the case of compounds, such as the end product L, comprises the treatment of two parts of the base with an excess of hydrochloric acid in methanol. The solvent is then removed in vacuo to drive off the excess acid which gives the unstable trihydrochloride salt. The salt is then redissolved in methanol and one part of free base added to the solution. The dihydrochloride salt is then precipitated from solution on the addition of a co-solvent, such as disclosed above.
Preferred among the compounds disclosed herein are those of the formula ##STR42## wherein R 1 is selected from the group consisting of lower alkyl; R 8 is selected from the group consisting of --O--(CH 2 ) n -- wherein n is 2 to 20, ##STR43## and ##STR44## and R 6 is selected from the group consisting of hydrogen or lower alkoxy, the racemates thereof and pharmaceutically acceptable salts thereof. Especially preferred are those compounds wherein R 1 is a branched chain alkyl, such as, isopropyl or tertiary butyl, R 8 is the group --O--(CH 2 ) n -- or ##STR45## wherein n is 2 to 10, most preferably 2, and R 6 is hydrogen.
The compounds of the present invention and their pharmaceutically acceptable salts are useful as α and β adrenergic blocking agents when utilized particularly in oral preparations. As contemplated by this invention the novel end products of the present invention and their pharmaceutically acceptable salts can be embodied in pharmaceutical dosage formulations containing from about 0.1 to about 50 mgs., most preferably 1-50 mg. with dosage adjusted to animal species and individual requirements. The novel end products and their pharmaceutically acceptable salts can be administered internally, for example, parenterally or enterally, in conventional pharmaceutical dosage forms. For example, they can be incorporated in conventional pharmaceutical dosage forms. For example, they can be incorporated in conventional liquid or solid vehicles such as water, gelatin, starch, magnesium stearate, talc, vegetable oils and the like to provide tablets, elixirs, capsules, solutions, emulsions and the like according to acceptable pharmaceutical practices. Although less preferred intravenous and intramuscular delivery systems may be utilized to provide the above novel compounds.
The disclosed compounds are in the general class of 1-aryloxy-3-alkylaminopropan-2-ols, many examples of which have been shown to possess β-adrenergic blocking activity. Since the class of compounds has an asymmetric center there are two enantiomeric forms. It has been found that the β-blocking activity of such compounds is to a large extent found in the isomer having the S-absolute configuration i.e. that isomer that is stereochemically equivalent to the naturally occurring β-agonist (R)-(-) epinephrine, whereas the racemic form exhibits approximately half of this activity, see, for example,
(1) R. Howe & B. S. Rao J. Med. Chem. 11, 1118, (1968);
(2) B. Ablad et al Acta. Pharmacol Toxicol. 25, 85 (1967);
(3) L. Almirante & W. Murmann, J. Med. Chem. 9 650 (1966);
(4) M. Dukes & L. H. Smith J. Med. Chem. 14 326 (1971);
(5) J. C. Danilewicz & J. E. G. Kemp 16, J. Med. Chem., 168, (1973).
The desired S-isomer of the disclosed compounds are available in two ways:
(a) by resolution of the racemic material via a fractional crystallization of its diastereoisomeric salts formed with an optically active acid, such as tartaric acid.
(b) by asymmetric synthesis using an optically active synthon of the appropriate absolute configuration. Two such synthons, IX and XV, which are readily available from D-mannitol, a naturally occurring sugar, have been used to construct the oxypropanolamine side chain in the disclosed compounds. Synthon IX is restricted to the syntheses of α, β-blockers, wherein the functionality of the final compound is compatable with the conditions required to remove the amine protecting group, R 3 i.e. reductive cleavage using a mixed metal hydride. When the functionality of the final compound is not compatable with these conditions, e.g. the amido group in compound L, the synthon XV is used to incorporate the oxypropanolamine side chain.
Applicants, in setting forth the disclosure of the above specification have cited the teaching of various articles and U.S. Patents. Such citations are meant to incorporate the teachings of these references for completeness of disclosure.
The following examples are illustrative but not limitative of the present invention. All temperatures are stated in degrees Centigrade unless otherwise indicated.
EXAMPLE 1
(2R,3R,4R,5R)-Mannitol-1,2;5,6-diacetonide
A mixture of 546 g powdered D-Mannitol (3.0 mol), p-toluenesulfonic acid (3.0 g) and 780 g dimethoxypropane (7.5 mol) in 900 ml dry DMSO was stirred at ambient temperature under anhydrous conditions. Within 30 min-1 hr, all the mannitol had dissolved. After 16 hours the reaction was poured into 900 ml saturated NaHCO 3 solution and then was diluted further with 2 liters H 2 O. The mixture was extracted with EtOAc (1×4.5 l; 3×3 l) and the extracts were washed in turn with H 2 O (3×1.5 l). The combined dried (Na 2 CO 3 ) EtOAc layers were concentrated in vacuo (bath temp ˜45° ) until the residue had solidified. The residue was then heated to reflux to redissolve the solids and the solution was diluted with ˜8 liters of hot hexane. The mixture was allowed to cool slowly overnight and the resulting crystalline material was filtered off and washed with an ether-hexane mixture (1:3; 4×500 ml) to give (2R,3R,4R, 5R)-mannitol-1,2,5,6-diacetonide, mp 115°-119°.
The mother liquors were concentrated to dryness. A solution of the resulting residue in ether (300 ml) was diluted with about 1.6 liters of hexane. This yielded additional diacetonide, mp 119°-120°.
EXAMPLE 2
(2S)-3-Isopropylamino-1,2-propanediol acetonide from (2R,3R,4R,5R)-Mannitol-1,2;5,6-diacetonide via the imine
Pb(OAc) 4 (263 g, 0.59 mol) was dispersed in 1500 ml dry benzene under argon. To the rapidly stirred mixture 140 g of the diacetonide was added in 5-10 g portions over 15 minutes and then further 1 g portions of diacetonide were added until the reaction gave a negative test for oxidant (KI-starch paper). A total of 150 g of acetonide (140 g+10×1 g) was used. The mixture was filtered through Celite and the filter cake was washed with 2×100 ml portions of dry benzene. The filtrate was stirred with 300 g anhydrous K 2 CO 3 for 30 minutes to neutralize HOAc which was produced in the oxidation. After a second filtration through Celite, the solution was treated with 450 ml isopropylamine and 300 gr of K 2 CO 3 . After stirring for 30 min., the mixture was filtered and the filtrate was hydrogenated over 15 g 10% Pd/C (1 atmos; 23°). The reaction essentially stopped after the uptake of 26.4 liters of H 2 . The catalyst was removed by filtration and concentration of the filtrate furnished the amine.
EXAMPLE 3
(2S)-3-N-Mesylisopropylamino-1,2-propanediol acetonide
90 ml (1.2 mol) mesyl chloride was added with stirring to a previously chilled (-10°) solution of (2S)-3-isopropylamino-1,2-propanediol acetonide (188 g; 1.087 mol) and triethylamine (288 ml; 1.63 mol) in dry THF at such a rate that the reaction temp did not exceed 5°. Reaction was then stirred at 10°-15° for 30 min whereupon it was diluted with 1.5 l brine. The layers were separated and the aqueous layers were extracted with ether (3×500 ml). The organic layers were washed in turn with brine (2×500 ml) and then were combined, dried (Na 2 SO 4 ), and evaporated to give the N-mesylate as an oil.
A small portion was recrystallized (3×) from hexane to give analytically pure material, mp 33°-34°; [α] D 25 -14.76° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 10 H 21 NO 4 S: C, 47.79; H, 8.42; N, 5.57; S, 12.76. Found: C, 47.87; H, 8.66; N, 5.72; S, 12.89.
EXAMPLE 4
(2S)-3-N-Mesylisopropylamino-1,2-propanediol
200 ml of prewashed (H 2 O and MeOH) Dowex 50W-8X ion exchange resin (H + form) was added to a solution of 264 g crude (2lS)-3-N-mesylisopropylamino-1,2-propanediol acetonide in methanol (1 liter) and water (325 ml). The mixture was stirred under reflux for 90 min. The cooled mixture was filtered and the filtrate was concentrated in vacuo. The residue was evaporated several times from benzene-EtOH mixtures to remove the last traces of water. The resulting solid was triturated with 2.5 l ether to give the diol, mp 67°-70°. Concentration of the ether furnished additional diol, mp 64°-66°. Crystallization from ethyl acetatehexane furnished the analytically pure material, mp 73°-74°; [α] D 25 -15.94° (c, 1.0, H 2 O).
Anal. Calcd. for C 7 H 17 NO 4 S: C, 39.79; H, 8.11; N, 6.63; S, 15.18. Found: C, 39.83; H, 8.40; N, 6.66; S, 14.96.
EXAMPLE 5
(S)-1-Mesyloxy-2-hydroxy-3-N-mesylisopropylaminopropane
19.1 g (90.5 mmol) N-mesyl-1,2-dihydroxy-3-isopropylaminopropane was dissolved in 150 ml anhydrous pyridine under argon and cooled to -45°. 7.0 ml (90.4 mmol) mesyl chloride was added dropwise over 5 minutes and the mixture was stirred at -45° for 5 hrs. The cold mixture was then diluted with 100 ml H 2 O followed by 200 ml 6 N HCl and extracted with EtOAc (3×). The EtOAc layers were washed in turn with 3 N HCl (1×250 ml), brine (2×) and NaHCO 3 solution (1×). The combined extracts were combined and evaporated to give the O,N-dimesylate as an oil which solidified on standing.
This material was contaminated with ˜2% trimesylate. A small sample was purified in the following way: 500 mg was dissolved in 10 ml water and filtered free of any undissolved trimesylate. The filtrate was extracted with ether (2×) and with EtOAc (2×). The EtOAc layers were combined, dried (Na 2 SO 4 ), and evaporated. Crystallization of the residue from ether furnished the analytical sample, mp 51°-52°, [α] D 25 -1.21° (c, 1.0, H 2 O).
Anal. Calcd. for C 8 H 19 NO 6 S 2 : C, 33.21; H, 6.59; N, 4.84; S, 22.16. Found: C, 33.33; H, 6.13; N, 4.76; S, 22.18.
EXAMPLE 6
(S)-1-Tosyloxy-2-hydroxy-3-N-mesylisopropylaminopropane
A stirred solution of 63.3 g (0.3 mol diol of Example 4 in 450 ml pyridine was cooled to -20° and 85.5 g tosyl chloride (0.45 mol) was added. The reaction mixture was stirred in an ice-water bath for 2 hr whereupon 5-10 g ice was added to the mixture and the stirring was continued for an additional 15 minutes before it was poured into a mixture of ice (1 kg) and concentrated HCl (500 ml) and extracted with CH 2 Cl 2 (1×1 l; 2×500 ml). The extracts were washed in turn with brine (1×500 ml) and 5% NaHCO 3 solution. The combined, dried (Na 2 SO 4 ) extracts were concentrated in vacuo to give the mono-tosylate as an oil. A small portion was purified for analysis by chromatography; [α] D 25 +5.65° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 14 H 23 NO 6 S 2 : C, 46.01; H, 6.34; N, 3.83; S, 17.55. Found: C, 46.11; H, 6.53; N, 3.67; S, 16.97.
EXAMPLE 7
(2S)-1-Chloro-2-hydroxy-3-N-mesylisopropylaminopropane
A mixture of 10.55 g (50 mmol) of diol of Example 4, 9.0 g (75 mmol) of trimethylorthoacetate and 0.4 g (3.27 mmol) of benzoic acid was heated with stirring at 80° for 45 min. The viscous reaction mixture was cooled and partioned between CH 2 Cl 2 and saturated NaHCO 3 solution. The CH 2 Cl 2 layer was dried (Na 2 SO 4 ) and evaporated to give 14.5 g of the crude orthoacetate which was then dissolved in 75 ml dry CH 2 Cl 2 and treated with 12 ml (95 mmol) trimethylchlorosilane and heated at reflux for 60 minutes. The solvent was removed in vacuo and the residue was dissolved in 100 ml 0.3 N methanolic HCl and the mixture was left at ambient temperature for ˜65 hrs. The solvent was removed under reduced pressure and the residual oil was chromatographed over silica gel (50 g) to give the pure chlorohydrin as an oil, [ α] D 25 -12.7° (c, 1.0 MeOH).
Anal. Calcd. for C 7 H 16 ClNO 3 S: C, 36.60; H, 7.02; N, 6.10; Cl, 15.43; S, 13.96. Found: C, 36.38; H, 7.32; N, 5.98; Cl, 15.15; S, 13.53.
EXAMPLE 8
(2S)-3-Benzyloxypropandiol, 1,2-acetonide
44 g of a 50% dispersion of NaH in oil was placed in a flask and washed with dry hexane. To the flask was then charged a solution of 120 g benzyl chloride in 1500 ml dry DMF. To this stirred mixture, a solution of (2S)-glycerol-2,3-acetonide (120 g) in dry DMF (500 ml) was added over 45 min at ambient temperature (initial reaction temperature was 17° and it rose to a maximum of 27° during the addition). Stirring was continued for 1 hr after the addition was completed and then MeOH (˜30 ml) was added dropwise to destroy excess hydride. The system was then equipped for distillation and the DMF was distilled off in vacuo (˜55°-60°; water aspirator). The residue was diluted with brine (2 liters) and extracted with CH 2 Cl 2 (3×1 liter). The organic layers were washed in turn with brine and then were combined, dried (MgSO 4 ) and evaporated to give an oil.
The oil was distilled in vacuo to give the benzyl ether (bp 78°-80°, 0.05 mm).
EXAMPLE 9
(2R)-3-Benzyloxy-1,2-propanediol
A suspension of 75 ml Dowex 50-8x (H + form) in a stirred solution of 254.6 g (1.15 mol) (2S)-3-benzyloxypropanediol, acetonide in 800 ml MeOH and 200 ml H 2 O was heated at reflux for 1 hr. The resin was filtered off and the filtrate was concentrated in vacuo. The diol was freed from residual H 2 O by evaporating it several times from ethanol-benzene mixtures to give it as a colorless oil.
EXAMPLE 10
2(R,S),4(S)-2-Methoxy-2-methyl-4[(benzyloxy)methyl)]-1,3-dioxolane
A stirred solution of 207 g (1.13 mol) (2R)-3-benzyloxy-1,2-propanediol in 200 g (1.66 mol) trimethylorthoacetate containing 3 g (0.024 mol) was heated in an oil bath at 75° in a flask fitted for downward distillation. Methanol thus was removed from the reaction as it was formed. After 40 min the reaction mixture was cooled and partitioned between CH 2 Cl 2 (800 ml) and 1 N NaOH solution (200 ml). The aqueous phase was extracted further with CH 2 Cl 2 (2×250 ml) and then the organic layers were washed in turn with 200 ml 0.5 N NaOH solution. The combined CH 2 Cl 2 layers were dried (Na 2 SO 4 ) and concentrated to dryness to give the cyclic orthoacetate as a colorless oil.
Analysis of its nmr spectrum showed it to be a 4:3 mixture of diastereoisomers. A small sample was distilled (˜165°/0.1 mm) to give the analytical sample [α] D 25 +7.4° (c, 1.0, MeOH).
Anal. Calcd. for C 13 H 18 O 4 : C, 65.53; H, 7.61. Found: C, 65.84; H, 7.76.
EXAMPLE 11
(2S)-3-Benzyloxy-2-acetoxy-1-chloropropane
155 ml (1.21 mol) trimethylchlorosilane was added to a solution of 270 g (1.13 mol) crude cyclic orthoacetate in 600 ml dry CH 2 Cl 2 and the mixture was heated at reflux in an inert atmosphere for 30 minutes. The solvent and excess reagent were removed under reduced pressure to give the crude chloroacetate as a mobile oil. This material was used without further purification.
A small portion was distilled (˜165°/0.1 mm) to give the analytical sample [α] D 25 +10.8° (c, 1.0, MeOH).
Anal. Calcd. for C 12 H 15 ClO 3 : C, 59.39; H, 6.23: Cl, 14.61. Found: C, 59.50; H, 6.31; Cl, 14.35.
EXAMPLE 12
(2S)-1,2-Epoxy-3-benzyloxypropane
A chilled solution of 115 g NaOH (2.875 mol) in 600 ml H 2 O was added dropwise over 20 minutes to a cooled solution of the crude chloroacetate of Example 11 (theory ˜1.13 mol) in MeOH (800 mol) with stirring. The reaction temperature was maintained at <12° during the addition. After stirring an additional 1 hr at ˜12°, the reaction was cooled to 5° and then neutralized to pH 7.0 using dilute H 2 SO 4 . The reaction was then concentrated in vacuo (bath temp. ˜25°) to remove MeOH and then it was diluted with 250 ml brine and extracted with CH 2 Cl 2 (1×750 ml; 1×400 ml). The CH 2 Cl 2 extracts were combined, dried (Na 2 SO 4 ) and evaporated to dryness. The resulting oil was distilled in vacuo to give the epoxide, bp 84°-86°/0.45 mm; [α] D 25 - 10.64° (c, 1.0, MeOH).
Anal. Calcd. for C 10 H 12 O 2 : C, 73.15; H, 7.27. Found: C, 73.21; H, 7.51.
EXAMPLE 13
(S)-1-(4-Benzyloxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane
Method A--Condensation of the product of Example 6 with benzyloxyphenol
A solution of (S)-1-tosyloxy-2-hydroxy-3-N-mesylisopropylaminopropane (103 g, 0.282 mol) and p-benzyloxyphenol (79 g, 0.395 mol) in 500 ml DMSO was treated with 93.7 ml 4 N NaOH (0.375 mol) and stirred at 100° under argon for 21/2 hr. The solution was cooled and 300 ml 1 N NaOH was added slowly to the vigorously stirred solution followed by 600 ml H 2 O. The resulting solid was removed by filtration and was washed with water. After partial air drying, the solid was dissolved in CH 2 Cl 2 and the solution was dried over MgSO 4 . The decolorized (charcoal) solution was evaporated to dryness and the resulting solid residue was triturated with hot ether (1.5 liters). Filtration of the colorless solid gave the end product, mp 91°-93°.
Recrystallization from CH 2 Cl 2 -ether gave the pure sample, mp 94°-95°; [α] D 25 -0.93° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 20 H 27 NO 5 S: C, 61.04; H, 6.91; N, 3.56. Found: C, 61.04; H, 6.90; N, 3.43.
EXAMPLE 14
Method B--Condensation of the product of Example 7 with benzyloxyphenol to give product of Example 13
A solution of 8.3 g (36.1 mmol) of (2S)-1-chloro-2-hydroxy-3-N-mesylisopropylaminopropane and 8.69 g (43.4 mmol) of p-benzyloxyphenol in 75 ml DMSO was treated with 10.86 ml 4 N NaOH (43.4 mmol) and the mixture was heated at 100° for 5 hours. To the cooled reaction mixture 40 ml 1 N NaOH and 60 ml H 2 O were added with stirring and the resulting solid was collected by filtration and was washed well with H 2 O. The dried crude product was recrystallized from EtOAc-hexane to yield the end product as white needles, mp 93°-94°.
EXAMPLE 15
(S)-1-(4-Hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane
A slurry of 10% Pd/C in 30 ml EtOAc was added to a solution of 38.4 g (S)-1-(4-benzyloxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane in 850 ml MeOH and the mixture was hydrogenated (760 mm; 20°). Within 1 hr the uptake of H 2 stopped (total 2.6 liters) and the catalyst was removed by filtration through Celite. The filtrate was concentrated under reduced pressure and the residue was crystallized from CH 2 Cl 2 -ether to give the phenol, mp 91°-93°. Recrystallization of a sample from EtOAc-hexane gave the analytically pure material, mp 92°-94°; [α]-1.93° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 13 H 21 NO 5 S: C, 51.47; H, 6.98; N, 4.62; S, 10.57. Found: C, 51.38; H, 6.89; N, 4.58; S, 10.46.
EXAMPLE 16
(S)-4-(2-Hydroxy-3-N-mesylisopropylaminopropoxy)phenoxyacetic acid
To a stirred solution of a 24 g (0.08 mol) of (S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane in 240 ml of absolute ethanol (argon atmosphere) was added at room temperature 9.04 g (0.08 mol) of potassium t-butoxide. After stirring for 15 min, 13.36 g (0.08 mol) of ethyl bromoacetate was added and the reaction mixture was heated under reflux overnight. It was then cooled and concentrated in vacuo. The residue was acidified to pH 2 with 1 N HCl, and was then dissolved in EtOAc. The organic layer was then washed twice with 1 N NaOH, once with H 2 O and dried (Na 2 SO 4 ). Evaporation of the solvent gave the crude ester as an oil which solidified on standing.
To a solution of 29 g (0.75 mol) of crude ester in 290 ml of MeOH, was added 40 ml of 4 N NaOH solution. The reaction mixture was refluxed for ten minutes and then allowed to cool to room temperature for one hour. Most of the solvent was evaporated in vacuo and the residue treated with 50 ml of 6 N HCl solution. The resulting solid was collected by filtration and crystallized twice from acetone-hexane to yield the end product, mp 128°-129°. Crystallization from acetone-hexane gave the analytical sample, mp 129°-130°; [α] D 25 +1.5° (c, 1.0, CH 3 OH).
Anal. Calcd. for C 15 H 23 NO 7 S: C, 49.85; H, 6.41; S, 8.87; N, 3.87. Found: C, 49.84; H, 6.58; S, 8.83; N, 3.80.
EXAMPLE 17
1-(2-Chloroethyl)-4-phenylpiperazine
To a stirred solution of N-phenylpiperazine (95% pure; 300 g; 1.85 mol) in 1 l MeOH previously chilled to -20° was added in one portion a chilled solution of ethylene oxide (150 ml) in MeOH (250 ml). The mixture was stirred in an ice-water bath overnight. After the solvent and excess reagent was removed in vacuo, the residue was taken up in toluene and re-evaporated to remove residual MeOH.
The crude 1-(2-hydroxyethyl)-4-phenylpiperazine (˜400 g) thus obtained was dissolved in dry CH 2 Cl 2 (3.5 l) containing triethylamine (400 ml; 2.9 mol) and the solution was cooled to -10°. A solution of 250 g (2.18 mol) mesyl chloride in 300 ml CH 2 Cl 2 was added to the stirred mixture over 30 min and then the reaction was allowed to warm up to room temp. It was then stirred at ambient temperature until the in situ conversion of the intermediate mesylate to the chloro compound was completed (16-40 hrs). Water (1 l) was added and the layers separated. The aqueous layer was washed with CH 2 Cl 2 (1×300 ml) and then the combined CH 2 Cl 2 phases were dried (K 2 CO 3 ) and evaporated. The residuw was triturated with hot hexane (1×1 l; 4×200 ml) and the combined extracts were decolorized (charcoal) and then cooled to 0° -5°. Filtration of the resulting colorless crystals afforded 1-(2-chloroethyl)-4-phenylpiperazine, mp 56°-58°. Concentration of the mother liquor to ˜400 ml furnished additional product, mp 55°-57°.
Recrystallization of a small sample from hexane furnished the analytically pure material, mp 59°-60°.
Anal. Calcd. for C 12 H 17 ClN 2 : C, 64.13; H, 7.62; N, 12.47; Cl, 15.78. Found: C, 64.30; H, 7.61; N, 12.41; Cl, 15.57.
EXAMPLE 18
1-(2-Chloroethyl)-4-(2-methoxyphenyl)-piperazine
In a procedure, analogous to the one described above, 50 mmol of N-(2-methoxyphenyl)piperazine was converted to 1-(2-chloroethyl)-4-(2-methoxyphenyl)-piperazine, mp 36.5°-37°.
Anal. Calcd. for C 13 H 19 ClN 2 O: C, 61.29; H, 7.52; N, 10.99; Cl, 13.92. Found: C, 61.22; H, 7.52; N, 11.02; Cl, 13.93.
EXAMPLE 19
1-[2-(4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine.
26.25 ml 4 N NaOH (0.105 mol) was added to a stirred mixture of 21.0 g (0.105 mol) 4-benzyloxyphenol and 22.5 g (0.1 mol) of 1-(2-chloroethyl)-4-phenylpiperazine in 250 ml DMSO and the reaction was heated at 60° for 60 min. After cooling, the stirred mixture was diluted with 50 ml 1 N NaOH solution and the resulting crystalline precipitate was collected by filtration and washed with water to give, after drying in vacuo, essentially pure end product, mp 116°-119°.
A small sample was recrystallized from ethyl acetate for analysis, mp 120°-121°.
Anal. Calcd. for C 25 H 28 N 2 O 2 : C, 77.29; H, 7.26; N, 7.21. Found: C, 77.19; H, 7.08; N, 7.12.
EXAMPLE 20
1-[2-(4-Hydroxyphenoxy)ethyl]-4-phenylpiperazine
Method A--By HCl cleavage of the benzyl ether of Example 19
35.75 g of 1-[2-(-4-benzyloxyphenoxy)ethyl]-4-phenylpiperazine was added rapidly with stirring to 75 ml concentrated HCl and the mixture was heated on a steam bath for 15 minutes. During this time starting material dissolved and then a white crystalline solid began to form and eventually the reaction mixture almost solidified. The reaction was cooled to ˜5° and then was diluted with 100 ml EtOH. The solids were filtered off and were washed in EtOH and ether to give 1-[2-(4-hydroxyphenoxy) ethyl]-4l-phenylpiperazine as its monohydrochloride. The salt was dissolved in 150 ml hot MeOH and 50 ml H 2 O and was then treated with 25 ml triethylamine. Water was then added to the refluxing mixture just to the cloud point whereupon the product began to crystallize from solution. The mixture was chilled and the solids were collected by filtration to give the end product, mp 142°-143°.
The analytically pure material, 143°-144°, was obtained by recrystallization from EtOAc.
Anal. Calcd. for C 18 H 22 N 2 O: C, 72.46; H, 7.43; N, 9.39. Found: C, 72.32; H, 7.23; ;l N, 9.25.
EXAMPLE 21
Method B--Hydrogenolysis of benzyl group in the product of Example 19 to produce the end product of Example 20
1-(4-Benzyloxyphenoxy)-4-phenylpiperazine (211.2 g; 0.544 mol) in 1 l HOAc was hydrogenolyzed over 20 g of 10% Pd/C (21°; 1 atmos). The absorption of H 2 essentially stopped after 3 hr (total uptake 15.1 l). The catalyst was filtered off through Celite and the filtrate was concentrated to dryness in vacuo. The crude material was dissolved in 750 ml hot MeOH and 250 ml warm (˜70°) H 2 O was added followed by 120 ml of triethylamine. H 2 O was then added to the cloud point whereupon the product started to crystallize rapidly from solution. The mixture was cooled to ˜5° and the crystalline material was removed by filtration and washed with MeOH-H 2 O (1:1) to give, the end product, mp 143°-144°.
EXAMPLE 22
(S)-1-[2-(4-(2-Hydroxy-3-N-mesylisopropylaminopropoxy)phenoxy)ethyl]-4-phenylpiperazine
Method A--Condensation of the compound of Example 15 with 1-(2-chloroethyl)-4-phenylpiperazine
11.0 ml 4 N NaOH solution (44 mmol) was added to a stirred solution of 13.3 g (43.9 mmol) (S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane and 10.0 g (44.4 mmol) 1-(2-chloroethyl)-4-phenylpiperazine in 100 ml DMSO. The mixture was heated at 60° under argon and then was cooled and diluted with 200 ml water. The resulting solid was collected by filtration, was washed with water and then was dissolved in CH 2 Cl 2 . The CH 2 Cl 2 solution was washed with 5% Na 2 CO 3 solution and then was dried (K 2 CO 3 ) before evaporation in vacuo to a white solid. Crystallization of the product from EtOAc furnished the end product in two crops: mp 104°-106°; mp 103°-105°.
A small sample of the second crop was recrystallized from EtOAc to give the analytically pure material, mp 104°-106°; [α] D 25 -0.5° (c, 1%, CHCl 3 ).
Anal. Calcd. for C 25 H 37 N 3 O 5 S: C, 61.08; H, 7.59; N, 8.55; S, 6.52. Found: C, 61.14; H, 7.74; N, 8.40; S, 6.41.
EXAMPLE 23
Method B--Condensation of the product of Example 6 and 1-[2-(4-hydroxyphenoxy)-ethyl]-4-phenylpiperazine
300 ml 4 N NaOH (1.2 mol) was added to a stirred mixture of 362 (0.99 mol) (S)-1-tosyloxy-2-hydroxy-3-N-mesylisopropylaminopropane and 298.4 g (1 mol) 1-[2-(4-hydroxyphenoxy)ethyl]-4-phenylpiperazine in 2.4 l DMSO and the reaction was heated at 95°-100° for 12 hrs. The cooled mixture was diluted with 1 l 1 N NaOH and 7 l H 2 O and was extracted using benzene (1×12 l; 1×2). The organic extracts were washed in turn with water (2×2 l) and then were dried (K 2 CO 3 ) and evaporated to dryness. A solution of the residue in hot EtOAc was charcoaled and, after concentration to ˜2.5 l was stored at 0°-5° overnight to give the end product of Example 22. The mother liquors were concentrated to ˜500 ml and diluted with 500 ml hexane which yielded additional product. The two crops were combined and recrystallized from acetone-hexane to give essentially pure material, mp 95°-100°.
EXAMPLE 24
(S)-1-(4-Benzyloxyphenoxy)-3-benzyloxy-2-propanol
4.5 g (0.04 mol) KOC(CH 3 ) 3 was added to a solution of 66.3 g (0.404 mol) (S)-1,2-epoxy-3-benzyloxypropane and 97.0 g (0.484 mol) p-benzyloxyphenol in 240 ml MeOH and the mixture was heated overnight at reflux. The reaction was cooled and then was diluted with the slow addition of 1 l 1 N NaOH. The resulting solids were recovered by filtration and were washed with 0.5 N NaOH and with water and air dried. The material was dissolved in 800 ml CH 2 Cl 2 and the solution was washed with H 2 O (3×150 ml). The water layers were backwashed in turn with 200 ml CH 2 Cl 2 and concentration of the combined, dried (Na 2 SO 4 ) CH 2 Cl 2 layers gave essentially pure product.
A small sample was crystallized from CH 2 Cl 2 -hexane (2×) to give the analytically pure material, mp 62°-63.5°; [α] D 25 +4.4° (c, 1.0, MeOH).
Anal. Calcd. for C 23 H 24 O 4 : C, 75.80; H, 6.64. Found: C, 75.82; H, 6.60.
EXAMPLE 25
(S)-3-(4-Hydroxyphenoxy)-1,2-propanediol
A solution of 138 g (0.378 mol) (S)-1-(4-benzyloxyphenoxy)-3-benzyloxy-2-propanol in 1.7 liters HOAc containing 36 ml concentrated HCl was hydrogenated over 14 g 10% Pd/C at normal temp and pressure. The uptake of hydrogen essentially stopped after 70 min (˜17.7 liters H 2 used). The catalyst was removed by filtration through Celite and concentration of the filtrate to dryness gave an oil which was then dissolved in 800 ml 0.5 N methanolic HCl and left at room temp overnight to hydrolyze the acetates which had been formed during the hydrogenation. The reaction was concentrated to dryness and the residue was evaporated several times from CH 2 Cl 2 to eliminate residual HCl. Trituration of the resulting solid with ether furnished the essentially pure end product.
0.5 g was crystallized from MeOH-CHCl 3 to give the analytically pure material, mp 149.5°-151°; [α] D 25 +8.01° (c, 1.0, MeOH).
Anal. Calcd. For C 9 H 12 O 4 : C, 58.69; H, 6.57. Found: C, 58.43; H, 6.73.
EXAMPLE 26
(R)-1-(4-Hydroxyphenoxy)-3-chloro-2-propanol
A stirred mixture of 62.15 g (0.337 mol) (S)-3-(4-hydroxyphenoxy)-1,2-propanediol (0.025 mol) and benzoic acid in 60 g trimethylorthoacetate was heated in an oil bath at 80°. Methanol was distilled from the system as it was formed. After 30 minutes the reaction mixture was cooled and partitioned between 750 ml benzene and 250 ml saturated NaHCO 3 solution. The benzene layer was washed with another 250 ml portion of NaHCO 3 solution and then the aqueous layers were backwashed with 250 ml benzene. The combined organic contracts were dried (Na 2 SO 4 ) and evaporated in vacuo to give the cyclic orthoacetate as an oil. The total crude material was then dissolved in 400 ml dry CH 2 Cl 2 and treated with 65 ml trimethylchlorosilane. After being heated at reflux for 30 minutes, the solution was concentrated to dryness under reduced pressure. The residue was evaporated from toluene to remove excess reagent to give crude (R)-3-(4-hydroxyphenoxy)-2-acetoxy- 1-chloropropane as an oil. The acetate was hydrolyzed by heating a solution of the crude product in 250 ml 0.5 N methanolic HCl at 55° for 30 min. The solvent was concentrated in vacuo and the residue was diluted with water and was extracted with EtOAc to give the crude chlorohydrin. The crude material was dissolved in 120 ml CH 2 Cl 2 and placed on a column of silica gel (800 g made up in CH 2 Cl 2 ). Three liters of CH 2 Cl 2 eluent were collected and discarded and the product was eluted using 3 liters of CH 2 Cl 2 -EtOAc (1:1) to give after evaporation of the solvent, the end product as an oil.
EXAMPLE 27
(S)-1,2-Epoxy-3-[4-(2-(4-phenyl-1-piperazinyl)ethoxy)phenoxy]propane
29.5 ml 4 N NaOH (0.118 mol) was added at a rapid dropwise rate to a stirring solution of 12 g (59 mmol) (R)-1-(4-hydroxyphenoxy)-3-chloro-2-propanol in 210 ml DMSO. During the addition the temp of the reaction was maintained <25° by means of a cooling bath. After the reaction had stirred at ˜20° for 10 min, 12.6 g (56.3 mmol) 1-(2-chloroethyl)-4-phenylpiperazine was added in one portion and the mixture was heated at 40° for 21/2 hr (after 20 min, a solid material began to crystallize from solution). The mixture was cooled and diluted with 30 ml H 2 O. The crystalline precipitate was collected by filtration and was washed with 100 ml DMSO-H 2 O (3:1) and with water. After air drying, the solids were dissolved in benzene (600 ml) and washed with H 2 O (3×150 ml). The aqueous layers were backwashed with benzene (1×200 ml). The combined benzene extracts were dried (K 2 CO 3 ) and evaporated to give the end product as a white solid.
A small sample from a previous run was filtered through a short silica gel column and crystallized from acetone to give the analytically pure material, mp 118°-119.5°; [α] D 25 -10.1° (c, 1.0, MeOH).
Anal. Calcd. for C 21 H 26 N 2 O 3 : C, 71.16; H, 7.39; N, 7.90. Found: C, 71.19; H, 7.28; N, 7.92.
EXAMPLE 28
(S)-1-(4-Benzyloxyphenoxy)-2-hydroxy-3-isopropylaminopropane
Under a flow of argon 318 ml of 70% Red-al solution was added over 15 min to a stirred solution of 86.5 g of (S)-1-(4-benzyloxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane in 800 ml dry benzene. After the addition was complete, the mixture was refluxed with stirring for 3 hours. The reaction was cooled using an ice-water bath and 30 ml 1 N NaOH was added dropwise to destroy excess hydride, followed by 800 ml 2 N NaOH. The phases were separated and the organic layer was washed in 1 N NaOH and with water. The aqueous phase and washings were back extracted with benzene (1×500 ml). The combined benzene extracts were dried (anhydr. K 2 CO 3 ) and evaporated to give a solid. The crude material was dissolved in 1500 ml ether and the solution was concentrated to ˜750 ml. The resulting crystalline amine was filtered off to give pure material, mp 93°-95°; [α] D 25 -6.26° (c, 1.0, CHCl 3 ).
Concentration of the mother liquors gave two additional crops of product: Crop #2, mp, 91°-93° and Crop #3, mp, 89°-93°.
Anal. Calcd. for C 19 H 25 NO 3 : C, 72.35; H, 7.99; N, 4.44. Found: C, 72.38; H, 8.16; N, 4.43.
EXAMPLE 29
(S)-1-(4-Hydroxyphenoxy)-2-hydroxy-3-isopropylaminopropane
Method A--From (S)-1-(4-benzyloxyphenoxy)-2-hydroxy-3-isopropylaminopropane
A slurry of 5.4 g 10% Pd/C in 50 ml benzene was added to a solution of 54.1 g of the amine in 600 ml MeOH. The attempted hydrogenolysis of this mixture resulted in very slow uptake of hydrogen due to catalyst poisoning by minor sulfur containing impurities in the amine. The poisoned catalyst was replaced by 5.4 g fresh Pd/C and then 4.2 liters of H 2 was taken up within 40 minutes. The catalyst was removed by filtration and the filtrate was concentrated in vacuo. Crystallization of the residue from acetone furnished the phenol amine, mp 125°-127°; [α] 25 D -22.1° (C, 1.0, 0.1 N HCl). The analytically pure sample, mp 125°-127°, was crystallized from acetone.
Anal. Calcd. for C 12 H 19 NO 3 : C, 63.97; H, 8.50; N, 6.22. Found: C, 63.81; H, 8.68; N, 6.40.
EXAMPLE 30
Method B--From (R)-1-(4-Hydroxyphenoxy)-3-chloro-2-propanol to produce the end product of Example 29
A solution of 50 g (0.247 mol) (R)-1-(4-hydroxyphenoxy-3-chloro-2-propanol in 300 ml methanol containing 100 ml isopropylamine was refluxed overnight. The solvent was removed in vacuo and the residue was evaporated twice from methanol to eliminate remaining isopropylamine. The crude was dissolved in 250 ml 1 N HCl and the solution was extracted with ether (2×) to remove non-basic impurities. The aqueous layer was chilled in an icewater bath and was treated with 13.5 g Na 2 CO 3 (0.255 equiv.). After 5 min the phenolamine began to crystallize from solution. The mixture was stirred in the ice-water bath for 30 min and then was stored at 0° for 1 hr. The product was collected by filtration and was washed with water to give the phenolamine, mp 124°-126°. 60 g of NaCl was added to the combined filtrate and washings and the resulting solution was extracted with 6×200 ml portions of EtOAc. The extracts were dried (K 2 CO 3 ) and evaporated to give an additional amount of phenolamine.
Crystallization of the total product from acetone (charcoal) furnished pure phenol mp 124°-126°; [α] D 25 -22.0° (c, 1.0, 0.1 N HCl).
EXAMPLE 31
(S)-1-[2-(4-(2-Hydroxy-3-(1-methylethyl)amino)propoxy)phenoxy)ethyl]-4-phenylpiperazine and its bis-maleate salt
Method A
A solution of 15.35 g (42.5 mmol) of (S)-4-(2-hydroxy-3-N-mesylisopropylaminopropoxy)phenoxyacetic acid in 170 ml of dry tetrahydrofuran was cooled (0°). To this solution (argon atmosphere) was added 5.16 g (51 mmol) of triethylamine followed by the dropwise addition of 4.61 g (42.5 mmol) of ethyl chloroformate. The reaction mixture was allowed to stir at 0° for one hr and was then filtered from the resulting precipitate. The filtrate was then treated with 10.35 g (63.8 mmol) of N-phenylpiperazine and the reaction mixture was allowed to stir under argon for 90 min at room temp. The solvent was then evaporated in vacuo and the residue was dissolved in methylene chloride and treated with 100 ml of 5 N HCl solution. The aqueous layer was extracted twice with methylene chloride. The organic layers were then washed twice with 5 N HCl solution and once with 5% NaHCO 3 solution. The combined organic layers were dried (Na 2 SO 4 ) and evaporated to give an oil which was dissolved in benzene and chromatographed on silica gel (400 g). The column was eluted with benzene-ethyl acetate mixtures, the product being eluted with benzene-ethyl acetate (3:1) and pure ethyl acetate. Evaporation of these solvent fractions yielded the intermediate amide 1-[(S)-4-(2-hydroxy-3-N-mesylisopropylaminopropoxy)phenoxyacetyl]-4-phenylpiperazine as an oil.
To a portion of this material (18 g, 35.7 mmol) in 600 ml of dry benzene was added dropwise (over 25 min) 113 ml of 70% sodium bis(2-methoxyethoxy)-aluminum hydride in benzene (Red-al). The reaction mixture was heated under reflux for 30 min and was then cooled and treated dropwise with 120 ml of 1 N NaOH solution followed by 1 l of H 2 O. The resulting mixture was extracted twice with 1500 ml of benzene and the organic layers were washed twice with water. The dried (Na 2 SO 4 ) organic layers were concentrated in vacuo to give a colorless solid, mp 88°-95°. Crystallization from methylene chloride-ether gave the end product, mp 99°-102°. Further crystallization from the same solvent system gave the analytical sample, mp 102°-104°; [α] D 25 -0.3° (c, 1.0, CH 3 OH).
Anal. Calcd. for C 24 H 35 N 3 O 3 : C, 69.70; H, 8.53; N, 10.16. Found: C, 69.73; H, 8.65; N, 10.00.
Method B--From (S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-isopropylaminopropane
18.75 ml 4 N NaOH (75 mmol) was added to a solution of 16.0 g (71.4 mmol) 1-(2-chloroethyl)-4-phenylpiperazine and 16.8 g (75 mmol) 1-(4-hydroxyphenoxy)-2-hydroxy-3-isopropylaminopropane, 150 ml DMSO and the mixture was stirred at 60° for 3 hours. 100 ml 1 N NaOH was added slowly to the cooled solution followed by 100 ml H 2 O and the resulting solid was recovered by filtration and was washed well with water. The crude solid was dissolved in CH 2 Cl 2 (600 ml) and the solution was dried (K 2 CO 3 ) and evaporated to give the crude product. The material was dissolved in 400 ml hot EtOAc and diluted with 400 ml hexane and was stored overnight 0°-5°. The resulting solid was collected by filtration and was washed with 200 ml EtOAc-hexane (1:1) to give the end product, mp 102° -104°.
23.3 g (56.4 mmol) of the amine was added to a hot solution of maleic acid (13.34 g; 115 mmol) in 300 ml MeOH. Hot EtOAc was added portionwise to the refluxing solution such that the volume remained at ˜500 ml until the salt began to crystallize from the solution. The mixture was cooled and the bis-maleate salt, mp 151°-153° was recovered by filtration.
Recrystallization from the same solvent raised the melting point to 153°-154°; [α] D 25 -10.8° (c, 1.0, MeOH).
Anal. Calcd. for C 24 H 35 N 3 O 3 2C 4 H 4 O 4 : C, 59.52; H, 6.71; N, 6.51. Found: C, 59.59; H, 6.55; N, 6.56.
Method C--From (S)-1-[2-(4-(2,3-epoxypropoxy)phenoxy)ethyl]-4-phenylpiperazine
A solution of 7.8 g (22 mmol) (S)-1-[2-(4-(2,3-epoxypropoxy)phenoxy)ethyl]-4-phenylpiperazine in 80 ml MeOH containing 20 ml isopropylamine was heated at 75° for 2 hr. The solvent was removed in vacuo and the residue was dissolved in 100 ml MeOH containing 5.1 g (44 mmol) maleic acid. The slightly hazy solution was filtered through Celite and then was concentrated to ˜60 ml, whereupon hot EtOAc was added until crystallization began. The resulting salt was recovered by filtration and washed with EtOAc to give the bis-maleate salt, mp 150°-151.5°.
Method D--From (S)-1-[2-(4-(2-hydroxy-3-N-mesylisopropylaminopropoxy)phenyl)ethyl]-4-phenylpiperazine
In an inert atmosphere, 82 ml Red-al (70% solution in benzene) was added dropwise to a stirred solution of 19.2 g (39 mmol) (S)-1-[2-(4-(2-hydroxy-3-N-mesylisopropylaminopropoxy)phenoxy)-ethyl]-4-phenylpiperazine in 100 ml benzene. After heating at reflux for 31/2 hr, the mixture was cooled in an ice-water bath and excess reagent was destroyed by the cautious dropwise addition of H 2 O. The mixture was then diluted with 2 N NaOH and CH 2 Cl 2 which resulted in the precipitation of some insoluble inorganic solids. The solids were removed by filtration through Celite and the filtrate was extracted with CH 2 Cl 2 (3×). The organic layers were washed in turn with 2 N NaOH solution (2×) and brine (1×) and then were combined, dried (K 2 CO 3 ) and evaporated to give the amine as a crystalline solid. A solution of the solids in 125 ml hot EtOAc was diluted with warm hexane (125 ml) and the product was allowed to crystallize slowly from solution. Filtration yield the amine, mp 100°-104°.
13.9 g (33.6 mmol) of the pure amine was added to a hot solution of 7.96 g (68.6 mmol) maleic acid in 100 ml MeOH. Hot EtOAc was added in portions to the refluxing solution until crystallization of the salt began. After cooling, the mixture was filtered to give the bis-maleate salt, mp 152°-154°.
EXAMPLE 32
(S)-1-[2-(4-(2-Hydroxy-3-tert-butylaminopropoxy)-phenoxy)ethyl]-4-phenylpiperazine and its bis-maleate salt
A solution of 7.8 g (22 mmol) of (S)-1-[2-(4-(2,3-epoxypropoxy)phenoxy)ethyl]-4-phenylpiperazine in 80 ml MeOH containing 25 ml tert-butylamine. The solvent was removed under reduced pressure to give an oily residue which crystallized on standing. The crude amine was dissolved in 60 ml hot MeOH containing 5.1 g (44 mmol) maleic acid. Almost immediately a crystalline solid began to form. The mixture was cooled and filtered to yield the bis-maleate, mp 180°-182°. A second crop, mp 172°-175° recovered from the mother liquors, was recrystallized from MeOH to give the salt, mp 179°-181°.
The first crop was recrystallized from MeOH to give the analytically pure salt, mp 182°-184°; [α] D 25 -6.03° (c, 0.58, H 2 O).
Anal. Calcd. for C 25 H 37 N 3 O 3 .2C 4 H 4 O 4 : C, 60.01; H, 6.88; H, 6.37. Found: C, 60.05; H, 6.97; N, 6.32.
1.3 g of the second crop bis-maleate salt from above was dissolved in 60 ml warm H 2 O and basified with 5 ml 2 N NaOH. The resulting solid was recovered by filtration, washed with water and dissolved in CH 2 Cl 2 . The CH 2 Cl 2 solution was dried (K 2 CO 3 ) and evaporated to give the free amine as a white solid. Crystallization from EtOAc furnished the pure base as a monohydrate, mp 82°-84°.
Anal. Calcd. for C 25 H 37 N 3 O 3 .H 2 O: C, 67.39; H, 8.82; N, 9.43; H 2 O, 4.21. Found: C, 67.22; H, 8.65; N. 9.13; H 2 O, 4.02.
EXAMPLE 33
(S)-1-[2-(4-(2-Hydroxy-3-isopropylaminopropoxy)phenoxy)ethyl]-4-(2-methoxyphenyl)piperazine and its bis-maleate salt
9.33 g 4 N NaOH (37.3 mmol) was added to a solution of 8.4 g (37.3 mmol) (S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-isopropylaminopropane and 9.0 g (35.4 mmol) 1-(2-chloroethyl)-4-(2-methoxyphenyl)piperazine in 75 ml DMSO and the mixture was heated at 60° for 90 min. After cooling, the mixture was diluted with 200 ml 0.5 N NaOH and extracted using benzene (3×200 ml). The organic extracts were washed in turn with H 2 O (2×100 ml) and then were combined, dried (K 2 CO 3 ) and evaporated.
8.6 g (74 mmol) of maleic acid was added to a solution of the residue in 40 ml MeOH and EtOAc was added to the cloud point. The compound did not crystallize and thus the solvents were removed in vacuo. The crude salt was redissolved in EtOH (40 ml) and EtOAc was again added just to the cloud point. The resulting crude solid was recrystallized from EtOH-EtOAc to give essentially pure product as its bis-maleate salt, mp 105°-110°. The analytically pure salt [mp 115°-117°; [α] D 25 -10.4° (c, 1.0, MeOH] was obtained from the same solvents.
Anal. Calcd. for C 25 H 37 N 3 O 4 .2C 4 H 4 O 4 : C, 58.66; H, 6.71; N, 6.22. Found: C, 58.52; H, 6.77; N, 6.50.
0.7 g of the bis-maleate salt was dissolved in 5 ml H 2 O and basified with 3 ml 1 N NaOH. The resulting crude free base was filtered off and dried. Crystallization from ether afforded the analytically pure material, mp 89°-90.5°.
Anal. Calcd. for C 25 H 37 N 3 O 4 : C, 67.69; H, 8.41; N, 9.47. Found: C, 67.97; H, 8.56; N, 9.42.
EXAMPLE 34
1-(2-Bromoethoxy)-4-(2-propenyloxy)benzene
To a solution of 45.0 g of 4-(2-bromoethoxy)-phenol (0.207 mol) in 310 ml of acetone was added 54 ml of allyl bromide (0.619 mol) and 45.0 g of anhydrous potassium carbonate (0.326 mol). The reaction mixture was stirred under reflux for eleven hours and was cooled and poured into 2500 ml of water. The mixture was extracted twice with 3:1 ether:methylene-chloride, and the organic layers were washed twice with 1 N NaOH, once with H 2 O, dried (Na 2 SO 4 ) and concentrated to dryness under reduced pressure to yield a colorless oil. The analytical sample was prepared by crystallization from hexane to give colorless crystals, mp 27°-28°.
Anal. Calcd. for C 11 H 13 BrO 2 : C, 51.38; H, 5.10; Br, 31.08. Found: C, 51.63; H, 5.27; Br, 31.22.
EXAMPLE 35
(R,S)-1-(2-Bromoethoxy)-4-(2,3-epoxypropoxy)benzene
To a solution of 48.0 g of 1-(2-bromoethoxy)-4-(2-propenyloxy)benzene (0.186 mol) in 960 ml of acetone and 125 ml of water was added 2.0 ml of 70% perchloric acid. To this stirred reaction mixture was added portionwise over a 12 min period 38.4 g (0.278 mol) of N-bromoacetamide. The stirred reaction mixture was maintained at 22° for 21/2 hr and was then treated with solid NaHSO 3 until a negative starch-KI reaction was achieved. The acetone was next removed in vacuo, and the residue was diluted with 1 of water. The mixture was extracted twice with methylene chloride and the organic layers were washed with water, dried (Na 2 SO 4 ) and concentrated to dryness under reduced pressure to yield the bromohydrin intermediate as a red oil.
The crude oil was redissolved in 1300 ml methanol and treated with 375.0 ml of 1 N NaOH. The reaction mixture was allowed to stand for two hours at room temperature under argon at which time the methanol was removed in vacuo and the residue was diluted with 1 l of water. The resulting precipitate was filtered and washed well with water. It was then redissolved in methylene chloride, dried (Na 2 SO 4 ), and concentrated to dryness under reduced pressure to yield a pale yellow solid. The crude solid was chromatographed on a column of Florisil using 1:1 C 6 H 6 --CH 2 Cl 2 as eluent. The eluted fractions were combined and concentrated to dryness to yield a yellow solid, mp 50°-61.5°. The solid was then rechromatographed through a column of Florisil in benzene and eluted again with 1:1 C 6 H 6 --CH 2 Cl 2 to yield a colorless solid, mp 56°-62°. Crystallization from ether:hexane yielded the end product as colorless crystals, mp 59°-62°. A second crop from the mother liquors yielded product, mp 58.5°-61.5°. Crystallization from ether:hexane gave the analytical sample, mp 62°-64°.
Anal. Calcd. for C 11 H 13 BrO 3 : C, 48.37; H, 4.80; Br, 29.26. Found: C, 48.40; H, 4.86; Br, 29.32.
EXAMPLE 36
(R,S)-1-(2-Bromoethoxy)-4-[2-hydroxy-3-isopropylaminopropoxy]benzene
To a stirred suspension of 15.0 g of (R,S)-1-(2-bromoethoxy)-4-(2,3-epoxypropoxy)benzene (0.055 mol) in 150 ml of methanol was added 10.2 ml of isopropylamine (0.122 mol). The reaction mixture was stirred and heated in an argon atmosphere at 55° for 3 hours and was then cooled to room temperature. The solvent was removed in vacuo to yield a pale yellow oil which crystallized on standing. The product was crystallized twice from methylene chloride-hexane to afford the end product as colorless crystals, mp 83°-87.5°.
Crystallization from methylene chloride-hexane gave the analytical sample, mp 87°-89.5°.
Anal. Calcd. for C 14 H 22 BrNO 3 : C, 50.61; H, 6.67; N, 24.05; Br, 4.22. Found: C, 50.50; H, 6.71; N, 24.05; Br, 4.09.
EXAMPLE 37
(R,S)-1-(4-Benzyloxyphenoxy)-2-hydroxy-3-isopropylaminopropane
To a solution of 200 g (1 mol) p-benzyloxyphenol in 2.5 DMSO was added 375 ml 4 N NaOH followed by 216 ml of epichlorohydrin and the resulting mixture was stirred at room temp for 3 hr. The reaction was poured into 6 l of an ice-water mixture and extracted with CH 2 Cl 2 (3×1 l). The organic extracts were washed in turn with H 2 O (3×500 ml), and then were combined, dried (Na 2 SO 4 ) and evaporated to dryness. The resulting crude solid was crystallized from ether to give (R,S)-1-[4-benzyloxyphenoxy)-2,3-epoxypropane in two crops. A solution of 135 g (0.527 mol) of the above epoxide in 1 l MeOH containing 135 ml isopropylamine was refluxed for 90 minutes. The solvents were then removed under reduced pressure and the residual solid was triturated with ether to give the end product amine, mp 99°-100°. A second crop, mp 98°-100° , was obtained by concentration of the ether extracts.
A small sample (1 g) of the second crop was recrystallized from ether to give the analytical sample, mp 100°-101°.
Anal. Calcd. for C 19 H 25 NO 3 : C, 72.35; H, 7.99; N, 4.44. Found: C, 72.42; H, 7.99; N, 4.41.
EXAMPLE 38
(R,S)-1 (4-Hydroxyphenoxy)-2-hydroxy-3-isopropylaminepropane
(R,S)-1-(4 Benzyloxyphenoxy)-2-hydroxy-3-isopropylaminopropane (124 g) in MeOH (1 l) containing 5 g 10% Pd/C was hydrogenated (21°; atmospheric pressure). The uptake of H 2 (total 9.6 l) essentially stopped after 1 hr. The catalyst was removed by filtration (Celite) and the filtrate was concentrated to dryness in vacuo. The resulting solid residue was crystallized from ethanol to give the end product, mp 158°-159°. A second crop of product was obtained by concentration of the mother liquor.
Anal. Calcd. for C 12 H 19 NO 3 : C, 63.98; H, 8.50; N, 6.22. Found: C, 64.03; H, 8.62; N, 6.09.
EXAMPLE 39
(R,S)-1-[2-(4-(2-Hydroxy-3-(isopropylaminopropoxy)phenoxy)ethyl]-4-phenylpiperazine and its bis-maleate salt
Method A--From the product of Example 36
A stirred mixture of 9.0 g of (R,S)-1-2-bromoethoxy)-4-[2-hydroxy-3-isopropylaminopropoxy]benzene (0.027 mol) and 9.0 g (0.055 mol) of N-phenylpiperazine in 135 ml of ethanol was refluxed under argon for seven hours. The reaction mixture was then cooled to room temp and the solvent was removed in vacuo. The residue was dissolved in benzene and washed twice with 1 N NaOH solution and once with water. The dried (Na 2 SO 4 ) organic layer was concentrated to dryness under reduced pressure to yield a crude solid which was crystallized twice from ether:hexane to yield the end product base as colorless crystals, mp 182.5°-186.5°. Crystallization from methylene chloride-ether gave the analytical sample, mp 87°-89.5°.
Anal. Calcd. for C 24 H 35 N 3 O 3 : C, 69.70; H, 8.53; N, 10.16. Found: C, 69.57; H, 8.45; N, 10.02.
A solution of 7.70 g (18.6 mmol) of the free base in 150 ml of absolute ethanol was treated with a solution of 5.10 g (43.9 mmol) of maleic acid in 80 ml of absolute ethanol. The reaction mixture was heated on the steam bath for two minutes and was then allowed to cool slowly to room temp. The solvent was removed in vacuo to yield a pale yellow solid which was crystallized twice from methanol-ethyl acetate to yield the bis-maleate salt as pale yellow crystals, mp 141.5°-144°. Crystallization from methanolethyl acetate gave the analytical sample as colorless crystals, mp 142°-144°.
Anal. Calcd. for C 32 H 43 N 3 O 11 : C, 59.52; H, 6.71; N, 6.51. Found: C, 59.56; H, 6.94; N, 6.53.
EXAMPLE 40
The end product of Example 39
Method B--From the end product of Example 38
To a stirred mixture of (R,S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-isopropylaminopropane (4.5 g; 20 mmol) and 1-(2-chloroethyl)-4-phenylpiperazine (4.6 g; 20.5 mmol) in 35 ml DMSO was added 5.0 ml 4 N NaOH (20 mmol). After stirring 3 hrs at 60° C., the reaction mixture was cooled and partitioned between CH 2 Cl 2 and dilute NaOH solution. The layers were separated and the aqueous layer was re-extracted with CH 2 Cl 2 (2×). The organic layers were then washed in turn with H 2 O (2×) and were combined, dried (K 2 CO 3 ) and evaporated in vacuo.
The crude free base thus obtained was dissolved in 75 ml MeOH containing 4.6 g (40 mmol) maleic acid and EtOAc was added portionwise to the boiling solution to the cloud point. After the solution was chilled, the resulting solid was recovered by filtration to give the bis-maleate salt. Recrystallization from MeOH-EtOAc furnished the pure salt, mp 143.5°-144°.
EXAMPLE 41
(S)-1-[6-(4-(2-Hydroxy-3-isopropylaminopropoxy)-phenoxy)hexyl]-4-piperazine
A solution of 25 g (0.128 mol) of 6-bromohexanoic acid and 12.7 g (0.125 mol) of triethylamine in 150 ml of ether was cooled (0°) and treated dropwise with 28.5 g (0.263 mol) of ethyl chloroformate. The reaction mixture was stirred for 1 hr and then filtered. To the cooled (0°) filtrate was added a solution of 21 g (0.129 mol) of N-phenylpiperazine in 50 ml of ether. The reaction mixture was then allowed to warm to room temperature for 30 min and was then washed once with 1 N NaOH solution and once with water. The dried (Na 2 SO 4 ) organic layers were concentrated in vacuo to give a yellow oil which was dissolved in benzene and chromatographed on silica gel (500 g). The column was eluted with benzeneethyl acetate mixtures, the product appearing in the benzeneethyl acetate (8.5:1.5) mixtures. Evaporation of those combined mixtures gave 1-(6-bromohexanoyl)-4-phenylpiperazine.
This material (4.55 g, 13.2 mmol) was added to a solution of 4.0 g (13.2 mmol) of (S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane in 30 ml of dimethylsulfoxide. To this stirred solution was added 3.33 ml of 4 N NaOH solution and the reaction mixture was heated at 70° for 30 min. It was then cooled, diluted with water and extracted three times with ethyl acetate. The organic layers were washed once in 1 N NaOH solution, twice with water, dried (Na 2 SO 4 ) and evaporated to give the intermediate condensation product as an oil.
To this material (7.4 g, 13.2 mmol) in 62 ml of dry benzene was added dropwise 42 ml of 70% sodium bis(2-methoxyethoxy)-aluminum hydride in benzene (Red-al). The reaction mixture was refluxed for 80 min and was then cooled and treated with 40 ml of 2 N NaOH solution followed by 100 ml of H 2 O. The mixture was extracted three times with benzene and the organic layers were washed twice with water, dried (Na 2 SO 4 ) and evaporated. The residue was crystallized from methylene chloride-ether to yield the end product (free base), mp 75°-76°. Crystallization from acetone-hexane gave the analytical sample, mp 78°-79°; [α] D 25 -3.52° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 28 H 43 N 3 O 3 : C, 71.61; H, 9.23; N, 8.95. Found: C, 71.69; H, 9.22; N, 8.79.
EXAMPLE 42
(S)-1-[6-[4-(2-Hydroxy-3-isopropylaminopropoxy)phenoxy]hexyl]-4-phenylpiperazine dihydrochloride
A solution of 4.265 g (9 mmol) of free base of Example 41 in 60 ml of ethanol was treated with 3.5 ml of 5.13 N ethanolic hydrogen chloride. The resulting solid was collected by filtration and washed with ethanol to give the end product, mp 183°-185°. Crystallization from ethanol gave the analytical sample, mp 183°-184°; [α] D 25 -11.4° (c, 0.5, CH 3 OH).
Anal. Calcd. for C 28 H 43 N 3 O 3 .2HCl: C, 61.98; H, 8.36; Cl, 13.07; N, 7.74. Found: C, 61.69; H, 8.30; Cl, 12.85; N, 7.61.
EXAMPLE 43
(S)-1-[11-(4-(2-Hydroxy-3-isopropylaminopropoxy)phenoxy)undecanyl]-4-phenylpiperazine
To a stirred solution of 13.26 g of 11-bromoundecanoic acid (50 mmol) in 75 ml of ether was added 6.95 ml (50 mmol) of triethylamine. The stirred solution was cooled to 0° and 4.80 ml of ethyl chloroformate (50 mmol) was added dropwise. The mixture was stirred for one hour at 0° and the resulting precipitate was filtered and washed with ether.
The filtrate was recooled to 0° and a solution of 8.10 g (50 mmol) of N-phenylpiperazine in 25.0 ml of ether was added with stirring. A precipitate formed and the ice bath was removed. Stirring was continued for an additional 25 minutes at room temp and the material was then collected by filtration and was washed well with ether to yield colorless crystals, mp 70°-74°. Crystallization from methylene chloride:ether gave 1-(11-bromoundecanoyl)-4-phenylpiperazine as colorless crystals, mp 73°-75.5°. Crystallization from methylene chloride-ether gave the analytical sample, mp 73.5°-75.5°.
Anal. Calcd. for C 21 H 33 BrN 2 O: C, 61.61; H, 8.13; N, 6.84; Br, 19.52. Found: C, 61.77; H, 8.14; N, 6.72; Br, 19.47.
To a stirred solution of 3.03 g (10 mmol) of (S)-1-(4-hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane and 4.09 g of 1-(11-bromoundecanoyl)-4-phenylpiperazine (10 mmol) in 20 ml of dimethylsulfoxide was added 3.0 ml (12 mmol) of 4 N NaOH solution. The reaction mixture was stirred and heated at 75°-78°, under argon for 35 minutes and was then cooled to room temperature and diluted with 100 ml of cold water. The mixture was extracted twice with ethyl acetate and the organic layers were washed once with 1 N NaOH, twice with water, and dried (Na 2 SO 4 ). The solvent was evaporated to dryness under reduced pressure to yield a colorless oil.
To a stirred solution of 6.50 g of this oil (10.4 mmol) in 55.0 ml benzene was added 36.6 ml of 70% sodium bis(2-methoxyethoxy)-aluminum hydride in benzene (Red-al). The reaction mixture stirred under reflux (argon atmosphere) for 21/4 hr, then cooled to room temp and treated with 35 ml of 2 N NaOH and 100 ml of water. The mixture was extracted twice with benzene and the organic layers were washed twice with water, dried (K 2 CO 3 ), and concentrated to dryness under reduced pressure to yield a colorless solid. The material was crystallized from acetone to yield the end product (free base) as colorless crystals, mp 99°-103°. Crystallization from acetone gave the analytical sample, mp 101.5°-104°; [α] D 25 -2.82° (c, 1.13, CHCl 3 ).
Anal. Calcd. for C 33 H 53 N 3 O 3 : C, 73.42; H, 9.90; N, 7.79. Found: C, 73.62; H, 9.91; N, 7.62.
EXAMPLE 44
(S)-1-[11-[4-(2-Hydroxy-3-isopropylaminopropoxy)phenoxyy]undecanyl]-4-phenylpiperazine dihydrochloride
To a warm (40°) solution of 2.83 g (5.2 mmol) of the free base of Example 43 in 95 ml of absolute ethanol was added at a rapid dropwise rate with swirling 2.03 ml (10.4 mmol) of 5.13 N ethanolic hydrogen chloride solution. The mixture was then cooled to 0° and the resulting colorless crystals were collected by filtration to yield the end product, mp 193°-196°. Crystallization from ethanol gave the analytical sample, mp 193.5°-196°; [α] D 25 -7.52° (c, 0.5, CH 3 OH).
Anal. Calcd. for C 33 H 53 N 3 O 3 .2HCl: C, 64.69; H, 9.05; N, 6.86; Cl, 11.57. Found C, 64.60; H, 9.10; N, 6.88; Cl, 11.37.
EXAMPLE 45
(S)-1-(2-Hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane
39.9 g (0.362 mol) of catechol was added to a solution of 14.5 NaOH (362 mmol) in 45 ml H 2 O and the mixture was stirred under argon. The pasty mixture was diluted with 100 ml of DMSO and after 10 min, a solution of 52.3 g (0.181 mol) of (S)-1-mesyloxy-2-hydroxy-3-N-mesylisopropylaminopropane in 100 ml of DMSO was added. The solution was stirred at 80° under argon for 21/2 hr and then it was cooled and diluted with 400 ml 1 N NaOH. The solution was extracted with CH 2 Cl 2 (3×250 ml) and the organic extracts were backwashed (1×) with dilute NaOH solution. The combined basic aqueous extracts were acidified using 70 ml concentrated HCl and extracted with CH 2 Cl 2 (2×500 ml). The organic extracts were then washed in turn with water (5×500 ml) and then were combined, dried (Na 2 SO 4 ) and evaporated to give the essentially pure monoalkylated end product as an oil.
EXAMPLE 46
(S)-1-[2-(3-Bromopropoxy)phenoxy]-2-hydroxy-3-N-mesylisopropylaminopropane
A mixture of 15 g (49.5 mmol) (S)-1-(2-hydroxy-phenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane, 30.6 g (˜150 mmol) 1,3-dibromopropane, and 10.6 g K 2 CO 3 in 60 ml acetone was stirred under reflux overnight. The reaction was diluted with water and extracted with CH 2 Cl 2 (4×). The CH 2 Cl 2 extracts were washed in turn with 1 N NaOH solution and then were combined, dried (Na 2 SO 4 ), and concentrated to dryness in vacuo to give 18.5 g of an oil. The oil was chromatographed on 200 g silica gel made up in hexane. The column was eluted successively with hexane, benzene, benzene-Et 2 O (19:1), benzene-Et 2 O (9:1) and benzene-Et 2 O (3:1). The fractions eluted with benzene-Et 2 O (9:1) and (3:1) were combined and evaporated to dryness to give chromatographically pure product, mp 95°-96°. Crystallization from EtOAc-hexane furnished the pure compound, mp 98°- 99°.
The analytical sample, mp 98°-100°; [α] D 25 -4.99° (c, 1.0, CHCl 3 ) was obtained from smaller experiment using the same solvent system.
Anal. Calcd. for C 16 H 26 BrNO 5 S: C, 45.29; H, 6.18; N, 3.30; S, 7.56; Br, 18.83. Found: C, 14.80; H, 6.16; N, 3.30; S, 7.60; Br, 18.32.
EXAMPLE 47
(S)-1-[3-(2-(2-Hydroxy-3-N-mesylisopropylaminopropoxy)phenoxy)propyl]-4-phenylpiperazine
A mixture of 10.5 g (24.7 mmol) (S)-1-[2-(3-bromopropoxy)phenoxy]-2-hydroxy-3-N-mesylisopropylaminopropane and N-phenylpiperazine (4.42 g; 27.3 mmol) in 50 ml ethanol was left at room temperature for ˜3 days. Tlc showed the reaction to be ˜50% completed but the ratio of starting materials and product did not change after 4 hrs at reflux. 4.0 ml 4 N NaOH was added and the reaction heated for 2 hours, and than an additional 1.5 ml 4 N NaOH [total used=22 equiv (95% of theory)] was added. After another 60 min at reflux, the reaction was cooled and evaporated. The residue was diluted with water and extracted with EtOAc. The EtOAc extract was dried (K 2 CO 3 ) and evaporated to given an oil. The oil was chromatographed over 200 g silica gel. The column was eluted with benzene and benzene-EtOAc mixtures (19:1; 9:1; 3:1 and 1:1) and then the product was eluted from the column using ethyl acetate to give the end product. Crystallization from ether afforded product in two crops, (mp 84°-85° and 82°-84°).
Recrystallization of a small amount from ether (2×) furnished the analytically pure material, mp 85°-86°; [α] D 25 -1.0° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 26 H 39 N 3 O 5 S: C, 61.76; H, 7.77; N, 8.31; S, 6.34. Found: C, 61.92; H, 7.85; N, 8.26; S, 6.29.
EXAMPLE 48
(S)-1-[3-(2-(2-Hydroxy-3-N-mesylisopropylaminopropoxy)phenoxy)propyl]-4-phenylpiperazine and its dihydrochloride
22 ml Red-al (60% solution in benzene) was added dropwise at first and then, once the bubbling had ceased, more rapidly to a stirred solution of 6.2 g (12.25 mmol) (S)-1-[3-(2-(2-hydroxy-3-N-mesylisopropylaminopropoxy)phenoxy)propyl]-4-phenylpiperazine in 100 ml dry benzene. The reaction was refluxed for 5 hrs under argon and then it was left overnight at room temp. Excess reagent was decomposed by the dropwise addition of 25 ml 2 N NaOH and then it was diluted with water (25 ml). The benzene layer was separated and the aqueous layer was extracted with benzene (2×). The benzene layers were washed in turn with 2 N NaOH solution (1×) and brine (2×). The combined extracts were dried (K 2 CO 3 ) and evaporated under reduced pressure to give the crude amine. Crystallization from acetone-hexane gave solids in two crops, which when recrystallized from the same solvent system afforded the pure amine, mp 87°-88°.
Anal. Calcd. for C 25 H 37 N 3 O 3 : C, 70.23; H, 8.72; N, 9.83.
Found: C, 70.27; H, 8.74; N, 9.70.
3.5 g of the amine in 150 ml absolute EtOH was treated with 2.2 molar equivalents of ethereal HCl and then the solution was diluted to 400 ml with ether. The resulting crystalline solid was collected by filtration to give the dihydrochloride salt, mp 192°-193°.
The analytically pure material, mp 192°-193°; [α] D 25 -5.39° (c, 1.0, H 2 O) was obtained by recrystallization from EtOH.
Anal. Calcd. for C 25 H 37 N 3 O 3 .2HCl: C, 59.99; H, 7.85; N, 8.40; Cl, 14.17. Found: C, 60.20; H, 8.13; N, 8.25; Cl, 14.28.
EXAMPLE 49
(S)-1-[6-(2-(2-Hydroxy-3-N-mesylisopropylamino)propoxy)phenoxy)hexanoyl]-4-phenylpiperazine
8.0 ml 4 N NaOH (32 mmol) was added to a solution of 9.5 g (31.35 mmol) (S)-1-(2-hydroxyphenoxy)-2-hydroxy-3-N-mesylisopropylaminopropane and 10.9 (32 mmol) 1-(6-bromohexanoyl)-4-phenylpiperazine in 70 ml DMSO and the mixture was heated at 80° under argon for 50 min. The reaction was cooled and poured into 500 ml H 2 O and extracted with benzene (2×250 ml). The benzene extracts were washed in turn with 1 N NaOH (2×) and H 2 O (1×), and then were combined, dried (K 2 CO 3 ) and evaporated to give an oil. The oil was chromatographed on 200 g silica gel made up in benzene. The fractions eluted with EtOAc:benzene (1:1 and 3:2) were combined and evaporated to yield essentially pure product as an oil.
A small sample was purified for analysis by preparative tlc.
Anal. Calcd. for C 29 H 43 N 3 O 6 S: C, 62.01; H, 7.71; N, 7.48; S, 5.71. Found: C, 62.02; H, 7.98; N, 7.23; S, 5.46.
EXAMPLE 50
(S)-1-[6-(2-(2-Hydroxy-3-isopropylaminopropoxy)phenoxy)hexyl]-4-phenylpiperazine and its fumarate salt
In an inert atmosphere 70 ml Red-al (70% solution in benzene) was added cautiously at first and then more rapidly to a stirred solution of 11.4 g (20.28 mmol) (S)-1-[6-(2-(2-hydroxy-3-N-mesylisopropylaminopropoxy)phenoxy)hexanoyl]-4-phenylpiperazine in 100 ml dry benzene. The reaction was then heated and stirred under reflux for 90 minutes. 50 ml 2 N NaOH solution was then added carefully to the cooled reaction mixture, followed by 100 ml H 2 O and 300 ml benzene. The aqueous layer was separated and extracted with benzene (2×300 ml). The benzene layers were then backwashed in turn with water (2×100 ml). The pooled organic extracts were dried (K 2 CO 3 ) and concentrated to give an oil which solidified when it was evaporated in vacuo from acetone. The residue was crystallized from acetone-hexane to give the pure amine, mp 69°-71°. Recrystallization from acetone-hexane gave the analytical sample, mp 69°-71°; [α] D 25 +3.5° (c, 1.0, CHCl 3 ).
Anal. Calcd. for C 28 H 43 N 3 O 3 : C, 71.61; H, 9.23; N, 8.95. Found: C, 71.82; H, 9.38; N,8.80.
4.0 g (8.55 mmol) of the amine and 0.99 g (8.55 mmol) of fumaric acid were dissolved in 25 ml MeOH at room temp and then the solution was diluted with 50 ml EtOAc. The resulting fumarate salt which slowly crystallized from solution was collected by filtration and was washed with EtOAc to yield the salt, mp 163°-165°.
The analytically pure specimen of fumarate, mp 164°-165° was obtained by recrystallization from MeOH-EtOAc.
Anal. Calcd. for C 28 H 43 N 3 O 3 .C 4 H 4 O 4 : C, 65.62; H, 8.09; N, 7.17. Found: C, 65.36; H, 7.92; N, 7.12.
EXAMPLE 51
Bromohydrins from 4-allyloxyphenylacetic acid
A solution of 5.00 g (0.0260 mol) of 4-allyloxyphenylacetic acid in 25 ml of acetone and 8 ml of water was cooled in an ice bath and treated with 5.00 g (0.0362 mol) of N-bromosuccinimide (NBS). The resulting mixture was allowed to warm to room temperature slowly and after 2.5 hour, an additional 0.5 g. of NBS was added. After a total of 3.5 hour, the reaction mixture was diluted with 150 ml of water and a small amount of citric acid. The product was extracted with methylene chloride and after evaporation of the solvent, gave a crude solid. Recrystallization from ethyl acetate-hexane gave a mixture of bromohydrins containing the end-products, m.p. 85°-99°. Several crystallizations from ethyl acetate-hexane gave an analytically pure sample of one of the isomers, m.p. 128°-133°.
EXAMPLE 52
(R,S)-4-(2,3-Epoxypropoxy)phenylacetic acid
Method A
A solution of 1.66 g (5.74 mmol) of the mixture of bromohydrins obtained in Example 51 in 100 ml of methanol and 5 ml of 4 N sodium hydroxide solution was stirred at room temperature for 2 hours. The resulting mixture was diluted with 1 M citric acid to pH 3 and extracted with methylene chloride. Crystallization of the crude product from methanol-water gave the end-product. Recrystallization from methanol-ether gave the analytical sample, m.p. 73°-77°.
Anal. (C 11 H 12 O 4 ) C, H.
Method B
A solution of 2.00 (10.4 mmol) of 4-allyloxyphenylacetic acid and 1.6 g. of NBS in 10 ml. of acetone and 4 ml. of water was stirred 30 minutes at 0° and allowed to warm to room temperature. After an hour 0.2 g of NBS were added and after a total of 2.5 hour, the mixture was cooled in an ice bath and 5.5 ml of 4 N sodium hydroxide were added. The mixture was warmed to room temperature, stirred one hour, and diluted with water, ice, and 10% citric acid solution. The solution was extracted with methylene chloride and the methylene chloride layers afforded the product as an off-white solid, m.p. 72°-76°.
EXAMPLE 53
Methyl 4-allyloxyphenyl acetate
A mechanically stirred suspension of 101.54 g (0.528 mol) of 4-allyloxyphenylacetic acid, 70 ml (1.12 mol) of iodomethane, and 100 g (0.756 mol) of potassium carbonate in 210 ml. of hexamethylphosphoramide was left at room temperature overnight. The resulting mixture was diluted with 1 liter of ether and the ethereal solution was washed 3×300 ml water and 1×300 ml. saturated brine. The ethereal solution was concentrated and the product was distilled to give a colorless oil, b.p. 120°-135°/0.05 mm.
EXAMPLE 54
(R,S)-Methyl-4-(2,3-epoxypropyl)phenyl acetate
Method A
To an ice cold solution of 4.50 g (0.0216 mol) of the product of Example 52 in 20 ml of dry methanol was added an excess of ethereal diazomethane. Evaporation of the resulting solution to dryness gave the ester.
Method B
A solution of 25.25 g (0.122 mol) of the product of Example 53 and 62 g (0.359 mol) of m-chloroperbenzoic acid in 200 ml of methylene chloride was stirred at room temperature. After 24 hours the reaction mixture was poured into 200 ml. of water made basic with 45% NaOH. The aqueous layer was extracted 2×300 ml CH 2 Cl 2 and the combined organic layers were washed 2×200 ml. H 2 O and 1×200 ml. brine. The crude product was evaporatively distilled to give the end-product, b.p. 180°-185°/0.1 mm. A portion was purified by preparative layer chromatography and distilled.
Anal. (C 12 H 14 O 4 )C, H.
EXAMPLE 55
Methyl 4-(2-hydroxy-3-isopropylaminopropoxy)phenyl acetate
A solution of 55.29 g (0.249 mol) of the product of Example 54 and 27.0 ml (0.334 mol) of isopropylamine in 200 ml. of methanol was stirred overnight at room temperature. The mixture was concentrated and the residue was dissolved in excess 1 M citric acid. The aqueous solution was washed 3×100 ml. CH 2 Cl 2 and was made basic by addition of 45% NaOH followed by extraction with 4×100 ml CH 2 CL 2 . The combined extracts were washed with saturated brine and were dried (K 2 CO 3 ). Evaporation gave the end-product, m.p. 72°-74°. Recrystallization from ether-hexane gave the analytical sample, m.p. 72°-74°.
Anal. (C 15 H 23 NO 4 ) C, H, N.
EXAMPLE 56
6-(4-Phenyl-1-piperazinyl)hexamide
A suspension of 9.85 g (0.060 mol) of phenylpiperazine, 11.6 g (0.060 mol) of 6-bromohexamide, and 6.35 g (0.060 mol) of sodium carbonate in 90 ml of toluene was heated reflux overnight. On cooling, the mixture was filtered and the filtrate was washed with water. Evaporation and crystallization of the crude product from methylene chloride-hexane gave analytically pure product, m.p. 129°-130°.
Anal. (C 16 H 25 N 3 O) C, H, N.
EXAMPLE 57
11-(4-Phenyl-1-piperazinyl)undecamide
A suspension of 13.1 g (0.0795 mol) of phenylpiperazine, 20.86 g (0.0795 mol) of 11-bromoundecamide and 8.45 g (0.0795 mol) of sodium carbonate in 120 ml of toluene was heated to reflux overnight. On cooling the solid which separated was collected and triturated with water to give the end-product, m.p. 128°-129°. Two recrystallizations from ethanol-ethyl acetate-hexane gave the analytical sample, m.p. 129°-130°.
Anal. (C 12 H 37 N 3 O) C, H, N.
EXAMPLE 58
1-(6-Aminohexyl)-4-phenylpiperazine
A solution of 38.3 g (0.139 mol) of the product of Example 56 in 400 ml of THF was treated with 500 ml. of 1 M borane in THF. The solution was refluxed for 8 hours and was cooled in an ice bath as 42 ml. of 12 N hydrochloric acid was added carefully. The excess THF was evaporated, the aqueous solution was made basic with potassium carbonate and was extracted with CH 2 Cl 2 . Evaporation of the organic layers gave an oil which gave a single spot on silica gel TLC and was used in the next example without further purification. A portion was further characterized as its dihydrochloride salt which crystallized from ethanol, m.p. 251°-253°.
Anal. (C 16 H 27 N 3 .2HCL) C, H, N.
EXAMPLE 59
1-(11-Aminoundecyl)-4-phenylpiperazine
1-(11-aminoundecyl)-4-phenylpiperazine was prepared similarly starting with 11.2 g (0.0322 mol) of the product of Example 57 to give the end-product as an oil. The dihydrochloride salt crystallized from ethanol, m.p. 197°-202°.
Anal. (C 21 H 37 N 3 .2HCl) C, H; N, calcd. 10.39; fd 9.87.
EXAMPLE 60
4-[(2-Hydroxy-3-isopropylaminopropoxy)phenyl]-N-[2-(4-phenyl-1-piperazinyl)ethyl]acetamide dihydrochloride
An intimate mixture of 5.00 g (0.0178 mol) of the product of Example 55 and 4.00 g (0.0190 mol) of 1-(2-aminoethyl)-4-phenylpiperazine* was heated to a bath temperature of 140°-145° overnight. The resulting solid was triturated with etherbenzene to give a tan solid, m.p. 100°-106°. Conversion to the hydrochloride salt gave the dihydrochloride salt, m.p. 173°-177°. Two recrystallizations from ethanol-ethyl acetate gave the analytical sample, m.p. 178°-181°.
Anal. (C 26 H 38 N 4 O 3 .2HCl), C, H, N, Cl.
EXAMPLE 61
4-[(2-Hydroxy-3-isopropylaminopropoxy)phenyl]-N-[6-(4-phenyl-1-piperazinyl)hexyl]acetamide dihydrochloride
An intimate mixture of 10.0 g (0.0384 mol) of the product of Example 58 and 10.0 g (0.0355 mol) of the product of Example 55 was heated to a bath temperature of 140° overnight. The crude brown solid was dissolved in CH 2 Cl 2 . and ether was added to precipitate a waxy solid. This material was passed through 50 g of grade III basic alumina eluting with 1% methanol-ethyl acetate to give a colorless wax which displayed a single spot on TLC. For conversion to the hydrochloride salt, a total of 9.1 g of material obtained as above was divided into portions of 6 g and 3.1 g and the 6 g portion was treated with excess hydrochloric acid and evaporated to dryness under high vacuum. This oil was taken up in alcohol and the 3.1 g portion was added. The resulting solution was concentrated and the residue was crystallized from ethanol-ether to give the end-product, m.p. 124°-6° (decomp). The analytical sample was obtained from ethanol-ether, m.p. 123°-126° (decomp).
Anal. (C 30 H 46 N 4 O 3 .2HCl) C, H, N, Cl.
EXAMPLE 62
4-[(2-Hydroxy-3-(isopropylaminopropoxy)phenyl]-N-[11-(4-phenyl-1-piperazinyl)undecyl]acetamide and its dihydrochloride
An intimate mixture of 9.4 g (0.030 mol) of the product of Example 59 and 8.45 g (0.030 mol) of the product of Example 55 were heated overnight at a bath temperature of 140°. The resulting brown solid was crystallized from methylene chloride-ether to give the free base, m.p. 107°-109°. A second crop, m.p. 101°-105° was obtained from the filtrate. The two crops were combined and acidified with hydrochloric acid to give a solid which was recrystallized from isopropanol to give the salt, m.p. 146°-150°.
Anal. (C 35 H 56 N 4 O 3 .2HCl) C, H, N, Cl.
EXAMPLE 63
(S)-4-(Dihydroxypropyl)phenylacetic acid, methyl ester
Sodium (2.3 g; 0.1 mol) was dissolved in 500 ml anhydrous MeOH and to this was added a solution of 194.3 g (1.17 mol) 4-hydroxyphenylacetic acid, methyl ester in 250 ml MeOH followed by a solution of 167.3 g. (1.018 mol) (S)-1,2-epoxy-3-benzyloxypropane in 250 ml MeOH. The solution was stirred under reflux for 12 hours. The cooled solution was treated with 8.3 ml (0.1 mol) of concentrated HCl and the methanol was removed in vacuo. The crude product was dissolved in benzene and washed with 2×200 ml portions of cold 1 N NaOH solution and with H 2 O (1×300 ml). The aqueous layers were backwashed with benzene (2×500 ml). The combined organic layers were dried (Na 2 SO 4 ) and evaporated in vacuo to give crude (S)-4-(3-benzyloxy-2-hydroxypropoxy)phenyl acetic acid, methyl ester.
The crude ester was then dissolved in 1 liter acetic acid containing 20 ml concentrated HCl and the mixture was hydrogenated over 10 g 10% Pd/C at normal temperature and pressure. After ˜100 minutes the absorption of H 2 ceased abruptly (total uptake ˜23.3 liters). The catalyst was removed by filtration through Celite and the filtrate was evaporated to dryness under reduced pressure. Since the product had undergone partial acetylation during the hydrogenolysis, it was dissolved in 1 liter 1 N methanolic HCl and left at room temperature for 1 hour. Evaporation of the solvent furnished the diol product as a white solid.
Crystallization of a small sample from ether-hexane furnished the analytically pure material, m.p. 64°-66°; [α] D 25 +6.55° (c, 1.0, EtOH).
Anal. Calcd. for C 12 H 16 O 5 : C, 59.99; H, 6.71. Found: C, 60.14; H, 6.75.
EXAMPLE 64
(R)-4-(2-Acetoxy-3-chloropropoxy)phenylacetic acid methyl ester
A stirred mixture of 223.3 g (0.916 mol) (S)-4-(2-dihydroxypropoxy)phenylacetic acid, methyl ester, 3.0 benzoic acid (0.024 mol) and 165 g (1.375 mol) trimethylorthoacetate was heated in an oil bath at 80°. Methanol was distilled from the reaction as it was formed. After 30 minutes, the reaction was cooled and the product was partitioned between 1 liter CH 2 Cl 2 and 300 ml cold saturated NaHCO 3 solution. The organic extract was washed with an addtional 200 ml NaHCO 3 solution and then aqueous layers were backwashed with CH 2 Cl 2 (1×200 ml). The combined CH 2 Cl 2 extracts were dried and evaporated to give the cyclic orthoacetate.
Without further purification this material (0.895 mol) was dissolved in 750 ml dry CH 2 Cl 2 followed by the addition of 151 ml (1.16 mol) of trimethylchlorosilane. The resulting solution was heated at reflux for ˜45 minutes, whereupon the solvent and excess reagent was removed in vacuo to give the chloroacetate as an oil.
A small portion of the product (1 g) was purified for analysis by chromatography on silica gel to give 950 mg of pure material, [α] D 25 -23.86° (c, 1.0, MeOH).
Anal. Calcd. for C 14 H 17 ClO 5 : C, 55.91; H, 5.70; Cl, 11.79. Found: C, 55.90; H, 6.04; Cl, 11.50.
EXAMPLE 65
(R)-4-(2,3-Epoxypropoxy)phenylacetic acid
A cold solution of 63 g (1.575 mol) NaOH in 200 ml H 2 O was added with stirring over ˜15 minutes to a previously chilled solution (0°) of 135 g (0.45 mol) crude (R)-4-(2-acetoxy-3-chloropropoxy)phenylacetic acid, methyl ester in 500 ml MeOH. The reaction temperature did not exceed 10° during the addition, and was then maintained at 0°-5° for 50 minutes and 10°-15° for an additional 20 minutes. The reaction was then rechilled and acidified using a solution of 32 ml concentrated H 2 SO 4 (1.15 equiv) in 200 ml. H 2 O. Some MeOH (˜250 ml) was removed by concentration of the reaction mixture in vacuo (bath temperature ˜25°) and then the solution was extracted with benzene (4×1 liter). The benzene layers were washed in turn with brine (1×250 ml) and were combined, dried (Na 2 SO 4 ) and concentrated to 500 ml in vacuo. The benzene solution was warmed to ˜40° and diluted to the cloud point with warm hexane and then it was stored at 0° for several hours. The resulting crystalline material was collected by filtration to give the epoxy acid end product, m.p. 70°-72°; [α] D 25 +10.6° (c, 1.0, MeOH). Concentration of the mother liquors gave additional epoxy acid.
Anal. Calcd. for C 11 H 12 O 4 : C, 63.45; H, 5.81. Found: 63.27; H, 5.89.
EXAMPLE 66
(R)-4-(2,3-Epoxypropoxy)phenylacetic acid, cyanomethyl ester
20.8 g (0.1 mol) of (R)-4-(2,3-epoxypropoxy)phenylacetic acid was suspended in 30 ml chloroacetonitrile and cooled to ˜10° in an ice water bath. Triethylamine (16 ml) was added to the stirred mixture at a rapid dropwise rate. The cooling bath was removed and after 30 minutes the temperature had risen to 30°. The temperature was maintained at 25°-30° by the intermittent use of the cooling bath. After 90 minutes the reaction was partitioned between toluene and H 2 O. The organic phase was washed with saturated NaHCO 3 solution and with water and then the aqueous layers were backwashed with toluene. The toluene extracts were combined, dried (MgSO 4 ) and evaporated to give the cyanomethyl ester end product as an oil. This material was used without further purification.
EXAMPLE 67
(R)-4-(2,3-Epoxypropoxy)phenyl-N-[2-(4-phenyl-1-piperazinyl)ethyl]acetamide
A mixture of 10.7 g (52.1 mmol) 1-(2-aminoethyl)-4-phenylpiperazine and 13.5 g (54.6 mmol) (R)-4-(2,3-epoxypropoxy)phenylacetic acid, cyanomethyl ester in 125 dry THF was stirred at room temperature for 40 hours. The solvent was removed in vacuo and the residue was triturated with ether to give the crude amide as a white solid. The solid was dissolved in 35 ml. CH 2 Cl 2 and placed on a column of 170 g Woelm basic alumina (grade 3) made up in CHCl 2 . Elution with 1 liter CH 2 Cl 2 furnished essentially pure material. Crystallization from acetone afforded the end product, m.p. 124°-125°. A second crop, m.p. 121°-123° was obtained from the mother liquors.
The analytical sample had been obtained from a previous batch by recrystallization from MeOH-H 2 O to give pure material, m.p. 123°-124°; [α] D 25 +5.64° (c, 1.0, MeOH).
Anal. Calcd. for C 23 H 29 N 3 O 3 ; C, 69.85; H, 7.39; N, 10.62. Found: C, 69.62; H, 7.40; N, 10.51.
EXAMPLE 68
(R)-4-(2,3-Epoxypropoxy)phenyl-N-[6-(4-phenyl-1-piperazinyl)hexyl]acetamide
A mixture of 9.4 g (38 mmol) (R)-4-(2,3-epoxypropoxy)phenylacetic acid, cyanomethyl ester and 9.4 g (36 mmol) 1-(6-aminohexyl)-4-phenylpiperazine in 75 ml THF was stirred for 60 hours at room temperature. The solvent was removed in vacuo and the residue was triturated with warm ether to give the crude amide. 12.4 g. of the crude amide in 25 ml CH 2 Cl 2 was placed on a column of 125 g Woelm basic alumina (grade 3). Elution with 750 ml. CH 2 Cl 2 furnished homogenous (tlc) material which was crystallized from acetone to give pure amide, m.p. 108°-110°.
The analytical sample, m.p. 108°-110°, was prepared in a previous run by crystallization from MeOH-H 2 0.
Anal. Calcd. for C 27 H 37 N 3 O 3 : C, 71.81; H, 8.26; N, 9.30. Found: C, 72.03; H, 8.13; N, 9.14.
EXAMPLE 69
(S)-4-(2-Hydroxy-3-isopropylaminopropoxy)phenyl-N-[2-(4-phenyl-1-piperazinyl)ethyl]acetamide and its dihydrochloride salt
A solution of 10.86 g (27.5 mmol) (R)-4-(2,3-epoxypropoxy)phenyl-N-[2-(4-phenyl-1-piperazinyl)ethyl]acetamide in 200 ml methanol containing 100 ml isopropylamine was refluxed for 90 minutes. The solution was evaporated to dryness and triturated with hot ether to give the amine, m.p. 121°-123°.
Crystallization of a small portion from EtOH-EtOAc furnished the analytically pure material, m.p. 123°-124°; [α] D 25 -0.8° (c, 1.0, MeOH).
Anal. Calcd. for C 26 H 38 N 4 O 3 : C, 68.69; H, 8.43; N, 12.32. Found: C, 68.90; H, 8.66; N. 12.15.
A portion of the above amine (8 g) was dissolved in 50 ml EtOH and treated with 35 ml 1.73 N methanolic HCl (60 mmol) and evaporated to dryness. Residue was swirled down 2× from ethanol solution which removed the excess HCl. The residue was then redissolved in 50 ml EtOH and the remaining portion of the above amine (4 g) was added. Upon the addition of 50 ml. EtOAc, crystals began to form to yield after cooling pure dihydrochloride salt, m.p. 160°-162°; [α] D 25 -12.75°. A second crop 159°-161° was obtained from the mother liquors.
Anal. Calcd. for C 26 H 38 N 4 O 3 : C, 59.20; H, 7.64; N, 10.62, Cl, 13.44. Found: C, 58.95; H, 7.49; N, 10.41; Cl, 13.62.
EXAMPLE 70
(S)-4-(2-Hydroxy-3-isopropylaminopropoxy)phenyl-N-[6-(4-phenyl-1-piperazinyl)hexyl]acetamide and its maleate salt
A solution of 7.8 g (R)-4-(2,3-epoxypropoxy)phenyl-4-[6-(4-phenyl-1-piperazinyl)hexyl]acetamide in 175 ml methanol containing 75 ml isopropylamine was heated under reflux for 75 minutes. The solution was evaporated to dryness and the residue was triturated with ether to give the amino-alcohol end product. Crystallization of the product from MeOH-EtOAc furnished pure material, m.p. 103°-104°.
The analytical specimen, m.p. 103°-104°; [α] D 25 -0.68° (c, 1.0, MeOH) was obtained from the same solvent mixture.
Anal. Calcd. for C 30 H 46 N 4 O 3 : C, 70.55; H, 9.08; N, 10.97. Found: C, 70.55; H, 9.06; N, 10.93.
4.4 g (8.615 mmol) of the amine was dissolved in acetone (100 ml) containing 1.0 g (8.615 mmol) of maleic acid. The solution was concentrated to ˜75 ml and then was cooled to 0°. The resulting crystalline salt was recovered by filtration to give the maleate, m.p. 107°-108°. Recrystallization from acetone gave the pure salt, m.p. 107°-108°; [α] D 25 -10.19° (c, 1%, MeOH).
Anal. Calcd. for C 30 H 46 N 4 O 3 .C 4 H 4 O 4 : C, 65.15; H, 8.04; N, 8.94. Found: C, 65.09; H, 8.15; N, 8.67.
EXAMPLE 71
N-(4-Hydroxyphenyl)-4-phenyl-1-piperazinepropanamide
A solution of 42.0 g (0.259 mol) of 1-phenylpiperazine and 40.0 g (0.245 mol) of N-(4-hydroxyphenyl)-2-propenamide in 600 ml of ethanol was heated under reflux overnight and then cooled. The resulting precipitate was collected and recrystallized from methanol to give the end product as colorless crystals, mp 172°-174°. The analytical sample was obtained by recrystallization from ethanol and had mp 174°-176°.
Anal. Calcd. for C 19 H 23 N 3 O 2 : C, 70.13; H, 7.12; N, 12.91. Found: C, 70.22; H, 7.09; N, 12.96.
EXAMPLE 72
(R,S)-N-[4-(3-Chloro-2-hydroxypropoxy)phenyl]-4-phenyl-1-piperazinepropanamide Hydrochloride
To a solution of 33.0 g (0.102 mol) of N-(4-hydroxyphenyl)-4-phenyl-1-piperazinepropanamide in 120 ml of 1 N sodium hydroxide was added 50 ml of epichlorohydrin. The reaction was stirred at room temperature overnight and then extracted three times with chloroform. The solvent was removed under vacuum and the crystalline residue was dissolved in 100 ml of concentrated hydrochloric acid. After standing at room temperature for 15 min the solution was concentrated to dryness under vacuum. The residue was recrystallized from methanol using a Soxhlet thimble to give the end product as colorless crystals, mp 242°-244°. Further recrystallization gave the analytical sample, mp 243°-245°.
Anal. Calcd. for C 22 H 28 ClN 3 O 3 .HCl: C, 58.15; H, 6.43; Cl, 15.61; N, 9.25. Found: C, 58.16; H, 6.51; Cl, 15.90; N, 9.18.
EXAMPLE 73
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazinepropanamide Bis-Maleate
A solution of 2.00 g (0.0044 mol) of (R,S)-N-[4-(3-chloro-2-hydroxypropoxy)phenyl]-4-phenyl-1-piperazinepropanamide hydrochloride and 20 ml of 1-methylethylamine in 20 ml of methanol was heated under reflux for 3 days and then concentrated under vacuum. The residue was mixed with dilute hydrochloric acid and the resulting solution was washed several times with chloroform and then made basic with sodium bicarbonate. The mixture was extracted several times with chloroform and the extracts were dried and concentrated to give (R,S)-N-[4-[3-[1-methylethyl)amino]-2-hydroxypropoxy]-phenyl]-4-phenyl-1-piperazinepropanamide as an amorphous solid. To a methanol solution of 0.80 g (0.0018 mol) of this solid was added 0.42 g (0.0036 mol) of maleic acid. The methanol was removed under vacuum and the residue was recrystallized several times from acetontrile to give the end product as colorless crystals, mp 159.5°.161.5°.
Anal. Calcd. for C 25 H 36 N 4 O 3 .2C 4 H 4 O 4 : C, 58.92; H, 6.59; N, 8.33. Found: C, 58.62; H, 6.78; N, 8.36.
EXAMPLE 74
6-Bromo-N-(4-hydroxyphenyl)hexanamide
A mixture of 39.0 g (0.20 mol) of 6-bromohexanoic acid and 39.0 ml of thionyl chloride was heated with a 90° oil bath until the temperature of the mixture had reached 80° and the initial gas evolution had essentially stopped. Excess thionyl chloride was distilled from the reaction mixture under aspirator vacuum. Toluene (25 ml) was added and this also was distilled under aspirator vacuum. The cooled reaction mixture was then added to a slurry of 43.6 g (0.40 mol) of 4-aminophenol in 500 ml of dioxane. After stirring for 30 min the mixture was filtered and the filtrate was concentrated under vacuum. The residue was recrystallized from trichloromethane using a Soxhlet thimble to give the end product as tan crystals, mp 127°-129°. The analytical sample was obtained from dichloromethane with charcoal; colorless crystals, mp 126°-128°.
Anal. Calcd. for C 12 H 16 BrNO 2 : C, 50,36; H, 5.64; Br, 27.93; N, 4.89. Found: C, 50.47; H, 5.69; Br, 27.92; N, 4.68.
EXAMPLE 75
N-(4-Hydroxyphenyl)-4-phenyl-1-piperazinehexanamide
A solution of 45.7 g (0.16 mol) of 6-bromo-N-(4-hydroxyphenyl)hexanamide, 26.0 g (0.16 mol) of 1-phenylpiperazine and 22.4 ml (16.3 g, 0.16 mol) of triethylamine in 400 ml of ethanol was heated under reflux overnight and then concentrated under vacuum. The residue was mixed with sodium bicarbonate solution and trichloromethane. The resulting suspension was filtered. The solid was recrystallized from ethanol-water and then from acetonitrile to give the end product as tan crystals, mp 157°-159°.
Anal. Calcd. for C 22 H 29 N 3 O 2 : C, 71.90; H, 7.95; N, 11.43. Found: C, 71.65; H, 7.99; N, 11.38.
EXAMPLE 76
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazinehexanamide
A mixture of 38.1 g (0.104 mol) of N-(4-hydroxyphenyl)-4-phenyl-1-piperazinehexanamide and 500 ml of 3 N sodium hydroxide was stirred at room temperature for 45 min. To the resulting solution was added 76 ml of epichlorohydrin and stirring was continued overnight. The heterogeneous reaction mixture was extracted with dichloromethane and the extracts were dried and concentrated to give 45.0 g of an oil. This was absorbed onto a column of 500 g of silica gel. Elution with 7 and 10% ethyl acetate in dichloromethane gave a colorless solid. A solution of 8.8 g of this colorless solid and 50 ml of 1-methylethylamine in 50 ml of methanol was heated under reflux for 4 hr and concentrated under vacuum. The residue was mixed with dichloromethane and sodium bicarbonate solution and the organic layer was dried and concentrated. The residue was precipitated several times from dichloromethane-ether to give the end product as a colorless amorphous solid, mp 125°-130°.
Anal. Calcd. for C 28 H 42 N 4 O 3 : C, 69.68; H, 8.77; N, 11.61. Found: C, 69.64; H, 8.48; N, 11.49.
EXAMPLE 77
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazinehexanamide Maleate
A methanol solution of 4.10 g (0.0085 mol) of (R,S)-N-[4-[3-[(1-methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazinehexanamide and 0.986 g (0.0085 mol) of maleic acid was concentrated and the residue was recrystallized from acetonitrile-ethyl acetate to give the end product as colorless crystald, mp 144.5°-146.5°.
Anal. Calcd. for C 28 H 42 N 4 O 3 .C 4 H 4 O 4 : C, 64.19; H, 7.74; N, 9.36. Found: C, 63.96; H, 7.74; N, 9.29.
EXAMPLE 78
11-Bromo-N-(4-hydroxyphenyl)undecanamide
A mixture of 94.7 g (0.357 mol) of 11-bromoundecanoic acid and 70 ml of thionyl chloride was heated with a 90° oil bath until gas evolution had essentially stopped. Excess thionyl chloride was distilled from the reaction mixture under aspirator vacuum. Toluene (50 ml) was added and this was also distilled under aspirator vacuum. The cooled reaction mixture was then added to a slurry of 78.0 g (0.715 mol) of 4-aminophenol in 500 ml of dioxane. After stirring for 30 min the mixture was filtered and the solid was washed with hot dioxane. The combined filtrates were concentrated and the residue was recrystallized from chloroform to give the end product as colorless crystals, mp 116°-117°.
Anal. Calcd. for C 17 H 26 BrNO 2 : C, 57.30; H, 7.36; Br, 22.43; N, 3.93. Found: C, 57.25; H, 7.28; Br, 22.42; N, 4.17.
EXAMPLE 79
N-(4-Hydroxyphenyl)-4-phenyl-1-piperazineundecanamide
A solution of 66.8 g (0.187 mol) of 11-bromo-N-(4-hydroxyphenyl)undecanamide, 30.3 g (0.187 mol) of 1-phenylpiperazine and 27.0 ml (19.6 g, 0.194 mol) of triethylamine in 600 ml of ethanol was heated under reflux overnight and then cooled. The resulting solid was shaken with sodium bicarbonate solution and dichloromethane and the suspension was filtered. The solid was recrystallized from 95% ethanol to give the end product as colorless crystals, mp 160.5°-162.5°.
Anal. Calcd. for C 27 H 39 N 3 O 2 : C, 74.10; H, 8.98; N, 9.60. Found: C, 74.28; H, 8.83; N, 9.42.
EXAMPLE 80
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazineundecanamide
To a stirring solution of 14.0 g (0.20 mol) of potassium methoxide in 400 ml of methanol was added 44.8 g (0.10 mol) of N-(4-hydroxyphenyl)-4-phenyl-1-piperazineundecanamide. Fifteen minutes later 90 ml of epichlorohydrin was added and stirring was continued overnight. The reaction was concentrated under vacuum and the residue was mixed with sodium bicarbonate solution and extracted with chloroform. The extracts were dried and concentrated and the solid residue was recrystallized from trichloromethane and from ethyl acetate to give 34 g of a colorless solid. This was dissolved in 200 ml of methanol, 200 l ml of 1-methylethylamine was added and the solution was heated under reflux overnight and then concentrated under vacuum. The residue was mixed with sodium bicarbonate solution and extracted with chloroform. The extracts were dried and concentrated to give a colorless solid. This was dissolved in chloroform and absorbed onto 500 g of silica gel. Elution with 1:1 methanol/chloroform gave material which upon recrystallization from methanol gave (R,S)-N-[4-[3-[(1-methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazineundecanamide as colorless crystals, mp 141.5°-142.5°.
Anal. Calcd. for C 33 H 52 N 4 O 3 : C, 71.70; H, 9.48; N, 10.13. Found: C, 71.92; H, 9.56; N, 10.04.
EXAMPLE 81
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazineundecanamide Maleate
A mixture of 0.200 g (0.36 mmole) of (R,S)-N-[4-[3-[(1-methylethyl)amino]-2-hydroxpropoxy]phenyl]-4-phenyl-1-piperazineundecanamide and 42 mg (0.36 mmole) of maleic acid was recrystallized from methanol-ethyl acetate to give the end product as colorless crystals, mp 141°-142°.
Anal. Calcd. for C 33 H 52 N 4 O 3 .C 4 H 4 O 4 : C, 66.44; H, 8.44; N, 8.38. Found: C, 66.59; H, 8.35; N, 8.28.
EXAMPLE 82
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazineundecanamide Hydrochloride (1:2)
Hydrogen chloride was bubbled into a solution of 5.53 g (0.010 mol) of (R,S)-N-[4-[3-[(1-methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazineundecanamide in a mixture of dichloromethane and chloroform. The mixture was concentrated under vacuum and the residue was recrystallized from methanolethyl acetate to give the end product, mp 210°-212°.
Anal. Calcd. for C 33 H 52 N 4 O 3 .2HCl: C, 63.34; H, 8.70; Cl, 11.33; N, 8.95. Found: C, 63.27; H, 8.58; Cl, 11.34; N, 8.79.
EXAMPLE 83
(R,S)-N-[4-[3-[(1-Methylethyl)amino]-2-hydroxypropoxy]phenyl]-4-phenyl-1-piperazinepropanamide
To a rapidly stirring solution of 2.243 g (0.01 mol) of 4-[2-hydroxy-3-[(1-methylethyl)amino]propoxy]benzenamine in 100 ml of dichloromethane was added dropwise a solution of 0.80 ml (0.91 g, 0.01 mol) of 2-propenoyl chloride. The reaction was stirred until the intermediate had settled out leaving a clear supernatant which was decanted. The residue was dissolved in 25 ml of ethanol, 5.0 ml (5.3 g, 0.33 mol) of 1-phenylpiperazine was added, and the solution was heated under reflux overnight. The reaction mixture was cooled and filtered. The solid was dissolved in water, and the solution was made basic with sodium bicarbonate and extracted with dichloromethane. The extracts were dried and concentrated and the amorphous residue was reprecipitated several times from ether to give the end product as a colorless amorphous solid, mp 151°-157°. Analyses were performed on this amorphous solid and subsequently the material was obtained crystalline and recrystallized from ether to give the end product as colorless crystals, mp 250°-252°.
Anal. Calcd. for C 25 H 36 N 4 O 3 : C, 68.15; H, 8.24; N, 12.72. Found: C, 68.33; H, 8.31; N, 12.65.
EXAMPLE 84
Tablet Formulations (Wet Formulation)
______________________________________Ingredients mg/tablet mg/tablet______________________________________(S)-1-[2-(4-(2-hydroxy-3-(1-methyl- 25 50ethyl)amino)-propoxy)phenoxy)ethyl]4-phenylpiperazine bis-maleate saltPregelatinized Starch 12.5 15Lactose 155 162AVICEL 30 40Modified Starch 25 30Magnesium Stearate 2.5 3 250mg 300mg______________________________________
Procedure:
Mix the first five ingredients in a suitable mixer. Granulate with water and dry in an oven. Mill through a Fitzmill. Add the magnesium stearate and mix for 5 minutes and compress on a suitable tablet press.
EXAMPLE 85
Tablet Formulation (Direct Compression)
______________________________________Ingredients mg/tablet mg/tablet______________________________________(S)-1-[-2-(4-(2-hydroxy-3-(1-methyl- 25 50ethyl)amino)-propoxy)phenoxy)ethyl]-4-phenylpiperazine bis-maleate saltLactose 147.5 157Modified Starch 25 30AVICEL 50 60Magnesium Stearate 2.5 3 250mg 300mg______________________________________
The first four ingredients are blended in a suitable mixer. The magnesium stearate is thereafter added and mixed for 5 minutes. The mixture is compressed on a suitable tablet press.
EXAMPLE 85
Capsule Formulation
______________________________________Ingredients mg/capsule mg/capsule______________________________________(S)-1-[2-(4-(2-hydroxy-3-(1-methyl- 25 50ethyl)amino)-propoxy)phenoxy)ethyl]4-phenylpiperazine bis-maleate saltLactose 125 170Cornstarch 40 60Talc 25 20 250 mg 300 mg______________________________________
The first three ingredients are blended in a suitable mixer and thereafter the talc is added. The mixture is blended for five minutes and filled on a suitable capsule machine.
EXAMPLE 87
Following the procedures outlined in Examples 84-86, the following preferred compounds and their pharmaceutically acceptable salts may be formulated into tablets or capsules:
(S)-4-[2-hydroxy-3-(1-methylethylamino)propoxy)-phenyl]-N-[2-(4-phenyl-1-piperazinyl)-ethyl]acetamide.
(S)-4-[2-hydroxy-3-(1-methylethylamino)propoxy)-phenyl]-N-[6-(4-phenyl-1-piperazinyl)-hexyl]acetamide.
(S)-1-[6-(4-hydroxy-3-isopropylaminopropoxy)-phenoxy)hexyl]-4-phenylpiperazine. | There are disclosed compounds of the formula ##STR1## wherein R 1 is selected from the group consisting of lower alkyl; R 8 is selected from the group consisting of --O--(CH 2 ) n --wherein n is 2 to 20, ##STR2## and ##STR3## and R 6 is selected from the group consisting of hydrogen or lower alkoxy, and ##STR4## wherein R 1 is selected from the group consisting of lower alkyl; R 8 is selected from the group consisting of --O--(CH 2 ) n --wherein n is 2 to 20, ##STR5## and ##STR6## and R 6 is selected from the group consisting of hydrogen or lower alkoxy and racemates thereof.
There are also disclosed processes and intermediates utilized to produce the end products.
The end products have utility as agents exhibiting both α and selective β adrenergic blocking action. | 2 |
FIELD OF THE INVENTION
The present invention relates to a process for knitting a single-faced pile fabric wherein the stitch forming work of needles in combination with sinkers is facilitated.
SUMMARY OF THE INVENTION
The process is characterised in that the knitting operation is effected with sinkers each having a throat longitudinally extended toward its closed end. A sloping shoulder on a lower edge of the throat and a re-entrant bevel on the leading portion of the upper edge of the throat, all of this supplemented by a notch on the upper edge of the sinker. To develop an operative cycle, starting from a feed stage wherein the sinker is in its position of maximum withdrawal, a base yarn is laid in the sinker throat threshold and a pile yarn is laid over a sinker by the corresponding yarnguide, a sinker is caused to move forwards, thereby aiding the needle latch to introduce the base yarn into the sinker throat with the aid of its leading bevel and cause said yarn to penetrate deeply into the throat, while the pile yarn is placed in the needle hook above the sinker. The needle is then drawn down, starting the sinking of both yarns, while the sinker is caused to push the base yarn with the sloping shoulder into the needle hook, whereafter the needle is drawn down to its lowermost position and forms a new stitch. Then the needle being raised, at the same time as the sinker is caused to continue its forward movement, thus preventing the previous stitch from being rehooked. Then the sinker being stopped until the needle reaches its uppermost position, thereby stretching the pile stitches at the expense of the corresponding loop by having made them pass over the thickest portion of the needle and the base stitches, having likewise been stretched, being caused to recover their normal length on being pulled by the take-up beam. Then the sinker being made to resume its forward movement, thereby pulling the pile stitch loop, hooked in the upper notch, thereby tightening the pile stitch around the needle stem, and eliminating the stretching. The needle finally being drawn down and the sinker being withdrawn backwards, closing the cycle with knocking off of the pile loops from this sinker.
Further objects and features of the invention will be disclosed in detail throughout the following description, with reference to the accompanying drawings, wherein:
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 to 10 illustrate schematically the successive stages of the movements of a needle and a sinker for knitting the pile fabric according to the process of the invention.
DETAILED DESCRIPTION OF THE INVENTION
According to the invention, there are used conventional needles 1 having a stem 2, hook 3 and latch 4, and sinkers 5 having a throat 6 on a circular knitting machine. Special features of the sinker 5 are the extension 7 for the throat 6, a sloping shoulder 8 on the lower edge of said throat 6 and a bevel 9 on the upper leading edge, supplemented by the notch 10 conventionally located on the upper edge forwardly relative to the closed end of the extension 7 of the throat 6.
There is described below the pile fabric knitting process as from the feed stage with the base yarn 11 and pile yarn 12, supplied through a yarnguide 13.
In FIG. 1, the sinker 5 is shown to be in its position of maximum withdrawal, while the needle 1 is at an intermediate height, leaving room for the yarnguide 13 to lay the base yarn 11 in the threshold of the throat 6 and the pile yarn 12 on top of the sinker 5, while the needle drags with it base yarn stitches 14d, 14c, . . . and pile yarn stitches 15c, 15b, . . . partly supermiposed on the base stitches and partly forming the corresponding loop.
In FIG. 2, the sinker 5 is seen to be moving forward and the base yarn 11, shown in section, as also is yarn 12, is pushed by the latch 4 of the needle 1 to enter the throat 6 with the aid of the front bevel 9 of the sinker.
Thereafter, as is seen in FIG. 3, the base yarn 11 (again shown in section) enters the throat 6 of the sinker 5 while the pile yarn 12 is located in the hook 3 of the needle 1, above the sinker.
Now, as seen in FIG. 4, the needle is drawn down to start knitting the base yarn 11 and pile yarn 12, while the sinker 5 continues moving forward to push the base yarn 11 into the hook 3 of the needle 1, with the aid of the sloping shoulder 8, to keep it separated from the pile yarn 12, and so be able to control the plating better in this way.
Then, as shown in FIG. 5, the needle 1 reaches its lowermost position to form a new stitch 14e.
In the following stage, shown in FIG. 6, the needle 1 starts to rise while the sinker 5 continues moving forward to prevent stitch 14d from being rehooked by the needle.
Then, as is seen in FIG. 7, the sinker 5 stops moving and the needle 1 reaches an intermediate position and, continuing upward, attains its uppermost position, as shown in FIG. 8, whereby the portions of stitches 15a, 15b, 15c and 15d superimposed over the base yarn stitches have been stretched by their passage over the thickest portion of the needle 1 at the expense of the corresponding loop portions extending therefrom that constitute pile, while the base yarn stitches 14a, 14b, 14c, 14d and 14e recover their normal position on being pulled by the take-up beam.
Thereafter, as shown in FIG. 9, the sinker 5 moves still further forward and pulls the pile loop of pile stitch 15d with the notch 10 until the stitch is tight around the stem 2 of the needle 1 and in the extension 7 of the throat 6, whereby that stitch recovers its normal dimension and, moreover, the stitch is prevented from passing over the latch and being rehooked by the needle in the drawdown movement.
Finally, as shown in FIG. 10, in the last stage of the cycle, the sinker 5 is drawn backwards at the same time as the needle reaches an intermediate point, while the pile loops are released from the sinker.
The foregoing description discloses the advantages provided by the novel features of the invention to fabric knitting, according to the special features introduced by the sinkers 5, which may be stated as preventing rehooking of the pile stitches when the needle is drawn down and positioning the pile yarn correctly relative to the base yarn, so that the former is located further from the needle and the latter is inside closer to the needle. | A process for knitting a single-faced pile fabric is disclosed, based on the raising and lowering of conventional needles and the movement of throated sinkers, each sinker having the throat extended and provided with a sloping shoulder in the lower edge thereof, a re-entrant bevel on the upper leading edge and a notch on the upper edge. | 3 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to electrostatographic color printing machines and, more particularly, to opposing corona wire chargers placed in the receiver path after the fusing process within a color printing apparatus.
[0003] 2. Description Relative to the Prior Art
[0004] Commercial reproduction apparatus include electrostatographic process copier-duplicators or printers, inkjet printers, and thermal printers. Such reproduction apparatus, pigmented marking particles, ink, or dye material (hereinafter referred to commonly as marking or toner particles) are utilized to develop an electrostatic image of information to be reproduced on a dielectric (charge retentive) member for transfer to a receiver member or directly onto a receiver member. The receiver member bearing the marking particle image is transported through a fuser device where the image is fixed (fused) to the receiver member, for example, by heat and pressure to form a permanent reproduction thereon.
[0005] Commonly, a primary charging device is used to uniformly place a charge on a dielectric member prior exposing the dielectric member to an imaging light pattern. Corona charging devices can serve as the primary charging devices, such as one or more parallel thin wires to which high voltage is applied, a housing partially surrounding the wires and open in a direction facing a dielectric member surface, and an electrically biased grid. A conductive housing is used for DC charging and an insulating housing is typically used for AC charging. A grid includes a metallic screen or mesh, mounted between the corona wires and the dielectric member, and is DC-biased for both DC and AC charging. The grid improves voltage control for the voltage that a primary charger imparts to the dielectric member. A grid also gives a resultant dielectric member voltage uniformity that is generally better than without a grid.
[0006] Corona wires having a high DC voltage applied to them can asymptomatically approach a cut-off voltage equal to the DC grid bias plus an overshoot voltage determined by grid transparency, grid/dielectric member spacing and corona voltage. This cut off voltage depends upon the amount of the time it takes for the moving dielectric member to pass under a gridded charger. If this time is longer than a characteristic time constant given by the product of the effective charging resistance and the capacitance of the dielectric member under the charger, the voltage on the dielectric member will asymptomatically approach the cut-off voltage. For tight grids (relatively low transparency) the cut-off of the charging current is very close to the grid bias; that is, the overshoot is small. Conversely, for open grids (relatively high transparency) the overshoot can be significant. Typically, grid overshoot is in the range 100-200 volts, depending on the grid to dielectric member spacing, with smaller overshoots for larger spacings.
[0007] In charging systems employing high voltage AC charging waveforms riding on low voltage DC offsets to charge corona wires, the cut-off voltage is generally close to the grid bias and is only weakly dependent on the grid transparency. The actual cut-off voltage is determined by the relative efficiencies of negative and positive corona emissions during the negative and positive AC voltage excursions. Moreover, a high duty cycle trapezoidal AC waveform can be used, as disclosed in U.S. Pat. No. 5,642,254 (issued Jun. 24, 1997, in the names of Benwood et al). In this patent, the cut-off voltage is also dependent on duty cycle, and the cut-off voltage steadily approaches a DC value if duty cycle is steadily increased from 50% (conventional AC) to 100% (DC).
[0008] A variety of gridded chargers are presently used in typical reproduction apparatus engines. Examples of grid designs include a continuous wire filament wound back and forth across a charger opening, grids (typically photoetched) mainly composed of thin parallel members that run parallel to or at an angle to the corona wire(s), and hexagonal opening mesh pattern grids. These different types of grids are applied in various types of corona chargers, for example, single or multiple corona wire chargers, pin corona chargers, chargers with insulating or conducting housings, and chargers that use AC or DC corona voltage. There are grids that are planar and grids that are curved to be concentric with a drum dielectric member.
[0009] Currently, there are a number of prior art systems that regulate the voltage of a corona wire purely by regulating the current. These current regulated prior art systems can, inadvertently, allow the corona wire voltage to increase to critically high values when a receiver element is between the two chargers. Furthermore, systems that employ current regulation of corona wire voltage can also have voltages vary when different receiver elements are used because of the difference in receiver resistivity. Additionally, current regulated systems can also have arcing develop between the opposing corona wires when a highly resistive sheet exits the charger. This can happen before the current regulation control of the power supply can reduce the output voltage of the supply to react to the change in resistance between the corona wires. Arcing results in undesired electrical noise radiated into the control system of the machine and, possibly, to the environment around the machine. Arcing can also be damaging to the machine hardware and materials.
[0010] Other prior art systems employ pure peak-to-peak voltage regulation that allows the current potentially to reach critical, high levels when the interframe is in between the two chargers. In this mode the charger will be operating at an unnecessarily high power level and generate excessive heat in the power supply. Corona wire emissions and the resulting chemical emissions will also be unnecessarily high.
[0011] From the foregoing, it should be apparent that there remains a need for a power regulation system of corona wires that can avoid the shortcomings of the prior art and provide a solution that prevents arcing and over-current loading for sheet fed applications.
SUMMARY OF THE INVENTION
[0012] The present invention is a high voltage power supply for electrostatically discharging prints from a sheet fed printing machine that addresses the prior needs for a power regulation system that can charge corona wires while preventing arcing and over-current loading for sheet fed applications. The power supply has two high voltage outputs that are RMS current regulated and peak-to-peak voltage limited. The current regulation provides a benefit for highly resistive receiver sheets. However, there is a potential for excess voltage that results when using highly resistive receiver sheets, which is corrected by voltage limiting. Each corona wire is connected to one of the two high voltage outputs of the high voltage power supply. The current flow through the ionized air neutralizes and reduces the electrostatic charge in the receivers to uncritical values.
[0013] These and other objects of the invention are provided by a power supply for driving opposing corona chargers comprising: a pair of transformers on the power supply, each of the transformers providing an output; a current sense element attached to each of the transformers; a current regulation circuit that is responsive to each of the current sense circuits in accordance with a predetermined parameter to adjust current flowing through the transformers; a voltage monitoring circuit for each of the transformers; and a voltage control circuit that is responsive to the output voltage monitoring circuit to limit the transformer voltage to less than a predetermined value.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The invention and its objects and advantages will become apparent upon reading the following detailed description and upon reference to the drawings, in which:
[0015] [0015]FIG. 1 illustrates a system having opposing wire chargers within a sheet transport system;
[0016] [0016]FIG. 2 illustrates the power supply concept of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] [0017]FIG. 1 illustrates a sheet transport system within the field of electrophotographic color printing machines, as envisioned by the present invention. Lower corona charger wire 22 and upper corona charger wire 23 are respectively contained within lower wire charger shell 20 and upper wire charger shell 21 . The opposing charger wires 22 , 23 are paired together and positioned such that they are after the fusing process in such a way that image receiver element 24 is guided through input paper guide 27 and into the space between the two opposing charger wires 22 , 23 . The charger wires are driven by the high voltage power supply 26 . The two charger wires 22 , 23 remove the electrostatic charge that is left over on the receiver 24 once the print has been made and after the fusing process is completed. If the left over charge is not removed from the receiver 24 , it can cause paper handling problems, like dishevelment in the stacking operation of the sheets, and difficulties in separating the sheets for the finishing operation because the sheets stick to each other.
[0018] The preset invention is directed towards the high voltage power supply 26 that is used for the electrostatic discharging of prints from a sheet-fed printing machine. The power supply envisioned has two high voltage outputs that are each RMS current regulated and peak-to-peak voltage limited. Each of the two high voltage outputs of the high voltage power supply 26 is connected to one of the corona charger wires 22 and 23 . The output voltage is trapezoidal with a 400 Hz AC frequency. The voltage waveforms of the upper and the lower charger are synchronized at 180 degrees apart to provide maximum current flow between the wires 22 and 23 . That current flow through the ionized air neutralizes and reduces the electrostatic charge in the receivers to uncritical values.
[0019] [0019]FIG. 1 illustrates the opposing corona charger wires 22 , 23 located within a sheet transport system, wherein the receiver 24 is a typical load to be driven by charging system. The receiver 24 is discharged as it passes through the two charger wires 22 , 23 . The basic problem in discharging the receiver 24 using charger wires 22 , 23 is that the resistivity between the two opposing charger wires 22 , 23 changes significantly once the receiver 24 is removed from the space between the charger wires 22 , 23 . As the receiver 24 passes through the paper guide 27 , there is no longer a load resistance between charger wires 22 , 23 .
[0020] It is not uncommon within the electrostatic discharging of prints from a sheet fed, printing machine that there be multiple stations having charging wiring configurations similar to the corona charger wires 22 , 23 seen in FIG. 1. When the receiver 24 is between these multiple stations, it is considered to be interframe, meaning that there is no sheet between the two charger wires 22 , 23 . Within the context of the present invention, current regulation features will determine the RMS current within the power supply 26 during this interframe period. The present invention also provides a voltage limiting function that determines the maximum peak-to-peak voltage allowed when the receiver 24 is present between charger wires 22 , 23 .
[0021] In a system having a power supply employing pure current regulation of the corona wire, the voltage between the chargers can increase to critically high values when a receiver is between the two chargers. The voltage will also vary with different receivers because of the variation in receiver resistivity. When a highly resistive sheet exits the charger, it is possible for an arc to develop between the opposing corona wires. The arc can develop before the current regulation used to control the power supply can reduce the output voltage of the supply as a response to the change in resistance between the corona wires. Arcing results in undesired electrical noise radiated into the control system of the machine and possibly to the environment around the machine. Arcing can also be damaging to the machine hardware and materials.
[0022] In the opposite case employing a pure peak-to-peak voltage regulating function, the current can reach critically high levels in the interframe period. In a peak-to-peak mode, the charger can be operating at an unnecessarily high power level and generate excessive heat within the power supply. The corona emission at the corona wire, and the resultant chemical emissions, will also be unnecessarily high. The combination of both output control methods provides a solution that prevents arcing and over-current loading for sheet fed applications.
[0023] Driven by the impedance between the two chargers, the power supply changes automatically from current regulation to voltage limit mode. The impedance between the two chargers refers to the load of the charger relative to wire conditions (clean vs. dirty), wire-to-wire spacing and the dielectric current between the wires (paper, plastic, plastic on paper etc.). The sample resistance is very small in comparison.
[0024] [0024]FIG. 2 illustrates the power supply concept. The preferred embodiment is comprised by two nearly identical circuits, one for driving each of the two of output transformers 1 for boosting a low voltage input to a high voltage (3-20 KVpp) AC output which energizes the corona wire chargers 10 . The present invention employs current sense elements 2 which, in the preferred embodiment, are a pair of resistors, each connected in series between the ground plane and the return of the high voltage secondary winding of the transformers, to obtain a reading of the voltage developed across the current sense elements 2 . This voltage across the current sense element reflects the current that is being sourced by the secondary coil of that transformer 1 . The voltage signal is then processed by conditioning circuitry 3 in a feedback loop. In the preferred embodiment the conditioning circuitry 3 is an RMS to DC converter. The conditioned signal is then compared to a regulation reference signal 14 at comparator 4 . The regulation reference signal 14 indicates the desired regulation and is an analog DC voltage signal, and the comparator 4 is an operational amplifier. The signal conditioning stage 3 , regulation reference signal 14 and comparator 4 sections of the preferred embodiment provide functionality that can be obtained using alternate methods that will be readily apparent to those skilled within the art. Among these methods are the use of pulse-width modulated signals, frequency modulated signals or series techniques with parallel or digital reference signals delivered to the power supply, or some combination of these methods. The regulation reference signal 14 may be generated internally to the power supply or provided by an external controller. An external controller is used in the preferred embodiment. The output of the comparators 4 provides control signals for each of the DC-to-DC converters 5 , which, in response, applies a voltage to nodes 50 that is connected at the input side of the primary coils to transformers 1 . The DC-to-DC converters 5 adjust the voltage on the primary of transformers 1 to provide a desired regulated current which is determined from the current sourced from the secondary of transformer 1 , as discussed above.
[0025] There is a potential for excess voltage that results when highly resistive receiver sheets are used, which is corrected by voltage limiting. The output of the DC-to-DC converter 5 is placed on nodes 50 and monitored by the voltage limit comparator 6 . The voltage applied to the primary of the transformer is compared to the voltage limit control reference signal 16 . Comparator 6 and voltage limit control reference signal 16 are analog in the preferred embodiment. As discussed previously, alternate methods may be used for this function. The voltage limit comparator 6 output imposes a limit on the maximum output voltage of the DC-to-DC converter 5 to node 50 , which limits the maximum voltage that can be applied to the corona wire. Alternately, the voltage limit comparison could be made by comparing the high voltage, secondary voltage with the limit reference.
[0026] The preferred embodiment of the invention uses two similar circuits in the double primary coils of transformer 1 , which are driven by a common clock circuit 7 . The clock signal 8 and inverted clock signal 9 are connected to polarity primary windings on the two transformers 1 that have opposite polarities. This can be seen by the circles adjacent to the primary windings indicating polarity. Accordingly, the voltages of the two transformer outputs 32 , 33 will be of opposite polarity. In the preferred embodiment, circuits are located on the same printed circuit board package. An alternate construction places the two circuits in different packages having the clock signal passed from printed circuit board package to the other via a wired connection. To insure that both packages are at the same electrical state, connections need to be provided for a clock output, a non-inverting clock input and an inverting clock input. The electrical wiring of the machine makes connection from the clock output of one unit to non-inverting clock input of that same unit and to the inverting input of the second unit. Alternately, the inverting and non-inverting clock inputs could be switched on both units.
[0027] The foregoing detailed description has detailed the best mode known to the inventors for practicing the invention. Other embodiments will be obvious to those skilled in the art. Therefore, the scope of the invention should be measured by the appended claims.
Parts List 1 transformer 2 current sense elements 3 conditioning circuitry 4 comparator 5 DC-to-DC converter 6 voltage limit comparator 7 common clock circuit 8 clock signal 9 inverted clock signal 10 corona wire chargers 14 regulation reference signal 16 voltage limit control reference signal 20 lower wire charger shell 21 upper wire charger shell 22 lower corona charger wire 23 upper corona charge wire 24 image receiver element 26 high voltage power supply 27 input paper guide 32, 33 transformer outputs 50 nodes | A method and apparatus for provision of a power supply that combines the advantages of current regulation with voltage limitation to enable corona chargers that can be run at higher current regulated set points for lower resistance sheets. The voltage limit will protect against arcing when high resistance media is used. This wider operation window can be provided without the need to track sheet types in the process and shift the operating set points, which would result in much more complicated machine control algorithms. The regulation and limit reference controls retain the ability of changing the operating set points of the power supply, such that it can be adapted to alternate physical configurations of the discharging system and the printing system. | 7 |
REFERENCE TO RELATED APPLICATIONS
This is a divisional application of application of Ser. No. 07/587,488 filed Sep. 20, 1990, abandoned, which is a continuation of parent application Ser. No. 07/255,078 filed Oct. 7, 1988, abandoned.
BACKGROUND OF THE INVENTION
The field of the invention is expandable batons, or night sticks and, more particularly, to expandable batons which comprise two or more rigid telescoping sections. This invention is also directed to a method of manufacture for the aforementioned expandable batons.
Expandable batons are commonly used by policemen as an alternative to fixed length, one piece night sticks. The latter are usually made of hardwood and measure approximately 26 inches long by 11/4 inch in diameter. Expandable batons are preferred because they are more convenient to carry than one piece night sticks. The expandable baton includes a hollow main section which serves as a handle. Each of the telescoping sections has a diameter progressively smaller than the inside of the handle. When collapsed, the telescoping sections are nested inside the handle.
Expandable batons come in a variety of sizes, but usually consists of three telescoping sections. The longest sizes of expandable batons extend to a length comparable to a one piece night stick. In the closed position, a three section expandable baton is just over one third of its extended length, owing to the overlap of the section.
Shorter expandable batons are also available for even greater carrying convenience at the expense of extended length. Such a short baton might measure, for example, six inches in length closed and 16 inches extended.
To be effective, the expandable baton must be capable of being extended and locked in place very quickly and simply. This is because the baton may be needed suddenly and in a crisis situation. The most common mechanism for locking the telescoping sections in place is a deadlock taper joint, comprising a swage on one end of an outer telescoping section and a mating flare on an inner telescoping section. In that case, the baton is simply extended by sharply swinging the handle in an arc. Doing so causes the inner telescoping sections to be thrust outward by centrifugal force, until the flares and swages engage. When swung hard enough, the sections are locked together so tightly that only a sharp axial blow on a very hard object, for example, a concrete wall or pavement, can break the deadlock joint between sections.
However, prior expandable batons have failed to gain widespread popularity, primarily because of manufacturing tradeoffs that had been necessary in their construction. Specifically, it was first desired to use relatively soft steel for the handle and telescoping sections to facilitate the swaging and flaring operations. This results in ease of manufacture and a corresponding low cost. While such batons continue to be manufactured, they suffer a serious drawback. While soft steel is easily worked, it is also relatively weak. When the telescoping sections are locked together there is a tremendous amount of stress at the joints, both from the locking tension and bending moments during use. Batons made of soft steel are therefore highly prone to separation at the joints. In fact, telescoping sections have been known to literally "fly apart" during the extension thrust as the soft metal of the swedge opens up and the soft metal of the flare collapses, thereby allowing the inner section to pass straight through the outer section at the joint.
Because of the circumstances under which expandable batons are used, the degree of unreliability imparted by the use of soft steel in their construction is totally unacceptable. Attempts have been made to produce batons from harder steels. Such batons perform satisfactorily, but are extremely expensive to manufacture. Special tooling is required and the service life of such tooling is reduced in working with hardened steels. Also, the rejection rate is high due to brittleness of the hardened steel as it is swaged and flared. In the finished expandable baton, this brittle steel tends to crack, allowing the same straight through separation as previously discussed.
SUMMARY OF THE INVENTION
The present invention provides a method for manufacturing an expandable baton which provides a strong yet easily manufactured baton. The method of this invention comprises the following steps. The first step is forming heat treatable alloy steel into a main section and a telescoping section. The second step is annealing the main section and the telescoping section by heat treating. After annealing the main section and the telescoping section, the next step is forming a portion of a joint on both the main and telescoping sections such that the joint portions on the main and telescoping sections form a complete joint when the baton is in an extended position. After forming the joint, the last step is hardening the main and telescoping sections by heat treating.
A main advantage of this invention is that an extremely strong baton is produced without the necessity of forming joints in hard, brittle steel. By using heat treatable alloy steel for the main and telescoping sections, the joints are easily formed after annealing, while the hardening step produces a strong, reliable joint. The hardening step may result, for example, in a hardness of 30 Rockwell C Scale or higher, and may be performed by an austempering process.
An object of the method of this invention is to produce a baton with an easily locked, strong, and reliable joint. The method of forming the joint portions on the main and telescoping sections may comprise the steps of swaging one end of the main section and flaring one end of the telescoping section. The flared end of the telescoping section is mated to form a deadlock joint with the swaged end of the main section.
Another object of the method of the invention is to produce a baton which includes a plurality of telescoping sections with progressively smaller diameters. In that case, each joint between the telescoping sections comprises a flare on one section in mating engagement with a swage on the adjoining telescoping section. The method of forming the swages and flares follows the same steps of forming the sections, annealing, forming the swages and flares, and then hardening.
Another aspect of this invention is the expandable baton produced by the method of this invention. An expandable baton of this invention includes a main section having a hollow interior. The main section is formed of a heat treatable alloy steel. A telescoping section formed of a heat treatable alloy steel and is movable between a retracted position and an extended position. The telescoping section is disposed within the interior of the main section in the retracted position. A joint is formed on portions of the main and telescoping sections for retaining the telescoping member in the extended position. The main and telescoping sections are first annealed by heat treating, then formed with the joint portions, and then hardened by heat treating.
The joint may comprise a swage on one end of the main section which mates with a flare on one end of the telescoping section. The expandable baton may further include a plurality of telescoping sections, each telescoping section being formed of heat treatable alloy steel, and each joint between the telescoping sections comprising a swage on one end of one of the telescoping sections in mating engagement with a flare on the adjoining telescoping section.
The advantages of manufacturing ease together with strength of the resulting baton provided by this invention result from the utilization of heat treatable alloy steel for the baton members. In any expandable baton of the type which includes a main section, at least one telescoping section, and a joint between each section for holding the baton in an extended position, this invention provides the improvement wherein the main section and all telescoping sections are formed of heat treatable alloy steel.
The foregoing and other objects and advantages of the invention will appear from the following description. In the description, reference is made to the accompanying drawings which form a part hereof, and in which there is shown by way of illustration a preferred embodiment of the invention. Such embodiment does not necessarily represent the full scope of the invention, however, and reference is made therefore to the claims herein for interpreting the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of an expandable baton of this invention in the retracted position; and
FIG. 2 is a sectional view of the expandable baton of FIG. 1 in the extended position.
DESCRIPTION OF THE PREFERRED EMBODIMENT
An expandable baton 1 according to the present invention is shown in a retracted position in FIG. 1 and in an extended position in FIG. 2. A main section 2 of the baton 1 serves as a handle and is formed from a hollow tube with an inner diameter d of approximately one inch. The main section 2 is covered by a padding material 3 to provide a comfortable, secure grip.
One end of the main section 2 is threaded to receive an end cap 4. The end cap 4 secures an end plate 5 across the threaded end of the main section 2. A leaf spring 6 is riveted to the center of the end plate 5 for holding the baton 1 in the retraced position.
Opposite the threaded end, the main section 2 is swaged down to a reduced diameter. The baton 1 includes to coaxial telescoping sections 10 and 11 of progressively decreasing diameter. The larger telescoping section 10 is flared on one end to mate with the swaged end of the main section 2 in the extended position (FIG. 2). The other end of telescoping section 10 is swaged to mate with a flare on the smaller telescoping section 11. A smooth knob 12 is threaded onto the end of the smaller section 11 to allow the baton 1 to be used for control or defense with a reduced risk of inflicting serious or permanent injury.
The diameter of each section 2, 10 and 11 is sized to allow nesting of each section 10 and 11 inside the next larger section 2 or 10, respectively, in the retracted position (FIG. 1). Although three sections 2, 10 and 11 are shown in this embodiment, it should be apparent to one skilled in the art that the number of sections, the retracted length, and the extended length are arbitrary. Batons of two or four sections are also practical. Batons of five or more sections are possible, but are not as practical. Three sections are preferred for providing a compact retracted size without an excessive number of joints 15 in the extended position.
Similarly, while the embodiment shown has a retracted length of approximately six inches and an extended length of approximately 16 inches, full length batons of 36 inches or more are popular as replacements for conventional fixed length night sticks. In fact, as the length increases, the need for rigidity and strength at the joints 15 increases dramatically, all of which imparts a greater importance to the strength and rigidity afforded by this invention.
Each joint 15 is a deadlock taper joint formed by a flared end of one section 10 or 11 being jammed tightly into the mating swage on the adjacent section 2 or 10, respectively. This type of joint 15 requires great strength to perform adequately.
In order to provide adequate strength for the joints 15 and the sections 2, 10 and 11, while still maintaining ease of workability for the sections 2, 10 and 11, a baton 1 according to this invention is constructed using a heat treatable alloy steel for the sections 2, 10 and 11. The particular steel preferred in this embodiment 4130 steel, and the method used for forming the sections 2, 10 and 11 is as follows.
Heat treatable steel has heretofore not been used in the manner of this invention and therefore has not been available as tubing stock. It has therefore been necessary for this invention to first fabricate the heat treatable steel alloy into the tubing sizes needed for the sections 2, 10 and 11. The preferred method is to form the tubing as seamless cold drawn 4130 alloy steel. The tubing is prepared in three sizes corresponding to the different basic diameters of the sections 2, 10 and 11 before swaging and flaring.
Once the tubing has been drawn and cut to an appropriate length for each respective section 2, 10 and 11, the tubing sections are annealed. The annealing softens the tubing and allows the swages and flares to be easily formed without cracking or introducing stress. The annealing is performed by maintaining the tubing at 1350° Fahrenheit (F) in an endothermic atmosphere for one hour, then gas cooling for about one hour until below 800° F.
After the tubing has been softened by the above described annealing process, the tubing is formed into the sections 2, 10 and 11. The smaller section 11 is flared on one end and tapped on the other end to receive the knob 15. The larger section 10 is swaged on one end and flared on the other. The main section 2 is swaged on one end and threaded on the other to receive the end cap 4.
After forming, the respective sections 2, 10 and 11 are hardened to give them the necessary rigidity and strength for the joints 15. Hardening is performed by an austempering process comprising the steps of heating in a neutral salt at 1500° F. for 30 minutes and then cooling in an agitated austempering salt for one hour at 650° F. The resulting hardness ranges from 38 to 43 Rockwell C scale, with hardness of 41-42 being typical.
The hardened sections 2, 10 and 11 are then assembled. The smaller section 11 is inserted through section 10 and the knob 15 is threaded onto section 11. The assembly of sections 10 and 11, and knob 15 is then inserted through main section 2. Finally, the end plate 5 is placed over the back of the main section 2 and the end cap 4 is threaded onto the main section 2.
It should be appreciated by those skilled in the art that many variations of the above described preferred embodiments are possible under this invention. For example, many techniques are known, other than those described, for annealing and hardening of heat treatable alloy steels which may be equally used with this invention. Specifically, induction heating as a part of the heat treating process is equally applicable. Similarly, other types of heat treatable steel may be used other than the specific type described. Finally, it should be appreciated that other types of joints 15 may be used, including twist lock, threaded, and many other types of known joints 15 for locking the baton in the extended position. Any joint 15 benefits from the increased strength afforded by this invention. | An expandable baton is constructed of heat treatable alloy steel and is formed according to a method which provides both ease of workability of the component materials and strength for the resultant baton. The disclosed method comprises the steps of first forming the sections from heat treatable alloy steel, then annealing the baton components to soften them, then forming the components into the desired shapes, and finally hardening the components. The resulting baton provides the strength and reliability required in such a device. | 5 |
This application is a continuation of U.S. Ser. No. 09/064,476 filed Apr. 22, 1998. Now U.S. Pat. No. 6,094,471.
The government has rights in this invention under grant No. N00014-95-1-1248.
BACKGROUND OF THE INVENTION
This invention relates to x-ray diagnostic systems and more particularly to a system which concentrates x-rays from a source and delivers them to an x-ray spectrometer.
Most focusing x-ray optics take advantage of total reflection at glancing angles of incidence. Total reflection occurs only when the angle of incidence is less than a critical angle that depends upon the properties of the reflecting material and the x-ray energy. Although prior art designs may vary according to application, most such designs have used metal or glass substrates with coatings of nickel, gold or iridium at glancing angles ranging from 10 to 150 arc minutes. Double-reflection geometries of the Wolter-I or Kirkpatrick-Baez types have been developed to focus a parallel beam of x-rays. The Wolter-I configuration consists of confocal parabaloid-hyperboloid shells and has been used most often for x-ray telescopes designed for high angular resolution. This optic is axially compact, has a moderate field of view and, in some cases, a large number of telescopes can be nested to fill a substantial fraction of the available entrance aperture. An approximation to the Wolter-I design replaces the precisely figured optics with simple cones. Telescopes based upon this approximation have been developed for various astrophysical payloads. The Kirkpatrick-Baez geometry uses two parabolic surfaces for parallel-to-point focusing, and it has been adapted to point-to-point geometries for x-ray microscopes. Recently, optics based upon bundles of glass capillary tubes have emerged as a method for focusing x-rays. The x-rays undergo numerous reflections as they travel through the glass channels causing these optics to have lower efficiency than the double reflection systems referred to above.
Electron microscopes are widely used in many applications including in the semiconductor fabrication industry. When targets are irradiated with electrons, x-rays are generated as a side effect. The x-ray spectrum provides information about elements contained in the target so that x-rays are often detected for analysis. In the prior art, it is known to place a detector such as a lithium-drifted silicon or germanium detector very close to the target in a scanning electron microscope. Such detectors are typically mounted on the end of a cold finger cooled by thermal conduction by means of a quantity of liquid nitrogen which boils at 77 kelvin. Higher resolution can be achieved utilizing detectors cooled to approximately 0.1 kelvin and in this context it may be desirable to locate the detector outside of the SEM enclosure. However, because of the well known square law dependence of intensity on distance from a source of x-rays, as a detector is moved farther from the source, the intensity drops which degrades the performance of a spectrometer receiving the x-rays. It is also known to use monolithic polycapillary glass optics within an SEM enclosure to concentrate x-rays for subsequent analysis but not to use any such concentrator beyond the confines of the SEM enclosure.
SUMMARY OF THE INVENTION
In one aspect, the x-ray diagnostic system of the invention includes a source of x-rays and an x-ray beam concentrator spaced apart from the x-ray source and disposed for receiving x-rays from the x-ray source. An x-ray spectrometer is disposed for receiving x-rays from the concentrator. The source of x-rays may be a point source such as a sample volume excited by an electron beam in a scanning electron microscope or excited by a focused synchrotron beam, an ion beam or a laser. The point source of x-rays may also be a commercial x-ray tube or may be produced by a small volume of hot gas produced in a laboratory plasma machine which may be of the magnetically and/or electrostatically confined type. The plasma can also be inertially confined. The x-ray source may also be a commercial electron impact device or even be a distant x-ray emitting object in space.
In preferred embodiments, the point-to-point x-ray concentrator is a single reflection concentrator made from either a nest of cylindrical surfaces or a surface wound into the form of a cylindrical spiral. The point-to-point concentrator may be a multiple reflection concentrator made either from opposed sets of nested conical surfaces or surfaces wound into the form of conical spirals. In another embodiment, the point-to-point concentrator is a single glass capillary bundle. The single glass capillary bundle may be monolithic. In another embodiment, the point-to-point concentrator includes a point-to-parallel glass capillary bundle coupled to a parallel-to-point glass capillary bundle and coupling occurs through vacuum or in gas over a variable distance.
It is preferred that the spectrometer be an energy dispersive x-ray detector such as a microcalorimeter, lithium-drifted silicon detector, germanium detector, cadmium zinc telluride (CZT) detector, gas scintillation proportional counter or gas proportional counter.
The spectrometer may also be a wavelength dispersive x-ray spectrometer which may use at least one flat Bragg crystal or may utilize at least one Bragg crystal in the Johann configuration or von Hamos configuration.
In yet another aspect, the invention is an x-ray concentrator comprising a ribbon of material having a reflecting surface and formed into a spiral having a plurality of windings. This concentrator may be either a single or a multiple reflection concentrator. It is preferred that the ribbon material be plastic foil, aluminum foil or quartz ribbon. A suitable plastic foil is polyester, kapton, melinex, hostaphan, apilcal or mylar. A particularly preferred plastic is available from the Eastman Kodak Company under the designation ESTAR™. Suitable foil thicknesses range from 0.004 to 0.015 inches as required. It is preferred that the ribbon material be coated with a thin layer of metal, preferably a high Z metal such as nickel, gold or iridium. The metal coating may be multilayer. In a preferred embodiment, the spiral configuration is maintained by a support structure made of metal, plastic or a composite material. Suitable metals are aluminum, beryllium, stainless steel, titanium or tungsten.
In yet another aspect, the invention is an x-ray concentrator comprising a plurality of nested, concentric cylinders or cones made of a ribbon material having a reflecting surface. The nested cylinders or cones may be made of glass, aluminum foil, plastic foil, silicon or germanium. Suitable plastic material is the same as described above in conjunction with the spiral aspect of the invention. The plastic material would also be coated as described above in conjunction with the spiral configuration.
The concentrators of the invention may be located, for example, outside the enclosure of an SEM and receive x-rays through an x-ray permeable window or through an evacuated pipe with no window between the SEM and concentrator. The x-rays are concentrated or focused onto a spectrometer which may be located several meters from the target within the SEM. Because of the separation, spectrometers such as microcalorimeters cooled to on the order of 0 . 1 kelvin can be more conveniently utilized thereby giving much greater spectral resolution.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic illustration of an embodiment of the invention employing single reflection cylindrical or cylindrical spiral foils.
FIG. 2 is a schematic illustration of an embodiment of the invention employing double or multiple reflection conical or conical spiral foils.
FIG. 3 is a schematic illustration of an embodiment of the invention utilizing a multiple reflection point-to-point capillary bundle.
FIG. 4 is a schematic illustration of an embodiment of the invention employing a multiple reflection point-to-parallel and parallel-to-point capillary bundle. This figure is also a schematic illustration of an embodiment of the invention that employs a point-to-parallel single or multiple reflection conical or conical spiral concentrator followed by a single or multiple reflection parallel-to-point conical or conical spiral concentrator.
FIG. 5 is an end-sectional view of a cylindrical concentrator.
FIG. 6 is an end-sectional view of a spiral concentrator.
FIG. 7 is a graph showing a ray tracing simulation for a cylindrical concentrator.
FIG. 8 is a graph-showing a ray tracing simulation for a spiral concentrator.
FIG. 9 is a projection of a trace of an x-ray reflected from a cylindrical foil telescope.
FIG. 10 is a projection of a trace of an x-ray reflected from a cylindrical spiral telescope.
FIG. 11 is a perspective, cut-away view of structure supporting the ribbon components of a cylindrical or cylindrical spiral concentrator.
FIG. 12 is a perspective view of an assembled structure for a cylindrical or cylindrical spiral concentrator.
FIG. 13 is an image from an optic produced with AlKα x-rays at 1.49 keV.
FIG. 14 is a graph of count rate versus energy with and without the telescope or concentrator of the invention.
FIG. 15 is a graph of the ratio of intensities of the curves in FIG. 14 .
FIG. 16 is a microanalysis spectrum obtained from a scanning electron microscope using a spiral optic and a microcalorimeter.
FIG. 17 is a graph of corrected gain versus energy using monolithic polycapillary glass optics.
FIG. 18 is a graph of a spectrum utilizing monolithic point-to-parallel, parallel-to-point polycapillary glass optics.
FIG. 19 is a graph of gain versus energy for monolithic point-to-parallel, parallel-to-point polycapillary glass optics.
FIG. 20 is a schematic illustration of an application of the invention to x-ray mammography.
FIG. 21 is a schematic illustration of an application of the invention to x-ray lithography.
FIG. 22 is a schematic illustration of an application of the invention to x-ray radiation therapy.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In applications where x-rays from a remote point source are being studied, the fall-off in photon flux with the square of the distance can seriously limit the sensitivity of the measurement. Two generic x-ray optic designs disclosed herein address the sensitivity problem. One design concept is based upon single or multiple reflection at grazing incidence from surfaces formed from nested cylindrical, conical, cylindrical spiral or conical spiral foils as shown in FIGS. 1 and 2. In these figures, a scanning electron microscope 10 generates a divergent beam of x-rays 12 . The x-rays 12 impinge upon a single reflection cylindrical or cylindrical spiral foil concentrator 14 and are focused on a spectrometer 16 . In FIG. 2 the diverging beam of x-rays 12 encounters a nested or multiple reflection conical or conical spiral foil concentrator 18 which similarly focuses the x-rays 12 on the spectrometer 16 . A second design concept is shown in FIGS. 3 and 4 and takes advantage of multiple reflections in glass capillary bundles. In FIG. 3, the diverging beam of x-rays 12 passes through point-to-point capillary bundle 20 which focuses the x-rays 12 onto the spectrometer 16 . In FIG. 4, multiple reflection point-to parallel, parallel-to-point capillary bundles 22 similarly focused the beam 12 onto the spectrometer 16 . FIG. 4 also represents a point-to-parallel single or multiple reflection conical or conical spiral concentrator followed by a single or multiple reflection parallel-to-point conical or conical spiral concentrator. Details of the embodiments shown in FIGS. 1-4 will be described hereinbelow and the performance from experiments are presented. Each of the x-ray optics embodiments shown in FIGS. 1-4 is compact and capable of providing a significant enhancement in the solid angle of collection. These embodiments are particularly adapted to laboratory astrophysics and x-ray microanalysis applications in which they can significantly improve coupling of a cryostat which contains a high resolution x-ray microcalorimeter to a plasma machine or the scanning electron microscope 10 . It will be readily apparent to those skilled in the art that the technology disclosed herein is applicable to space-borne astrophysical applications. Because the concentrators 14 , 18 , 20 and 22 focus a diverging beam, acceptable intensities are presented at the spectrometer 16 .
Two embodiments of the foil concentrators of the invention are shown in FIGS. 5 and 6. In FIG. 5, a cylindrical or conical concentrator 24 includes nested concentric cylinders or cones 26 , 28 , 30 , etc. The concentric cylinders or cones are formed from a thin ribbon of a gold-coated plastic. The nested cylinders or cones 26 , 28 , 30 , . . . , may also be made of glass, aluminum foil, silicon or germanium. A spiral concentrator 32 shown in FIG. 6 is formed of a long single ribbon 34 that is wound into a spiral. The ribbon 34 may be gold-coated plastic, aluminum foil or quartz ribbon. Suitable plastic materials for the embodiments in FIGS. 5 and 6 include polyester, polyimide, kapton, melinex, hostaphan, apilcal, mylar or any suitably smooth, flexible material. A particularly preferred plastic is available from the Eastman Kodak Company under the designation ESTAR™. Such plastic foil may range from 0.004 to 0.015 inches thick, for example. The plastic material is coated with a thin layer of metal, preferably a high Z metal such as nickel, gold or iridium and may be coated with multilayers. A suitable thickness for the metal coating is approximately 800 Å. Evaporation or sputtering is a suitable technology for applying the metal coating to the plastic ribbon material 34 . The embodiments of FIGS. 5 and 6 may be configured for single reflection as illustrated in FIG. 1 or for multiple reflections as illustrated in FIG. 2 .
The embodiments shown in FIGS. 5 and 6 both use a point-to-point geometry to obtain significant gain and solid angle in the energy band of 0.1 keV to 10 keV. The gain depends upon the x-ray reflectivity, focal distance, the width of the ribbon material and the number of windings of the spiral or the number of nested cylinders. The x-ray reflectivity of the concentrators 24 and 32 can be improved by depositing multilayers of W—C, Co—C, or Ni—C for example, on the uncoated or metal-coated plastic which allow the designs to include larger grazing angles.
An embodiment of the cylindrical spiral concentrator 32 has been built and tested in a microanalysis application at the Smithsonian Astrophysical Observatory in Cambridge, Mass. in which the distance between an x-ray source (scanning electron microscope, SEM) and an energy dispersive detector (lithium-drifted silicon detector and/or x-ray microcalorimeter) was approximately two meters. The constructed embodiment used single reflection in a point-to-point geometry. For the spiral concentrator 32 the ribbon was wound with a pitch of 0.05 inches and had 19 windings within an entrance aperture with diameter of 50 mm. For the cylindrical concentrator 24 , the ribbon would be cut into 20 lengths to form concentric cylinders. FIG. 7 shows the results of a ray tracing computer program which simulated the shape of images produced by the cylindrical concentrator 24 with a ribbon width of 25 mm and focal length of 1.5 m. FIG. 8 depicts a simulated image expected from the cylindrical spiral concentrator 32 . In contrast to the cylindrical geometry, the spiral optic 32 forms an annular image as shown in FIG. 8 because the ray that connects the center of the spiral to the reflecting surface of the ribbon is not the same ray that describes the normal vector at the ribbon surface. This relationship is schematically illustrated in FIGS. 9 and 10 in which the reflection geometry of the cylindrical optics of FIG. 5 and the spiral optics of FIG. 6 are compared.
With reference to FIG. 11, the cylindrical spiral concentrator 32 comprises front and back discs 40 and 42 supported in spaced apart relation by a central hub 44 . In this embodiment, each disc 40 and 42 has eight spokes which extend radially from the central hub 44 . Holes (not shown) are drilled into the spokes to hold thin stainless steel pins 46 . The pins 46 locate and support the gold-plated plastic ribbon 34 (not shown in FIG. 11 ). One end of the ribbon 34 is clamped to the central hub 44 and the other end is clamped to one of the outer ones of the support pins 46 . FIG. 12 shows an assembled concentrator 32 . It should be noted that the ribbon 34 may be supported by grooves machined into the radial spokes of the front and back discs 40 and 42 . The structure supporting the ribbon 34 may be made of metal, plastic or a composite material. Suitable metals are aluminum, beryllium, stainless steel, titanium or tungsten.
The spiral optic 32 shown in FIG. 12 was evaluated in the context of an x-ray microanalysis application. The optic (or concentrator) 32 was mounted on a kinematic base which was attached to a stage with five degrees of freedom—three translational and two rotational axes. The stage was located midway (52 inches) between the axis of a scanning electron microscope and a microchannel plate detector or lithium-drifted silicon detector. These instruments were used to measure the image characteristics and spectral transmission properties, respectively.
FIG. 13 shows an image measured with an imaging detector at an energy of 1.5 keV. The annular image structure predicted by the simulation of FIG. 8 is evident. The spectral count rates obtained with and without the x-ray concentrator 32 are shown in FIG. 14. A lithium-drifted silicon detector was used for these measurements. The three peaks are Cu Lα at 930 eV, Cu Lα at 8.04 keV and Cu Lβ at 8.9 keV, respectively. The ratio of the intensities recorded with and without the telescope is a measure of the gain provided by the x-ray optic 32 and is shown in FIG. 15 . In this particular case, a 1 mm diameter aperture was placed over the detector to mimic the size of a smaller x-ray detector such as a microcalorimeter. The gain of approximately 200 below 2 keV means that, at a distance of 2 meters from the source, the telescope can provide an x-ray intensity that is equivalent to placing the detector fourteen times closer to the source (14 cm). An example of a high resolution microanalysis spectrum taken with a cryogenic microcalorimeter instead of a lithium-drifted silicon detector is shown in FIG. 16 .
Monolithic polycapillary glass optics have been adapted by others for many laboratory applications including microflorescence analysis and protein crystallography [references]. These tapered glass optics have made it possible to intercept x-rays from a point source over an angular range as much as 6 degrees and focus them to a spot with dimensions on the order of 0.2 mm FWHM.
These monolithic polycapillary glass optics may be used for microanalysis with an SEM and an energy dispersive detector such as a lithium-drifted silicon detector, germanium detector or a cryogenically cooled microcalorimeter. As depicted schematically in FIGS. 3 and 4, there are two ways to produce point-to-point focusing with capillary bundles. The first as shown in FIG. 3 is with a single monolithic polycapillary bundle 20 . We have tested such a capillary bundle with x-rays over an energy range extending to 6 keV. The optic used in this test had a point-to-point focal distance of 14 inches. The gain in intensity measured as a function of energy is as high as 400 as shown in FIG. 17 .
The second method uses two monolithic polycapillary bundles 22 shown in FIG. 4 . The input optic intercepts the x-rays from the point source 10 and directs the radiation 12 into a parallel bundle. The output lens portion intercepts the parallel portion of x-rays and refocuses them to a spot. This technique has the advantage that the distance between the source and the image is variable and does not require a specific monolithic polycapillary bundle to be manufactured each time an experimental configuration is modified. A spectrum from a polycapillary glass optics setup is shown in FIG. 18 and the gain as a function of energy is presented in FIG. 19 .
The concentrators of the present invention may have application in the field of radiography, x-ray lithography and radiation therapy. For example, in conventional mammographic machines, a point source of Mo K x-rays forms a divergent beam that passes through the breast and is recorded on a photographic plate. Lesions in the breast tissue show up in the image as regions of contrasting intensity. Since the breast tissue is thick, the lesion can be located at varying distances along the beam path. The beam divergence will cause the recorded size of the lesion to vary according to its location along the beam path. This effect causes a loss of spacial resolution and can affect the resulting diagnosis of the mammogram. This effect would be absent if, instead of being divergent, the x-ray beam was parallel.
Large diameter parallel x-ray beams are not commonly available since most conventional x-ray sources are derived from point-like geometries. The solution to this problem is to introduce an optical system between the source and the breast that makes a parallel beam from the x-rays diverging from the point source. This can be accomplished either by a set of nested cones that have been multi-layered to reflect Mo K x-rays with high efficiency as shown in FIG. 20 or a point-to-parallel bundle of glass capillary tubes. Both are suitable approximations to a parabolic lens and will provide a quasiparallel beam with small angular divergence. Some angular divergence is required to allow the x-rays reflected from successive cones to-overlap and remove any shadows of the cones. For this parallel beam, the image of a lesion will not be affected by its location along the beam path and a degree of uncertainty will be removed from the diagnosis.
Similarly, as shown in FIG. 21, concentrators of the invention may form an optic for x-ray micro-lithography. Low energy x-rays are generally used for micro-lithography and multi-layering will not be necessary. A quasiparallel beam insures that the mask will be imaged with accuracy on a substrate. The lack of beam divergence means that it will be possible to construct features with thinner lines on the substrate.
For applications where x-ray therapy is required to destroy lesions located deep in tissue, the normal approach is to use a finely collimated beam that intersects the location of the lesion. This approach causes all the tissue along the line of sight to receive roughly the same high dose of radiation. One approach to provide lower doses to the surrounding tissue than for the lesion is to have the radiation enter the body within the volume of a cone whose apex is located at the lesion. This can be achieved mechanically by rotating the patient about the apex of the cone centered on the lesion. The pencil beam always goes through the apex, but with a variety of directions thus reducing the exposure to the healthy surrounding tissue. Another approach that achieves the same goal is to use an optic that will refocus a diverging beam from an x-ray source as shown in FIG. 22 . The focal point of the optic is located at the lesion and the conical, refocusing beam will put maximum intensity on the lesion and much less on the healthy surrounding material. The optic can be made as an approximate point-to-point lens. The approximation can be in the form of nested cylinders or two opposed sets of nested cones. In either case, the mirrors are made from thin foils that have been multilayered to reflect the x-rays of interest.
It is recognized that modifications and variations of the disclosed invention may be apparent to those skilled in the art and it is intended that all such modifications and variations be included within the scope of the appended claims. | X-ray diagnostic system. The system includes a source of x-rays which communicates with an x-ray beam concentrator spaced apart from the x-ray source and disposed for receiving x-rays from the x-ray source. An x-ray spectrometer is disposed for receiving x-rays from the concentrator. In a preferred embodiment, the concentrator is formed of a cylindrical spiral of a metal-coated plastic material having a surface for reflecting x-rays. In another embodiment, the concentrator includes a plurality of concentric nested cylinders of a metal-coated plastic material for reflecting x-rays. In yet another embodiment, the concentrator is a glass capillary bundle. The concentrator allows the spectrometer to be spaced away from the source of x-rays such as scanning electron microscope. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 11/673,430, filed Feb. 9, 2007, entitled, “Electronic Game with Overlay Card,” which claims the benefit of provisional application No. 60/766,769, filed Feb. 9, 2006, which is incorporated herein by reference in its entirety.
BACKGROUND OF THE DISCLOSURE
1. Field of the Disclosure
The present disclosure relates to electronic games. In particular, it relates to electronic games having tangible overlay card.
2. General Background
Portable or hand-held game machines continue to increase in popularity. Typically, these portable game machines include a hand-held game machine housing a processing unit and memory for executing a stored game program, as well as associated hardware such as a display for displaying images of the game and controls for implementing user interaction. The game program itself is typically contained in a game program memory such as, for example, a semiconductor memory (e.g., ROM, EPROM, and the like) that is part of a removable cartridge. User input to general-purpose computers is generally implemented through keyboards and control buttons. Graphical user interfaces implement pointing devices such as mice and touch pads that are commonly used with general-purpose computers, but less frequently used in game consoles. Game consoles support special purpose user input devices such as joysticks, special purpose buttons, rocker switches and the like.
More recently, handheld game devices have been introduced that include touch screen input devices. Touch screens comprise a display device together with touch-sensitive overlays that typically comprise either pressure-sensitive (resistive), electrically sensitive (capacitive), acoustically sensitive (SAW—sufface acoustic wave) or photosensitive (infrared). The touch-sensitive overlays allows a display to be used as an input device, removing the keyboard and/or the mouse as the primary input device for interacting with the display's content. Such displays can be attached to computers or, as terminals, to networks. One example of a game console incorporating a touch screen as a user interface is the Nintendo® DS™ available from Nintendo of America, Inc.
Touch pads and touch screens enable user input via a pointer such as a finger or more commonly a stylus. A touch pad is akin to a graphics tablet in that it does not include an active display and instead presents a blank surface to the user. In the case of a touch screen, the display beneath the touch screen overlay displays one or more graphic controls that a user selects by touching a portion of the screen overlay above the displayed control with the stylus or other device. In a manner similar to clicking on a screen element using a mouse in a conventional computer, processes executing on the game console detect the selection of the graphic control by the user and launch a programmed responsive behavior. In the context of a game, the selection may cause a character in the game to take a particular action, load a new background, or any desired programmed response.
Computer games often involve the gradual revelation of information and/or additional tools as a game progresses and a player's character gains experience, for example. An entirely self-contained game provides some means to for a player to obtain all of the tools and reveal all of the information contained in the game. However, some games require outside information such as “cheat codes” in order to obtain particular tools, weapons, modes of play, or to learn secret information that is not otherwise available by simply playing the game itself. Because these codes are very much a part of the game to many players, web sites and books have become available to give, sell, or exchange these cheat codes.
Such books are examples of auxiliary products that can enhance the overall user experience and market value of a game. Other examples of auxiliary products include trading cards, stickers, tattoos, tip sheets and the like that can be purchased with a game or separately. In the case of trading cards, secondary games have been developed using the trading cards. The trading card games are substantially separate from the electronic game played on a console, although characters, scenes and situations may be common between them. While existing forms of auxiliary products provide some enhancement of the user experience, they do not directly affect game play of the computer game implemented on the game console.
Accordingly, a need exists for products that interact more directly with a game console and a game implemented on a game console. More specifically, a need exists for systems and methods for providing new ways of user interaction with a computer game using auxiliary products such as trading cards, game cards, coupons and other forms of touch screen overlays.
SUMMARY
Briefly stated, the present invention involves systems and methods related to game consoles, game software and games for play on a game console having a touch screen interface. A card having a pattern defined therein is overlaid on the touch screen. The defined pattern is used to activate portions of the touch screen by guiding user interaction with a touch pad or touch screen. The activated portions of the touch pad or touch screen launch responsive activity in a computer program implemented on the game console.
In another aspect the present invention involves a card that is sized to interface with a touch pad or touch screen of a computing device. A pattern is formed in or on the card, wherein the pattern is traceable by a user to guide the user's interaction with the touch pad or touch screen. The pattern comprises a point, line, two-dimensional shape or a combination of thereof. The pattern may be cut into the card, printed on a card surface, or a protrusion from the card surface. The card may be whole or may be cut in smaller pieces that can be assembled in to form a whole card.
In yet another aspect the present invention involves a computer game comprising computer-implemented code having code constructs implementing an interface to a touch pad or touch screen of a computer executing the software. Game play processes within the computer-implemented code are responsive to user inputs from the touch screen to determine whether pre-specified patterns are input through the touch pad or touch screen. The pre-specified patterns are embodied in an overlay card that physically overlays the touch pad or touch screen in operation.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates a game system in accordance with an embodiment of the present invention,
FIG. 2A - FIG. 2D illustrate several exemplary implementations of overlay cards in accordance with the present invention;
FIG. 3A - FIG. 3C illustrate in cross section alternative mechanisms for implementing an overlay card in accordance with the present invention; and
FIG. 4 illustrates a card point area defined by software in a particular implementation of the present invention.
DETAILED DESCRIPTION
FIG. 1 shows an embodiment of a game device or console 10 suitable for use in conjunction with the present invention. Console 10 includes a main body 12 and a cover body 14 connected to each other along an upper edge of the main body 12 and a lower edge of the cover body 14 . In the implementation shown in FIG. 1 , hinge elements on main body 12 mesh with hinge elements on the cover body 14 , with a hinge pin (not shown) extending through the aligned hinge elements.
In the example of FIG. 1 a first display screen 32 is recessed within the upper face 26 of the main body 12 . Display screen 32 comprises, for example, a backlit, color liquid crystal display (LCD). Display screen 32 is touch sensitive and may be activated by a stylus 71 . Stylus 71 comprises a plastic pencil-shaped device with a rounded tip that is used to activate the touch screen 32 . The transition at the edge 30 of display screen 32 may be tapered, curved or abrupt. Edges 30 provide a convenient mechanism for registration of the overlay card 31 in accordance with the present invention by aligning edges 33 of overlay card 31 with edges 30 of display screen 32 .
In the upper right corner of the main body 12 , there are side-by-side “start” and “select” buttons 38 , 40 , respectively, with X/Y/A/B buttons 42 located adjacent and below the “start” and “select” buttons, Buttons 38 , 40 and 42 are also used for game play control. A cross-shaped directional control button 36 is located adjacent and below the power button 34 , and is used for game play control. Additional control buttons may be located on the peripheral edge of main body 12 or at other desired locations on the upper face 26 .
FIG. 2A - FIG. 2D illustrate several exemplary implementations of overlay cards in accordance with the present invention. FIG. 2A illustrates an embodiment similar to that shown in FIG. 1 in which an overlay card 31 contains a pattern 201 . Overlay card 31 is constructed from a material such as paper, pressboard, cardboard, plastic, metal or the like. In a particular implementation overlay card 31 is roughly the thickness of a playing card, but may be substantially thicker or thinner in particular applications.
In one embodiment overlay card 31 is sized to fit snugly within the recess defined by edges 30 of a particular game console. In this manner, one face of card 31 contacts touch screen 32 and card 31 is registered with a relatively high degree of precision with touch screen 32 . In an alternative embodiment overlay card 31 may be sized smaller than touch screen 32 and some other means of registering card 31 with screen 32 is used. For example, touch screen 32 may display one or more alignment marks or images allowing card 31 to be aligned with touch screen 32 using the visible alignment marks. Card 31 may be larger than touch screen 32 by forming it of a sufficiently flexible material such as paper, foil, plastic film, and the like.
Pattern 201 is defined by punched holes 201 in the implementation of FIG. 2A . Holes 201 may extend completely through card 31 as shown in FIG. 3A or may extend partially through card 31 as shown in FIG. 3B . Alternatively, pattern 201 may be printed only, without punched or holes, when the material chosen for card 31 is sufficiently conformable so that activity of a stylus on the printed pattern is translated to touch screen 32 .
In this manner user input to touch screen 32 and in turn a game or other process executing on console 10 is guided by the pattern 201 . In FIG. 2A the user places a cursor in or on each of the elements of pattern 201 and thereby specifies a sequence of inputs specified by that particular pattern 201 . A large number limitless number of patterns may be defined to fit the needs of a particular application. Because the pattern 201 is physically encoded into or on card 201 , the information is easy to enter as it does not require memorization of complex sequences of buttons or controls. Overlay card 31 can be manufactured and distributed efficiently and inexpensively, and the many materials available for overlay card 31 enable a wide range of product differentiation to further engage customers.
FIG. 2B illustrates an embodiment in which pattern 201 must be accessed by the user in a particular order indicated by printed indicia on a surface of card 31 . A simple sequence of numbers is shown in FIG. 2B , however, the indicia may comprise other printed symbols or images that guide or prompt a user to select the desired sequence.
In the examples of FIG. 2A and FIG. 26 the pattern is defined by a collection of points or dots. FIG. 2C shows an embodiment in which pattern 201 comprises a line, arc and/or two-dimensional shape. A one- or two-dimensional pattern may be a line or an area that guides a user to follow the pattern with a stylus once card 31 is placed in contact with screen 32 . In the case of an area such as the star shape in FIG. 2C , use of the card may require tracing the perimeter of the shape or may require the user to “fill in” the shape by scrubbing the area with a stylus. Additionally, a particular game may require the user to trace the card pattern 201 in a particular direction, or to trace the pattern multiple times such as back and forth. In any embodiment the game may require that a particular pattern be followed within specified time constraints.
Optionally an overlay card may be implemented as multiple pieces such as shown in FIG. 2D . Once the pieces are fit together they form a complete overlay card 31 that can be used to interact with a game. The pieces can be formed so as to fit together in jigsaw fashion if desired. Such an implementation may be useful when the card pieces are distributed as a part of a retail incentive program to encourage repeat business, or similar distribution scheme.
FIG. 3A - FIG. 3C illustrate in cross section alternative mechanisms for implementing an overlay card in accordance with the present invention. In the embodiment of FIG. 3A pattern 201 extends entirely through the thickness of card 31 . This can be accomplished by punching, die cutting, laser cutting, etching, or other technique suitable for a particular card material and production process. In the embodiment of FIG. 3A the card 31 can be used by placing a stylus 71 completely through the pattern 201 to contact the touch pad or touch screen. One or more elements of pattern 201 may be used as alignment marks as described hereinbefore.
In the embodiment of FIG. 3B pattern 201 comprises cavities that extend less than completely through card 31 to leave a thinner membrane portion. The membrane portion is sufficiently thin such that a touch pad or touch screen 32 can sense a stylus 71 . The implementation of FIG. 3B can be formed by cutting patterns 201 partially through card 31 or by cutting a pattern 201 completely through card 31 and applying a layer of paper, plastic, or similar material to form the membrane portion. In this manner the pattern 201 can be obscured during distribution if desired to deter copying.
In the embodiment of FIG. 3C a pattern is formed by protrusions or bumps 303 on one surface of card 31 . Bumps 303 may be formed by screen-printing, adhesives, or other available technique. In the case of a pressure sensitive screen bumps 303 allow a user to input a pattern into a touch pad or touch screen by rubbing the upper surface (i.e., a surface that faces a user) of card 32 . This may allow a user to input complex patterns involving near simultaneous activation of a number of points on the touch screen 32 in a manner that would be difficult to perform using a stylus alone.
FIG. 4 illustrates a card point area defined by software in a particular implementation of the present invention. In the embodiment of FIG. 4 the touch pad or touch screen writeable area is segmented into a 15×11 array. The granularity of this segmentation is a matter of design choice and is constrained only by the granularity permitted by the touch pad or touch screen mechanism. Less granular arrays may be easier to use and will be more forgiving to misalignment whereas more granular arrays allow more complex patterns to be defined and used. In operation the array may be fully populated such that all areas are active, or sparsely populated such that less than all of the areas are active. For example, if a game is at a point where only a certain card can be played, only elements corresponding to that card may need to be active. On the other hand, activating the entire array allows the program to detect when an incorrect sequence is entered indicating that an incorrect card has been played. Processes executing on the game console may take responsive action for incorrect use.
In operation a game program can be constructed such that a character obtains some benefit. For example, a character may grow stronger or more robust. A character may be given extra life or vitality, or be given new tools or weapons. A character may evolve or grow up more rapidly than permitted by normal game progression. Conversely, a card may signal a negative effect on a character such as weakening the character or stealing a tool or weapon.
Game developers program the effect of a particular card when designing a game. A particular effect is dormant until a particular pattern is applied to the touch pad or touch screen 32 . The game may define specific times at which a card pattern may be applied such as at the beginning of a game or round. Alternatively or in addition a game may be designed to prompt a user to use a card if available.
Card 31 can be distributed entirely separate from the particular game with which it is associated. Moreover, a specific card 31 may be useful in more than one game. A game designer will publish, sell, or license the information about various features that can be activated by a game card, and any entity with sufficient rights in the pattern 201 for a particular game can manufacture and distribute cards 31 as desired. This separation of the game and card overlay is not required, but enables great flexibility in providing auxiliary products for a game that enhance the overall user experience.
It is apparent that the present invention is useful in a variety of applications other than computer games. The card overlay is generally useful for entering information using touch pad or touch screen input devices to computers where it is desirable for the user to trace a pattern or activate a sequence of points on the touch screen. Such operation might be useful in activating software or activating features in a software program.
Although certain illustrative embodiments and methods are disclosed herein, it will be apparent from the foregoing disclosure to those skilled in the art that variations and modifications of such embodiments and methods may be made without departing from the true spirit and scope of the art disclosed. Accordingly, it is intended that the art disclosed shall be limited only to the extent required by the appended claims and the rules and principles of applicable law. | Systems and methods related to game consoles, game software and games for play on a game console having a touch screen interface. A card having a pattern defined therein is overlaid on the touch screen. The defined pattern is used to activate portions of the touch screen by guiding user interaction with a touch pad or touch screen. The activated portions of the touch pad or touch screen launch responsive activity in a computer program implemented on the game console. | 0 |
FIELD OF THE INVENTION
The invention relates to an optical element that comprises a substrate, an interlayer and at least one functional layer and is suitable for recovery of the substrate. The invention further relates to a method for recovering a substrate of an optical element comprising a substrate, an interlayer and at least one functional layer.
BACKGROUND OF THE INVENTION
When optical elements are produced, not only flat substrates but also spherical or aspherical substrates may be used. In these cases, the costs of the substrate may exceed the coating costs by a multiple. It is therefore useful in development work if a substrate can be used repeatedly. In production, too, it may be advantageous if coatings that do not meet the specifications can be removed again and the substrate reused. The important thing is that the original form of the substrate is not changed and that the roughness of the substrate surface is not increased. Flawed optical elements can, for instance, have inadequate reflectivity or cause image distortion.
The optical elements can have one or more functional layers, which in turn comprise one or several layers. An example to be cited is a mirror for soft x-rays, which is provided with a coating of molybdenum and silicon films on a silicon substrate to reflect the soft x-rays, whereupon a single-layer protective coating is applied.
The requirements for the substrates, including recovered substrates, are discussed in D. P. Gains, et al, SPIE Vol. 1547 (1991) 228-238. This paper also introduces two methods for repairing optical elements. On the one hand, the flawed layers may be covered with additional correct layers. On the other hand, an interlayer between substrate and functional layer may be etched away and the coating thereby removed. Both of these methods have drawbacks. In the first method, flaws in the surface characteristics and the form of the optical element may be propagated through the individual layers. In addition, cracks may form through stresses and cause the coating to be partially detached. The second method has the drawback that removal takes a long time if the surfaces are relatively large.
A good interlayer must be homogenous and have a surface roughness that is as low as possible. In addition, it must be capable of being etched by substances that do not attack the substrate. For this reason, the aforementioned paper proposes aluminum as the interlayer on a silicon-based substrate. This aluminum interlayer is etched by a solution of hydrochloric acid and copper sulfate. However, optical elements with an aluminum interlayer have lower reflectivity than optical elements without this interlayer.
As mentioned above, the removal of functional layers of an optical element by etching away an interlayer is very time-consuming. For in order to be able to etch away the interlayer, the solution must first penetrate through the functional layer(s). Depending on the substance used, the at least one functional layer can also completely prevent the etching of the interlayer.
Another option to remove the coating from a substrate is dry etching. Such methods are described, for instance in WO 97/31132 and European Application EP 0 422 381 A2. In optical elements, however, it has thus far not been possible to optimize the dry etching process in such a way that the functional layers are removed while the substrate is left intact.
Chemical removal has also been attempted on objects other than optical elements.
German Patent DE 31 10 931 describes a method for removing a flawed copper sulfide coating applied to a cadmium sulfide layer, particularly in a process for producing solar cells. The substrate carrying the two layers is immersed into an aqueous cyanide-ion-containing solution until the flawed copper sulfide coating is completely dissolved, forming copper tetracyanide ions. The cadmium sulfide layer is not dissolved.
German Application DE 37 37 483 A1 describes a method for reusing glass substrates for optically readable compact storage masters. The disk-shaped glass substrates are coated with a layer of photoresist, which is partially exposed and developed. They are subsequently provided with an electrically conductive metal coating and a galvanically applied reinforcement. The latter two metal layers are then removed and serve to produce, either directly or after additional duplicating steps, the optically readable disk-shaped information carriers. This method provides that after removal of the photoresist layer, any residues of the electrically conductive metal coating and the galvanically applied reinforcement adhering to the glass plate be removed by rinsing with an acid and water mixture that attacks the metals.
A similar approach is used in German Patent DE 43 18 178 C2, which deals with a process for chemically removing a coating applied to the surface of a substrate made of glass, glass ceramic or ceramic. The decorated glass is brought into contact with hydrochloric acid and/or sodium hydroxide solution or with sulfuric acid and potassium hydroxide.
U.S. Pat. No. 5,265,143 describes an optical element comprising a substrate, an interlayer and a multilayer coating in which the interlayer dissolves 1000 times faster than the substrate material in an etchant solution at a temperature of 130° C. This interlayer consists particularly of germanium. The multilayer coating is typically made of molybdenum and silicon. The etchant solution used is an aqueous solution of 0.88 mol potassium hexacyanoferrate and 1 mol potassium hydroxide. At room temperature, only the molybdenum dissolved; if the solution is heated to above 60° C., the silicon is dissolved as well. However, re-coated recycled substrates partly showed reflectivities that were only 80% of the reflectivity of the original optical elements. This was attributed to increased surface roughness. To counteract this, a barrier layer of a chemically inert material, e.g. ruthenium, was applied between the interlayer and the substrate. For the production of iridium on glass ceramic mirrors it is suggested to use chromium as the interlayer. However, this should be done only in conjunction with a barrier layer since the surface roughness will otherwise excessively increase.
SUMMARY OF THE INVENTION
Against this background, it is the object of the invention to find an optical element, the substrate of which can be reused while retaining an optimal surface quality, as well as a method for recovering the substrate.
This object is attained by an optical element comprising a substrate, an interlayer and at least one functional layer, which is suitable for recovering the substrate and is characterized by an interlayer consisting of at least one layer of chromium and one layer of scandium.
DETAILED DESCRIPTION OF THE INVENTION
This object is further attained by a method for recovering a substrate of an optical element comprising a substrate, a chromium- and scandium-based interlayer and at least one functional layer, wherein the optical element is immersed in a 15%-30% aqueous hydrochloric acid solution.
If an optical element with an interlayer consisting of at least one layer of chromium and one layer of scandium is immersed into a 15%-30% hydrochloric acid bath, the interlayer dissolves with strong gas formation. The parts of the interlayer and particularly the at least one functional layer which are not dissolved by the hydrochloric acid are split off, as it were, by the gas development. This causes both the interlayer and the at least one functional layer to be virtually completely removed from the substrate. This is all the more surprising since chromium is known to passivate when it comes into contact with hydrochloric acid, so that it does not dissolve in hydrochloric acid.
The first layer on the substrate can be either chromium or scandium. The last layer before the functional coating can likewise be either scandium or chromium.
The advantage of the method according to the invention is that the substrate, which is made of silicon, glass or quartz, is not attacked and therefore retains both its shape and its original surface roughness. As a result, optical elements with high reflectivities can be produced even if they are recycled. It has proven to be advantageous if the interlayer comprises about 15-25 layers each of chromium and scandium. Preferably one layer of scandium and one layer of chromium have a combined thickness of 2-3 nm. At these small thicknesses, no crystal growth can take place, which would result in an increased surface roughness. Particularly preferred are equal layer thicknesses for chromium and scandium. Such interlayers have the effect on the one hand that the gas development during etching of the interlayer is sufficient to split off even relatively thick functional layers. On the other hand they have the effect that the substrate is better protected against any reactions with the hydrochloric acid.
To perform the method according to the invention, it has proven to be advantageous if the temperature of the hydrochloric acid bath is greater than 70° C., preferably 78° to 82° C. This increases the reaction rate and makes it possible to keep the optical element in the hydrochloric acid bath for less than 25 minutes while the interlayer and the functional layer(s) are nevertheless dissolved.
In large-area optical elements with thick functional layers, the optical element is preferably cleaned in addition with a mixture of equal parts of 35%-40% aqueous potassium hydroxide solution and 15%-25% aqueous potassium hexacyanoferrate solution. For this purpose, a rag or a wad of cotton wool or some other cleaning item is impregnated with this mixture and is used to wipe the optical element or the now remaining substrate to remove any residues of the interlayer and the at least one functional layer.
The invention will now be described in greater detail by means of the following examples.
EXAMPLE 1
A silicon substrate with an area of 3.14 cm 2 , which is provided with an interlayer of 15 3 nm thick chromium and scandium layer pairs and a 350 nm thick functional coating of molybdenum and silicon layers, has a reflectivity of 68% at a wavelength of 13.4 nm. To remove the functional layer and the interlayer from the substrate, this multilayer system is immersed for 15 minutes in a 75° C. 25% aqueous hydrochloric acid solution. Thereafter, the recovered silicon substrate is re-coated with an interlayer of 15 chromium and scandium layer pairs having a thickness of 3 nm and with a molybdenum and silicon based functional layer having a thickness of 350 nm. At a wavelength of 13.4 nm a reflectivity of 68% is again reached.
EXAMPLE 2
A silicon substrate with an area of 12.5 cm 2 , which is provided with an interlayer of 25 2.5 nm thick chromium and scandium layer pairs and aB functional layer of 100 tungsten and silicon layers each having a periodic thickness of 3 nm, has a reflectivity of 35% at a wavelength of 0.99 nm. To remove the functional layer and the interlayer from the substrate, the multilayer system is immersed for 20 min in an 80° C. 30% aqueous hydrochloric acid solution. Thereafter, the recovered silicon substrate is re-coated with an interlayer of 25 chromium and scandium layer pairs having a thickness of 2.5 nm and a tungsten and silicon based functional coating having a thickness of 300 nm. At a wavelength of 0.99 nm a reflectivity of 35% is again reached.
EXAMPLE 3
A silicon substrate with an area of 6.25 cm 2 , which is provided with an interlayer of 30 2 nm thick chromium and scandium layer pairs and a 225 nm thick functional coating of nickel and carbon layers, has a reflectivity of 29% at a wavelength of 4.47 nm. To remove the functional layer and the interlayer from the substrate, the multilayer system is immersed for 18 minutes in a 70° C. 20% aqueous hydrochloric acid solution. Subsequently, the silicon substrate is cleaned by wiping with a wad of cotton wool dipped into a solution of 2 equal parts of 40% aqueous potassium hydroxide solution and 20% aqueous potassium hexacyanoferrate solution. Thereafter the recovered silicon substrate is re-coated with an interlayer of 30 chromium and scandium layer pairs having a thickness of 2 nm and a nickel and carbon based functional layer having a thickness of 225 nm. At a wavelength of 4.47 nm, a reflectivity of 29% is again reached.
EXAMPLE 4
A quartz substrate with an area of 6.25 cm 2 , which is provided with an interlayer of 30 2 nm thick chromium and scandium layer pairs and a 240 nm thick functional layer of molybdenum and boron carbide layers, has a reflectivity of 30% at a wavelength of 6.76 nm. To remove the functional layer and the interlayer from the substrate, the multilayer system is immersed for 20 minutes in an 80° C. 23% aqueous hydrochloric acid solution. Subsequently, the quartz substrate is cleaned with a rag using a solution of equal parts of 35% aqueous potassium hydroxide solution and 25% aqueous potassium hexacyanoferrate solution. Thereafter, the recovered quartz substrate is re-coated with an interlayer of 30 chromium and scandium layer pairs having a thickness of 2 nm and a molybdenum and boron carbide based functional layer having a thickness of 240 nm. At a wavelength of 6.76 nm a reflectivity of 30% is again reached.
EXAMPLE 5
A glass substrate with an area of 12.5 cm 2 , which is provided with an interlayer of 25 3 nm thick chromium and scandium layer pairs and a 272 nm thick functional coating of molybdenum and silicon layers, has a reflectivity of 66% at a wavelength of 13.4 nm. To remove the functional layer and the interlayer from the substrate, the multilayer system is immersed for 15 minutes in an 85° C. 15% aqueous hydrochloric acid solution. Subsequently the glass substrate is cleaned with a solution of equal parts of 45% aqueous potassium hydroxide solution and 15% aqueous potassium hexacyanoferrate solution. Thereafter the recovered glass substrate is re-coated with an interlayer of 25 chromium and scandium layer pairs having a thickness of 3 nm and a molybdenum and silicon based functional layer having a thickness of 272 nm. At a wavelength of 13.4 nm a reflectivity of 66% is reached. | In the production of optical elements, not only flat substrates but also spherical or aspherical substrates are used. The costs of such a substrate can exceed the coating costs by a multiple. Particularly in development work, cost savings may be achieved if a substrate can be used repeatedly. To recover a substrate, it is proposed to provide an interlayer between the substrate and the functional layers, which comprises at least one layer of chromium and one layer of scandium. By immersing the optical element into a hydrochloric acid solution, this interlayer is dissolved, so that the functional layer is also removed from the substrate and the substrate is ready for reuse. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Division of application Ser. No. 13/065,183, filed Mar. 16, 2011, publication No 2012-0234745A1 with a notice of allowance on Jun. 12, 2013. International Patent Application filed with the USPTO on Mar. 16, 2012, No. PCT/US12/29439.
FEDERALLY SPONSORED RESEARCH
[0002] Not Applicable
SEQUENCE LISTING OR PROGRAM
[0003] Not Applicable
BACKGROUND
[0004] 1. Field
[0005] This application relates to hollow fiber membrane fluid transport devices, specifically to the method of manufacturing such membrane fluid transport devices, and even more specifically to the means of assembling the hollow fibers into bundles and sealing the ends of the hollow fibers to make suitable contactors.
[0006] 2. Background of the Invention
[0007] Membrane contactors are useful devices for separation processes, contacting processes, or as filters. A membrane contactor includes a membrane or membranes held in such a manner as to separate two regions of flow and enable the membrane to act as a separation means between the two phases, and a housing to enclose the membrane and contain and direct the flow of the multiple phases. The membrane acts as a barrier between the two fluid phases and selectively allows or prohibits the transport of one or more chemical species or particles from one fluid stream to the other. The housing has one or more ports to allow flow to and from the membrane. Membrane contactors can be considered as a subclass of the more general class of fluid or fluid/gas transport devices.
[0008] Membrane contactors have applications as filters, separation systems, or contacting devices in many industries such as chemical, pharmaceutical, food and beverage, environmental, water treatment, and semiconductor processing. Membrane separation processes such as gas/liquid separation or membrane distillation are replacing their bulk counterparts (distillation towers, stripping columns) due to improved energy efficiency, scalability, the ability to operate isothermally, and smaller physical footprints. In addition, membrane filters, separators, and contactors generally have no moving parts and are physically simple and rugged, resulting in low maintenance cost.
[0009] Hollow fiber membrane devices are one class of membrane modules that employ membranes in hollow fiber form. While many types of membranes are available in sheet form, the ability to create significantly higher surface area per unit volume with a hollow fiber membrane is of major advantage to the designer and user of a membrane filter or contactor. A hollow fiber membrane is also typically self-supporting in contrast to flat sheet or thin film membranes that usually require a skeletal structure for support. In addition, typical contactor designs employing hollow fiber membranes, whether constructed as a cross flow element or in a dead-end configuration, offer more uniform flow and fewer regions for the flow to stagnate.
[0010] The usefulness and efficiency of a membrane contactor is determined by the available surface area of the membrane per unit volume of the device and the rate at which the transfer or removal of the species of interest occurs; this is generally governed by the flux (flow per unit area, per unit time, per unit pressure gradient) of the process stream. The available surface area for a hollow fiber membrane module is dictated by the packing density of the fibers (the ratio of the sum of the cross sections of the individual fibers to the total available cross sectional area). The higher the packing density and the greater the surface area to volume ratio generally results in a more efficient module.
[0011] Two other useful parameters for defining the performance of a porous membrane are the pore size distribution and the porosity. The pore size distribution is a statistical distribution of the range of pore diameters found in the membrane wall. The largest pore size is also generally characterized by a measurement called a bubble point, which is defined in the below detailed description of the invention. The smaller the mean pore size, the smaller the particle a membrane filter will separate.
[0012] The porosity of a hollow fiber membrane may be defined as the percentage of free volume in the membrane, or, for PTFE hollow fiber membranes, as (1−(membrane density/2.15)*100 where 2.15 is the density of solid PTFE. The higher the porosity, the more free volume and generally the higher the flux rate through the membrane wall.
[0013] For a given pore size distribution, higher porosities are often desirable as they lead to higher flux rates. Unfortunately higher porosities also generally lead to softer membrane walls, causing the hollow fibers to be structurally very soft and prone to deformation and collapse, especially during a potting process. Heating the ends of the hollow fibers reduces the porosity and hardens the heated portion of the fibers, reducing the likelihood of the fibers being crushed or deformed on compression.
[0014] The elements of a hollow fiber membrane contactor include the hollow fiber membrane itself, the housing, and a means to bind the fibers to one another and to the housing. A hollow fiber membrane is a porous or non-porous, semi-permeable membrane of defined inner diameter, defined outer diameter, length and pore size, and generally of a very high aspect ratio, defined as the ratio of the length to the diameter of the fiber. A hollow fiber membrane contactor is generally comprised of a plurality of fibers.
[0015] The housing is an outer shell surrounding the membrane that secures and contains a potted bundle of hollow fibers. The housing is equipped with one or more inlets and one or more outlets, such that the potted bundle of hollow fiber membrane acts as a barrier and separates the two phases or process streams. The design of the housing, and specifically the relationship of the inlets and outlets, regulates the flow of the process fluid into or out of the fiber lumens and directs the processed fluid away from the device. There are typically two common modes of designing the housing, which relate to how the fluids interact with the membrane. What are known to those well versed in the art as dead-end elements consist of a housing that directs all of the volume of one fluid to pass through the membrane walls to reach the discharge or exit of the housing. The dead-end design is a very common design employed for membrane filtration. For dead-end hollow fiber membrane filters, both ends of each hollow fiber membrane are potted or bound at one end of the housing. In dead-end hollow fiber membrane filters the process fluid either enters the lumens of the hollow fibers and discharges out through the walls of the hollow fiber membrane, or enters through the walls and discharges out of the lumens. In either case, this ensures that the entire process stream passes through the membrane wall.
[0016] A dead-end hollow fiber membrane filter configuration is contrasted to a cross flow configuration in which the lumens are open at both ends, and only a portion of the process stream entering the upstream lumens passes through the membrane wall, while the remainder of the fluid discharges through the downstream lumen openings. The portion of the fluid discharging from the downstream lumen end may be passed along to another membrane element, recycled to the beginning of the unit, or discarded. The cross flow configuration mode is employed with both filtration as well as membrane contacting or separation processes.
[0017] A hollow fiber membrane bundle may be integral to the housing or may be designed so that the potted hollow fiber membrane bundle may be installed and removed.
[0018] To create a membrane filter or membrane separator or contactor module, one must establish a suitable means for binding the hollow fiber membranes into an integral bundle and sealing the exposed ends of the hollow fibers from the body of the module, a process hereafter referred to as potting the fibers. Potting the hollow fiber membranes may occur prior to, or during the operation of mounting the hollow fiber membranes into the housing. To bind the ends of the hollow fibers to one another, a potting compound is employed. A potting compound is a material that when applied around the ends of hollow fibers, bonds them together into a solid, cohesive mass that isolates and fixes the hollow fibers from the remainder of the bundled assembly of fibers.
[0019] A potted bundle of hollow fibers is a plurality of hollow fiber membranes bound together or potted at least at one end. Both ends may be potted, or the ends of each individual fiber may be looped back in a U-shape and potted at or near one end. One potential configuration can be where the bundled fibers are first twisted 180 degrees and then folded into itself to form a closed end and an open end with the open end potted, i.e.—embedded in a solid mass providing a fluid-tight seal around each fiber. There may be several themes and variations on these basic configurations.
[0020] Membranes for contactors or filters have been developed from a variety of synthetic polymers and ceramics and have been known in the industry for many years. While ceramic membranes offer the chemical resistance and high service temperature required by aggressive acidic, alkali, or organic solvent applications, in their present-day state they are very fragile, very expensive, and very difficult to work with, a combination of features that keeps ceramic membranes out of many applications.
[0021] The vast majority of state of the art polymeric membranes are limited as they are not inert, they possess inadequate chemical purity, thermal stability and chemical resistance, and occasionally have undesirable surface properties, preventing their use in certain important applications. This is because these very same membranes are spun from solution, and the fact that they must be soluble in certain solvents to convert to a membrane means that the final membrane itself is susceptible to attack by those same classes of solvents.
[0022] It has long been desired to be able to have membranes manufactured from fluorinated or perfluorinated resins due to their high service temperatures, chemical stability, inertness, and chemical resistance to a wide range of solvents, acids and alkali systems. However, membranes produced from non-fully fluorinated polymers still require aggressive solvent systems and very high processing temperatures to manufacture, increasing cost and generating environmental and waste issues. Membranes manufactured from Polytetrafluoroethylene (hereafter referred to as PTFE) are most desirable because, as a fully fluorinated polymer, they offer the best combination of thermal and chemical stability of all the fluorinated and perfluorinated resins commercially available. In addition, the method by which they are converted to membranes does not employ hazardous solvent systems; instead using a stretching and orientation method.
[0023] It is also desirable to have membranes manufactured from fluorinated or perfluorinated resins, especially fully fluorinated resins, due to their low surface energy Filtration of organic liquids, separating organic from aqueous systems, or removing vapor from aqueous systems all favor low energy membranes. PTFE offers the lowest surface energy of all the fluorinated or perfluorinated polymeric membranes—less than about 20 dyne-cm.
[0024] Current potting materials have many limitations such as inadequate chemical resistance, lack of chemical purity and inertness, and poor thermal stability. They are also very difficult to use, and produce inefficient and costly modules. One such class of inadequate potting systems consists of low viscosity materials including urethanes and epoxies which are easy to apply but are chemically very impure and are not chemically resistant, nor do they offer high service temperatures.
[0025] It is also therefore highly desirable to have a potting compound that has excellent chemical resistance and high service temperatures that would match those of the fluorinated, perfluorinated, or fully fluorinated membrane, because the effectiveness of a contactor constructed with a fluorinated or perfluorinated membrane for a thermally or chemically aggressive system is limited by the weakest part of the device. An effective combination of a potting system for a fluorinated or perfluorinated membrane has hitherto been unavailable. Current potting methods are not amenable to the use of fluorinated or perfluorinated compounds; they cannot produce membrane modules with high fiber packing density, or with economical manufacturing cycle times; nor can they be employed to make contactors with relatively soft fibers or contactors containing many thousands of fibers, something necessary for many commercial membrane applications.
PRIOR ART
[0026] In the art, various adhesives, such as epoxies, polyurethanes, cyanoacrylates, etc. have been used for bonding or potting the ends of hollow fibers together into an integral assembly (for example, H. Mahon, U.S. Pat. No. 3,228,876, Mahendran et al. U.S. Pat. No. 6,685,832). These systems offer the advantage that the potting compound flows readily between the fibers, but methods utilizing these adhesives for potting fluoropolymer membranes in general and PTFE membranes in particular suffer from serious limitations. The adhesion of epoxies, cyanoacrylates, and polyurethanes to fluoropolymer fibers, in general, and PTFE in particular, is very limited, resulting in assemblies that suffer from fiber pullout and failure due to pressure or thermal cycling. More importantly, materials such as epoxies, polyurethanes, cyanoacrylates, etc. suffer from very limited chemical and thermal stability, thus greatly limiting the types of high temperatures or harsh or aggressive chemical environments for which one would want to use PTFE hollow fibers.
[0027] Some practitioners avoid the use of potting compounds such as epoxies, polyurethanes, cyanoacrylates, etc. via melt bonding the fibers, eliminating the use of potting compounds all together. Melt bonding has it's own limitations.
[0028] Muto et al. (U.S. Pat. No. 5,066,397), Suzuki et al. (U.S. Pat. No. 7,291,204B) and other practitioners teach methods for assembling thermoplastic hollow fiber membranes via a fusion process. In both the Suzuki and the Muto fusion process at least one set of the ends of the hollow fibers are bundled together and heated above the softening point of the hollow fibers allowing the ends to form into a solid end terminal block. PTFE however will not fuse with itself unless exposed to temperatures in excess of 340 C and very high pressures (greater than 50 bar). Exposure to the extreme temperatures and pressures would crush the fibers and destroy the porous structure, thus rendering the Muto process and others like it, that require a melting or softening of the hollow fiber membrane, unsuitable for PTFE. The fusion method employed by Muto, Suzuki, and others also suffers from the limitation of not being able to control the fiber spacing, something necessary for high solids filtration applications or larger high flow rate contactors where the tightness may restrict the flow.
[0029] Spiegelman et al. (U.S. Pat. No. 7,625,015) teaches the use of a connector with a series of pre-drilled holes through which fibers are placed and then crimped in place via an external swaging ring. A major limitation of the Spiegelman method is that the fibers must have a significant degree of rigidity to maintain the seal. Sealing with a tight clamp as required by Spiegelman would crush the soft PTFE fibers and a tight, leak proof seal would not be achieved. This method would not be suitable for contactors with desired high packing density.
[0030] U.S. Pat. No. 5,695,702 (Niermeyer) teaches a technique for building and sealing the ends of hollow fiber membranes into a module by contacting an array of hollow fibers with an extruded molten thermoplastic polymer. The molten thermoplastic polymer flows over and in between the hollow fiber ends as they are assembled into an array. The process as described by Niermeyer is not effective for PTFE hollow fibers and not as efficient as the present invention herein for any fluoropolymer fiber for several important reasons. The Niermeyer process requires that the molten thermoplastic polymer be heated and applied at a contact temperature higher than the melting point of the hollow fiber membrane. This allows the material to flow between the fibers and more importantly results in at least partial melting of the hollow fiber membrane wall to form an integral bundle. For PTFE hollow fiber membranes, heating the fiber or exposing the fiber to temperatures near or at its melting point (327 C-345 C depending on degree of sinter) would destroy the integrity of the fiber, changing the pore structure of the hollow fiber.
[0031] In addition, as known by those practiced in the art, the type of thermoplastic polymers cited in Niermeyer that are capable of being extruded into an unsupported molten web, are very viscous in their molten state; and thus, it would require large gaps between the fibers to allow the melt to flow between the fibers; a critical requirement to form a leak free potted assembly. The Niermeyer technique requires that the molten polymer flow quickly between the fibers before the next layer is applied on top or the unit will leak. This flow is driven strictly by gravity, as there is no means of forcing the melt between the fiber. The spacing between the adjacent fibers and between layers of fibers is large, resulting in poor fiber packing density and loss of efficiency of the finished unit.
[0032] Huang et al. (U.S. Pat. No. 5,284,584) teaches a method very similar to Niermeyer, as Huang also utilizes a melt extrusion potting method. However, in Huang, the molten thermoplastic extrudate used for potting must have a melting point 10° C. or lower than that of the fiber, while in Niermeyer the extrudate is at a higher temperature than that of the fiber. Although this overcomes the limitation of having to use extreme temperatures for extrusion potting utilized in the Niermeyer patent, Huang does not address the issue that the use of a melt for potting prohibits high packing density of the fibers. However, this imparts another limitation, as cited by Niermeyer, the lower temperature used for potting in Huang limits the use temperature of the finished device made by such a technique. Most limiting is that Huang also claims that the fiber tubes are only thermoplastic. Huang also only claims polyolefinic tubes, and more highly prefers (in the specification) polyolefin tubes as well as polyolefinic potting agents.
[0033] Cheng et al. (U.S. Pat. No. 6,663,745 and its patent family) teaches a method employing a perfluorinated polymer for potting perfluorinated hollow fibers which overcomes only some of the difficulties outlined earlier. In Cheng, a solid mass of a perfluorinated polymer is heated and degassed in an oven to a molten state and a set of looped hollow fibers are suspended in a hole created in the molten polymer. Driven by gravity, the molten potting polymer flows between the hollow fibers, filling the voids between the fibers. The resultant mass is cooled, annealed, and the bottom of the potted mass is cut off to reveal the open lumens. The Cheng method contains severe method and practical limitations for commercial hollow fiber modules. Cheng teaches that preparation of the potting polymer requires that the polymer be held at elevated temperatures 16 to 72 hours, and preferably 24 to 48 hours, to allow melting and degassing in the oven. The Cheng process requires the use of a polymer with a low enough melt viscosity to flow freely through the fibers, greatly limiting choices of potting materials, an additional 16 to 24 hours for the polymer to diffuse in amongst the hollow fibers, and an additional 16 to 24 hour annealing step following potting for a combined assembly time from 48 hours to five days.
[0034] The Cheng patent is also limited to smaller bundle diameters as the time required to diffuse into the center of larger units would be excessive, resulting in burnt polymer, very high assembly costs and the risk of voids in the potted assembly. Because Chung requires the unaided flow (other than gravity) of a highly viscous fluid between the fibers, the fiber packing density cannot be high, severely limiting the use of the contactor due to surface area limitations. Cheng also cites examples where the addition of a wire grid for spacing is required to achieve a packing density of only 60% for this reason. Addition of grids and other fiber spacing techniques adds cost and time to construction, as each fiber must be individually threaded through the mesh. The use of such grids would be unimaginable for typical commercial modules that employ thousands of fibers.
[0035] In WO2000/044483A2 (Yen, filed Jan. 27, 2000), Yen claims a method similar to Niermeyer, but for potting an all perfluorinated thermoplastic fiber membrane device. The Yen method also claims that a TFE/HFP or TFE/Alkoxy tape can be used in a potting method. However, Yen specifically prohibits the use of PTFE hollow fibers in his patent application, even excluding the use of PTFE in the claims: Yen states that PTFE is not a thermoplastic and that it is difficult to mold and form into various shapes. Of equal commercial concern is that the packing density in the Yen device is very low (as is the packing density of other potted systems in the literature carried out via a melt extrusion process) compared to the packing density of the invention herein. All of the polymer melt flowing potting methods are limited by the need to maintain significant spacing between the fibers to accommodate the flow of the very viscous polymer. Yen specifies 45-65% packing density in the preferred mode with the stated reason as to avoid incomplete potting and the formation of voids. Like the Niermeyer potting method, the Yen method has no control of packing thickness and packing density, and requires considerable time to assemble even a small unit. The Yen method also calls for a required post-potting heat treatment to ensure no voids or leaks in the potted end, a step that adds considerable additional costs for assembly.
[0036] In comparison to Niermeyer and Huang, the polymeric film potting method stated herein has the advantage of eliminating the need to allow space and time for a molten polymer to flow between the fibers. The film potting method also offers additional advantages over the Niermeyer process when applied to PTFE hollow fibers, in that the fibers may be spaced significantly closer to one another as no unessential space is needed for the flow of a very viscous fluid. In addition, polymeric film as a potting agent doesn't typically flow into the open holes at the end of the hollow fibers, so one doesn't have to add the additional method step of cutting and removing open fibers filled with potting agent.
[0037] The invention herein also overcomes limitations of Cheng. The film potting method is suitable over a wide variety of bundle diameters, including the number of fibers and choice of potting polymers. Furthermore, the present invention allows the designer to generate tightly packed fiber bundles or to deliberately create spacing between the fibers to enhance flow on the shell side of the module. In addition, larger units with greater numbers of fibers and the ability to control packing density offer significant design advantages to the end user. The film potting method stated herein also has advantages over the methods in the Muto and Spiegelman patents as it is a more gentle process and it does not lead to the crushing of the fibers. The film method also does not result in fiber contamination, as does methods using epoxies, polyurethanes, cyanoacrylates, and other non-fluoropolymers as potting agents.
[0038] As is apparent from the limitations cited in the above art, for fluorinated, and perfluorinated hollow fiber membranes in general, and PTFE hollow fiber membranes in particular, there exist many needs for improvements in potting methods that have not yet been satisfied. The limitations in the art and current day commercial potting needs are reemphasized below.
[0039] The ideal potted end has a long lasting and robust bond between the potting medium and the hollow fiber (the fiber must have strong adhesion to the potting compound so that the fibers cannot be pulled or pushed out under the temperature and pressure cycles of normal operation). Preferably, the potting method minimizes or eliminates any distortion or deformation that would otherwise damage or hurt the integrity of the hollow fiber. If the fiber is collapsed or distorted, a flow restriction may result, and the ensuing module would be less efficient. If the fiber is collapsed or damaged, the fiber may leak under subsequent operation, resulting in a defective module. A distorted fiber may not fully bond with the potting material, resulting in a flow path between the fiber wall and the potting compound, or between the fiber and shell, or potting material and shell, resulting in a leak and a defective module.
[0040] The ideal potting material is of a nature that it's thermal resistance, chemical resistance, chemical inertness, and chemical composition, do not limit the use of the hollow fibers, that is, the chemical resistance and service temperature of the potting material ideally would match or come close to matching that of the membrane itself. The potting compound generally is as chemically robust as the hollow fiber membrane or the range of applications of the module will be diminished and the end user will not be able to capitalize on the desired properties of the membrane.
[0041] The ideal potting method allows for efficient packing of fibers, meaning that the fibers can be packed closely together, accommodating as many fibers in the cross sectional area of the module as possible. The ideal potting method allows for control over the packing density of the fiber so that the designer can accommodate high solids level applications, high flow applications, and other conditions that may dictate larger spacing between fibers. The ideal potting method accommodates or is adaptable to any number of fibers as filters and contactors may range from a few fibers up to many thousands. The ideal potting method accommodates a wide range of fiber diameters without having to sacrifice module construction efficiency or packing density. The ideal potting method accommodates a wide range of fiber porosities and of varying softness. Finally, the marketplace dictates that the potting method should be cost effective, low in labor and short cycle times.
[0042] As will be disclosed, the invention that is the subject of this patent overcomes inadequacies of prior art as well as meeting desired characteristics outlined above.
DESCRIPTION OF THE DRAWINGS
[0043] The operation of the present invention should become apparent from the following description when considered in conjunction with the accompanying figures, in which:
[0044] FIG. 1 : Illustration of a typical array of hollow fibers
[0045] FIG. 2 : Support frame with hollow fibers wound over ends
[0046] FIG. 2 a Examples of frame end elements with varying spacing
[0047] FIG. 2 b Examples of frame end elements with varying spacing
[0048] FIG. 3 : Support frame with hollow fiber being wound over ends
[0049] FIG. 4 : End view of hollow fibers with first weave tape
[0050] FIG. 5 : Isometric view of hollow fibers and first weave tape
[0051] FIG. 6 : Isometric view of hollow fibers with two weave tapes
[0052] FIG. 7 : End view of hollow fibers with first weave tape and upper cross tape
[0053] FIG. 8 : End view of hollow fibers with first weave tape and one cross tape
[0054] FIG. 9 : Isometric view of hollow fiber web with completed tapes
[0055] FIG. 10 : End view of spiral wrapped hollow fiber web
[0056] FIG. 11 : End view of spiral wrapped hollow fiber web with collet compression
[0057] FIG. 12 : End view of spiral wrapped hollow fiber web with adjustable sleeving
[0058] FIG. 13 : End view of compressed and fused hollow fiber bundle
[0059] FIG. 14 : View of cross flow potted hollow fiber bundle
[0060] FIG. 15 : View of web prepared for dead end filter element
[0061] FIG. 16 : Completed dead end filter element
SUMMARY OF THE INVENTION
[0062] The posited challenges of potting or sealing soft hollow PTFE fiber membranes are addressed by the system of the present set forth below. The system reliably and rapidly seals PTFE hollow fibers together and fills the interstices between the fibers. Materials are identified that are chemically and physically compatible with both the hollow fiber membrane and the process fluids to be used in the contactor module. Additionally, the present system provides a device that incorporates the said potting system. The polymeric film potting system presented herein overcomes the challenges listed above by: not requiring the fiber wall to be softened (by excessive heating), by ensuring the bonding thermoplastic resin (in the form of a polymeric film) is in between each adjacent fiber, and by allowing very close fiber spacing, and high packing densities (due to the compressing means). This is also accomplished without the longer processing time necessary for a viscous material to flow under gravity in between the fibers.
[0063] The potting method described herein offers advantages over potting methods disclosed in the art for fluoropolymer membranes in general and PTFE membranes in particular. These advantages include: the ability to economically produce potted fiber bundles with high packing densities regardless of the diameter of the fiber or of the unit, applicability regardless of how soft the hollow fiber membrane, the ability to economically produce a wide variety of diameters and length modules, and short cycle times, regardless of the nature of the fiber or size of the unit.
[0064] The potting polymeric film utilized in the present system can be defined as any type of generally flat material whose length and width are significantly greater than its thickness, and usually, although not a requirement, whose length is far greater than its width. The potting film can have a thickness that is less than the diameter of the hollow fibers down to less than one hundredth of the diameter of the hollow fibers. It is ideal that the film be as thin as possible. In fact, the film can be very thread like in thickness, as long as it can be handled during manufacture. The length of the potting film (along the length of the hollow fiber) can be less than, or equal to, the diameter of the bundled fibers down to less than one hundredth of the diameter of the bundled array of fibers. Thinner film results in a higher fiber packing density. The width of the film can be equal to the length of the film, although the width is variable, as the more fibers that are used, the more film is needed to surround each fiber. It is preferred that the film be applied as close to the ends of the hollow fibers as possible, so that upon melting it does not flow into the hollow fibers. It is most preferred that the length of the portion of the film along the length of the hollow fiber is even with the ends of the hollow fiber, so that upon melting, the melted film does not flow into the ends of the hollow fibers. Any type of chemically resistant thin film can be used to form a web over the ends of fiber bundled in a generally parallel configuration. Herein, the film may be very chemically resistant and can be chosen from the list of perfluorinated copolymers of: TFE/HFP, TFE/Alkoxy, TFE/PPVE, TFE/CTFE, and copolymers of Ethylene such as Ethylene/TFE, Ethylene/FEP, and other similar fluorinated polymers such as DuPont™ SF-50 and Solvay™ Hyflon 940 AX, or fluorinated terpolymers of Ethylene/VDF/HFP (Dyneon™ THV).
[0065] In another embodiment the fluoropolymer or other polymer used for the film or potting compound may be dissolved in a solvent such as acetone, butyl acetate, ethyl acetate, N-methyl pyrrolidone, or methyl ethyl ketone to create an adhesion promoter or primer solution. One preferred polymer solution is comprised of fluorinated terpolymers of Ethylene/VDF/HFP (Dyneon™ THV) and butyl acetate. The dilute adhesion promoter solution may be applied to the ends or near the ends, or for that matter on any portion of the porous PTFE hollow fibers where the film will be applied, allowing the adhesion promotion solution to wick or infuse into the pore structure of the hollow fiber. Upon drying or removal of solvent, the residual polymer or adhesion promoter that is infused into the inner pores of the fiber promotes enhanced adhesion between the potting film and hollow fibers.
[0066] According to one aspect, the present invention provides a fluid transport device having a plurality of perfluorinated polymer fibers that have an inner diameter and an outer diameter. At least one end of each fiber is open for fluid entrance or exit. The fibers are substantially parallel to one another and a length of polymeric film bonds the fibers together by contacting outer surface areas of the fibers adjacent ends of the fibers and filling interstitial volume between the fibers
[0067] According to another aspect, the present invention provides a hollow fiber membrane fluid transport device comprising a cylindrical containment shell containing polytetrafluoroethylene hollow fibers treated with a solvent polymer solution. The solution comprises a polymer used to prepare a potting film so that after solvent removal by drying, the fibers are bound together in bundles by at least one segment of film interwoven through interstitial spaces between the fibers and contacting each fiber near or at the ends of the bundles of the fibers.
[0068] According to yet another aspect, the present invention provides a method for producing a hollow fiber membrane fluid transport device. The method includes the step of laying polytetrafluoroethylene hollow fibers in an array or a row. Fluorinated homopolymer, copolymer, or terpolymer film is applied to the hollow polytetrafluoroethylene fibers interwoven between the fibers near one end or both ends of the hollow polytetrafluoroethylene fibers. The fibers and film are rolled into a bundle. A portion of the bundle is then heated and compressed to melt the film such that the film melts and flows between the hollow fiber to form an integral bundle of hollow fibers. The bundle is the cooled to form a solid mass providing a fluid-tight seal around each fiber such that the ends of the hollow fibers are open on one side of the solid mass and the open fiber ends are isolated from the fiber walls of the membrane.
[0069] According to a further aspect, the present invention provides a method for producing a hollow fiber membrane fluid transport device. According to the method, a plurality of polytetrafluoroethylene hollow fibers are arranged in an array or a row. A fluorinated homopolymer, copolymer, or terpolymer film on the hollow polytetrafluoroethylene is applied to the fibers so that the film is interwoven with the fibers near one end or both ends of the hollow polytetrafluoroethylene fibers The fibers and film are rolled into a bundle. The bundle is heated and compressed to melt the film such that the film is applied to the fibers at a contact temperature lower than the melting point of the fibers thereby causing the hollow fibers to form a bundle of hollow fibers. The bundle is then cooled to form a fluid-tight seal around the fibers such that the ends of the hollow fibers are open on one side of the solid mass and the open fiber ends are isolated from the fiber walls of the membrane.
DETAILED DESCRIPTION OF THE INVENTION
[0070] This invention provides a simple, fast, and reliable method for producing a membrane contactor comprising a plurality of hollow fiber membranes produced from polytetrafluoroethylene or other fluoropolymers employing a potting compound comprising of a perfluorinated or fluorinated thermoplastic to seal the ends of the hollow fibers and bind them into a solid mass. The invention further provides for the membrane contactor or filter module made by the inventive method.
[0071] The hollow fiber membranes used in this invention are produced from polytetrafluoroethylene homo or copolymers, but the technique is applicable to any polymeric or inorganic hollow fiber membrane, and represents an excellent technique for potting ceramic hollow fiber membranes as it minimizes risk of breakage of the fragile fibers.
[0072] The potting film that is used in this invention may be produced from any fluorinated or perfluorinated thermoplastic such as: PFA (polytetrafluoroethylene perfluoropropyl vinyl ether), FEP (perfluoroethylene propylene polymer), MFA (polytetrafluoroethylene perfluoro methyl vinyl ether), PVDF (polyvinylidene fluoride), THV (tetrafluoroethylene, hexafluoropropylene, vinylidene fluoride terpolymer), EFEP (ethylene perfluoroethylene propylene polymer), ECTFE (ethylene chlorotrifluoroethylene polymer), ETFE (ethylene tetrafluoroethylene polymer), or other fluorinated or perfluorinated thermoplastics. Preferred compounds are EFEP and THV for lower temperature applications (below 120° C.), MFA and PVDF for applications up to 150° C., and FEP or PFA for applications up to 200° C.
[0073] The potting film may be any of a variety of commercially available fluoropolymer or perfluropolymeric films manufactured from the resins listed above (DeWal Industries, Ajedium, are examples of commercial suppliers) or may be extruded as a film via a melt extrusion and calendaring operation known to those practiced in the art or produced by compression molding granules, powder, or pellets into a thin film between two heated platens, or cast from a solution prepared from granules, powder, or pellets of the resins listed above. The preferred method is a film produced via extrusion and calendaring operation.
[0074] The film is prepared to a thickness of between 0.01 mm and 2.5 mm, with the preferred thickness between 0.076 mm and 0.125 mm and is generally dependent on the spacing desired between the fibers and the diameter of the fibers.
[0075] Shown in FIG. 1 , the construction of a two dimensional plane of fibers 10 is the starting point for the film potting method and this two dimensional plane of fibers is hereafter referred to as the web 5 . The web can be prepared via different techniques. A number of hollow fibers of a given diameter and porosity are placed in a substantially parallel arrangement by either securing individual fibers to a support frame, or by wrapping a single length of hollow fiber multiple times around a support frame or by any other such means as to generate a two dimensional plane of fibers held stationary and parallel to one another.
[0076] The support frame may be one of any number of suitable types of designs, but generally consists of three or four sides lying in the same plane, approximating a rectangle where each of the opposite pairs of sides are substantially parallel to one another. As shown in FIG. 2 , the pair of sides opposite to one another that serve as either the terminal points for the fibers or the ends over which the fiber is wrapped around are referred to collectively as the frame end elements 12 . The other side or pair of sides opposite to one another that are substantially parallel to the hollow fibers are referred to as the side elements of the frame 14 . It is preferred that the side element 14 or elements 14 are adjustable, allowing the frame end elements to be move apart from one another, enabling the frame to be used for multiple module lengths. It is also preferred that the end frame elements 12 are removable to allow either the spacing between the fibers to be adjustable or to adjust the width of the web being prepared. FIGS. 2 a and 2 b show two such types of end frame elements.
[0077] While individual fibers may be arranged along the perimeter of a frame and secured, one embodiment as shown in FIG. 3 is to wind a single hollow fiber 10 around the end frame elements 12 , creating two webs 5 of fibers, an upper web and a lower web, or one long web of double the length of the frame. The frame may be stationary and the fiber wrapped around the frame, or the frame may be rotated about an axis running parallel to the end frame elements 12 as the fiber is fed to the frame. The hollow fibers may be wound around a cylindrical mandrel, however, the use of the cylindrical mandrel is not as preferred as it inhibits the later weaving process and requires a different cylinder for each length of module desired.
[0078] It is also preferred that the spacing between fibers is maintained at a distance approximately equal to or slightly greater than the thickness of the potting film being employed, allowing the assembler the ability to control the spacing between the fibers and hence control the spacing between fibers in the final module. The spacing may be controlled by utilizing a few different methods. One method to control the spacing is to use frame end elements, examples of which are shown in FIGS. 2 a and 2 b that have a series of parallel grooves 15 or slots perpendicular to the major axis of the frame end element. A second method is to use a series of circular disks of known thickness placed in between adjacent fibers. In lieu of circular discs a variety of fin or comb-like structures that allow the fibers to be indexed at uniform spacing along the length of the frame end element can also be used. It is generally desirable that the spacing be equal at the two opposite frame end elements to ensure equal spacing between the fibers in the completed potted assembly.
[0079] A primer may be applied to further improve bonding between the potting film and the porous fiber. A dilute solution of the potting resin used to manufacture the potting film is prepared by dissolving either the film, pellets, granules, or powder forms of said potting resin in a suitable solvent. For a film produced from THV 220 may be suitably dissolved in acetone or methyl ethyl ketone. The percent solids in the solvent will be a function of the molecular weight of the polymer, but the solution should be suitably dilute to allow the film deposited to penetrate the pore structure of the fiber. A solution of 6 to 10% solids by weight is suitable, but solutions more dilute, down to 1% solids by weight are also acceptable and as high as 15% solids by weight will work. As the solids level increases, the penetration into the pore structure decreases and the thickness of the dried primer on the outside of the fiber increases.
[0080] If used, the primer solution is brushed or wiped onto the fiber ends where the potting film is to be applied, preferably covering the entire circumference of the fiber membrane. Additionally, preferably the primer solution is limited to covering only the portion which will eventually be covered by the potting film, because the primer penetrates the pore structure of the membrane and can block pores. The primer is allowed to dry in air for a minimum of two hours at 20° C. to 30° C. While application of heat will accelerate the drying process, this is less preferable as there is risk of forming bubbles from the solvent being released too quickly. After the primer has dried, the fiber array is ready for application of the film for the next step in the potting process.
[0081] Whether or not a primer is employed, the next step in the film potting process is to begin applying strips of potting film to the ends of the fiber web. As shown in FIG. 4 , typically a length of thin film 20 , preferably a fluoropolymer, is inserted between the fibers 10 in a direction substantially perpendicular to the major axis of the fibers at or near either of the frame end elements. FIG. 5 shows an isometric view of the fibers with one strip of film woven between them. The film 20 is first fed over the top of the first fiber 10 and underneath the adjacent fiber 10 . This sequence repeating itself in such a way as to ensure that each fiber has at least one layer of the film between that fiber and each adjacent fiber until all the fibers have been separated from one another by one layer of film.
[0082] The thin film 20 may be a single strip woven between the fibers, or, as shown in FIG. 6 , may consist of two or more strips 20 of film woven between the fibers in alternating directions next to one another, with the first strip passing over alternate fibers, the adjacent strip passing under those same alternate fibers, resulting in a longer potted portion of fiber. A second strip of film or set of film strips may then be woven in a similar manner at the opposite frame end element, depending on the type of module to be constructed. If the element is to be a cross flow element or a dead end filter element, both ends are fitted with the strips of film. If the web is to be unfolded to a double length, then no strips are applied at the opposite frame end element.
[0083] Following the insertion of one or more lengths of thin film alternating between the fibers, a length of thin film 22 is then placed perpendicularly to the major axis of the fiber as shown in FIG. 7 , on top of the array of fibers and along the same axis as the strips of film previously woven between the fibers. This strip of film may be wider or narrower than the band of woven strips, but preferably is of the same width as the combined width of the woven strips and is referred to as a crossing film. The thickness of this first crossing film may be of variable thickness, chosen by the assembler to control the distance between the fibers as they are bundled. Use of a crossing film is not necessary, but can help to ensure that the potted end is leak-free and also helps to control spacing between the fibers.
[0084] The crossing film and the woven film are then heated at a temperature that is greater than 10° C. above the melting point of the polymer from which the film was made until the crossing film fuses with the woven film strip or strips.
[0085] After bonding crossing strips to the woven strips at either or both ends of the frame, the frame may be flipped over and the process repeated on the reverse side at top and bottom, creating two identical webs ready for the last step prior to bundling. For a single web of double length, only one end on the reverse side is potted.
[0086] After applying the weave strips and the crossing strips, the web is removed from the frame. If the web was prepared by wrapping a hollow fiber, the fibers are cut along the major axis of the frame end elements separating the fibers into two webs, one formed on the top of the winding rack, one on the bottom. If only one end of the top web and bottom web were prepared with the fluoropolymer films, then the web is opened up on itself to form a single web of a length double that of the winding frame.
[0087] The single web or the two matching webs are then placed on a flat surface, with the face having the upper crossing film face down. A second crossing strip 24 is then placed along the woven strips, as shown in FIG. 8 , parallel to the previously applied crossing strip, but on the opposite sides of the fibers. If the opposite ends of the fibers were fitted with film, then a second crossing tape is applied to that end as well. FIG. 9 shows the completed web 5 of fibers 10 with woven film 20 and upper 22 and lower 24 crossing strips applied at both ends of the web.
[0088] On completion of the individual web, it is carefully rolled up upon itself as shown as an end view in FIG. 10 , allowing the ends of the fibers fitted with the strips of film to wind up in a spiral 30 . Additional webs may then be wound onto the roll simply by abutting the end of one web with the beginning of the other, having trimmed any excess of the film from the ends of each. Additional webs are applied until the final fiber count is achieved. The web may be wound up on itself or may be wrapped around a core piece to provide support or structure. The core piece may be a fluoropolymer rod or may be machined from stainless steel or other compatible metals or polymers. If one uses a metal core, it is important that the surface be roughened or pre-coated with a fluoropolymer that is compatible with the film used for potting to ensure good adhesion and no leakage between the fibers and the solid core piece.
[0089] The potted fiber bundle is completed by a combination of applied heat and compression. Radial compression of the taped end by heating and compressing means causes the fiber ends to translate radially toward the centerline of the cylindrical bundle, reducing the distance between adjacent fibers until all interstitial volume between the fibers is eliminated and the fused tape contacts all outer surfaces of the membranes. This results in a leak proof potted end. The compression and applied heat are essential for establishing void-free, leak free high packing density potted ends.
[0090] The radial compression may be achieved by any number of means taking into account several factor. It is desirable to compress the bundle at a rate that limits or avoids deforming the hollow fibers and/or causes the fibers to become closed off. It is also desirable to compress the bundle in a manner that maintains a substantially rectangular cylindrical shape to the potted end. The end fitted with the strips of film is heated to a temperature at least 10° C. above the melting point of the film and allowed to reach equilibrium. The time required to reach equilibrium is dictated by the size of the module.
[0091] The compressing means may be by several methods, all of which achieve a gradual compression and maintain a cylindrical shape while being heated: including but not limited to: heat shrinkable sleeving, various collet systems, adjustable centerline roller systems, and an adjustable sleeving system. There are other methods of achieving the compression that would be obvious to those skilled in the art on understanding the function of the compression.
[0092] Achieving compression via a collet system as shown in FIG. 11 consists of placing the rolled end 30 of the fibers fitted with the woven and crossing films in a collet system 31 of a diameter large enough to accommodate the rolled and uncompressed bundle whose closed diameter is equal to or less than the desired final compressed diameter of the fiber bundle. The collet assembly holding the bundle of fiber fitted with the potting films is placed in an oven or heated chamber and brought up to a temperature at least 10° C. above the melting point of the film used for potting.
[0093] Achieving the compression via an adjustable sleeving system as shown in FIG. 12 is achieved by placing a suitable band 35 of tempered steel around the rolled bundle 30 . The band consists of a strip of metal that has preferably been coated with PTFE or similar release agent. The width of the band should be no wider than the length of the potted region of the fibers. The band should overlap on itself by at least 5% and preferably about 25% to maintain a uniform circle and so when radially compressed via a circular clamp 23 , the end of the band slides over top of itself and reduces in diameter in proportion to the tightening of the outer band clamp. The thickness of the tempered steel is between 0.1 mm to 0.127 mm, but may be as thin as 0.0254 mm for smaller bundles and as thick as 0.05 mm for larger diameter bundles.
[0094] The fiber bundle is compressed until the desired final diameter is achieved and all the voids between the fibers have been eliminated. The final diameter may be simply where all the voids are eliminated but may be reduced more by further tightening of the bundle. The compressed potted end is removed from the heat source and allowed to cool at which time the compression means is removed from the potted end.
[0095] Depending on the number of fibers, the diameter of the fibers, the softness of the fibers, and the final diameter desired in the bundle, the compression means may be achieved in a single step or multiple applications. For larger bundles, generally exceeding 50 to 80 mm in diameter, benefit from multiple applications of the compression means during build-up of the fibers. FIG. 13 shows an end view of the potted fibers 10 in the solid mass of potting compound 35 .
[0096] For a cross flow module, the final bundled assembly has two potted ends 40 , each of which resembles the potted cross section shown in FIG. 13 . FIG. 14 shows a drawing of such a potted bundle.
[0097] To achieve a similar configuration for a dead-end or single potted end, one prepared end of the web 5 is flipped over on itself ( FIG. 15 ) while holding the other end stationary, resulting in the web 5 being twisted along the plane of the web with the result that the top strip 22 at one end of the web no longer lies in the same plane as the top strip 22 on the other end of the web. The web is then rolled and compressed in a manner similar to that previously outlined resulting in a potted bundle with looped fibers 10 shown in FIG. 16 .
Fiber Potting Characterization
[0098] To validate the integrity of the potted end, a test may be provided to show there is no leakage around the fibers between the fiber wall and the potting compound at elevated pressures. In the present instance, a method common to those practiced in the art was employed which involves the determination of the bubble point of the fiber using isopropyl alcohol. The bubble point method includes a number of steps. In the first step the fiber is wetted in isopropyl alcohol (IPA) and pressurized to ensure there is no trapped air in the pores of the fiber. The fiber is then looped and immersed in a clear container of IPA with the two lumen ends above the level of the IPA. Air pressure is applied to the lumen ends in small increments until the first bubble of air is observed on the outside of the fibers. The resulting pressure is the bubble point pressure and is an indication of the largest pore in the fiber as the IPA in that pore is the most readily (lowest pressure) displaced by the incoming air pressure.
[0099] The integrity of a potted end may be tested by sealing the potted end in a clear tube of plastic or glass and immersing the pendant hollow fibers in IPA. Air pressure is applied to the open lumen ends of the hollow fibers and the potted end is observed as well as observing the first appearance of a bubble on the fiber walls. If no bubbles appear at the wetted face of the potted end and the bubble point pressure matches that of the single fiber, the integrity of the potted seal has been shown.
[0100] To test the strength of the bond between the fiber and the potted assembly, a pull test has been developed that measures the force required to extract a single fiber from the potted end of the bundle (or break the fiber attempting extraction). The test consists of using a Chatillon Force Gauge on an individual fiber from one of the potted ends of the bundle. The bundle is placed under the slotted support bracket to hold it in place. An individual fiber is randomly selected, placed through the slotted support bracket, and tied to a “J” hook attached to the top of the force gauge. The force gauge is activated and extends upward pulling on the individual fiber to achieve separation from the potted bundle or breaking of the individual fiber, whichever comes first. Once the end point is reached, the machine automatically stops and displays the break force value in Newtons.
Comparative Example 1
[0101] Twenty hollow fibers with an outer diameter of 1.5 mm and an inner diameter of 1.0 mm and a porosity of 55% were potted using an epoxy potting compound formulated by Henkel Corporation (Loctite®) for use with fluoropolymer resins.
[0102] Two samples were prepared, with the fibers for the first sample left untreated while the fibers for the second sample were treated with a Corona Discharge to promote adhesion with the epoxy. The corona discharge consisted of five second exposures four times followed by rotation of the fiber by 90° and repeating the treatment until the fiber had been rotated 360°.
[0103] The epoxy was Loctite product X263572, developed expressly for use with fluoropolymers and other low surface energy polymers. Approximately 350 grams of resin were mixed with 122 grams of hardener. A fixture was made to suspend the fibers in a 100 ml beaker so that they did not touch the sides or the bottom of the beaker. The fibers were looped over the top of a rod so that the ends of the fibers were suspended in the resin.
[0104] The epoxy was cured for 10 hours at 22° C. followed by 2 hours at 65° C. and 2 hours at 120° C. to achieve a complete cure. Following cooling to room temperature for 4 hours, the beakers were removed and the bottom 2-cm was cut off from each potted end. The ends were polished to achieve a clean finish on the potted ends.
[0105] The adhesion between the fiber and the potting resin was tested using a Chatillon force gauge attached to an individual fiber and pulled to failure. In each case the failure mode was the fiber pulling free of the epoxy. For the untreated fiber, the average pull force required to pull out the fiber was 3.37 lbf or 15 Newtons. The treated fibers had an average pullout force of 7.53 lbf or 33.5 Newtons.
Example 1
[0106] In this example, the film potting method is used to make a cross flow module of 110 hollow fibers potted at both ends of the bundle.
[0107] 110 loops of a hollow fiber membrane prepared from polytetrafluoroethylene with an inner diameter of 1.5 mm and an outer diameter of 1.9 mm with a porosity of 40% were wrapped around a winding frame 400 mm from end to end and 250 mm wide. The winding frame was fitted with slotted rods at each end, with spacing between slots of 2.0 mm, ensuring spacing between the hollow fibers of 0.1 mm.
[0108] A potting film pre pared from Ethylene Fluorinated Ethylene Propylene copolymer (EFEP, Daikin RP 4020) with a thickness of 0.0762 mm, a width of 25.4 mm, and a length of 220 millimeters was woven between each individual fiber at the end of the winding frame. The film was passed underneath the first fiber on the frame and then alternately passed over the top of the next fiber and underneath the following fiber. This pattern was repeated until the film was passed between each fiber on the winding rack. The excess tape was trimmed off. A second strip of tape of similar size was placed on top of the hollow fibers (referred to as the top tape), directly above the woven strip. The end of the winding rack containing the tape was heated above its melting point of 160° C. by means of a forced air heat gun set at 450° C. for 45 seconds. The potting tapes melted sufficiently to attach to each other and to the hollow fibers.
[0109] The weaving process was repeated at the other end of the winding rack, followed by application of a top layer of film heated and bonded to the fibers and the woven film. The process was again repeated on the two ends on the back side of the winding rack.
[0110] The fibers were removed from the winding rack by cutting the fibers along the major axis of the slotted ends containing the tape, forming two webs of fibers bound by the potting tape. Each woven web containing 110 fibers was laid on a flat surface with the side fitted with the top tape facing downward. A third piece of potting film of similar dimensions (bottom film) was placed over the hollow fibers directly above the other two films and heated in a similar manner, bonding the two strips of film to one another and to the hollow fiber.
[0111] The first web was subsequently wound into a tight cylinder, being careful that the ends remained parallel and that the diameters of each end were identical. The second web was subsequently added to the end of the first web and continued to be wrapped, resulting in a final diameter of approximately 38 mm in diameter.
[0112] To compress the bundle ends and occlude any voids, each taped end was fitted with a sleeve of a fluoropolymer heat shrink with an inner diameter of 38 mm (FEP 160 DuPont, 1.3:1 expansion ratio) approximately 25 mm long. Each taped end was then placed in an oven at 232° C. for 30 minutes. The heat shrink tubing reduced in diameter, compressing the bundle of fibers into a contiguous mass. The resulting mass was allowed to cool for 30 minutes. The fluoropolymer heat shrink was then cut from the potted end.
[0113] The potted bundle final diameter was 32 mm with a packing density of 78%. Examination of the potted ends via optical microscopy revealed no voids in the potted ends and good contact between the EFEP potting resin and the fibers. The resulting module was pressure tested by using the method outlined above and found to be fluid tight.
[0114] Subsequent testing of the individual fibers showed a pull strength of greater 75 Newtons, with the fiber failing before the bond with the potting.
Example 2
[0115] In this example, the film potting method is used to produce a dead-end filter module. A continuous length of porous PTFE hollow fiber with the dimensions of 1.0 mm inner diameter and 1.5 mm outer diameter, with a specific gravity of 0.9 grams/cm 3 was employed for this module. Using the winding apparatus previously described in Example 1, the fiber was wound between the two end pieces 120 times to create two 120-fiber webs on the top and bottom of the winding frame. The spacing between the fibers was maintained by machined grooves in the end pieces of the winding frame. The spacing between the fibers was set at 1.6 mm. The spacing between the two end elements of the frame was 610 mm. This process was repeated several times to generate sufficient fibers to make the unit.
[0116] A strip of 0.051 mm thick THV-220G film (Dyneon) with a width of 50 mm was woven in between the porous hollow fibers following previously described methodology at the two ends of the winding frame. After weaving one strip of film at each end of the winding frame, another strip of film of identical dimensions was placed directly over the top of the fibers. Using an industrial heat gun set at 450° C., hot air was passed over the film for approximately 30 seconds. The film was fused to the individual fibers as well as to the underlying film. This process was repeated on the opposite end of the frame. The frame was rotated to expose the opposing side and a second strip was applied over the woven strips at both ends of the frame as described above.
[0117] The fibers are then cut along the length of the two end pieces creating two individual webs of 100 fibers each that were approximately 610 mm long. Both webs were laid out on a flat surface with the sides without the 2 nd strip of film facing downward. A third piece of film was then bonded in a similar fashion on top of the woven film on both ends of the web, creating two 120 fiber webs with each end secured by a top film, a bottom film, and a woven film.
[0118] To prepare the dead-end filter, a section of a web containing 16 fibers was cut from a larger web. While holding the web on both ends, one end was rotated 180°. The web was then folded in half, laying the taped ends on top of one another. By this action the exit lumen of one fiber at the start of the web is placed adjacent to the entrance lumen of the furthest most fiber on the other side of the web. The web is rolled up at the taped ends to create a tight cylinder.
[0119] To compress the bundle into a solid mass, a 50 mm length of 12 mm ID FEP (1.3 to 1 ratio) heat shrinkable sleeve was subsequently placed over the bundled end placed into a tunnel heater at 218° C. for fifteen minutes. The bundle was removed and allowed to cool at room temperature for approximately 20 minutes. The heat shrink sleeve was carefully scored and removed from the bundled end.
[0120] Another small web of thirty-one fibers was twisted and folded in the same fashion as the first web and rolled around the original bundle. A 50 mm length of 38 mm ID FEP (1.6 to 1 ratio) heat shrink sleeving was placed over the bundle and heated at 218° C. for fifteen minutes. The bundle was removed and allowed to cool at room temperature for approximately twenty minutes, followed by removal of the FEP heat shrink sleeve. The process of preparing and folding web sections was repeated using webs of 63 fibers, 70 fibers, 80 fibers, 123 fibers, 50 fibers, each followed by compression with the appropriately sized FEP heat shrink and heating in the oven.
[0121] The final bundling process involves wrapping a 2,750 mm×5 mm wide strip of 0.127 mm THV 500G film/tape around the bundle and then placing a 5 mm long piece of 76 mm diameter FEP heat shrink sleeving over the tape and heat at 232° C. for thirty minutes. The bundle is removed from the oven and allowed to cool for forty-five minutes.
[0122] Following removal of the heat shrink sleeve, the final step in the method can comprise trimming off 25 mm of the potted end for a fresh clean finished bundle, exposing the open lumen ends. This finished “dead-end” cartridge produces an outside diameter of 67 mm, containing 433 individual fibers with 886 open lumen ends with an active filtration length of 250 mm. Pull strength of individual fibers were measured as described and averaged 70 N.
Example 3
[0123] In this example, the film potting method is used to produce a double ended cross flow module using double weaves. 200 loops of a hollow fiber membrane prepared from polytetrafluoroethylene with an inner diameter of 1.5 mm and an outer diameter of 1.9 mm with a porosity of 65% were wrapped around a winding frame 1000 mm from end to end and 400 mm wide, fitted with slotted rods at each end, with spacing between slots of 2.0 mm, ensuring spacing between the hollow fibers of 0.1 mm.
[0124] A potting tape prepared from Dyneon THV-220 with a thickness of 0.0762 mm, a width of 25.4 mm, and a length of 600 millimeters (referred to as the weave tape) was woven between each individual fiber at the end of the winding frame starting by passing under the first fiber, over the adjacent fiber, and continuing across the frame, resulting in a strip of potting film being interlaced between the fibers. The excess tape was trimmed off.
[0125] After completing the initial weaving step, a second piece of the THV 220 film of similar dimensions was woven next to the first piece of THV tape, reversing the weaving pattern from the first film. The second piece of film was woven by first passing the film over the first fiber, under the second fiber, and on until the second strip has been woven between all the fibers. This weaving process was repeated at the opposite end of the frame.
[0126] A strip of film that is double the width of the individual weaving strips but of the same length was placed on top of the hollow fibers (referred to as the top tape), directly above the woven strip. The end of the winding rack containing the tape was heated so that the film was brought above its melting point of 160° C. by means of a forced air heat gun set at 450° C. for 60 seconds. The potting tapes melted sufficiently to attach to each other and to the hollow fibers. This process was repeated at the other end of the winding rack. The process was again repeated on the two ends on the back side of the winding rack.
[0127] The fibers were cut at the ends of the winding frame to create two individual webs of fiber. Each web was placed on a flat surface with the top strip facing downwards and another strip of film applied across the woven strips and bonded in a similar fashion to the first side.
[0128] On completion of applying the potting film, the web is rolled up on itself. After rolling the 200 fiber web a diameter of approximately 46 mm was achieved. A 50 mm long piece of 38 mm (1.3/1) FEP heat shrink and slide over each end of the bundle. Each potted end is placed in an oven at 233° C. for a period of 30 minutes to achieve a finished diameter of approximately 39 mm after removing the FEP heat shrink.
[0129] The bundle was removed from the oven and allowed to cool for 30 minutes. Once cooled, the FEP heat shrink was removed and the second 200 fiber web was rolled onto the compressed bundle resulting in a diameter of approximately 56 mm. Another 50 mm long piece of 60 mm FEP heat shrink was placed over each end of the bundle and placed in an oven at 232° C. for a period of 30 minutes to achieve a finished diameter of 51 mm. The bundle was removed from the oven and allowed to cool for 30 minutes. The FEP heat shrink was removed and approximately 25 mm was trimmed off of each bundled end resulting in a clean flush cut with open lumen ends. The average pull-out strength was measured at 68 Newtons.
Example 4
[0130] In this example the tape potting method utilizing a spring steel compression is used to produce a dead-end filter module.
[0131] 200 loops of a hollow fiber membrane prepared from polytetrafluoroethylene with an inner diameter of 1.0 mm and an outer diameter of 1.4 mm with a porosity of 43% were wrapped around a winding frame equipped with slotted ends spaced at 1.5 millimeters, ensuring spacing between the hollow fibers of 0.1 mm.
[0132] A potting film prepared from Dyneon THV-220 with a thickness of 0.0762 mm, a width of 25 mm, and a length of 400 mm was woven between each individual fiber at the end of the winding frame resulting in a pattern wherein the tape was alternately passed over the top of one fiber and underneath the adjacent fiber. A strip of film of similar size was placed underneath the hollow fibers, directly beneath the woven strip. A third strip of film was placed above the woven strip. The end of the winding rack containing the film was heated via a hot air gun set at 450° C. for 45 seconds. The potting films melted sufficiently to attach to each other and to the hollow fibers.
[0133] The fibers were removed from the winding rack by cutting the fibers along the major axis of the slotted end containing the film. One end of the hollow fiber membrane web was then folded over on itself resulting in a 180 degree twist in the web. The two taped ends were laid on top of one another. The entire taped web was subsequently wound into a tight cylinder with the taped fiber ends wrapping up on themselves.
[0134] To achieve compression, the taped end was fitted with a sleeve of spring steel (0.178 mm 1095 grade tempered spring steel) approximately 130 mm long by 5 mm wide. The sleeve of spring steel was in turn fastened with two hose clamps to allow compression of the spring steel. Each taped end was then placed in an oven at 232° C. degrees for 30 minutes. Following 15 minutes of heating, the bundle was removed and the hose clamps tightened, resulting in a 10% reduction in the spring steel sleeve diameter, compressing the bundle of fibers and molten tape into a contiguous mass. The process was continued 2 times. The resulting mass was allowed to cool for 30 minutes.
[0135] The potted bundle final diameter was 35 mm with a packing density of 78% in a dead end configuration. The resulting module was pressure tested by observing the bubble point of the hollow fibers as outlined above and it was found to have a fluid tight seal.
[0136] Subsequent testing of the individual fibers showed an average pull strength of 71 Newtons.
Example 5
[0137] The following example illustrates the use of a primer solution of the potting resin to promote adhesion between the potting film and the porous PTFE hollow fibers being assembled into a module.
[0138] 110 loops of a hollow fiber membrane prepared from polytetrafluoroethylene with an inner diameter of 1.5 mm and an outer diameter of 1.9 mm with a porosity of 65% were wrapped around a winding frame 400 mm from end to end and 250 mm wide, fitted with slotted rods at each end, with spacing between slots of 2.0 mm, ensuring spacing between the hollow fibers of 0.1 mm.
[0139] After the fibers are secured to the winding rack, the ends of the individual fibers are pretreated with a solution of the potting resin, in this example a solution of Dyneon THV 220 prepared by dissolving 3 grams of THV 220 per 40 ml of acetone.
[0140] Using a synthetic bristle brush, a thin layer of the THV 220 solution is applied to both ends of each fiber, ensuring that the full circumference of each fiber was coated. The coating was applied from the end of each fiber in a distance equivalent to that of the potting film, in this case 25 mm. Following application of the primer coating, the THV solution was allowed to dry at room temperature for 120 minutes. After drying a second layer of the THV solution was applied to the fibers. The second coating was allowed to dry at room temperature for an additional 120 minutes.
[0141] A potting tape pre pared from Dyneon THV-220 with a thickness of 0.0762 mm, a width of 25.4 mm, and a length of 600 millimeters (referred to as the weave tape) was woven between each individual fiber at the end of the winding frame starting by passing under the first fiber, over the adjacent fiber, and continuing across the frame, resulting in a strip of potting film being interlaced between the fibers. The excess tape was trimmed off.
[0142] After completing the initial weaving step, a second piece of the THV 220 film of similar dimensions was woven next to the first piece of THV tape, reversing the weaving pattern from the first film, that is, passing over the first fiber, under the second fiber, and on until the second strip has been woven between all the fibers. This weaving process was repeated at the opposite end of the frame.
[0143] A strip of film that is double the width of the individual weaving strips but of the same length was placed on top of the hollow fibers (referred to as the top tape), directly above the woven strip. The end of the winding rack containing the tape was heated above its melting point of 160° C. by means of a forced air heat gun set at 450° C. for 60 seconds. The potting tapes melted sufficiently to attach to each other and to the hollow fibers. This process was repeated at the other end of the winding rack. The process was again repeated on the two ends on the back side of the winding rack.
[0144] The fibers were cut at the ends of the winding frame to create two individual webs of fiber. Each web was placed on a flat surface with the top strip facing downwards and another strip of film applied across the woven strips and bonded in a similar fashion to the first side.
[0145] On completion of applying the potting film, the web is rolled up on itself. After rolling the 110 fiber web a diameter of approximately 35 mm is achieved.
[0146] A 127 mm piece of 0.178 mm thick 1095 tempered spring steel was wrapped around each end of the bundle and secured with two standard hose clamps. The potted ends were placed in an oven at 233° C. for a period of 30 minutes. The bundle was removed and the hose clamps were tightened approximately 9 times to achieve an outside diameter of approximately 26.5 mm or 25% of the original starting diameter. The potted ends were allowed to cool for approximately 30 minutes and the clamps and tempered spring steel strip was removed. Approximately 25 mm was trimmed off each potted end resulting in a clean flush cut with open lumen ends. An average pull strength of 81 Newtons was measured.
[0147] It should be noted that throughout this patent application, for the sake of brevity, we use the term X/Y to represent a copolymer of X and Y, and the term X/Y/Z to represent a terpolymer of X and Y and Z. | A hollow fiber membrane fluid transport device's method of manufacture is disclosed wherein the fibers are comprised of Polytetrafluoroethylene (PTFE), and the potting materials are comprised of fluoropolymer based materials. The potting method described herein, utilizes a compressed chemically resistant fluorocopolymer and or fluoroterpolymer film, allows for ease of manufacture without destruction of the PTFE hollow fibers, with high packing densities, and without the processing complexity of pre-melting, extruding, or chemical crosslinking of any polymeric adhesives. Furthermore, the PTFE hollow fibers can be treated with a fluoropolymeric solvent solution before the chemically resistant film is applied to enhance the adhesion of the PTFE fiber to the film. PTFE hollow fibers, and its respective fluoro-co and terpolymers as potting films, impart high packing densities, superb chemical resistance and temperature resistance without membrane contamination, or low fiber pull strength, as is sometimes observed with standard potting materials such as polyurethane and epoxy. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to an image database apparatus and to a method of controlling the operation of the database apparatus.
2. Description of the Related Art
There are a variety of types of image database apparatus available. In one example of such an apparatus, keywords corresponding to images are registered in advance. When an image search is performed, a keyword is entered, whereby the image corresponding to the keyword is found. With an image database of this kind, however, appropriate keywords are entered in accordance with the sought images and therefore a great deal of labor is involved.
In another example of an image database apparatus, an image is drawn using draw software and an image that resembles the drawn image is found by a search. However, drawing an image that resembles the sought image is not always easy. Finding a desired image is difficult.
SUMMARY OF THE INVENTION
Accordingly, an object of the present invention is to find a desired image with comparatively little labor.
According to the present invention, the foregoing object is attained by providing an image database apparatus comprising an extraction device (extraction means) for extracting representative image data, which represents representative images of a plurality of frames, from an image database in which image data of a number of frames has been stored; a first display control device for controlling a display device in such a manner that the representative images of the plurality of frames represented by the representative image data extracted by the extraction unit are displayed in a coordinate area in a form in which they are distributed in accordance with characteristics of each of the representative images; a designating device (designating means) for designating a desired image from among the images of the plurality of frames distributed in the coordinate area based upon display control performed by the first display control device; a search device (search means) for searching the image database for an image having characteristics that resemble the characteristics of the image designated by the designating device; and a second display control device for controlling the display device in such a manner that retrieved images, which result from the search performed by the search device, are displayed in the coordinate area in conformity with the characteristics thereof.
The present invention provides also an operation control method suited to the image database apparatus. Specifically, the method comprises the steps of: extracting representative image data, which represents representative images of a plurality of frames, from an image database in which image data of a number of frames has been stored; displaying the representative images of the plurality of frames represented by the extracted representative image data on a display device in a form in which the images are distributed in a coordinate area in accordance with characteristics of each of the representative images; designating an image of a desired frame from among the images of the plurality of frames distributed in the coordinate area; searching the image database for images having characteristics that resemble the characteristics of the image designated; and controlling the display device in such a manner that retrieved images, which result from the search, are displayed in the coordinate area in distributed form.
In accordance with the present invention, representative images (representative image data) of a plurality of frames are extracted from images (image data) of a number of frames that have been stored in an image database. The extracted representative images of the plurality of frames are displayed by being distributed in a coordinate area (also referred to as a coordinate plane in which the characteristics of images are placed along the coordinate axes, which may or may not be displayed) in accordance with the characteristics of each of the representative images (color characteristics, lightness characteristics, saturation characteristics and dates of photography of the representative images).
An image resembling a sought image (an image whose characteristics resemble those of the sought image) is designated by the user from among the plurality of representative images displayed in the coordinate area. Images (usually a plurality) having characteristics that resemble those of the designated image are searched from the image database, and the images retrieved by the search are displayed in the coordinate area.
Since representative images of a plurality of frames are displayed in the coordinate area in distributed form, an image resembling the image sought by the user can be readily ascertained visually. Designating the sought image is comparatively easy. When the image is designated, images of a plurality of frames having characteristics that resemble the characteristics of the image are displayed in the coordinate area. The sought image can be selected from the images that have been re-displayed.
Since the labor involved in entering a keyword suited to an image is unnecessary, less effort is required to create the image database. Further, since images of a plurality of frames are displayed and the sought image is selected from these images, the desired image can be found relatively simply as compared with the case where an image resembling the sought image is drawn and an image resembling the drawn image is found.
Preferably, the apparatus further includes a device for performing control so as to repeat the designating of images by the designating device, searching by the search device and display control by the second display control device.
It is preferred that at least one of the first and second display control devices controls the display device so as to display images, in conformity with the characteristics thereof, in a coordinate area that is formed over the entire surface of one window.
Since the coordinate area itself is formed over the entire surface of one window (display screen), the size of one frame of an image appears larger in comparison with a case where one window is split into multiple areas and the coordinate area is formed in one of these areas. A plurality of representative images and other images, etc., displayed in this coordinate area become easier to view.
By way of example, the extraction device extracts the representative image data from image data obtained by applying a KL (Karhunen-Loéve) expansion to image data representing images of a number of frames that have been stored in the image database.
Representative images represented by representative image data extracted by the extraction device are extracted randomly, by way of example.
Preferably, coordinates axes in the coordinate area in which images are displayed in accordance with their characteristics based upon display control by the second display control device are more detailed than coordinate axes in the coordinate area in which images are displayed by being distributed based upon display control by the first display control device.
Even if images of a plurality of frames displayed in distributed form based upon display control by the second display control device have similar characteristics, these images are displayed in a form separated from one another. This makes it easier to find the sought image.
The number of frames of representative images displayed in the coordinate area based upon display control by the first display control device and the number of frames of images displayed in the coordinate area based upon display control by the second display control device may be made the same.
Since the number of frames of images to be displayed will not change, images can be maintained in an easy-to-view state by setting the number of frames of images to be displayed to a suitable number.
Other features and advantages of the present invention will be apparent from the following description taken in conjunction with the accompanying drawings, in which like reference characters designate the same or similar parts throughout the figures thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram illustrating the electrical structure of an image database apparatus according to the present invention;
FIG. 2 is a flowchart illustrating processing executed by the image database apparatus; and
FIGS. 3 to 5 diagrams showing examples of images displayed on a display screen in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Preferred embodiments of the present invention will now be described with reference to the drawings.
FIG. 1 is a block diagram illustrating the electrical structure of an image database apparatus embodying the present invention.
The overall operation of the image database apparatus is controlled by a CPU 2 .
The image database apparatus includes an image database 4 storing image data representing a number of color images (or monochrome images). Data representing the characteristics of the image data also is stored in the image database 4 in correspondence with the image data that has been stored. The characteristics of the image data include the percentage of color in an image, the average lightness of an image, the average saturation of an image and the date of photography of the image.
An output signal from an input unit 3 such as a keyboard or mouse is applied to the CPU 2 . The input unit 3 outputs a signal representing an image search command, a signal indicative of the fact that a specific image has been designated, etc.
Also connected to the CPU 2 is a VRAM (Video Random-Access Memory) 1 for temporarily storing image data representing an image to be displayed on the display screen of a display unit 6 . The display of an image on the display unit 6 is controlled by a display controller 5 .
FIG. 2 is a flowchart illustrating processing executed by the image database apparatus, and FIGS. 3 and 4 are diagrams showing examples of images displayed on the display screen of the display unit 6 .
The image database apparatus according to this embodiment is such that a plurality of images having different characteristics are displayed on the display screen of the display unit 6 as representative images from among the number of images that have been stored in the image database 4 . An image resembling a sought image is designated by the user from among the plurality of representative images thus displayed. A plurality of images having characteristics close to those of the designated image are re-displayed on the display screen of the display unit 6 . By repeating this processing, the required image is found by the user. Since the required image can be found from among images being displayed on the display screen of the display unit 6 , the required image can be found in comparatively simple fashion. Other features of the image database apparatus according to this embodiment will become obvious from the description that follows.
As mentioned above, the image database apparatus according to this embodiment is such that a plurality of representative images are displayed on the display screen of the display unit 6 . The representative images selected for this display have various characteristics. The representative images are displayed as follows, by way of example: Consider multidimensional space in which the image characteristics are placed along the coordinate axes. In such case the images are disposed in this multidimensional space. The distances and directions of respective ones of the images from the origin of this multidimensional space are calculated as feature vectors. Representative images having a variety of feature vectors are selected.
However, in actuality, images of a multiplicity of frames have been stored in the image database 4 , and the image characteristics of these images are actually multifarious. In order to calculate feature vectors of images of such a large number of frames, a great deal of calculation is required and calculation takes a long period of time. Accordingly, in the image database according to this embodiment, a KL (Karhunen-Loéve) expansion is applied to the image data that has been stored in the image database 4 , thereby reducing the number of dimensions (number of coordinate axes) of the space in which the images are placed (step 11 ). Since the images that have been stored in the image database 4 are disposed in space in which the number of dimensions has been reduced, the time required for calculation of feature vectors can be shortened.
The images that have undergone the KL expansion are disposed in space, after which representative images are extracted based upon the feature vectors of respective ones of the images (step 12 ). The representative images extracted are displayed on the display screen of the display unit 6 (step 13 ).
FIG. 3 illustrates the manner in which extracted representative images are displayed.
As shown in FIG. 3 , a coordinate area 23 has been formed over the entire surface of a display screen 21 . Ten frames of thumbnail images (representative images) Ir are displayed in the coordinate area 23 . The coordinate axes of the coordinate area 23 indicate characteristics of the images. The horizontal axis of the coordinate area 23 indicates image photography date, and the vertical axis indicates image lightness. It goes without saying that other image characteristics may be used on the coordinate axes. Further, the coordinate axes need not be displayed on the display screen 21 . It will suffice if the representative images Ir are displayed on the display screen 21 in distributed form in accordance with fixed image characteristics. In addition, a cursor 22 for designating a specific image is also displayed on the display screen 21 .
Using the input unit 3 , the user designates a representative image Ir having characteristics close to those of the required image from among the representative images Ir being displayed on the display screen 21 (step 14 ). More specifically, the cursor 22 is moved onto the desired representative image Ir and the image is doubled-clicked, for example, using the mouse included as part of the input unit 3 , whereby the image is designated. In this embodiment, it is assumed that the user has designated a representative image Is 1 in FIG. 3 .
When this is done, images possessing characteristics near those of the representative image Is 1 designated by the user are extracted from the image database 4 (step 15 ). Images of a number of frames identical with the number (ten) of frames of the representative images Ir displayed on the display screen 21 are extracted. It goes without saying that the number of frames of images extracted need not be the same. The extracted images (thumbnail images), denoted by reference characters It in FIG. 4 , are displayed in the coordinate area 23 on the display screen 21 by being distributed in accordance with the characteristics thereof, as illustrated in FIG. 4 (step 16 ). The coordinate axes of the coordinate area 23 that displays the extracted images It are made the same as the coordinate axes of the coordinate area 23 that displays the representative images Ir (i.e., the same image characteristics are used). However, the coordinate axes used in the coordinate area 23 that displays the images It extracted based upon the selected image Is 1 are more detailed than the coordinate axes used in the coordinate area 23 that displays the representative images Ir. More specifically, whereas a period from January to December and a lightness of from 0 to 7 are specified along the horizontal and vertical axes, respectively, of the coordinate area 23 shown in FIG. 3 , a period from July 1 st to July 31 st and a lightness of from 3.0 to 4.0 are specified along the horizontal and vertical axes, respectively, of the coordinate area 23 shown in FIG. 4 .
As shown in FIG. 4 , ten frames of images having characteristics resembling those of the image Is 1 selected by the user are displayed on the display screen 21 . If the thumbnail image (e.g., thumbnail image Is 2 ) of the required image is present among the images of the ten frames thus displayed, the thumbnail image of this required image is designated by the cursor 22 (“YES” at step 17 : end of search). As a result, the image representing the image that corresponds to the designated thumbnail image is displayed on the display screen of the display unit 6 . If a thumbnail image of the required image is not present among the images of the ten frames displayed (“NO” at step 17 ), then the image having the characteristics resembling those of the required image is designated again using the cursor 22 . As a result, thumbnail images of ten frames of images having the characteristics of the designated image are displayed on the display screen 21 . It goes without saying that the coordinate axes of the coordinate area appear in even greater detail also when the coordinate area is displayed on the display screen 21 again. For example, in a case where a thumbnail image It 1 having a lightness of 3.5 and a photography date of Jul. 10, 2000 has been selected, a coordinate area having a horizontal axis covering a period of from 00:00 to 24:00 on July 10 th and a vertical axis covering a lightness of from 3.4 to 3.6 would be displayed on the display screen 21 .
In the embodiment described above, a KL transform is applied to the image data and representative images are extracted from the images obtained by the KL transform. However, the KL transform need not necessarily be applied. Further, it may be so arranged that representative images are extracted randomly and not based upon feature vectors.
FIG. 5 illustrates an example of images displayed on the display screen 21 according to another embodiment of the present invention.
As shown in FIG. 5 , the display screen 21 is split into a left-half area that serves as a coordinate area 24 and a right-half area that serves as a detailed-image display area 25 .
Ten frames of thumbnail images are displayed in the coordinate area 24 by being distributed in accordance with their characteristics in the manner illustrated in FIGS. 3 and 4 . Detailed images (images having a higher image quality than thumbnail images) corresponding to the thumbnail images displayed in the coordinate area 24 are displayed in the detailed-image display area 25 . The right edge of the detailed-image display area 25 is provided with a scroll bar 26 . By scrolling up or down using the scroll bar 26 and by employing the cursor 22 , a detailed image that does not appear in the detailed-image display area 25 can be displayed in the detailed-image display area 25 from among detailed images I corresponding to the thumbnail images being displayed in the coordinate area 24 .
Since detailed images are thus displayed, the user can ascertain the details of an image that are not apparent from the thumbnail image thereof.
As many apparently widely different embodiments of the present invention can be made without departing from the spirit and scope thereof, it is to be understood that the invention is not limited to the specific embodiments thereof except as defined in the appended claims. | Ten representative images are extracted from an image database storing images of a number of frames. The extracted representative images are displayed in a coordinate area, along the coordinate axes of which the image characteristics of the images are plotted, in a form in which the images are distributed in accordance with the image characteristics possessed by the extracted representative images. An image having characteristics resembling those of a required image is designated from among the representative images displayed. Images of ten frames having characteristics resembling those of the designated image are again displayed in distributed form in a coordinate area having image characteristics plotted along the coordinate axes thereof. The coordinate axes of the coordinate area displayed the second time are made more detailed than those of the coordinate area displayed the first time. As a result, images having slightly different characteristics are displayed in separated form, thereby making it easier to find the required image. | 6 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the invention
[0002] The present invention relates to an embroidery machine, and more particularly to a multi-functional embroidery machine, which can simultaneously embroider sewing objects having various shapes, including a flat object, an object having a shape of a usual processed cloth, an object having a shape of a cap, etc., without replacement or addition of the machine or any separate part for the machine.
[0003] 2. Description of the Prior Art
[0004] As generally known in the art, embroidery machines can be classified into flat type embroidery machines and tubular type embroidery machines. In the flat type embroidery machine, a flat object is secured on a rectangular frame and is then embroidered by the cooperation between a sewing head and a reel unit In the tubular type embroidery machine, an object having a shape of a usual processed cloth, such as T-shirt, or a sewing object shaped like a cap is secured and embroidered by a processed cloth supporting flame or a cap flame. The flat type embroidery machine has a bed structure suitable for embroidering of a flat sewing object, and the tubular type embroidery machine has a structure suitable for embroidering of a tubular object and a sewing object for a cap. However, it is impossible for only one conventional embroidery machine to simultaneously embroider more than one kind of sewing objects (e.g., including at least two of a flat sewing object, a tubular sewing object, and a cap-shaped sewing object).
[0005] That is, in a conventional embroidery machine, a plurality of sewing heads and a plurality of reel units provided corresponding to the sewing heads are synchronized and operated by one driving source. The conventional embroidery machine has one driver which drives an embroidering frame. Thus, one embroidery machine cannot simultaneously embroider multiple kinds of sewing objects including flat objects, tubular objects, and sewing objects for caps.
[0006] In order to solve such problems, it has proposed an embroidery machine, which can embroider multiple kinds of sewing objects.
[0007] The embroidery machine is a flat type embroidery machine including a plurality of independent driving embroidering frames which are separately installed. In the embroidery machine, a plurality of sewing heads are divided into at least two head groups separately mounted on an upper beam. Each of the head groups includes an embroidering frame for securing a sewing object and an embroidering frame driver for driving the embroidering frame in X and Y directions.
[0008] In operation of the flat type embroidery machine, a flat object is secured to each embroidering frame corresponding to each head group, and then corresponding embroidering frame drivers are individually driven. Accordingly, sewing objects having different patterns can be simultaneously embroidered by one embroidering machine to maximize operation efficiency and mass production.
[0009] However, the independent-type driving embroidery machine as described above includes a shuttle bed having a short length suitable to embroider flat objects and has a difficulty m embroidering a tubular object such as a cap or a T-shirt
[0010] The shuttle bed and the embroidering frame driver (X and Y axis drivers) have structures in which a driving unit of a cap frame and a tubular round frame support member can not be mounted to the embroidering fame driver.
[0011] An embroidery machine has been required to solve such problems occurring as in the disclosed machine and to have a construction capable of simultaneously embroidering multiple kinds of sewing objects, including flat objects, tubular objects, and cap-shaped objects.
SUMMARY OF THE INVENTION
[0012] Accordingly, the present invention has been made to solve the above-mentioned problems occurring in the prior art and an object of the present invention is to provide an embroidery machine, which can simultaneously embroider sewing objects having various shapes, including a flat object, an object having a shape of a usual processed cloth, an object having a shape of a cap, etc.
[0013] Another object of the present invention is to provide an embroidery machine, which allows a worker to conveniently embroider a sewing object
[0014] A further object of the present invention is to provide an embroidery machine, which has a structure suitable for production of various kinds and small amounts of goods, can facilitate the production of goods, and thereby can reduce the manufacturing cost
[0015] In order to accomplish this object, there is provided an embroidery machine comprising: a plurality of sewing heads installed at an upper portion of a working table while being spaced a predetermined distance apart from each other, a plurality of shuttle beds being located at positions vertically corresponding to the sewing heads, the shuttle beds being arranged in a line; a plurality of embroidering frames installed between the sewing heads and the shuttle beds while being movable in X- and Y-axis directions; a plurality of X-axis drivers for moving each of the embroidering frames in the X-axis direction; a plurality of Y-axis driver for moving each of the embroidering frames in the Y-axis direction; a controller for controlling driving of the X and Y axis drivers; and an operating panel for displaying all information required for an embroidery pattern and an operation of embroidering and enabling input of the information, and wherein the sewing heads are grouped into at least two working groups, each of the embroidering frames is arranged for one of the working groups, and the embroidering frames have structures either identical to each other or at least two different structures.
[0016] Each of the embroidering frames includes at least one of a border frame unit, a tubular frame unit, and a cap frame drive unit A plurality of units corresponding to the plurality of heads are installed at each of the work groups are integrally formed on each other when the embroidery frame is the tubular frame unit or the cap frame drive unit Each of X and Y axis drivers includes a moving member and a driving source for moving the moving member, and the moving member of the X axis drivers includes a frame holder for securing the embroidering frame therein and mounted on the moving member of the respective Y axis driver. The frame holder reciprocates in an X direction by driving the X-axis driver.
[0017] Each of X and Y axis drivers includes a moving member and a driving source for moving the moving member, and the driving source is a rotary motor. The controller allows a worker to operate or stop one of the X and Y-axis drivers. The controller allows the plurality of embroidering frames to selectively embroider one pattern or different patterns, respectively.
[0018] One operating panel is provided in the plurality of working groups. The operating panel is located at a boundary between two working groups when the two working groups are used. The operating panel simultaneously or sequentially embroidering pattern and progress information for all working groups being in progress. One controller controls driving of the X and Y axis drivers.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The above and other objects, features and advantages of the present invention will be more apparent from the following detailed description taken in conjunction with the accompanying drawings, in which:
[0020] FIG. 1 is a perspective view for showing an embroidery machine according to an embodiment of the present invention;
[0021] FIG. 2 is a front view of the embroidery machine shown in FIG. 1 ;
[0022] FIG. 3 is a plan view of the embroidery machine shown in FIG. 1 ; and
[0023] FIG. 4 is a side view of the embroidery machine shown in FIG. 1 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] Hereinafter, a preferred embodiment of the present invention will be described with reference to the accompanying drawings. In the following description and drawings, the same reference numerals are used to designate the same or similar components, and so repetition of the description on the same or similar components will be omitted.
[0025] An embodiment of the present invention will be now explained referring to the FIGS. 1 through 4 .
[0026] FIG. 1 is a perspective view for showing an embroidery machine according to an embodiment of the present invention. FIG. 2 is a front view of the embroidery machine shown in FIG. 1 . FIG. 3 is a plan view of the embroidery machine shown in FIG. 1 . FIG. 4 is a side view of the embroidery machine shown in FIG. 1 .
[0027] As shown in FIGS. 1 through 4 , at least two working groups, each of which includes a plurality of sewing heads 110 , are installed on a front side of an upper beam 120 while being spaced a predetermined distance apart from each other. The sewing heads 110 in each of the working groups are spaced a predetermined distance apart from each other. A plurality of shuttle beds 130 , which cooperate with the sewing heads 110 to perform embroidering on multiple sewing objects, are installed at positions corresponding to the sewing heads 110 . Here, it is preferred that each of the shuttle beds 130 has a cylindrical shape.
[0028] Further, it is noted from the drawings that the embroidery machine includes a working table 200 , a plurality of embroidering frames, embroidering frame drivers 230 , controllers 320 , and an operating panel 310 . Each of the embroidering flames is disposed on the working table 200 to hold a sewing object so that the embroidering frames enable the embroidery machine to simultaneously embroider multiple kinds of sewing objects. Each of the embroidering frame drivers 230 moves each of the embroidering frames in X-direction or Y-direction. Each of the controllers 320 controls the embroidering frame drivers 230 to individually operate, so as to allow the embroidering frames to either embroider the same patterns or multiple patterns different from each other. The operating panel 310 displays all information required for progressing of the embroidering and allows input of such information. Here, the operating panel 310 may include a display device and a key input section, preferably a touch screen.
[0029] Also, a plurality of operating panels 310 may be separately installed for all working groups. However, in order to simplify the structure of the embroidery machine and reduce manufacturing cost, it is preferred that only one operating panel is installed for all the working groups. The operating panel 310 is arranged at a predetermined position on the working table 200 , which allows a worker to control all working groups by using the operating panel 310 . For example, as shown in FIG. 1 , the operating panel 310 is located at a boundary between two working groups, namely, at a center of the working table 200 when the two working groups are used.
[0030] Further, the worker inputs information required for embroidering operations of all working groups through the operating panel 310 . While all working groups are in progress, the worker simultaneously or sequentially displays embroidering patterns and progress information with respect thereto through the operating panel 310 . A display screen is divided into a plurality of screens corresponding to the number of the working groups and all information which the worker wants is simultaneously displayed on the divided screens. So, the worker simultaneously confirms embroidering situations of a plurality of working groups being in progress on one screen. If necessary, the progress information of the working groups is controlled to be displayed sequentially.
[0031] With reference to FIG. 3 , each of the X and Y-axis drivers 230 includes an X-axis moving member 240 , a Y-axis moving member 250 , an X-axis driving motor 220 , and a Y axis driving motor 210 .
[0032] A frame holder 260 is mounted in the X-axis moving member 240 , and secures the embroidering frame on the X-axis moving member 240 . Two Y-axis moving members 250 are vertically arranged at both ends of the X-axis moving member 240 . Since the X-axis moving 240 is mounted on the two Y axis moving members 250 , the X axis moving 240 and the two Y axis moving members 250 reciprocate the embroidering frame in X direction (left and right) and Y direction (front and back) by driving the X and Y axis driving motors 220 and 210 .
[0033] The X-axis moving member 240 includes a Y-axis driving motor 210 and X-drive timing pulleys 214 . The Y-axis driving motor 210 is installed at a rear center of the working table 200 by sewing head groups. The X-drive timing pulleys 214 are installed at left and right ends of a driving shaft of the Y-axis driving motor 210 . Each of the timing pulleys 214 is connected to each of Y-drive timing belts 212 .
[0034] Left and right ends of the X-axis moving member 240 are supported and fixed on the Y-drive timing belt 212 using connecting bracket 216 and a timing belt fixing plate (not shown). An X-axis driving motor 220 is mounted at an upper end of the X-axis moving member 240 .
[0035] The Y-drive timing belt 212 is connected to a driving source of the Y-axis driving motor 210 . The X-axis moving member 240 is directly connected to the Y-axis driving motor 210 on the Y-dive timing belt 212 . The X-axis moving member 240 reciprocates into a Y-axis direction (front and back directions) by driving the Y-axis driving motor 210 .
[0036] The X-axis driving motor 220 is mounted at an upper end of the X-axis moving member 240 . An X-drive timing belt 222 is connected to the driving source of the X-axis driving motor 220 . A frame holder 260 is mounted at the X-rive timing belt 222 using a belt bracket (not shown) and an L/M block connecting plate (not shown).
[0037] At this time, the frame holder 260 is connected to a border frame using a known locking member when the worker sews flat objects. The flame holder 260 is connected to a tubular frame unit by the known locking member when the worker sews tubular objects. The frame holder 260 is connected to a cap frame driving unit by the known locking member when the worker sews cap shaped sewing objects.
[0038] The frame holder 260 reciprocates in an X direction (left and right directions) by driving the X-axis driving motor 220 .
[0039] As described above, the X and Y axis drivers 230 moves the X axis moving member 240 into the Y direction by driving the Y axis driving motor 210 . Simultaneously, the X and Y axis drivers 230 moves the frame holder 260 into the X direction by driving the X axis driving motor 220 mounted on the X axis moving member 240 .
[0040] Each of the X and Y driving motors 220 and 210 includes a rotary motor such as an AC servo-motor and a stepping motor. When the rotary motor is used for the X driving 220 or the Y driving motor 210 , manufacturing cost, machine weight, and machine size are significantly reduced.
[0041] The controller 320 controls the driving of the X and Y driving motors 220 and 210 . The controller 320 controls the X and Y driving motors 220 and 210 which allows one of the X and Y axis drivers 230 to be operated or stopped according to the worker's instruction.
[0042] Regardless of the number of working groups each having a plurality of head groups, one controller 320 is preferably installed at one embroidery machine. X and Y locations of the X and Y drivers 230 are determined according to the direction and distance of the movement by the X and Y driving motors 220 and 210 under the control of the controller 320 .
[0043] Also, each of the sewing heads 110 installed at each of the working groups can selectively use a plurality of needle bars under a color converting control of each color changer 140 , so as to use sewing threads of various colors.
[0044] An upper surface of each sewing head 100 and an upper surface of the working table 200 are formed at the same surface. Needle plates are provided at upper front srufaces of the sewing head 100 and working table 200 .
[0045] In the embroidery machine 100 according to the present invention, a tubular frame unit 500 is mounted at X and Y-axis drivers 230 , which are installed at one side of the working, table 200 . The tubular frame unit 500 functions as a support member of a tubular round flame. A cap frame driving unit 400 is mounted at X and Y-axis drivers 230 , which is installed at the other side of the working, table 200 . Thus, the embroidery machine 100 simultaneously embroiders tubular objects as T-shirts and cap shaped sewing objects using the tubular flame unit 500 and cap frame driving unit 400 .
[0046] In another embodiment of the present invention, at least one of embroidering frames having different structures from each other are selectively mounted at the X and Y-axis drivers 230 . The embroidering frames include a tubular frame unit 500 which is a support member of a tubular round frame, a cap flame driving unit 400 , and a border flame (not shown) for securing flat sewing objects. If necessary, embroidering frames having identical structures are mounted at the X and Y-axis drivers 230 every working group, so that the same embroidering operations are simultaneously performed at all the working groups.
[0047] When the embroidery flame mounted at the X and Y axis drivers 230 is a cap flame driving unit 400 or a tubular flame unit 500 , the above embodiment of the present invention has been described for each unit installed to correspond to each sewing head 110 for one separately working group. According to another embodiment of the present invention, a plurality of units corresponding to a plurality of sewing heads for a working group are integrally formed on each other, and are attached and detached to and from the X and Y axis drivers 230 by the lump, respectively. In the case, it is very easy to attach and detach the units to and from the X and Y-axis drivers 230 , respectively, causing saving an operating time.
[0048] After performing the above-mentioned process, the worker selects embroidering pattern data to be embroidered on sewing objects, which are secured to the X and Y-axis drivers 230 .
[0049] According to the selected embroidering pattern data, the controller 320 moves the X and Y-axis drivers 230 which allows them to embroider each sewing objects. Since one embroidery machine simultaneously embroiders various kinds of sewing objects, the present invention is particularly advantageous in producing various kinds and small amounts of goods.
[0050] According to the present invention as described above, various kinds of sewing objects can be simultaneously embroidered by one embroidery machine. In addition, either identical sewing objects or different sewing objects, according to a worker's selection, can be simultaneously embroidered by one embroidery machine, so that productivity and operating efficiency can be maximized. Therefore, an embroidery machine according to the present invention is suitable for production of various kinds and small amounts of goods.
[0051] Further, an embroidery machine according to the present invention employs a rotary motor as the driving sources for X and Y-axis drivers, so that its manufacturing cost, machine weight, and machine size can be significantly reduced.
[0052] Furthermore, an embroidery machine according to the present invention may include only one operating panel installed at a predetermined location, for all working groups, which simplifies the structure of the embroidery machine and reduces manufacturing cost.
[0053] Although a preferred embodiment of the present invention has been described for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. | An embroidery machine can simultaneously embroider sewing objects having various shapes, including a flat object, an object having a shape of a usual processed cloth, an object having a shape of a cap, etc. The embroidery machine comprises a plurality of sewing heads grouped into at least two working groups, and the embroidering frames, each of which is arranged for one of the working groups. The embroidering frames have structures either identical to each other or different from each other. Therefore, one conventional embroidery machine can simultaneously embroider more than one kind of sewing objects, including at least two of a flat sewing object, a tubular sewing object, and a cap-shaped sewing object | 3 |
RELATED APPLICATION
This application is a continuation-in-part of U.S. Ser. No. 415,249 filed Nov. 12, 1973, and now abandoned.
1. Field of the Invention
This invention relates to polymerizable macrocyclic compounds containing 1 to 3 aza substituents and oxa substituents.
2. The Prior Art
The preparation of 3,3,-disubstituted oxacyclobutanes (oxetanes by preferred nomenclature) and their polymerization by electrophilic catalysts such as boron fluoride has been described by A. C. Farthing, J. Chem. Soc. 3648 (1955).
The reaction of the sodium salt of guaiacol with the tetra(para toluene sulfonate) derivatives of pentaerythritol in dimethyl sulfoxide has been reported to produce cyclic polyethers some of which contain spirooxetane rings by A. W. Archer and P. A. Claret Chem. & Ind. 1271 (1969).
C. J. Pedersen, J. Am. Chem. Soc. 89 7017 (1967) has described cyclic polyethers known as crown compounds which are capable of complexing cations, especially alkali metals.
B. Dietrich et al., Tetrahedron Letters, No. 34 2885 (1969), have described the preparation of macrocyclic polyethers containing two nitrogen atoms in the ring.
SUMMARY OF THE INVENTION
The compounds of the present invention have the formula: ##EQU3## WHERE Y is --XCH 2 CH 2 --X--, --X(CH 2 CH 2 X) 2 -- or ##EQU4## p is 1 to 4, and each X separately is O, NH, N-alkanoyl, N-benzoyl where the benzene ring is optionally substituted with --NO 2 , --NH 2 or --CH 3 ; N-alkyl, or N-β-hydroxyalkyl each of up to 8 carbon atoms with the proviso that the number of nitrogen atoms is from 1 to 3.
DETAILED DESCRIPTION OF THE INVENTION
The present invention is directed to macrocyclic compounds containing both oxa and aza linkages in the macrocyclic ring and also containing 1 or 2 spirocyclic oxetane rings. The presence of the nitrogen atoms in the ring enhances the complexing ability of the compound with heavy metal ions while the presence of the spirocyclic oxetane rings provide the capability for polymerization either directly by catalysis with electrophilic catalysts which open the oxetane rings, or indirectly by hydrolysis of each oxetane ring to a diol followed by reaction with diacid halide to form polyester, or with diisocyanates to form polyurethanes or the like.
In preferred compositions only simple oxa or aza (--NH--) linkages are present and the number of ring heteroatoms is 5-6, i.e., p = 1 in the generic formula examples are: ##EQU5##
2,9,12,15-tetraoxa-6,18-diazaspiro[3.15]nonadecane ##EQU6##
2,6,9,15,18-Pentaoxa-12-azaspiro[3,15]nonadecane ##EQU7##
2,6,12,16,19,25-Hexaoxa-9,22-diazadispiro [3.9.3.9] hexacosane ##EQU8##
2,6,12,15,21-Pentaoxa-9,18-diazaspiro[3.18]docosane
The spirooxetanes of this invention are prepared by reaction of 3,3-bis(chloromethyl)oxetane or 3,3-bis-(bromomethyl)oxetane with an aminoether in a polar, non-interfering solvent such as t-butanol, dimethylformamide, or tetrahydrofuran. The aminoether is terminated at each end by hydroxyl or amine groups. To the extent that the aminoether component has hydroxyl end-groups a base such as potassium t-butoxide or sodium hydride must be used to convert the hydroxyl to a reactive alkoxide. Bases such as sodium hydroxide and potassium hydroxide can also be used with only a small lowering of yield.
It is preferred to conduct the reaction at temperatures of 50°-100°C at 1 atm pressure for 1-24 hours. The temperature may vary, however, between 25°-100°C. If a pressure vessel is used, the pressure can be above 1 atm. Reaction times, depending on the temperature, may vary from a few minutes to a week.
The amine groups of the spirooxetanes can react with acid halides such as acetyl chloride, benzoyl chloride, p-nitrobenzoyl chloride, p-methylbenzoyl chloride and the like to yield alkanoyl derivative or benzoyl derivatives which may be substituted with alkyl, or nitro groups. The nitro groups can be catalytically reduced with hydrogen to yield aminobenzoyl compounds. Alkyl halides, particularly when the halogen is chlorine, bromine or iodine can be employed to alkylate the amino groups to form alkyl derivatives. The reaction of alkene epoxides with the amino groups gives β-hydroxy alkyl derivatives.
The products of this invention are isolated from their reaction mixtures by standard procedures of filtration, distillation, crystallization and extraction.
UTILITY
The monomeric azapolyoxasubstituted macrocyclic compounds of the invention find generic utility in their ability to complex metal ions. Their particular ability to complex with the heavier metals such as Cu + + , Ag + and Hg + + and transition metals such as Ni + + , Co + + and Pd + + is a distinction and advantage over the macrocyclic polyethers. These compounds may also be employed as monomers in cationic polymerizations to yield polymers which are capable of complexing metal ions.
SPECIFIC EMBODIMENTS OF THE INVENTION
The following examples are intended to illustrate this invention, but not to fully delineate the scope thereof.
EXAMPLE 1
2,9,12,15-Tetraoxa-6,18-diazospiro[3.15]nonadecane ##EQU9##
A mixture of 15.5 g (0.10 mol) of 3,3-bis(chloromethyl)oxetane, 19.2 g (0.10 mol) of 1,11-diamino-3,6,9-trioxaundecane, 38.7 g (0.30 mol) of diisopropylethylamine, and 500 ml of n-propanol was refluxed under nitrogen for 3 days. The mixture was cooled, treated with 21.2 g (0.20 mol) of anhydrous sodium carbonate, and refluxed an additional 5 hrs. The reaction mixture was then filtered and distilled in a molecular still to give 4.6 g (17%) of an approximately equimolar mixture of the isomers 2,9,12,15-tetraoxa-6,18-diazaspiro[3.15]nonadecane and ##EQU10## N-(11-amino-3,6,9-trioxaundecyl)-2-oxa-6-azaspiro[3,3]heptane. bp 108°-110° (0.1 μ). Ir 2.98 (sh) and 3.02 (NH), 6.26 (NH 2 rel weak), 8.9 (broad COC), 10.28 and 10.61 μ (oxetane ring); nmr indicated a mixture of oxetanes for which assignments could be made as described below.
Anal. Calcd for C 13 H 26 N 2 O 4 : C, 56.91; H, 9.55; N, 10.21; M.W., 274. Found: C, 56.92; H, 9.16; N, 9.88; 56.88 9.23 9.93; M.W. 274 (field ionization mass spec).
The mixture of isomers was separated by isolation of 2,9,12,15-tetraoxa-6,18-diazaspiro[3.15]nonadecane as the crystalline complex with NaSCN. A solution of 1.2 g (0.0044 mol) of the mixture and 0.32 g (0.004 mol) of NaSCN in 10 ml of acetone was evaporated to ca 5 ml, 5 ml of ether was added and the mixture was allowed to stand overnight. The supernatant liquid was decanted and the solid recrystallized from acetone/ether, then from acetone to give the 1:1 complex as large colorless cubes, mp 154.5°-155.5°. Ir (Nujol) 3.08 (HN), 4.85, (SCN), 8.8-9.5 (COC), 10.21 and 10.60 μ (oxetane); nmr (acetone-d 6 ) 1 H 4.43 (s, 2H oxetane CH 2 ), 3.67 (s, 4H, OCH 2 CH 2 O), 3.12 (s, 2H, C-CH 2 N), and 2.43 ppm (broad, 1H, NH) with rough triplets of an AA'BB': pattern at 225, 220.5 (hidden), 216 Hz (2H, NCH 2 CH 2 O) and 177, 172.5, 168 Hz (2H, NCH 2 CH 2 O).
Anal. Calcd. for C 14 H 25 N 3 NaO 4 S: C, 47.31; H, 7.37; N, 11.82; Na, 6.47. Found: C, 47.49; H, 7.21; N, 11.62; Na, 7.33.
The mother liquid from complex formation was evaporated to a viscous residue and the residue extracted with 50 ml of benzene. Evaporation of the benzene gave a residue which was extracted with 50 ml of pet ether. Evaporation of the pet ether gave an oil, nearly pure N(11-amino-3,6,9-trioxaundecyl)-2-oxa-6-oxaspiro[3,3]-heptane. Nmr (acetone-d 6 ) 1 H 4.60 (s, 2H, oxetane), 3.57 and 3.54 (both s, combined with 6H, NCH 2 CH 2 OCH 2 CH 2 OCH 2 CH 2 ), and 3.31 ppm (s, 2H acetidine) with rough triplets of an AA'BB' pattern hidden near 200 Hz and at 155.5, 150, and 144 Hz; NH 2 resonance uncertain due to impurity peaks.
EXAMPLE 2
2,6,9,15,18-Pentaoxa-12-azaspiro[3.15]nonadecane ##EQU11##
Preparation of the required 3,9-dioxa-6-azaundecan-1,11-diol was carried out as follows: ##EQU12##
A mixture of 450 g (3.6 mol) of 2-(2-chloroethoxy)-ethanol, 400 g of ammonia and 2 l. of absolute ethenol was heated at 125° for 15 hours under autogenous pressure in a 3-gallon autoclave. The dark reaction mixture was refluxed for 4 hours with 600 g of anhydrous Na 2 CO 3 , filtered and distilled to give 16.4 g (43%) of 1-amino-3-oxapentane-5-ol, bp 60°-65° (0.2 mm), and 145.3 g (42%) of 3,9-dioxa-6-aza-undecan-1,11-diol, bp 140°-145° (15μ). ##SPC1##
A solution of 62.0 g (0.40 mol) of bis(chloromethyl)oxetane, 94.0 g (0.84 mol) of potassium butoxide, and 77.2 g (0.40 mol) of 3,9-dioxa-6-aza-undecan-1,11-diol in 1 l. of t-butanol was refluxed and stirred under N 2 for 6 days. Filtration and evaporation of the reaction mixture to 50° (0.5 mm) gave a residue which crystallized on cooling. The crude 2,6,9,15,18-pentaoxa-12-azaspiro-[3,15]-nonadecane was kept molten at 90° and extracted continuously with heptane for 1 day. The cooled extract was filtered, and solid so isolated was recrystallized from ether to give 74.2 g (67%) of product mp 79°-81°. An analytical sample, mp 80°-81°, was recrystallized from ether. Ir (Nujol): 3.01 (NH), 8.6-9.1 (COC), 10.22 and 10.74 μ (ocetane). Nmr ((CD 3 ) 2 CO): 4.32 (singlet, 4, oxetane CH 2 ), 3.65(singlet, 4, C-CH 2 O), 3.57 (singlet, 12 with underlying OCH 2 CH 2 N, OCH 2 CH 2 ) and 2.32 ppm (broad singlet, 1, NH) with OCH 2 CH 2 N appearing as A 2 B 2 at 214 (hidden), 209, and 204 Hz (OCH 2 ) and 162, 157, and 152 Hz (4, CH 2 N). Addition of D 2 O moved the NH resonance downfield.
Anal. Calcd for C 13 H 25 NO 5 : C, 56.71; H, 9.15; N, 5.09; mol wt, 275. Found: C, 56.61; H, 8.88; N, 5.04; mol wt, 272 (cry. φH)
A 1:1 complex of this macrocycle with NaSCN was prepared in acetone, crystallized by concentration and addition of a small amount of ether and isolated in 93% yield, mp 113°-114°. A recrystallized sample had mp 113°-114°. Ir (Nujol): 3.03 (NH), 4.86 (SCN), 8.7-9.5 (COC), 10.36, 10.57 and 10.75 μ (oxetane). Nmr (CD 3 ) 2 CO: 4.43 (singlet, 4, oxetane CH 2 , 3.98 (singlet, 4, C-CH 2 O), and 3.73 (singlet, 12 with nearby OCH 2 CH 2 N, OCH 2 CH 2 O), with OCH 2 CH 2 N appearing as A 2 B 2 at 221, 216.5 and 211.5 Hz (OCH 2 ) and 174.5, 169.5, and 165 Hz (4, CH 2 N).
Anal. Calcd for C 14 H 25 N 2 NaO 5 S: C, 47.18; H, 7.07; N, 7.85; Na, 6.45. Found: C, 47.41; H, 7.14, N, 8.16; Na,6.06.
a. Alkylation of 2,6,9,12,18-Pentaoxa-12-azaspiro[3.15]-nonadecane ##SPC2##
A mixture of 27.5 g (0.10 mol) of 2,6,9,15,18-pentaoxa-12-azaspiro[3,15]nonadecane, 10 g (0.21 mol) of ethylene oxide and 200 ml of methanol was heated in a bomb tube at 100° for 6 hours under autogenous pressure. Solvent was evaporated, and the product was volatilized in a very short path still at 190° (˜20 μ), giving 27.6 g (87%) of N-hydroxyethyl-2,6,9,15,18-pentaoxa-12-azaspiro[3.15]nonadecane as a nearly colorless oil. Ir: 2.90 (OH), 8.7-9.5 (COC, COH), 10.23 and 10.80 μ oxetane). Nmr ((CD 3 ) 2 CO): 4.29 (singlet, 4, oxetane CH 2 ), 3.74 (singlet, 4, C-CH 2 O), 3.6-3.3 (multiplet, 15, OCH 2 CH 2 O + OH + OCH 2 CH 2 N), 2.85-2.5 ppm (multiplet, 6, CH 2 N).
Anal. Calcd for C 15 H 29 NO 6 : C, 56.41; H, 9.15; N, 4.39. Found: C, 56.43; H, 8.80; N, 4.54.
b. 12-(4'-Nitrobenzoyl)-2,6,9,15,18-pentaoxa-12-azaspiro-[3.15]nonadecane
A solution of 1.86 g of p-nitrobenzoyl chloride and 2.75 g of 2,6,9,15,18-pentaoxaspiro[3.15]nonadecane in 50 ml of benzene was treated with small portions of a solution of 1.10 g of triethylamine in benzene over a period of 5 minutes. The solution became cloudy and fine crystals deposited. After 2 hr the mixture was shaken with two 30 ml portions of water. The benzene layer was separated and dried (MgSO 4 ). Solvent was stripped under reduced pressure and the resulting colorless oil was analyzed. It did not crystallize and appeared to retain some solvent.
______________________________________Anal. Calcd for C.sub.20 H.sub.28 N.sub.2 O.sub.8 : C, 56.59; H, 6.65; N, 6.60Found: C, 58.23; H, 6.80; N, 5.59 58.64 6.89 5.73 58.05______________________________________
Nmr spectrum- δ 7.67 [4H] quartet (aromatic), δ 4.40 [4H] singlet (oxetane CH 2 ), δ 2.80 [4H] (spiro CH 2 ), δ 3.63 [16H] broad (OCH 2 and NCH 2 of macrocyclic ring). This agrees well with the assigned structure.
c. 12-(4'-Aminobenzoyl)-2,6,9,15,18-pentaoxa-12-azaspiro-[3.15]nonadecane
A solution of the nitro compound above in 100 ml of ethanol was hydrogenated on a Parr shaking apparatus using 10% palladium on charcoal catalyst. The mixture was filtered, and solvent was remove under reduced pressure. The resulting colorless oil (3.276 g) crystallized on standing to form a mass of silky needles. A 2.866 g portion was recrystallized from 25 ml of benzene to yield 1.78 g of white crystals which melted at 114.5°-117.5°.
______________________________________Anal. Calcd for C.sub.20 H.sub.30 N.sub.2 O.sub.6 : C, 60.89; H, 7.67; N, 7.10Found: C, 59.56; H, 7.57; N, 6.63 59.78 7.60 7.00______________________________________
d. Polymerization of N-hydroxyethyl-2,6,9,15,18-pentaoxa-12-azaspiro[3.15]nonadecane
Treatment of N-hydroxyethyl-2,6,9,15,18-pentaoxa-12-azaspiro[3.15]nonadecane with a slight excess of CF 3 SO 3 H over that required to neutralize the amine group led to polymer formation, as follows:
A solution of 18.5 g (0.058 mole) of N-hydroxyethyl-2,6,9,15,18-pentaoxa-12-azaspiro[3.15]nonadecane and 9.3 g (0.062 mol) of CF 3 SO 3 H in 300 ml of glyme had pH ˜6. Addition of a small amount of CF 3 SO 3 H did not increase pH, indicating rapid addition to the oxetane ring. The homogeneous solution was allowed to stand for 4 days at 25°, when two phases were present. Nmr showed oxetane to be nearly all reacted. After an additional 2 days at 25°, 2.6 g (0.035 mol) of lithium carbonate was added, and the mixture was refluxed for 3 hr. The lower layer was extracted with 50 ml of glyme, and the combined upper layer and glyme extract evaporated to give 24.8 g of glassy residue. Distillation at 160°-175° (0.05 mm) for 2 weeks removed only 1.6 g of oil; the residue was a hard glass which was insoluble in hot water.
e. Addition of Hydroxylic Compounds to Oxetane Ring of 2,6,9,15,18-Pentaoxa-12-azaspiro[3.15]nonadecane
The oxetane ring in 2,6,9,15,18-pentaoxa-12-azaspiro[3.15]nonadecane was shown to add hydroxylic compounds by acid-catalyzed reaction with 2-chloroethanol to give 1-hydroxymethyl-1-(4-chloro-2-oxabutyl)-2,5,11,14-tetraoxa-8-azacyclopentadecane. ##EQU13##
A solution of 27.5 g (0.10 mol) of the nonadecane and 7.9 g (in 400 ml of conc. H 2 SO 4 ) of 2-chloroethanol was heated at 100° for 31/2 days, after which time the nmr spectrum of an aliquot detected no oxetane ring. Solvent was evaporated, 900 ml of water added, and another 250 ml of distillate taken. The resulting solution was treated with 24.4 g of Ba(OH) 2 -8H 2 O, then carbonated to pH = 9 and filtered. The filtrate was diluted to 2500 ml with water, refluxed under N 2 for 3 days and evaporated to give 46 g of viscous residue. Product was acidic, indicating sulfate esters not completely solvolyzed, so the residue was dissolved in water, 40 g of BaCO 3 added and the mixture refluxed 2 hr. Isolation of the organic product and volatilization in a short-path still at 140°-145° (0.03 mm) gave 9.7 g (29%) of crude product. Mass spec (disilylated derivative): m/e 499 (M + ), 484 (M +-CH 3 ), 450 (M +-CH 2 Cl); empirical formula established as C 21 H 46 NO 6 ClSi 2 by high resol. mass spec.
EXAMPLE 3
2,6,12,16,19,25-Hexaoxa-9,22-diazadispiro[3.9.3.9]hexacosane ##EQU14##
A solution of 105.0 g (1.0 mol) of diethanolamine, 155.0 g (1.0 mol) of 3,3-bis(chloromethyl)oxetane, and 233 g (2.08 mol) of potassium t-butoxide in 2.5 l. of t-butanol was refluxed and stirred under N 2 for 2 days. The addition of oxetane, glycol, and butoxide was repeated, and reaction continued for 4 days. Filtration and evaporation of the filtrate to 60° (0.5 mm) gave a semisolid residue which was kept at 90° and extracted continuously with heptane for 3 days. Removal of heptane from the extract and recrystallization from ether gave 63.6 g (17%) of 2,6,12,16,19,25-hexaoxa-9.22-diazadispiro[3.9.3.9]hexacosane, mp 118.5°-119°. An analytical sample was recrystallized from tetrahydrofuran, mp 118.5°-119°. Ir (Nujol): 3.04 (NH), 8.6-9.5 (COC), 10.07, 10.29, 10.52 and 10.75 μ (oxetane). Nmr ((CD 3 ) 2 CO): 4.36 (singlet, 1, oxetane CH.sub. 2), 3.68 (singlet, 2 along with underlying OCH 2 CH 2 N, CCH 2 O), 2.30 ppm (very broad NH) with A 2 B 2 branches at 221 (hidden), 216.5 and 211 Hz (OCH 2 CH 2 N) and 172, 166.5 and 162 Hz (OCH 2 CH 2 N).
Anal. Calcd for C 18 H 34 N 2 O 6 : C, 57.73; H, 9.15; N, 7.48; mol wt, 374.5. Found: C, 57.62; H, 8.86; N, 7.61; mol wt, 398 (ebul φH).
a. Formation of Stable Complex of 2,6,12,16,19,25-Hexaoxa-9,22-diazadispiro[3.9.3.9]hexacosane
The presence of nitrogen in the macro rings of these products extends their ability to form stable complexes to ions of heavy metals such as copper and silver, as well as transition metals. For example, 2,6,12,16,19,25-hexaoxa-9,22-diazadispiro[3.9.3.9]hexacosane gives a 1:1 complex with cupric acetate.
A solution of 0.36 g (0.001 mol) of 8 and 0.20 g (0.001 mol) of Cu(OAc) 2 .H 2 O in 25 ml of absolute ethanol was deep blue in color. Removal of nearly all the ethanol and addition of 25 ml of ether gave 0.52 g (93%) of violet 1:1 complex, mp 156°-158° (dec). Recrystallization from ether/tetrahydrofuran gave an analytical sample, mp 159°-160.5° (dec). Ir (Nujol): 3.08 and 3.16 (NH), 6.21 and 6.29 (CO 2 - ), broad 9 (COC), and 10.24 and 10.77 μ (oxetane). Nmr ((CD 3 ) 2 SO): very broad peaks due to paramagnetic Cu + + .
Anal. Calcd for C 22 H 40 CuN 2 O 10 : C, 47.51; H, 7.25; N, 5.04; Cu, 11.43. Found: C, 47.64; H, 7.59; N, 4.95; Cu, 11.51
EXAMPLE 4
2,6,12,15,21-Pentaoxa-9,18-diazaspiro[3.18]docosane ##EQU15##
Preparation of the required 6,9-dioxa-3,12-diazatetradecane-1,14-diol was carried out as follows
HOCH.sub.2 CH.sub.2 NH.sub.2 + ClCH.sub.2 CH.sub.2 OCH.sub.2 CH.sub.2 OCH.sub.2 CH.sub.2 Cl→ (HOCH.sub.2 CH.sub.2 NHCH.sub.2 CH.sub.2 OCH.sub.2 ).sub.2
Two kilos (33 mol) of ethanolamine and 374 g (2.0 mol) of 1,8-dichloro-3,6-dioxaoctane were stirred and heated at 130° for one day. The mixture was cooled, 163 g (4.0 mol) of NaOH pellets were added, and the mixture was heated slowly with stirring to 100° and held there for 30 min. Most of the ethanolamine was then stripped off, 500 ml of tetrahydrofuran added, and the mixture filtered. Evaporation of the filtrate to 80° (0.5 mm) gave a concentrated product which was recrystallized from 1 l. of cold tetrahydrofuran to give 432.3 g (92%) of 6,9-dioxa-3,12-diazatetradecane-1,14-diol as an extremely hygroscopic solid, mp 49°-55°. An analytical sample was obtained by two recrystallizations from tetrahydrofuran, mp 53.5°-55°. Nmr ((CD 3 ) 2 CO): 3.7-3.4 (multiplet with major peak at 3.59, 3, OCH 2 ), 3.23 (broad, OH + NH), and 2.85-2.6 ppm (multiplet, 2, NCH 2 ). Addition of D 2 O moved the active H peak to 4.17 ppm (singlet, 1, OH + NH).
Anal. Calcd for C 10 H 24 N 2 O 4 : C, 50.83; H, 10.24; N, 11.86. Found: C, 51.22; H, 10.15; N, 11.67.
A solution of 202 g (0.855 mol) of 6,9-dioxa-3,12-diazatetradecane-1,14-diol, 132.8 g (0.855 mol) of 3,3-bis(chloromethyl)oxetane, and 191.5 g (1.71 mole) of potassium t-butoxide in 2.35 l. t-butanol was stirred and refluxed under N 2 for 5 days, cooled and filtered. The filtrate was concentrated to 50° (0.5 mm) and the residual oil extracted continuously with pentane for 4 days. Concentration of the extracts gave 198.4 g (71%) of a crude thick yellow oil. This product could not be purified by distillation, but nmr and ir indicated it to be 2,6,12,15,21-pentaoxa-9,18-diazaspiro[3.18]docosane. The structure was confirmed by isolation of the 1:1 complex with NaSCN in high yield as follows.
A solution in acetone (15 ml) of 3.18 g (0.01 mole of crude product and 0.81 g (0.01 mol) of NaSCN was evaporated to a volume of 10 ml and 5 ml of ether added. The cloudy solution was seeded with previously prepared complex and on standing gave 3.20 g (80%) of 1:1 complex, mp 147°-150°. Recrystallization from a small amount of acetone gave 2.63 g of complex, mp 151°-153.5°, shown by mixed mp to be the same as authentic complex. An analytical sample of similarly prepared complex had mp 151°-153°. IR (Nujol): 2.97 and 3.04 (NH), 4.82 (SCN), 8.5-9.5 (COC), 10.03, 10.48 and 10.53 μ (oxetane). Nmr (CCD 3 ) 2 CO): 4.36 (singlet, 2, oxetane CH 2 ), 3.90 (singlet, 2, CCH 2 O), 3.75-3.5 with major singlet at 3.64 for OCH.sub. 2 CH 2 O (multiplet, 6, OCH 2 ), and 2.23 ppm (broad, 1, NH), with one branch of A 2 B 2 at 173.5, 168, and 164 Hz (4, NCH 2 ).
Anal. Calcd for C 16 H 30 N 3 NaO 5 S: C, 48.11; H, 7.57; N, 10.52; Na, 5.75. Found: C, 47.76; H, 7.57; N, 10.60; Na, 5.65.
A 1:1 complex with NaI was similarly obtained as hygroscopic crystals, mp 143°-145°. IR (Nujol): 3.09 (NH), 8.5-9.5 (COC), 10.07 and 10.57 μ (oxetane). Nmr ((CD 3 ) 2 CO): 4.38 (singlet, 2, oxetane CH 2 ), 3.95 (singlet, 2, C-CH 2 O), 3.7-3.55 with major singlet at 3.67 (multiplet, 6, OCH 2 ), 3.0-2.7 (multiplet, 2, NCH 2 ), and 1.83 ppm (singlet shifted downfield by D 2 O, 1, NH).
Anal. Calcd for C 15 H 30 N 2 NaO 5 I: C, 38.47; H, 6.46; N, 5.98; I, 27.10. Found: C, 38.36; H, 6.37; N, 5.77; I, 26.90.
a. Acid-Catalyzed Hydrolysis of 2,6,12,15,21-Pentaoxa-9,18-diazaspiro[3.18]docosane
The oxetane ring in these macrocycles can be opened, by addition of water as well as of alcohols. For example, acid-catalysed hydrolysis of 2,6,12,15,21-pentaoxa-9,18-diazaspiro[3.18]docosane yields 12,12-bis(hydroxymethyl)-1,4,10,14-tetraoxa-7,17-diazacyclononadecane. ##EQU16##
A solution of 99.1 g (0.31 mol) of crude 2,6,12,15,21-pentaoxa-9,18-diazaspiro[3.18]docosane and 39.2 (0.4 mol) of conc. H 2 SO 4 in 2 l. of distilled water was refluxed for 3 days, treated with 32.0 g (0.80 mol) of NaOH pellets, and concentrated to low volume. Then 2 l. of xylene was added and distillation continued until the head temperature was 138°. The hot xylene was decanted and the residue was extracted with 2 × 500 ml hot xylene. Evaporation of the xylene extracts to 50° (0.5 mm) yielded 69.5 g (67%) of crude bis(hydroxymethyl)-1,4,10,14-tetraoxa-7,17-diazacyclononadecane as indicated by the ir spectrum (loss of oxetane band and appearance of hydroxyl absorption). A previous attempt to distill the diol resulted in considerable loss of product, but fractions with bp 188°-200° (0.15 μ) were obtained. A sharply melting 1:1 complex with NaSCN was obtained as follows:
A sample of crude bis(hydroxymethyl)-1,4,10,14-tetracoxa-7,17-diazacyclononadecane (3.4 g, 0.01 mol) and 0.81 g (0.01 mol) of NaSCN were dissolved in acetone and acetone evaporated to give a heavy oil. Addition of 10 ml of ether and scratching induced crystallization. Ether was decanted and the largely solidified residue was recrystallized from acetone to give 2.46 g (59%) of 1:1 complex, mp 137°-140°. An analytical sample was recrystallized from acetone, mp 141.5°-142.5°. Ir (Nujol): 2.98 (OH), 3.06 (NH), 4.88 (SCN), 8.7-9.5 μ (COC, COH). Nmr ((CD 3 ) 2 SO): 3.6-3.3 (multiplet with major peaks at 3.53 and 3.36, 5, OCH 2 ), 3.14 ppm (broad, 1, OH + NH, shifted downfield by D 2 O) with one branch of A 2 B 2 at 165, 160, and 155.5 Hz (2, NCH 2 ).
Anal. Calcd. for C 16 H 32 N 3 NaO 6 S: C, 46.03; H, 7.73; N, 10.06; Na, 5.51. Found: C, 46.41; H, 7.81; N, 10.24; Na, 6.24.
b. Acylation of 2,6,12,15,21-Pentaoxa-9,18-diazaspiro-[3.18]docosane
The amine function in these macrocycles can be acylated as well as alkylated, as shown by the following addition of a bridge to the two nitrogen atoms in 2,6,12,15,21-pentaoxa-9,18-diazaspiro[3.18]docosane under conditions of high dilution.
Solutions of 31.8 g (˜ 0.10 mol) of crude 4 in 200 ml of dry benzene and 17.1 g (0.10 mol) of diglycolyl dichloride in 210 ml of dry benzene were added dropwise and simultaneously to a vigorously stirred mixture of 50 ml of triethylamine and 1 l. of dry benzene. After addition was completed (3.5 hr), stirring was continued an additional 15 min, the mixture was filtered to remove polymer and amine salts, and the filtrate was evaporated to give 26.3 g of viscous residue. Crystallization from acetone gave 12.3 g (30%) of ##EQU17## mp 178°-181°. An analytical sample was obtained from acetone, mp 180.5°-182°. Ir (Nujol): 6.03 (C=O), 8.6-9.6 (COC), 10.27 and 10.78 μ (oxetane). Nmr ((CD 3 ) 2 SO): 1 H 4.3-4.0 (multiplet, 1) and 3.7-3.2 (multiplet, 2).
Anal. Calcd for C 19 H 32 N 2 O 8 : C, 54.79; H, 7.75; N, 6.73; mol wt, 416. Found: C, 54.88; H, 7.92; N, 6.50; mol wt, 417. (ebul φH). | Compound having the formula ##EQU1## WHEREIN Y is --XCH 2 CH 2 --X--, --X(CH 2 CH 2 X) 2 or ##EQU2## p is 1 to 4, and each X is O or NH, N-alkanoyl, N-benzoyl wherein the benzene ring is optionally substituted with --NO 2 , --NH 2 , or --CH 3 , N-alkyl or N-β-hydroxyalkyl each of up to 8 carbons and wherein the total number of N is 1 to 3 are disclosed. The compounds can be polymerized by opening of the oxetane ring in the presence of electrophilic agents, or the oxetane ring can be hydrolyzed to a dihydroxy group and reacted with diacid halides to form polyesters or with diisocyanates to form polyurethanes. Both monomers and polymers complex metal ions and can be used to separate such ions from solutions. | 2 |
BACKGROUND OF THE INVENTION
The present invention relates to a photometric system applied to an image pick-up device such as a still camera, a moving camera, a television camera, an industrial television camera and the like.
In case of photographing an object by a camera, it has often occurred that the object becomes too dark with rear light or the object becomes too bright when photographing at night. As a photometric system for eliminating such conventional disadvantage, Japanese Patent Laid-open No. 129,221/75 discloses such system that provision is made of a light receiver having a number of light-receiving elements consisting of an image sensor such as CCD (charge coupled device) or the like for receiving light present on the whole surface of the field of an object, thereby deriving a luminance signal of a previously selected necessary photometric portion among luminance signals corresponding to positions of an object successively obtained from the light receiver and carrying out spot photometry. Such photometric system, however, requires to designate a photometric portion, so that its operation is troublesome, and it is necessary to derive a luminance signal corresponding to respective photometric portions, so that its circuit construction becomes complicated and large. In case of photographing a moving object, it is difficult to correspond the object to a desired photometric portion, so that it is almost impossible to carry out precise spot photometry.
SUMMARY OF THE INVENTION
An object of the present invention is to eliminate the above described disadvantages of the conventional photometric system.
Another object of the present invention is to provide a photometric system capable of obtaining a desired light quantity with a simple construction.
A further object of the present invention is to provide a photometric system capable of constantly obtaining a proper light quantity in usual daytime photographing.
According to the present invention a photometric system comprises steps of forming an image focussed by a photo-optical system on a light receiver consisting of a plurality of charge transfer elements arranged in a picture element array; selectively deriving luminance signals of amplitude having a value within a range of a predetermined exposure value from luminance signals provided by the light receiver around a reference exposure value corresponding to a mean value between a maximum value and a minimum value of the amplitude of the luminance signals; and seeking a mean value of the selected luminance signals to photometrically measure the light of automatically selected portions on the average. A photometric system comprises the steps of forming an image focussed by a camera lens system on a light receiver consisting of a plurality of charge transfer elements arranged in a picture element array; selectively deriving luminance signals of amplitude having a value within a range of about ±2 exposure values around a reference exposure value corresponding to a mean value between a maximum value and a minimum value of the amplitude of the luminance signals; and seeking a mean value of the selected luminance signals to photometrically measure the light of automatically selected portions on the average. The reference exposure value corresponding to the mean value between the maximum value and the minimum value of the amplitude of the luminance signals can be varied within a range of about ±1 exposure value.
A photometric apparatus for use in an image pick-up device comprises a light receiver arranged at a focal plane of a camera lens optical system for receiving an image focussed by the camera lens optical system; a reference light quantity setting and generating circuit connected to the light receiver for generating a reference light quantity by obtaining a mean value between a maximum value and a minimum value of the amplitude of the luminance signals from the light receiver; a logarithmic compression circuit connected to the light receiver for logarithmically compressing the luminance signals from the receiver; a window comparator circuit connected to the logarithmic compression circuit and the reference light quantity setting and generating circuit for selecting luminance signals of amplitude having a value within a range of predetermined exposure value; a signal treating circuit connected to the window comparator circuit and the logarithmic compression circuit for treating the signals from the these circuits to obtain an average value of the amplitude of the luminance signals to the reference light quantity set in the reference light quantity setting and generating circuit; an information circuit for generating signals of exposure factors; an arithmetic circuit connected to the signal treating circuit and the information circuit for calculating the mean value output of the signal treating circuit and the exposure factors of the information circuit; a control device connected to the arithmetic circuit for controlling the shutter speed and the iris of the image pick-up device; and a display device connected to the arithmetic circuit for displaying the shutter speed value and the iris value of the image pick-up device. The light receiver comprises a plurality of light receiving elements consisting of an image sensor. The image sensor consists of a charge coupled device or a bucket brigade device. The reference light quantity setting and generating circuit comprises a rotary switch having three terminals, and these terminals are so switched that a proper light quantity for a daytime, a nighttime and a rear light photographing can be obtained.
As described above, the invention is to derive a luminance signal of an amplitude within the range of a predetermined exposure value and photometrically measure it on the average around a reference exposure value corresponding to a mean value between the maximum value and the minimum value of the luminance signal obtained from a light receiver.
The present inventors have confirmed from various experiments in usual daytime photographing what a good photograph can be obtained by how to set the range of the exposure value around a reference exposure value and found out that the range of about ±2 EV is proper.
BRIEF DESCRIPTION OF THE DRAWING
A single FIGURE is a circuit diagram showing one embodiment of a photometric system according to the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawing one embodiment of a photometric system according to the present invention will be described. In the present embodiment the case of applying the invention to a camera is explained.
A light receiver 1 is arranged to receive an image focussed on a focal plane of a camera lens which is not illustrated. The light receiver comprises a number of light-receiving elements (hereinafter referred to as picture element) consisting of image sensors such as CCD, BBD (bucket brigade device) or the like. The light receiver 1 receives predetermined signals from a clock signal generator 2 and a drive circuit 3 and successively supplies luminance signals of each picture element to a multiplexer 4. The drive circuit 3 and the multiplexer 4 are controlled by signals from a control circuit 5. The successive luminance signals in the first one frame of the light receiver 1 are supplied to a reference light quantity setting and generating circuit A through the multiplexer 4.
The reference light quantity setting and generating circuit A sets a voltage for selecting a luminance signal of an amplitude having a value within a predetermined range at a window comparator circuit B which will be explained later on, based on a mean value (reference light quantity) between the maximum value and the minimum value of the amplitude of the input luminance signal as a reference. To this end, the maximum value and the minimum value of the amplitude of the luminance signal applied through the multiplexer 4 are detected by a maximum value hold circuit 6 and a minimum value hold circuit 7, respectively, these maximum and minimum values are added by an adder 8, its mean value is sought by a divider 9, and a voltage corresponding to the mean value is delivered to an input terminal 12 of a switch 11 through an amplifier 10. The switch 11 comprises three switch contacts a, b and c, in which the contact a is grounded through resistors 13, 14, 15, 16 and 17 having predetermined resistance values, respectively, the contact b is connected to a junction point of the resistors 13 and 14, and the contact c is connected to a junction point of the resistors 14 and 15, respectively. A junction point of the resistors 16 and 17 and that of the resistors 15 and 16 are connected to two reference input terminals, respectively, at the window comparator circuit B, to supply reference voltages V 1 and V 2 for selectively deriving a luminance signal having an amplitude within a predetermined range based on the mean value as a reference.
In the present embodiment, when the terminal 12 of the switch 11 is connected to the contact b, a reference exposure value corresponding to the mean value is obtained, and when the terminal 12 is connected to the contact a or c, the reference exposure value is varied by ±1 EV (exposure value), and the reference voltages V 1 and V 2 are of values for deriving a luminance signal having an amplitude within the range of about ±2 EV around the exposure value at the connection of the switch 11 to the contacts.
The above described reference voltages V 1 and V 2 are set by scanning the light receiver 1 by one frame.
When the one frame scanning of the light receiver 1 is completed and the next scanning is started by the drive circuit 3 under control of the control circuit 5, the luminance signal at that time is supplied to a logarithmic compression circuit C through the multiplexer 4. This logarithmic compression circuit C comprises an operational amplifier 20, a diode 21 having a logarithmic characteristic and a variable voltage supply source 22, so as to connect a positive input terminal of the operational amplifier 20 to an output terminal of the multiplexer 4, to ground through the diode 21 connected in forward direction and the variable voltage supply source 22 or to connect a negative input terminal to an output terminal of the operational amplifier 20 and to supply a logarithmic compressed luminance signal as an output signal. This output signal is supplied to the window comparator circuit B and also to an A/D converter 25 through a gate circuit 24.
The window comparator circuit B comprises comparators 27, 28, amplifiers 29, 30 and an AND gate 31, so as to supply the above described two reference voltages V 1 , V 2 to one input terminal of the comparators 27 and 28, and to supply output signals of the logarithmic compression circuit C to the other input terminal of the comparators, respectively. The outputs of the comparators 27 and 28 are amplified to predetermined values in accordance with the outputs by respective amplifiers 29 and 30 and supplied to the AND circuit 31. The AND circuit 31 supplies a digital signal of a high level only when two input signals are in high level, that is, the output voltage V m of the logarithmic compression circuit C has a relation of V 1 <V m <V 2 .
The gate circuit 24 is controlled by the output of the window comparator circuit B and the output of the AND circuit 33 which receives a clock signal from the clock signal generator circuit 2, and supplies the output of the logarithmic compression circuit C to the A/D converter 25 by opening the gate 24 when the output of the AND circuit 33 is in high level. Further, the number of delivers for the digital signals of high level in one frame, that is, the number of picture elements in the logarithmically compressed luminance signals having the amplitude V m within a range of V 1 <V m <V 2 are counted by an adder 34.
The output of the logarithmic compression circuit C supplied to the A/D converter 25 is converted into a train of pulses having its number in accordance with the amplitude of the output and the output of the converter 25 is supplied to an adder 35. The adder 35 adds all the pulse numbers of the outputs of the logarithmic compression circuit C supplied to the A/D converter 25 in one frame and supplies the result thereof to a divider 36. The divider 36 divides the output of the adder 35 by the counted value of the adder 34. Therefore, the output of the divider 36 becomes a digital mean value of the luminance signal of an amplitude having a value within the range of about ±2 EV around a reference light quantity set by the reference light quantity setting and generating circuit A.
An arithmetic circuit 40 operationally treats the mean value output from the divider 36 together with exposure factors such as a shutter speed value, an iris value, an ASA sensitivity or the like supplied from an information circuit 41, controls a control system 42 of the shutter speed and the iris based on the result thereof and indicates these values in a display system 43.
According to the above described embodiment, if the contact b is connected to the terminal 12 of the switch 11 provided in the reference light quantity setting and generating circuit A, the luminance signal of an amplitude having a value within the range of about ±2 EV is automatically selected around the reference exposure value corresponding to the mean value between the maximum value and the minimum value of the amplitude of the luminance signals from the light receiver 1, that is, the field portion within the range of about ±2 EV is automatically selected, and the thus selected portion is photometrically measured on the average, so that a precise light quantity can always be obtained in usual daytime photographing. In case of obtaining a proper light quantity at a bright portion or a dark portion, that is, in the nighttime photographing or rear light photographing, a desired light quantity can be obtained by only connecting the terminal 12 of the switch 11 to the contact c or a.
As stated above in detail, according to the present invention, the photometric portion is automatically selected and the proper light quantity can be obtained, so that there is not required any troublesome operation for selecting a photometric portion as in the conventional system, the circuit construction becomes simple and small, and even in such a case that a moving object is photographed, a desired light quantity can easily be obtained.
In addition, the invention is not limited to the above embodiment, but can be modified or altered in various ways. For example, if the resistors 13 and 14 connected between the contact a of the switch 11 in the reference light quantity setting and generating circuit A and the ground in series are replaced by a variable resistor, the reference exposure value can optionally be changed within the range of ±1 EV or more than that. Further, it is preferable to form an image focussed by a camera lens optical system on the light receiver 1, if an image focussed on a focal plane is guided by an optical fiber or the like, the light receiver can be set at any optional position. In the above embodiment, the photometry is carried out by arithmetic mean, but it can be possible to construct it by seeking geometric mean, harmonic mean, square mean, median or the like. Further, in the above embodiment, the luminance signal at the selected portion was A/D converted to obtain a mean value, but it can be possible to obtain a mean value with an analog signal as it is, or the whole circuit is made as a digital circuit to photometrically measure the selected portion on the average. | A photometric system for use in an image pick-up device is disclosed. The photometric system comprises the steps of forming an image focussed by a camera lens system on a light receiver consisting of a plurality of charge transfer elements arranged in a picture element array; selectively deriving luminance signals of amplitude having a value within a range of about ±2 exposure values around a reference exposure value corresponding to a mean value between a maximum value and a minimum value of the amplitude of the luminance signals; and seeking a mean value of the selected luminance signals to photometrically measure the light of automatically selected portions on the average. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the conversion of non-ferrous metal mattes to the metal or metal sulphide.
2. Description of the Prior Art
The Pierce-Smith converter has been used widely for this purpose, since the turn of the twentieth century, and so converting in this vessel will be used to exemplify the present invention. The operation of this apparatus is described in some detail in Extractive Metallurgy of Copper by Newton, Chapter V, Converting; in Extractive Metallurgy of Sulfide Ores by J. Boldt and P. Queneau, pages 249-252 (1967) and more of the complexities of the converting operation may be found in papers such as "Metallurgy of the Converting Process in the Thompson Smelter," a paper prepared for presentation at the 14th Annual Conference of Metallurgists, Edmonton, Alberta in August 1975, the contents of these publications being hereby incorporated by reference.
Fundamentally, the Pierce-Smith converter is made up of a horizontal cylinder providing within it an elongated sealed refractory lined chamber having a cylindrical sidewall and circular endwalls. The sidewall is provided with a hooded opening for charging and discharging located between the endwalls and a row of injection pipes, or tuyeres, entering the chamber through the refractory lining at one side. The vessel is rotated between a charging position in which the opening is accessible from the side that it can be charged and a blowing position in which the charging opening faces upward and is hooded and forms an off-gas outlet. With the vessel in blowing position air or air slightly enriched with oxygen is blown in through the tuyeres at low pressure, typically 15 psig to oxidize iron and sulfur in the matte and, thus, effect separation from the matte to form slag and release off-gases, namely, sulfur dioxide. The iron is converted to iron-oxide, fluxed with silica and removed as a slag while the sulfur is oxidized to sulfur dioxide which leaves the converter in the off-gas. Further details of the converting operation in the Pierce-Smith converter are contained in the publications referred to and some of the complexities of chemical reactions, heat transfer and other relatively complex changes in conditions are described. Through the many years of operation of this type of converter, a manner of operation has developed which has undergone little change in the past few years.
There are certain disadvantages that have always plagued the use of this converter. For example, the tuyeres become plugged quickly and thus require clearing on a regular basis by punching with a metal rod which is forced through the tuyere. Another problem is that severe refractory wear occurs along the tuyere line, above the tuyeres in the backwall and the endwalls. This refractory wear is sufficiently excessive that a converter typically operates for only three months out of four, the other month being required for refractory repair. This results in high maintenance costs and necessitates excess converter capacity in a smelter operation. A further problem is accretion build-up in the converter mouth, resulting from the accumulation of particles entrained in the off-gases and which is a function of the airflow. This build-up requires frequent cleaning. These problems seem to have been accepted as a fact of life in non-ferrous metal converting using the Pierce-Smith converter.
Attempts to improve refractory life have been in the area of using better, more wear-resistant refractories as for instance discussed in "The Copper Refractory Symposium" held in New York in 1968. At that Symposium various factors were described which adversely affect refractory life and which must be controlled, for example, wide rapid temperature variations, low-grade matte with resultant large slag volumes, fine or extremely coarse flux, punching and fluxing practice, low blowing rates, methods of cleaning the converter mouth, and modifying the normal converter heating periods.
SUMMARY OF THE INVENTION
In the face of the state of the art, the applicants have now found that tuyere plugging and refractory wear are related to the behavior of the gas jets discharging from the tuyere. At pressures at which air is normally blown into non-ferrous metal converters, that is between 12 and 15 psig, the air issues from the tuyere tip in the form of discrete bubbles at a frequency of 10 to 12 s -1 . The bubbles rise more or less vertically from the tuyere, break up into smaller bubbles, and wash against the backwall refractory, while the exothermic oxidation reactions promoted by the injection of the oxidizing gas and resulting from the oxidation of sulfur and iron take place in close proximity to the refractory wall. Moreover, the heat and pumping action of the rising bubbles combine to create rapid wear in the backwall area and also in the endwalls. The backwall refractory wear is relatively uniform axially above the tuyeres because there is considerable overlap of bubbles forming at adjacent tuyeres. The overlap is caused by the normal close tuyere spacing, for example, 6 to 7 inches, required to achieve sufficient air throughput.
Between the formation of successive bubbles at a given tuyere, the bath washes against the tuyere mouth and promotes the formation of accretions due to local freezing and magnetite formation. Successive deposits of accretions quickly plug the tuyere, and punching is required. Because the accretions attach themselves to the refractories, their abrupt and forced removal by the punching rod leads to pieces of the refractory breaking off with the accretions. In addition, repeated bubble formation causes rapid thermal cycling at the tuyere line, which stresses the refractory and accelerates local wear.
The applicants have developed a process which overcomes these disadvantages, as will be apparent from the following description. The converter, in charging position, is charged to a blowing level with non-ferrous molten metal matte. The converter is rotated until the tuyeres are submerged, with the control regulated, with sufficient air being introduced to keep the tuyeres open. Then the global air supply is adjusted so that an amount of air is supplied effective to carry out an autogenous converting reaction at temperatures within the capacity of the converter and at normal ambient pressure, without overheating, through several tuyeres whose number and individual cross-sectional area is such that the air is underexpanded and enters the bath horizontally in discrete steady jets extending some distance downstream from the tuyere tip before disintegrating into bubbles. The applicants have found that a preferred injection pressure is from about 50 to about 150 psig, desirably through 3 to 6 tuyeres spaced-apart so as to avoid merging of the jets. The tuyeres may be in the form of a single group of 3 to 6 tuyeres spaced from the endwall and spaced from the mouth of the converter. Alternatively, the tuyeres may be divided into two groups of tuyeres with each group spaced from an endwall and from the mouth of the converter. Desirably, the tuyeres will have a cross-sectional area from about 1 square inch to about 3 square inches and are spaced-apart from about 8 inches to about 24 inches. The closest tuyere to the endwall should be spaced from it at not less than about 36 inches. The spacing of the tuyeres away from the mouth of the converter reduces the turbulence in this area and reduces the accretion formation at the mouth of the converter.
It is thus seen that, according to the invention, air or air enriched with oxygen is injected with pressures such that underexpanded conditions are achieved in the tuyere, as compared with the employment of low pressure gas which issues from the tuyere fully expanded, that is, with the pressure at the tuyere mouth equal to the local bath pressure. The effect of increasing pressure to create underexpanded conditions is to raise the pressure at the tuyere mouth to a value in excess of the local bath pressure so that the air discharging from the tuyeres behaves as a steady rather than a pulsating jet and bubbles do not form regularly at the tuyere tip, but instead form some distance downstream from it. The jet penetrates further into the bath and the tip of the tuyere is continuously surrounded by gas. The higer pressures ensure that the jet is pushed further from the backwall because the momentum of the gas from the horizontally positioned tuyeres is greatly increased with increasing pressure. The high pressure injection reduces the problem of backwall refractory erosion by forcing the gas jet further into the bath. The continuous presence of gas at the tuyere mouth also inhibits the formation of accretions. Moreover, accretions that do form are broken off by the action of the jet. Accordingly, the frequency of tuyere punching is reduced or eliminated altogether as refractory wear at the tuyere line is reduced.
In the light of normal Pierce-Smith converter practice, one skilled in the art would expect that the increased pressure at which the air is introduced would increase splashing and accretion build-up at the mouth of the converter. This may be overcome by limiting the pressure to a maximum of about 150 psi and by placing the reduced number of tuyeres away from the converter mouth so that material ejected by the blowing falls back into the bath before reaching the mouth. One familiar with conventional blowing practice would also expect that concentrating the gas in fewer tuyeres would encourage local refractory wear through higher temperatures being generated in the region of the tuyere and that the flow of the liquid up the backwall above the horizontally directed tuyeres would be greater. The applicants have found, however, that with the steady jet penetrating further into the bath away from the backwall, that the extra heat generated is dissipated in the body of the bath and not at the backwall. One accustomed to the use of a large number of tuyeres at normal pressures would also expect that injecting the air through fewer tuyeres and in the form of jets rather than subdividing it into bubbles would provide a decrease in oxygen efficiency through lessened interface between the gas and liquid. However, provided their effective submergence within the molten metal is ensured the higher pressure jets have proven very active and provide good gas-liquid contact. The tips should be at a level from about 18 to about 36 inches beneath the surface of the molten metal.
The applicants' operation in the underexpanded jet regime, by raising the pressure to the range from about 50 psig to about 150 psig, should not be confused with operating in the expanded jet regime at small pressure increases over normal, for example, up to about say 10 to 15 psig as proposed by L. M. Shalygin and V. B. Meyerovich: Tsvet. Metal, 1960, vol. 33, No. 7, pp. 16-19. In order to achieve the results described by the applicants, pressure must be high enough to provide an underexpanded jet regime in which the jet differs in kind from those created at lower pressures while maintaining the total amount of oxidizing gas within the range required for the metallurgical operation by reducing the number of jets over that normally employed and maintaining their cross-sectional area within appropriate limits. This requires pressures of at least about 50 psi.
Nor should the applicants' procedure be confused with proposals in the non-ferrous metal field to protect the injectors from the severe results of injecting pure oxygen by employing the Joule-Thomson effect created at high pressures of 400 psi or more. The applicants' range of pressure is directed merely to changing the jetting conditions from fully expanded to underexpanded, while maintaining the total oxidizing gas injected within normal limits of non-ferrous operations.
BRIEF DESCRIPTION OF THE DRAWINGS
Having thus generally described the invention, it will be explained more specifically by reference to the accompanying drawings which should be considered as exemplifying preferred embodiments, and in which:
FIG. 1 is a schematic perspective view of a Pierce-Smith converter equipped according to the invention;
FIG. 2 is a schematic diagram of the inside of the converter showing one preferred arrangement of tuyeres according to the invention set in the refractory; and
FIG. 3 is a schematic diagram showing another arrangement of tuyeres according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring more particularly to the drawings, the Pierce-Smith converter shown is made up of a cylindrical vessel A provided with spaced-apart circular supporting rings 15 riding on rollers 17 suitably journalled in an infra structure (not shown). A toothed ring 19 adjacent one of the rails 15 is engaged by a pinion 21 driven by the shaft 23 by a suitable drive source so that the vessel A may be rotated about its axis between a charging position and a blowing position.
The vessel A provides an internal cylindrical chamber having a refractory lined sidewall 25 and refractory lined endwalls 27. The sidewall 25 is provided with a charging opening 29 surrounded by a skirt 31 and provided with a hood 33.
A number of tuyeres B enter the chamber through its sidewall 25 and are supplied with oxidizing gas from a header 35 which receives its supply of compressed air or other oxidizing gas from an air inlet pipe 37 connected with a suitable source of such gas.
Each tuyere B extends through the iron shell or sidewall 25 and the refractory lining 26 to terminate in a tip 24 at the surface of the refractory 26. The tuyere B may be provided with a tuyere puncher.
In accordance with the invention, the number of tuyeres is reduced considerably as compared with the number used conventionally. One preferred arrangement is shown in FIG. 2. Here there are two groups of 2 to 3 tuyeres each spaced from the endwalls 27 and from the mouth of the converter. Another preferred arrangement is shown in FIG. 3 where there is a single group of from 4 to 6 tuyeres spaced from one endwall and to one side of the mouth of the converter.
The tuyeres B may be perpendicular to the sidewall so as to operate in horizontal blowing position. Alternatively, special effects may be obtained by angling the tuyeres so that the steady jets are injected at an angle of up to about 15° from perpendicular to the refractory wall of the vessel. For example, downward injection may increase the efficiency of the oxidizing gas. Injection at an angle away from the endwall will remove the heating effect of the jet away from the endwall. Injection at an angle away from the mouth of the vessel will reduce turbulence in that zone and thus reduce accretions.
VARIABLE FACTORS
Converters
The Pierce-Smith converter has been described to characterize the invention, although it may be applied to any non-ferrous furnace using tuyere side injection of air or of oxygen enriched air.
A typical converter has external dimensions of 13 feet to 15 feet in diameter by 30 feet to 35 feet in length and is made with a 1 inch thick outer iron shell, a 1 to 11/2 inch thick insulating layer of magnesite (MgO), 15 inches of chrome magnesite (MgO--35% Cr 2 O 3 ) refractory bricks, except the same material is thicker, say about 18 inches, near the tuyeres.
Injectors
The injectors or tuyeres, basically the same as in current practice may be employed, are made from iron and have a straight bore. A typical injector has a 11/2 inch to 2 inch inside diameter and is in excess of 18 inches to pass through the steel shell, insulating bricks and chrome magnesite bricks and to project some distance outside the vessel. The injectors are horizontal when the converter is in blowing position. In a conventional converter there are usually two sets of injectors on either side of the mouth with, for example, 40 tuyeres and two sets of 20 tuyeres each with spacing approximately 7 inches. All the injectors are the same. According to the present invention the number of active tuyeres is reduced with a preferred range from 4 to 6 with a spacing of at least about 15 inches apart.
Each tuyere may blow the same amount of air with several tuyeres linked to a common manifold. Preferably a separate control is provided for each tuyere so that the flow rate may be varied along the bath, provided that the flow rate is kept within the range stated. The diameters of the respective tuyeres may be varied as may their position in the converter. While the invention has been described and illustrated in connection with a furnace equipped with a smaller number of tuyeres than normally employed in the prior art, the furnace may be equipped with a larger number of separately regulatable tuyeres so that a few can be used at a time with the others cut off. This has the advantage that if eventually the refractory wear becomes a problem in the region of an active tuyere or set of tuyeres, it or they can be plugged externally and another set activated. In this way, lining life may be prolonged substantially.
In accordance with the invention the submergence of the tuyeres should be at least about 18 inches.
The tuyere arrangement pattern is to keep the tuyeres away from the endwall to minimize refractory erosion and away from the furnace mouth to minimize splashing problems and accretion build-up at the higher gas injection rates employed.
Control of the flow through the tuyeres is based on pressure in the tuyeres and/or temperature of the bath. Feedback control using pressure measurement may be used to activate tuyere punchers, if found necessary.
Feed Materials
The materials treated are non-ferrous mattes, that is a mixture of sulphides of copper and iron, and nickel and iron. The common denominator is the elimination of sulfur as sulfur-dioxide gas, and iron as a siliceous liquid slag of the type fayalite, (FeO) x .SiO 2 , where 1<x<2; this slag also contains variable amounts of Fe 3 O 4 . The matte changes its composition during the cycle, as Fe and S are oxidized, and subsequently eliminated from the matte. The pressure range of the bath is atmospheric.
One ferrous metal which may be treated according to the invention is copper matte which usually contains from 20 to 60% copper (as Cu 2 S), 2 to 6% oxygen (as iron oxides) with the remainder FeS and minor impurities. Another is nickel matte with usually from 10 to 50% nickel (Ni 3 S 2 ) with usually small amount of copper (as Cu 2 S), 2 to 6% oxygen (as iron oxides) with the remainder FeS and minor impurities.
A preferred flux is a siliceous flux containing not less than 80% SiO 2 , to improve the heat balance. Flux containing as low as 65% SiO 2 is acceptable.
Oxidizing Gas
The oxidizing gas may be air or air enriched with up to about 40% oxygen. Enrichment with oxygen may be used so as to maintain the autogenous nature of the process and to melt the quantity of cold material that is charged, i.e. to adjust the heat balance. The gas is injected at a pressure, effective to provide underexpanded conditions with the tuyere, from about 50 to about 150 psi and a linear speed above about 0.9 Mach. The overall flow rate is within the range from about 25,000 to 30,000 SCFM for furnaces of the size mentioned. The oxidizing gas jet is unshielded and is projected into the fluid charge in the form of a steady underexpanded jet as opposed to a pulsing jet. "Underexpanded jet" may be further explained as follows. When a gas is injected through a tuyere at low pressures, the pressure decreases along the tuyere in the direction of flow, until at the tip it is equal to the surrounding pressure (atmospheric plus pressure due to bath height). The gas jet is thus fully expanded. As the driving pressure is increased, the gas accelerates and the pressure drop along the tuyere becomes steeper. However, there is a limit to the velocity that the gas can attain in a straight-bore tuyere, i.e. the speed of sound (Mach 1). Thus at a sufficiently high back-pressure the gas reaches a terminal velocity (usually less than Mach 1 owing to frictional effects in the tuyere). Under these conditions the pressure inside the tuyere cannot be released by a further acceleration of the gas, and the pressure at the tip is greater than the ambient pressure. Thus the gas is not fully expanded (underexpanded) relative to the surrounding pressure. The excess pressure is released outside the tuyere by a multidirectional expansion of the gas.
Conditions
The conditions in the furnace during blowing in furnaces of the type and size exemplified are as follows. The range of temperature of which converters operate according to the invention is from about 1100° C. to about 1300° C. The blowing time is from 6 to 20 hours depending on the grade of matte. The input may range from about 100 to 200 metric tons of matte depending on the matte grade, with 20 to 60 metric tons of flux (again depending on the matte grade). At this feed rate the oxygen necessary for the oxidation will be at a rate of 4,000 to 8,000 SCFM of oxygen in the oxidizing gas. The output ranges from about 70 to about 120 metric tons of copper per cycle and 30 to 80 metric tons of slag per cycle. The punching frequency with the conventional process is every 15 to 60 seconds. According to the applicants' procedure punching is usually not necessary until the end of the blow.
Punching will not normally be required during most of the converter cycle. However, the normal punchers are desirably included in the apparatus since they may be required towards the end of the cycle, especially for copper, when the gas flow, and hence temperature decreases.
Through the high pressure injection of the invention, the total gas flow rate may be increased up to about 30,000 SCFM in which case the reduction of cycle time will be roughly proportional to the increase in flow rate.
When the furnace is rotated from charging to blowing position, until the desired submergence is reached, it is desirable to maintain the pressure through the tuyeres at from about 10 to about 20 psig with about 15 psig preferred. Then the pressure may be increased to the desired level.
Th working of the invention will be explained in more detail by reference to the following examples of preferred procedures.
It should be borne in mind that an important factor in determining the length of a cycle is the grade of the starting material. The grades vary from about 20 to about 60% Cu (in the case of copper). This also affects converter operation. Therefore, the operation cycle will be described for both cases.
High grade mattes are obtained when the concentrates are rich in copper due to a high content of chalcocite (Cu 2 S) and/or when flash melting methods are used to melt the solid concentrates. In such case, it is common to obtain a matte with say 55% Cu content. Since a higher content of Cu implies a lower content of Fe in the matte, smaller amounts of slag will be produced and the volume of the converter will be occupied to a larger extent by the value metal, i.e. Cu 2 S (obtained in the first stage of a copper-converting cycle). In such a case, the fresh matte (or starting matte) will be added fewer times (twice for 55% Cu matte) and the cycle length will be shorter, since there is less FeS to be oxidized in the first stage of converting.
EXAMPLE 1
A Pierce-Smith converter was employed 35 feet long by 13 feet in diameter using 6 tuyeres about 1/2 inch internal diameter. The feed material was copper matte (55% Cu). The flux contained 85% SiO 2 . The oxidizing gas was air.
The following describes a treatment cycle.
First Stage:
1. The converter is hot, having just been emptied from the cycle.
2. 80 to 100 tons of matte are added through the mouth using ladles moved by cranes. 4 to 5 full ladles were needed to charge the converter. The matte was at a temperature of from 1100° to 1150° C.
3. With the converter in loading position (the tuyeres not immersed in the bath) air is blown through the tuyeres at low pressure, not higher than 15 psi.
4. The converter is rotated until it reaches blowing position with the tuyeres submerged 18 inches in the molten matte.
5. The blowing pressure is increased to 120 psi immediately after converter reaches blowing position.
6. Air flow is maintained at a rate of about 25,000 SCFM for approximately 45 minutes. At this point, the converter temperature is approximately 1200° C. depending on the starting matte temperature.
7. The blowing pressure is decreased to 15 psi, the converter is rotated to loading position and the air flow turned off.
8. 15 to 20 tons of siliceous flux are added through the converter mouth.
9. Blowing is restarted, following the same steps described in 3, 4 and 5 above.
10. After 20 to 30 minutes of blowing, air is shut off according to step 7.
11. At this point, the converter temperature is between 1220° to 1240° C. The matte grade would be between 72 to 75% Cu. About 35 tons of slag will have been produced.
12. Approximately 30 tons of slag (2 ladles) are skimmed off.
13. If the temperature of the converter in step 11 is higher than say 1230° C., about 10 tons of cold charge (solid recycle material) are loaded in the converter.
14. 40 to 60 tons of fresh matte (55% Cu) are added to the converter (2 to 3 ladles).
15. Some 10 to 20 tons of flux are commonly added at this point.
16. Blowing is started, following steps 3, 4 and 5.
17. Step 6 is repeated.
18. Steps 8 and 9 may or may not be necessary, depending on whether step 15 has been performed.
19. After 60 to 80 minutes of blowing (since step 16) the air is shut-off according to step 7.
20. At this point, the converter temperature will be about 1220° C. to about 1240° C. The matte grade is 78 to 80% (most of FeS, if not all has been oxidized and about 30 tons of slag have been produced) and this slag is skimmed off into ladles.
21. End of Stage 1; product left in the reactor 80 to 110 tons of Cu 2 S.
Second Stage:
Basically Cu 2 S is the starting raw material. The same FeS and/or flux may be present.
22. If the temperature at the end of Stage 1 has been too high (over 1240° C.) and/or if relatively pure copper reverts are available (80% Cu or more) add about 10 tons of cold reverts to the reactor.
23. Blowing is started following steps 3, 4 and 5 of the first stage.
24. The air flow is maintained at about 25,000 SCFM at 120 psi. Usually there are no interruptions in the second stage. The temperature will rise slowly from about 1180° C. to about 1220° C. The blowing time will vary depending on the amount of Cu 2 S present in the beginning of Stage 2, but it is expected to be 3 to 4 hours (overall blowing time for the cycle about 5 to 8 hours). Note: This is blowing time. Overall time for the cycle, including charging, waiting for cranes, etc. will make the cycle 1 to 2 hours longer.
25. When the bath reaches 97 to 98% Cu (an experienced operator can tell the precise point) pressure is decreased to not more than 15 psi.
26. After about 5 minutes the converter is rotated to loading position and the gas is turned off. Some flux may be added to account for any iron oxide that may be present.
27. The final product is 60 to 90 tons of blister copper (98.5 to 99.5% Cu).
Low Grade Matte
Low grade mattes are obtained when the concentrates are rich in chalcopyrite and are melted in a reverberatory furnace. In such case it is common to obtain a matte of say 30% Cu content. This means larger amounts of FeS in the matte, a larger volume of slag to be produced and smaller amounts of Cu (as Cu 2 S) in the reactor.
To overcome this problem, fresh matte is added to the converter several times during the first blowing stage (perhaps 5 times for a 30% Cu matte) and the amounts of flux charged and slag produced change correspondingly. However, the converter is operated following the same principle: temperatures not higher than 1250° C. and good estimates of the matte grade during the blowing.
EXAMPLE 2
In this case a matte of grade having 30% Cu is treated in a converter similar to that of Example 1 using the same flux and air as the oxidizing gas.
The cycle was as follows:
Steps 1, 2, 3 and 4 were the same as in Example 1.
For steps 5 and 6, since the blowing time is longer, the temperature of the converter exceeds 1250° C. This is avoided by reducing the blowing pressure to about 80 psi, through 6 tuyeres, and decreasing the overall flow to not more than 20,000 SCFM. Alternatively, the blowing pressure may be 120 psi, but employing 4 tuyeres and, again, decreasing the overall flow to not more than 20,000 SCFM.
A further way of avoiding high temperatures is to use 120 psi blowing pressure, 25,000 SCFM total air injection, and 6 tuyeres, and the addition of larger amounts of cold recycled materials. This may be undesirable, due to the more frequent interruptions in the blowing that would be required. It may also not be feasible, if cold materials are not available in large enough amounts.
Apart from these exceptions, the procedure continues as in Example 1, but the blowing time would be greater (i.e. approx. 60 minutes).
7. The same as in Example 1.
8. 30 tons of flux are required.
9. The same as in Example 1.
10. Blowing time 30 to 45 minutes.
11. The same as in Example 1, except that the matte grade is 45% Cu.
12. 60 tons of slag are produced.
13. Add 10 to 20 tons of cold charge.
14. 60 tons of fresh matte (30% Cu)
15. 30 tons of flux
16. The same as in Example 1.
17. The same as in step 6 for low grade matte as described above.
18. The same as in Example 1.
19. 60 minutes, matte is 55 to 60% Cu.
20. Repeat as from step 12 above to step 19 above but change.
12. To about 40 tons of slag.
13. To about 10 tons of cold charge.
14. To about 40 tons of matte.
15. To 20 tons of flux.
16. and 17. The same as in Example 1.
19. 60 minutes, the matte is about 70% Cu.
20. Repeat steps 12 to 17, but change:
12. 30 tons of slag
13. 10 tons of slag cold revert (may not be necessary).
14. 20 tons of fresh matte
15. 10 tons of flux (otherwise 16 through 21 are the same as in Example 1 to end the first stage.)
The second stage will be the same as in Example 1.
The following are variables which affect the operation.
The use of enriched oxygen-enriched air improves the heat balance and shortens the cycle length. It will be useful when,
(a) the matte grade is higher than 50%, and therefore the lower content of FeS in fresh matte does not allow a large heat generation (cold mattes) in the first stage;
(b) although low grade mattes are available, large amounts of cold materials (recycled charge) or even concentrates need to be melted;
(c) during the second stage, specially if a higher flow per tuyere, due to the increased pressures, causes some freezing of the melt in the tuyere zone.
The use of increased gas flow (30,000 SCFM or more) produces a similar effect to an increase in the O 2 concentration, i.e. improves heat generation. However, in addition, it may cause excessive amounts of material from the bath to be carried by the off-gases. It would also shorten the cycle length. It would be convenient when,
(a) the tuyeres are located near end of the reactor, and the mouth is near the other end;
(b) there is a need for larger heat generation as specified above in connection with the use of oxygen-enriched air;
(c) no fine materials (such as concentrates) are charged into the reactor.
Reference has been made to the first stage of a copper converting cycle. So far Cu can be changed to Ni, bearing in mind that copper is present as Cu 2 S and nickel as Ni 3 S 2 . The operation is basically the same in each case.
However, once all the iron has been removed as slag, the method to obtain the respective metals differs. In the case of copper, Cu 2 S is oxidized by further blowing of air (or oxygen-enriched air) to obtain Cu. But this cannot be done in the case of nickel since that would cause oxidation of Ni to Ni oxides (this can be avoided at higher temperatures, but that is not central to the present invention, since it requires a different reactor). Therefore, in the case of nickel, the final product, according to the present invention, will be Ni 3 S 2 (nickel sulfide) that later is converted into Ni by a completely different technique. In the case of copper, the production of the pure copper sulfide, Cu 2 S means the end of the first stage of converting, the second stage being the obtaining of Cu. | A method of converting a charge of non-ferrous metal matte in a Pierce-Smith or similar converter. The fluid charge is blown with a total flow of oxidizing gas effective to maintain autogenous converting temperatures through a plurality of spaced-apart tuyeres limited in number and individual cross-sectional area effective to maintain the gas underexpanded at a pressure within the range from about 50 to about 150 psig so that it penetrates the bath in the form of discrete steady jets to positions remote from the tuyere tips thereby reducing degradation of the refractories and build up of accretions. The gas is injected through from three to six tuyeres. | 2 |
BACKGROUND OF THE INVENTION
1. Field of Invention
This invention discloses an adsorbent material fabricated into a self-supported coherent sheet and configured for use as a parallel passage contactor.
2. Prior Art
Traditional mass transfer devices for adsorption process include monoliths (e.g. honey combs), cloth (e.g. activated carbon fiber cloth) and packed bed of adsorbent particles. The packed bed is cheap and versatile, but quite inefficient in operation at high flow rate regimes due to the high costs associated to the large internal pressure drop. Calculations by Ruthven and Thaeron (in Gas. Sep. Purif. vol. 10, (1996) p. 63) have shown that a significant improvement in the mass transfer/pressure drop characteristics over the packed bed configuration could be achieved with parallel passage contactors. These are mass transfer devices in which the gas passes in laminar flow through straight channels between equally spaced parallel sheets of adsorbent. Rapid mass transfer enables rapid cycling and smaller devices. One application of parallel passage contactors is Pressure Swing Adsorption (PSA).
PSA has become of interest for small-scale gas separation applications because of its potential for high separation performance (product purity and recovery) compared with other gas separation technologies. Depending on the actual mechanism, PSA separations could be categorized as equilibrium or kinetically (diffusion) controlled. An example for the first category is separation of air on zeolite 5 Å into almost pure nitrogen and oxygen streams based on differences in equilibrium adsorption isotherms between nitrogen and oxygen. An example for the second group is the same separation carried out on zeolite 4 Å, where the mechanism is based on the differences in diffusion rates between nitrogen and oxygen, which have different effective kinetic diameters (3.46 Å and 3.64 Å, respectively). While the equilibrium based PSA separation has been relatively well established theoretically and already commercialized for some applications, the diffusion-induced PSA still needs theoretical development and is not fully commercialized. The reader is referred to several recent publications such as by Shin and Knaebel, in AlChE Journal, vol. 33, p. 654 (1987), and vol. 34, p. 1409 (1988); by Chung and others, in Computers Chem. Engn. Vol. 22, Suppl., p. S637 (1998); and to the “Pressure Swing Adsorption” monograph book by Ruthven, Farooq and Knaebel, VCH Publisher, 1994.
Another way for optimization of PSA in terms of enhancing the adsorbent productivity at equal recovery and product purity parameters is through shortening the cycle times. Enhanced adsorbent productivity results in reducing the cost and foot print size of PSA beds. When the intra particle diffusion limits the rate of mass transfer in PSA, one way to shorten the cycle times is by using adsorbent with very small particle sizes. This was demonstrated first in U.S. Pat. No. 4,194,892, where relatively small particles of adsorbent were used in a packed bed configuration at cycle times of less than 30 seconds, with substantially higher product recovery than in previous art. U.S. Pat. No. 4,354,859 demonstrated a further increase in productivity by executing rapid cycle PSA with two pistons operating out-of-phase at the ends of the adsorption column.
However, the gas separation efficiency in rapid cycle PSA, as described by U.S. Pat. Nos. 4,194,892 and 4,354,859, is limited by the pressure drop in the randomly packed bed column. To circumvent this, Farooq, Thaeron and Ruthven (Sep. Pur. Tech., vol. 13 (1998) p. 181–193) suggested combining piston-driven rapid cycle PSA with parallel passage contactors, thus providing an economical solution to older separation technologies such as air drying, air separation, and VOC removal. Based on numerical simulation models developed by Ruthven and Thaeron (Gas Sep. Purif. vol. 10 (1996) 63–73), for example, a parallel passage contactor with sheet thickness of about 500 to 800 μm and sheet spacing of about 100 μm should be well suited to rapid cycle adsorption processes for CO 2 /N 2 separation. The adsorbent described by Ruthven and Thaeron was activated carbon fiber (ACF) sheet with fiber diameters of 10–15 μm. For this adsorbent characteristic length, the optimal cycle frequency was 10–20 rpm, the rate being limited by the inter particle, macro pore diffusion. However, it became evident for those who tried to use carbon fiber adsorbent in woven or non-woven form in rapid cycle PSA systems that a great disadvantage of these materials is that they are not dimensionally stable.
Further increase in cycle frequency and thus more performance improvement of the separation process is possible in principle by using even smaller adsorbent particles (about 10 μm in size). Problems with small particles in packed beds subjected to high flow velocities include particle break up, particle attrition from the bed, and particle fluidization. U.S. Pat. No. 6,176,897 teaches a high frequency pressure swing adsorption system in which granular adsorbent beds are replaced by a high surface area adsorbent monolith or layered support, with adsorbent elements formed of layered or laminated sheet materials using fibrous reinforcements (such as glass, carbon or kevlar fibers) which support zeolite loaded composites in adsorbent sheets. However, the availability of materials that could be successfully used for fabrication of such adsorbent structures is limited. Also, the use of reinforcement materials limits the adsorption capacity per volume of adsorption bed, because a relatively large fraction of the adsorbent bed volume, associated with the reinforcement structures, is not effectively used for adsorption.
It was demonstrated that inorganic adsorbent particles with sizes in the range of tens to hundreds of nanometers (also called adsorbent nanoparticles) have enhanced adsorption and chemical surface reactivity due to the very high ratio of surface atoms to bulk atoms. For more information, the reader is directed to the recently published book entitled “Nanoscale Materials in Chemistry” (Wiley, 2001) by Klabunde. However, integrating adsorbent nanoparticles into usable sorptive materials has been a challenge so far. Efficient means for binding, stabilizing or incorporating adsorbent particles with sizes in the nanometer range in structures that can be used for adsorption and separation applications are deemed necessary.
Recently, sorptive materials based on polytetrafluoroethylene (PTFE) matrix have been described in the patent literature. U.S. Pat. Nos. 4,810,381 and 4,906,378 describe a chromatographic sorptive material composed of PTFE fibril matrix and non-swellable adsorbent particles enmeshed in the matrix U.S. Pat. Nos. 4,153,661 and 5,071,610 disclose manufacturing methods and uses of composite sheet materials comprised of fine, non-swellable adsorbent particles held by a fibrillated polymer matrix, and methods for the control of internal porosity. The resulting sheet is extremely pliable and it is said to be useful as an electronic insulator or semi permeable membrane. U.S. Pat. No. 4,373,519 discloses a composite wound dressing comprising hydrophilic absorptive particles enmeshed in a PTFE matrix. U.S. Pat. Nos. 4,565,663 and 4,460,642 disclose water swellable composite sheets having a PTFE matrix in which are enmeshed swellable hydrophilic sorptive particles. However, sorptive materials obtained by enmeshing particulate sorbents, in a fibrillated PTFE matrix with specification for use as a parallel passage contactor have not been disclosed.
Self-supported porous membranes obtained by compacting micron-size carbon particles and fibrillated PTFE could also be used as porous electrodes in electrochemical applications. The U.S. Pat. No. 4,585,711 teaches a hydrogen electrode for a fuel cell obtained by roll compaction of granular PTFE and platinum-covered carbon black particles. The U.S. Pat. No. 4,379,772 disclosed a method for forming an active layer electrode for fuel cells in which granules of active carbon are mixed with fibrillated PTFE and rolled into a self-supported, coherent sheet form. U.S. Pat. No. 4,468,362 discloses a method for preparing a self-sustained electrode-backing layer with excellent electrical conductivity through dispersing PTFE particles and finely divided carbon black particles (50 to 3000 Å). U.S. Pat. No. 4,500,647 teaches the preparation of three-layer matrix electrodes for fuel cell or other electrochemical applications in which active carbon particles are present within an unsintered carbon black-fibrillated PTFE material. U.S. Pat. No. 5,636,437 discloses a fabrication method of solid carbon porous electrodes from various carbon powders and thermoset resin binders. These un-reinforced, self-supporting sheets have not been specified for use as a parallel passage contactor. The prior art is limited to adsorbent cloths or reinforced sheets for parallel passage applications.
BRIEF SUMMARY OF THE INVENTION
This invention discloses an adsorbent material fabricated into a reinforcement-free, self-supported coherent sheet, and configured for use as a parallel passage contactor. The adsorbent material is obtained by enmeshing fine adsorbent particulates, including but not limited to carbon particles, inorganic oxide particles, or ceramic particles, or synthetic polymer resins. For the purpose of the present invention, the characteristic length of these particles is in the range from 0.01 μm to 100 μm. The sheet material is a high surface-to-volume composite, characterized by sheet surface area to total sheet volume ratio in the range of 200 to 2500 m 2 /cm 3 and the sheet micro pore volume to total sheet volume ratio is in the range of 0.1 to 0.9. For use as a parallel passage contactor, the sheet material is configured in the form of flat parallel layers with gaps between adjacent sheets, or is corrugated, or is embossed, or is spiral wound, or is in any other form that allows the gas to flow parallel to the sheet surface. The material configured as parallel passage contactor can be used in many gas separation applications, or liquid applications, where fast adsorption, low pressure drop, and minimal mass transfer resistance are essential, such as in rapid cycle pressure swing adsorption. Examples of preferred uses of parallel passage contactor devices manufactured with the material disclosed in the present invention include but are not limited to hydrogen purification and air separation by rapid cycle pressure swing adsorption, air desiccation and VOC abatement by HVAC rotary wheel technology, rapid gas capture and controlled release for adsorbed natural gas fueled vehicles or analytical sampling purposes.
OBJECT AND ADVANTAGES
When parallel passage contactor elements are built, they must combine thin adsorbent sheets of high micropore volume capacity with a porous, low pressure drop separator (or no separator at all). The first requirement is introduced by the need to maximize the adsorption capacity of the sheet adsorbent; the second ensures that a low pressure drop device is being obtained. For fast cycle PSA application, the intra-particle diffusion must be minimized, which can be realized by using very small adsorbent particles, preferably in sub-micron size. Based on all these considerations, a means for manufacturing thin sheets of adsorbent materials, which hold very small adsorbent particulates, was deemed highly necessary for further improving the efficiency of PSA systems through rapid cycle technology. Calculations showed that to be useful, the adsorbent sheet must have a sheet thickness less than about 0.8 mm, a void volume fraction in the range of about 0.3 to 0.9, particle sizes smaller than about 0.7 μm, and an linear driving force mass transfer coefficient larger than about 1 sec −1 . The contactor must withstand the high velocity flow associated with rapid cycling PSA, in conditions where pelletized powders fluidize and suffer from attrition, and woven cloths do not have sufficient stability or structural integrity.
It is therefore an object of this invention to provide an adsorbent material, which immobilizes and incorporates a multitude of fine adsorbent particulates, with characteristic dimensions in the nanometer or micrometer range, which otherwise are too small to be used alone for adsorption applications.
Another object of this invention is to provide an adsorbent material that maintains much of the adsorptive properties of the starting adsorbent particles, thus that one can take full advantage of the high reactivity and fast adsorption or reaction rates associated to small adsorbent particles in the nanometer and micrometer range.
Yet another object of this invention is to provide an adsorbent material configured as a reinforcement-free, self-supported, flexible thin sheet layer or membrane.
Yet one more object of this invention is to teach the use of the above said thin sheet reinforcement-free adsorbent material as an element of parallel passage contactors for adsorption or separation applications in gas or liquid phase.
In this application, “reinforcement” means an essentially freestanding, sizable structure that adds integrity and mechanical stability to a manufactured object, does not necessarily have adsorption properties, and on which one can support with appropriate binders a variety of adsorbent particulates.
In this application, “binder” means a component that, when added in a small amount to a manufactured object, provides structural integrity by gluing together a multitude of component particles, but which does not possess structural integrity by itself, e.g. without the presence of a multitude of particles.
In this application, “self-supporting” means that no rigid backing support is needed for the manufactured object.
In this application, “particles” or “particulates” means solid shapes (not including PTFE) with a diameter from about 0.010 μm to about 100 μm.
One advantage of this invention over prior art consists in the effective immobilization of nanosized adsorbent particulates, in general starting from about 10 nm, for more efficient use in adsorption and separation applications. Also, this invention teaches the manufacturing of a reinforcement-free, self-supported, coherent, and dimensionally stable adsorbent material which can be configured as an element of a parallel passage contactor. An obvious advantage of this material, which comes from the lack of any structural reinforcement, is that its apparent volume is essentially filled with adsorbent particles, thus maximizing the adsorption capacity per volume of adsorbent sheet. Yet, the parallel passage contactors made from material, when used for adsorption or separation applications, combine good mass phase transfer properties with low pressure drop. Another advantage of this invention comes from the fact that the adsorbent material can be obtained as a thin and flexible sheet, which makes it useable in many forms, such as parallel sheets, corrugated sheets, embossed sheets, spiral wound or in a honeycomb configuration, as elements of a parallel passage contactor. Yet a more distinct advantage of this invention is that it provides a means for using small adsorbent particulates, with sizes in the nanometer or micrometer range, in a free-standing, reinforcement-free, dimensionally stable material which becomes suitable for manufacturing parallel passage contactors to be used in rapid cycles pressure swing adsorption.
Further objectives and advantages of this invention will become apparent from a consideration of the following full description of embodiments.
FIGURES
FIG. 1 is a scanning electron microscope picture of the adsorbent sheet material obtained according to the procedure outlined in Example 1. The primary carbon nanoparticles of less than 20 nm are randomly distributed and enmeshed by the polymer fibrils (not seen in the picture). The scale bar length is 100 nm.
FIG. 2 is another scanning electron microscope picture of the adsorbent sheet materials obtained according to the procedure outlined in Example 1. It shows that carbon nanoparticles form an open structure, with very little attachments and contact points to polymer fibrils. A polymer binder fibril about 1000 nm long and less than 40 nm in diameter is also seen. The scale bar length is 200 nm.
FIG. 3 is a scanning electron microscope picture of the adsorbent sheet material obtained according to the procedure outlined in Example 2. It shows a mixture of activated carbon particles of various sizes, forming a reinforcement-free open structure held together by polymer fibrils (not seen in the picture). The scale bar length is 2 μm.
FIG. 4 is a schematic drawing showing a parallel passage contactor element configured as a multitude of flat adsorbent sheets 1 in a parallel arrangement. Air inlet 2 and air outlet 3 are arranged such that the direction of airflow is parallel with the surface of flat sheets.
FIG. 5 is a schematic drawing showing a parallel passage contactor element configured as a spiral structure made from an adsorbent sheet 1 . Air inlet 2 and air outlet 3 are arranged such that the direction of airflow is parallel with the surface of adsorbent sheet.
FIG. 6 is a schematic drawing showing a parallel passage contactor element configured as a honeycomb structure consisting of alternating flat sheets 1 and corrugated sheets 4 . Air inlet 2 and air outlet 3 are arranged such that the direction of airflow is parallel with the surface of corrugated and flat sheets.
FIG. 7 compares results on CO 2 breakthrough from a packed bed of 1 mm granular carbon and a parallel passage contactor element made from a carbon adsorbent sheet manufactured according to Example 2, and configured as a spiral structure according to Example 7.
FIG. 8 shows thermogravimetric data on raw Na—X zeolite powder and two samples of zeolite powder processed in sheet form according to the procedure outlined in Example 10. It shows that domains of thermal stability for zeolite sheet samples are between 300 and 400 C.
FIG. 9 shows results on drying at 350 C. followed by N 2 adsorption/desorption cycles at 45 C. on raw Na—X zeolite powder.
FIG. 10 shows results on drying at 350 C. followed by N 2 adsorption/desorption cycles at 45 C. of zeolite processed in sheet form according to the procedure outlined in Example 11.
FIG. 11 shows results on drying at 350 C. followed by N 2 adsorption/desorption cycles at 45 C. of zeolite processed in sheet form according to the procedure outlined in Example 11.
DETAILED DESCRIPTION OF THE INVENTION
By employing a process like the one disclosed by U.S. Pat. Nos. 4,153,661 and 5,071,610, a sheet material is obtained, containing a first type of adsorbent particulates, either alone or admixed with a second type of adsorbent particulates, or the second type of adsorbent particulates alone, and a polymer binder.
The first type of adsorbent particulates includes but is not limited to carbon nanoparticles and inorganic oxides nanoparticles and is characterized by particle sizes in the range of about 10 to about 200 nm. Examples of carbon nanoparticles include but are not limited to carbon black particles, carbon fullerences, and multiwalled carbon nanotubes. Examples of inorganic oxide nanoparticles include but are not limited to silica, alumina, alumino-silicates (e.g. natural or synthetic zeolites), magnesia, zirconia, titania, ceria.
The second type of adsorbent particulates is comprised of activated carbon, such as particles or fibers, inorganic oxides, ceramic materials, or synthetic polymeric resins with particle sizes in the range from about 0.2 to about 100 μm.
The adsorbent particulates from the first and second group are characterized, in general, by adsorptive properties that make them suitable for use as adsorbents in the parallel passage contactor after incorporation in the sheet form. Although the nature of these adsorbent particulates may vary within quite large limits, the adsorptive properties are expected to correlate with their specific surface area and micropore volume, as measured by nitrogen adsorption. The acceptable limits for specific surface area are between 200 and 2500 m 2 /g and the acceptable limits for the micropore volume are between 0.2 and 1 cm 3 /g. For practical applications where the device footprint or the device volume should be minimized, a more convenient measure of the adsorptive properties is based on the apparent or bulk volume of the adsorbent, which can be contained in the working volume of the adsorption device. Thus, when the bulk density of obtained sheet materials is property accounted for, the adsorption capacity could also be expressed as the total BET surface area or total micropore volume of the adsorbent material per apparent unit volume of the adsorbent material. The corresponding range for sheet surface area to total sheet volume ratio is 200 to 2500 m 2 /cm 3 and the range for the sheet micropore volume to total sheet volume ratio is 0.1 to 0.9.
Examples of polymer binder include but are not limited to polyethylene, polypropylene, polytetrafluoroethylene (PTFE), polyamide, cellulose acetate, polyvinyldifluoride (PVDF) or any other natural or synthetic polymer that is capable of suspending other particles in a random manner.
The optimal ratio of adsorbent particulates to polymer fibril binder can be varied, but should be kept, in general, in the range from 98:2 to 60:40 by weight. Under these conditions, the composite sheet is obtained with porosity in the range of 30 to 95% void volume, and the mean pore size in the range of 0.002 to 2 μm. Fugitive pore formers such as salts, or excess solvents, or polymers may be added to increase the pore size and porosity.
The obtained sheet material can be formed with sheet thickness in the range from 50 to 1000 μm, but it is convenient for the purpose of the present invention to manufacture it in very thin sheets. When the particulate adsorbent particles are preponderantly in the form of nanoparticles with large surface area to volume ratio it is preferable to manufacture the composite sheet material with small thickness in order to take advantage of the properties of individual nanoparticles.
One important advantage offered by thin sheet nanocomposite is the ability to freely access the particle and interparticle surfaces, which thus can efficiently be used for gas or vapor adsorption, pathogen annihilation, surface chemical reactions, or electrochemical energy storage, to name a few.
EXAMPLE 1
This example demonstrates that processing the nanoparticulate carbon black in a sheet form does not substantially reduce the surface area and mesopore volume of the starting carbon black material. According to one of preferred embodiments, a nanoparticulate carbon sheet containing 85% furnace carbon black (such as Black Pearls 2000 available from Cabot Corporation) and 15% PTFE (available commercially as Teflon 30 or Teflon 601A) was obtained by blending the particulate adsorbent material with PTFE in the presence of water, followed by intensive mixing to cause PTFE fibrillation, biaxial calendaring to form the sheet, and drying. A carbon sheet with thickness of 250 μm was obtained. FIG. 1 shows a SEM (scanning electron microscopy) image of the obtained material; carbon black nanoparticles with sizes in the 20–50 nm range are visible. A polymer fibril about 1000 nm long and 20 nm in diameter is seen in FIG. 2 . The carbon nanoparticles bound around and between polymer fibrils form an open, essentially reinforcement-free structure. The carbon black used in this example had a surface area of 1500 m 2 /g, and a total pore volume of 1.65 cm 3 /g distributed mostly (54%) in the mesopores (2–50 nm), see Table 1. The resulted nanoparticulate carbon black sheet had a total surface area of 1200 m 2 /g and a total pore volume of 1.55 cm 3 /g, from which more than 70% is distributed in the mesopores, (see Table 1). The BET surface area was calculated from nitrogen adsorption data at liquid nitrogen temperature, and the pore volume distribution was calculated using the DFT method (as developed by Micromeritics) and nitrogen adsorption data. While the average particle size of the starting carbon black was approximately 12–15 nm, it is estimated that pore sizes of greater than 50–100 nm exist in the obtained carbon sheet, as pores between complex strands and agglomerates of particles (see FIG. 1 ). The material was tested for static VOC adsorption capacity (see Example 3).
TABLE 1
Surface area and pore volume distribution of starting
particulate materials and sheet processed carbon materials
Carbon
Carbon
Activated
Activated
black
black
carbon
carbon
(BP 2000)
sheet
(MSP 20)
sheet
BET surface area (m 2 /g)
1500
1200
2400
1900
Total pore volume (< 120
1.65
1.55
0.88
0.83
nm) (cm 3 /g)
Ultra micropores (<1.18
0.19
0.15
0.45
0.33
nm) (cm 3 /g)
Super micropores (1.18–2
0.13
0.14
0.33
0.26
nm) (cm 3 /g)
Total micropores (<2 nm)
0.32
0.29
0.78
0.59
(cm 3 /g)
Micropores fraction (%)
19.39
18.71
88.64
71.08
Mesopores (2–50 nm)
0.89
1.11
0.07
0.12
(cm 3 /g)
Mesopore fraction (%)
53.94
71.61
7.95
14.46
EXAMPLE 2
This example demonstrates that processing high surface area activated carbon particles in a sheet form does not substantially reduce the surface area and micropore volume of the starting activated carbon material. According to another embodiment, a carbon sheet containing 80% activated carbon particles (such as MSP20 activated carbon available from Kansai Coke & Chemical Company), 10% carbon black (such as Black Pearls 2000 available from Cabot Corporation) and 10% PTFE (available commercially as Teflon 30 or Teflon 601A) was prepared according to the procedure from Example 1. A carbon sheet with thickness of 200 μm was obtained. FIG. 3 shows a SEM (scanning electron microscopy) image of the obtained material; carbon particles of various sizes and irregular shape form an open, reinforcement-free structure. The BET surface area and the pore volume distribution were calculated as explained in Example 1. The initial activated carbon was characterized by a BET surface area of 2400 m 2 /g and a total pore volume of 0.88 cm 3 /g, of which 88% was comprised in micropores (below 2 nm), see Table 1. The resulted activated carbon sheet material was characterized by a surface area of 1900 m 2 /g and a total pore volume of 0.83 cm 3 /g, of which 71% was comprised in micropores (below 2 nm) and 15% in mesopores (2–50 nm), see Table 1. The material was tested for static VOC adsorption capacity (see Example 4) and CO 2 adsorption capacity and kinetics (see Example 5).
EXAMPLE 3
This example demonstrates that processing carbon black material in sheet form does not significantly reduce the static VOC adsorption capacity of starting carbon black. Static adsorption of volatile organic compounds (VOC) was measured on the starting carbon black material (Black Pearls 2000) and on the derived carbon sheet material from Example 1. The samples (0.3–0.5 g) were dried at 180 C., and accurately weighed in capped glass bottles. The capped bottles were placed in desiccators containing a beaker with a few milliliters of liquid VOC (either one of toluene, carbon tetrachloride, and trimethylpentane). The lids of the desiccators were tightly closed and the bottles were uncapped. The adsorbent samples were allowed to equilibrate with the respective VOC vapors for 3 hours at room temperature. After 3 hours, the bottles were capped, removed from desiccators and accurately weighed. The weight gain represents the amount of VOC adsorbed plus the weight of saturated vapors trapped inside the capped bottles. In order to correct for the weight of saturated vapors, the adsorbent samples were replaced in the desiccators, uncapped, and the desiccator's lids were partially open to the ambient. After one more hour, the bottles were re-capped, removed from the desiccators and weighed. The weight gain versus the initial weight of dried samples represents the capacity for static VOC adsorption at the pressure of saturated vapors of respective VOC, at room temperature. The results are shown in Table 2. It is seen that the static VOC capacity of carbon sheet materials derived from carbon black are within 80–95% if the VOC capacity of the starting carbon black material.
TABLE 2
Static VOC adsorption data on carbon black and carbon black derived sheet
materials
Toluene
Carbon tetrachloride
Trimethylpentane
Carbon
Carbon
Carbon
black
Adsorbent
black
Adsorbent
black
Adsorbent Carbon
BP2000
Carbon Sheet
BP2000
Carbon Sheet
BP2000
Sheet
Weight of initial sample (g)
0.3914
0.4241
0.3704
0.4650
0.3733
0.3868
Weight of dried sample (g)
0.3823
0.4117
0.3616
0.4541
0.3642
0.3753
Weight of sample after
0.7614
0.8058
0.7362
0.8527
0.6198
0.5839
adsorption (g)
Amount adsorbed (%)
99.16
95.73
103.60
87.78
70.18
55.58
EXAMPLE 4
This example demonstrates that processing the material in sheet form does not significantly reduce the static VOC adsorption capacity of activated carbon material. Static adsorption of volatile organic compounds (VOC) was measured on the starting activated carbon material (MSP 20) and on the derived activated carbon sheet material from Example 2. The procedure was similar to that from Example 3. The results are shown in Table 3. It is seen that the static VOC capacity of activated carbon sheet materials derived from activated carbon materials are within 85–90% if the VOC capacity of the starting activated carbon material.
TABLE 3
Static VOC adsorption data on activated carbon and activated carbon derived
sheet materials
Toluene
Carbon tetrachloride
Trimethylpentane
Activated
MSP-20
Activated
MSP-20
Activated
MSP-20
Carbon
Adsorbent
Carbon MSP
Adsorbent
Carbon
Adsorbent
MSP 25
Carbon Sheet
25
Carbon Sheet
MSP 25
Carbon Sheet
Weight of initial sample (g)
0.3911
0.5698
0.3911
0.5698
0.3375
0.5699
Weight of dried sample (g)
0.2413
0.5350
0.3905
0.5515
0.3371
0.5514
Weight of sample after
0.4227
0.8907
0.9050
1.1630
0.5356
0.8299
adsorption (g)
Amount adsorbed (%)
75.18
66.49
131.75
110.88
58.88
50.51
EXAMPLE 5
This example demonstrates that the activated carbon sheet material is characterized by faster adsorption kinetics and higher adsorption capacity for CO 2 adsorption in comparison with granular activated carbon and activated carbon fibers. A carbon sheet material was obtained as shown in Example 2. The adsorption of CO 2 at room temperature was measured by the volumetric method, in which the adsorption is monitored through pressure variations following successive gas dose introductions in a close, calibrated volume. The activated carbon sheet material of Example 2 was tested against a 12×30 mesh granular activated carbon (GAC) sample obtained from coconut shell (bulk density 0.4 g/cm 3 ) and an activated carbon fiber (ACF) cloth (bulk density 0.2 g/cm 3 ). The results are shown in Table 4. It is seen that the activated carbon sheet obtained according to Example 2 is characterized by a substantially higher isothermal adsorption capacity for CO 2 , on a weight basis and on a volumetric basis, as well as by a faster mass transfer coefficient. The increased capacity, coupled with the faster mass transfer coefficient, demonstrates the advantage of using activated carbon sheet materials as components of parallel passage contactors for rapid cycle pressure swing adsorption systems. The improvement over GAC and ACF cloth comes from the open access of gas to sub-micrometer sized carbon particles immobilized in the sheet form, according to the present invention disclosure.
TABLE 4
Isothermal capacity and kinetic constant of CO 2 adsorption on activated
carbon adsorbent sheet and other forms of adsorbent carbon for reference
MSP-20
Adsorbent
Coconut Shell
Activated
Carbon
Granular Carbon
Carbon
Sheet
(12 × 30 mesh)
Fiber Cloth
Isothermal CO 2 working ca-
5.9
4.1
4.7
pacity @ 30 C. (0.5 to 5
atm) (mmole/g)
Isothermal CO 2 volumetric
2.54
1.64
0.94
capacity @ 30 C. (0.5 to 5
atm) (mmole/cm 3 )
Mass transfer coefficient of
1.4
0.7
1.4
CO 2 uptake (sec −1 )
EXAMPLE 6
This example shows the making of a parallel passage contactor with flat sheets configuration. Reference is made to FIG. 4 . The adsorbent material obtained as disclosed in this invention was manufactured as a multitude of flat sheets 1 stacked together with gaps between adjacent sheets to allow the flow of gas parallel to the sheet surface from the direction of gas inlet 2 to gas outlet 3 . A separator material was used between adjacent layers of carbon sheet. In this example the separator was a 230 μm thick polypropylene mesh.
EXAMPLE 7
This example shows the making of a parallel passage contactor with spiral configuration. Reference is made to FIG. 5 . The adsorbent material obtained as disclosed in Example 2 of this invention was manufactured as a long and continuous sheet 1 which was then rolled into a spiral with gaps between adjacent layers. The gas was allowed to flow parallel to the sheet surface from the direction of gas inlet 2 to gas outlet 3 . A separator material was used between adjacent layers of carbon sheets. In this example the separator was a 230 μm thick polypropylene mesh. The parallel passage contactor was tested for CO 2 /N 2 separation (see Example 9).
EXAMPLE 8
This example shows the making of a parallel passage contactor with honeycomb configuration. Reference is made to FIG. 6 . The adsorbent material obtained as disclosed in this invention was manufactured as a multitude of corrugated sheets 1 and flat sheets 4 . A multitude of alternating corrugated and flat sheets was assembled as shown in FIG. 6 . The gas would be allowed to flow parallel to the sheet surface from the direction of gas inlet 2 to gas outlet 3 .
EXAMPLE 9
This example demonstrates the performance of adsorbent materials manufactured according to the methods disclosed in Examples 1 and 2 when assembled as parallel passage contactors. Various activated carbon powders (such as MSP 20 from Kansai Coke & Chemicals Company; WPH from Calgon Carbon Corporation; and Picactif PCO from Pica USA), together with carbon black nanoparticles (Black Pearls 2000 from Cabott Corporation), were selected as raw materials for manufacturing adsorbent sheet materials according to the general procedures described in Examples 1 and 2. The properties of the obtained adsorbent sheet materials are outlined in Table 5. The manufactured materials were spiral wound around a central rod (0.63 cm diameter) to form parallel passage contactors as described in Example 7. The separator between adjacent adsorbent layers was a 230 μm thick polypropylene mesh. The typical length of the spiral wound rolls was 10.2 cm and the outer diameter was 2.22 cm. The resulted rolls were inserted in cylindrical canisters, which were connected to the gas line. In this configuration, the gas flow direction is parallel to the carbon adsorbent surface, as shown schematically in FIG. 5 .
TABLE 5
Properties of adsorbent carbon sheet materials made with carbon
particulates from various sources
Bulk
Areal
BET surface
Micropore
Total pore
Activated
Carbon
Thickness
density
weight
area
volume
volume
carbon source
precursor
(mm)
(g/cm 3 )
(m 2 /g)
(m 2 /g)
(cm 3 /g)
(cm 3 /g)
Cabott Corp.
Furnace
0.29
0.369
107
1200
0.257
1.60
BP2000
carbon
black
Kansai coke
Phenolic
0.20
0.525
105
1870
0.687
1.03
Maxsorb
resin
MSP20
Calgon
Bituminous
0.22
0.673
145
685
0.289
0.683
Carbon WPH
coal
Picactif PCO
Coconut
0.33
0.596
197
907
0.404
0.606
shell
Pressure drop tests were performed for each cartridge using nitrogen, with the outlet at atmospheric pressure. The flow rate was increased to a maximum of 4.5 L/min and the pressure drop across the canisters was measured using a differential pressure transducer. The permeability of canisters was calculated from the following equation:
β
=
μ
Ql
A
Δ
P
where Q (cm 3 /min) is the flow rate,/(cm) is the length, and A (cm 2 ) is the cross section of parallel passage contactors, ΔP (Torr) is the pressure drop, and μ=1.83×10 −5 Pa·s is the gas viscosity. The permeability values expressed in Darcy units (1 Darcy=0.987× 10− 10 Pa·s) are given in Table 6. The higher the permeability, the lower the pressure drop across canister at equal volume flow rates.
Breakthrough tests were measured with 1% CO 2 in nitrogen, at atmospheric pressure and room temperature. The canisters were purged several hours with pure nitrogen before each test. The tests consisted in injecting a step of 1% CO 2 concentration in the nitrogen feed, and recording the gas composition at the outlet of the contactor. The gas composition in the feed was adjusted by varying the volume flow of nitrogen (between 1500 and 4500 Ncm 3 /min) and carbon dioxide (between 5 and 60 Ncm 3 /min). The gas composition downstream the contactor was analyzed using a Stanford Research Systems residual gas analyzer model RGA-100. The gas was continuously sampled from the discharge flow and directed into the analyzer via a 0.76 mm capillary and a differential pumping system. The sampling rate of the mass spectrometer was 2 seconds. The breakthrough profiles were analyzed according to the model developed by Yoon and Nelson (Am. Ind. Hygiene Assoc. J., 45 (8), 509, 517 (1984)) based on gas adsorption kinetics in a bed of solid sorbent. The main equation of the Yoon-Nelson model is:
C
out
C
in
=
{
1
+
exp
[
-
k
′
(
t
-
τ
)
]
}
-
1
It relates the concentration of contaminant that enters (C in ) or escapes (C out ) the contactor with τ, the time at 50% breakthrough, and k′, an apparent kinetic constant that indicates the slope of the breakthrough curves. With τ and k′ measured from experimental data, an intrinsic kinetic constant k (independent on flow rate and concentration conditions) and an equilibrium adsorption capacity W e (at the corresponding gas concentration) can be calculated:
k
′
=
k
C
in
Q
W
e
=
k
τ
The calculated values are given in Table 6. Large k values indicate fast mass transfer kinetics.
The separation efficiency of each contactor was evaluated from the number of theoretical plates, N, calculated as the ratio of the total column length to the height equivalent to a theoretical plate (L HETP ). The L HETP values were calculated following the theoretical analysis of Ruthven and Thaeron (Gas. Sep. Purif. 10, 63 (1996)) from the first and second moments of the experimental breakthrough curves:
L
HETP
=
σ
2
μ
2
where μ and σ are defined as follows in case of a step concentration variation:
μ
=
τ
=
∫
0
∞
(
1
-
C
out
C
in
)
ⅆ
t
σ
2
=
∫
0
∞
2
(
1
-
C
ouy
C
in
)
t
ⅆ
t
-
μ
2
Examples of calculated values are given in Table 6. The smaller the L HETP value, the higher the separation efficiency of the parallel passage contactor.
The energy efficiency of the contactors was calculated in terms of pressure drop per theoretical stage, ΔP HETP /L HETP , as suggested in the above cited reference by Ruthven and Thaeron. For this calculation we used the experimental permeability values (β) of each canister:
Δ
P
HETP
L
HETP
=
v
β
where v is the linear velocity. Examples of calculated values are given in Table 6. The smaller the (ΔP HETP /L HETP ) value, the lower is the energy penalty for circulating the gas through the parallel passage contactor.
TABLE 6
Performance of various adsorbent sheet materials when assembled in
parallel passage contactors for CO 2 /N 2 separation
Carbon
packing
Capacity @
L HETP @
density
Contactor
Intrinsic
7.6 Torr
4.5
Activated
(g carbon /
permeability
kinetic
CO 2
L/min
ΔP HETP /L HETP
Example
carbon source
cm 3 )
(Darcy)
constant
(mmol/cm 3 )
(cm)
(mTorr/cm)
9
Granular 1 mm
0.56
1645
2.82
0.038
3.71
1.6
activated
carbon
9
Cabott Corp.
0.22
234
10.07
0.016
2.95
12.5
BP2000
9
Kansai Coke
0.35
160
8.39
0.030
1.68
18.3
Maxsorb
MSP20
9
Calgon Carbon
0.41
213
11.33
0.029
1.57
13.8
WPH
9
Picactif PCO
0.42
211
11.81
0.037
1.37
13.9
10
Kansai Coke
0.32
794
7.67
0.028
1.63
3.9
Maxsorb
MSP20 (no
spacer)
The results in Table 6 show that, with one exception, all canisters have almost constant adsorption capacity for CO 2 at 7.6 Torr CO 2 in gas phase. This is a consequence of the intrinsic adsorption properties of various carbon materials and of the packing densities that can be achieved with them.
A comparison of CO 2 breakthrough curves from 1 vol % and 2 vol % CO 2 in N 2 at several flow conditions is shown in FIG. 7 for equal volume canisters containing a bed of 1 mm granular activated carbon and a parallel passage contactor structure made from Kansai Coke Maxsorb MSP 20 activated carbon, according to this Example. Both canisters have almost equal capacity for CO 2 , but the breakthrough profile is much sharper for the parallel passage contactor made according to this invention. Similar results were found for all contactors made with adsorbent material sheets. Data in Table 6 show that they all have faster adsorption kinetics (higher intrinsic kinetic constant values) than the 1 mm granular activated carbon. This allows for using the PSA system at shorter cycle times when the contactors are made with carbon sheet materials. The sheet materials also show improved separation performance over granular carbon, as indicated by shorter HETP lengths in Table 6. However, the permeability of packed granular beds is higher than that of contactors made from spiral wound adsorbent layers plus separator mesh structures. As a result, the pressure drop per theoretical plate is lower for the granular carbon bed. In conclusion, at comparable adsorption capacity for CO 2 , the contactors made with adsorbent sheet materials afford faster kinetics (shorter cycle times) and better separation (require tower column length), at the expense of higher pressure drop.
EXAMPLE 10
This Example shows the making of a parallel passage contactor with spiral configuration and without using a separator between adjacent layers of carbon adsorbent sheets. A 400 μm thick carbon adsorbent sheet containing 80 wt % MSP 20 from Kansai Coke & Chemicals Company, 10 wt % Black Pearls 2000 from Cabott Corporation and 10 wt % PTFE binder was manufactured according to Example 2. The carbon sheet was then aligned parallel to a 200 μm thick stainless steel perforated plate containing a pattern of alternating circular holes of 500 μm diameter separated by distances no shorter than 2 mm. The carbon layer and the patterned perforated plate were passed together between the rolls of a calender. As a result, the carbon sheet acquired a regular pattern of imprinted bosses, with heights of about 100 μm, and the overall thickness of the carbon layer, including the elevated bosses, became 300 μm. This carbon layer was then spiral wound around a central rod (0.63 cm diameter) to form parallel passage contactors as described in Example 7, with the difference that a polypropylene spacer was not used. The results of CO 2 breakthrough data analysis are shown in Table 6. In comparison with all other parallel passage contactors containing a polypropylene mesh spacer, the embossed structure without spacer demonstrates higher gas permeability at comparable carbon packing density, CO 2 adsorption capacity, and intrinsic kinetic constant values. As a result of all these factors, the separation efficiency was higher and the energy penalty (expressed as pressure drop per theoretical plate) was lower than for all other contactors made with an inert separator mesh.
Examples 11–13 show that processing zeolite in a sheet form does not substantially reduce the N 2 adsorption properties of the raw zeolite powder.
EXAMPLE 11
A zeolite sheet material contained 90% zeolite 13X in Na form and 10% PTFE was obtained by blending 100 g of raw Na—X zeolite powder with 16.6 g of Teflon T30 in presence of water, followed by intensive mixing to cause PTFE fibrillation, biaxial calendaring to form the sheet, and drying. The sheets (0.25 mm thick) were air dried overnight at room temperature and for 3 more hours in air at 125 C.
EXAMPLE 12
A zeolite sheet material contained 90% zeolite 13X in Na form and 10% PTFE was obtained as described in Example 11, except that water was replaced by white gas. The sheets (0.25 mm thick) were dried for 3 hours in nitrogen at 125 C.
EXAMPLE 13
The zeolite containing sheet materials from Examples 11 and 12 were subsequently heat treated at higher temperatures in a TGA apparatus under a He stream. For comparison, the raw Na—X zeolite powder was treated in the same way. The results are shown in FIG. 9 . All samples eliminate water between about 100 and about 250 C. The water content is about 1 wt % for raw zeolite powder and between 5–8 wt % for sheet zeolite materials. The dried zeolite powder is stable above 400 C., while the PTFE component of the sheet zeolite materials from Examples 11 and 12 starts to decompose above a temperature of about 400 C.
Based on this result, drying of raw zeolite powder and sheet formed materials was carried out at 340 C. under a He stream in a microbalance. After drying, the temperature was reduced to 45 C. and He gas was replaced by N 2 . A sudden weight increase was seen with all samples. The weight uptake represents the amount of N 2 adsorbed, and the derivative of the weight change is a measure of instantaneous rate of adsorption. The data are shown in FIG. 9 for the raw Na—X zeolite and in FIGS. 10 and 11 for zeolite sheets made according to procedures from Examples 11 and 12, respectively. For all samples, the cycles of adsorption and desorption of N 2 are very reproducible. The equilibrium amounts of N 2 adsorption were 0.0095 g N 2 /g zeolite for powdered Na—X zeolite ( FIG. 9 ) and 0.0073 g N 2 /g zeolite for the two zeolite sheet formed samples ( FIGS. 10 and 11 ). The rate of adsorption were estimated to about 0.008 g N 2 min −1 /g zeolite for raw Na—X zeolite ( FIG. 9 ) and about 0.006 g N 2 min −1 /g zeolite for the two zeolite sheet formed samples ( FIGS. 10 and 11 ). | An adsorbent material fabricated into a reinforcement-free, self-supported coherent thin sheet and configured for use as a parallel passage contactor element in adsorption/separation applications with gases and liquids is disclosed. The adsorbent sheet material is obtained by enmeshing fine adsorbent particulates in a polymer binder. Particulates include but are not limited to carbon particles, inorganic oxides particles, or ceramic particles, or synthetic polymer resin particles. The adsorbent sheet advantageously contains a large volume percentage of active adsorbent particles. The parallel passage contactor device fabricated from the adsorbent sheet material is characterized by minimal mass transfer resistance and better separation efficiency expressed as height equivalent to a theoretical plate, while it maintains most of the adsorptive properties of the starting particulates, and can be used in gas separation applications with short adsorption cycles, such as rapid pressure swing adsorption, rotary concentrators, rapid electric swing adsorption. | 1 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation application of U.S. application Ser. No. 12/369,640 filed Feb. 11, 2009, which is a divisional application of U.S. application Ser. No. 11/189,120 filed Jul. 25, 2005, now U.S. Pat. No. 7,501,256 issued Mar. 10, 2009, which claims the benefit of U.S. provisional application Ser. No. 60/590,631 filed Jul. 23, 2004; and a continuation-in-part application of U.S. application Ser. No. 11/670,882 filed Feb. 2, 2007, which is a continuation-in-part of U.S. application Ser. No. 11/189,120, which claims the benefit of U.S. provisional application Ser. No. 60/590,631 filed Jul. 23, 2004; all of which prior applications are incorporated herein by reference to the extent not inconsistent herewith.
BACKGROUND OF THE INVENTION
[0002] Appendicitis is a common acute surgical problem affecting human beings of a wide age range. There are approximately 700,000 cases annually in the United States. A large proportion of cases occur in the 10 to 30 age group. An accurate diagnosis at a sufficiently early stage is a significant factor in achieving a successful outcome.
[0003] Many people present to their physician with symptoms suggestive of appendicitis but caused by other ailments such as viral infections. Differentiating the appendicitis patients from those affected with other ailments is a daunting clinical task that physicians face daily. While medical science has an excellent understanding of appendicitis and its treatment, it is very limited in its ability to accurately recognize or diagnose the disease.
[0004] Complicating the goal of an accurate and early diagnosis is the considerable overlap of genuine appendicitis with other clinical conditions. There appears to be no individual sign, symptom, test, or procedure capable of providing a reliable indication of appendicitis. Imaging technology is inadequate in identifying and characterizing the appendix, especially in the early stages of the disease when treatment is likely to be most effective. Imaging technology is further handicapped by its expense and its dependence upon the availability of highly trained and experienced people to interpret the studies. This limitation affects thousands of people every year by inaccurately diagnosing their problem or by delaying the accurate diagnosis. In cases of appendicitis, delays in diagnosis are the single most important factor leading to worsening of the condition and more complications related to the disease. The misdiagnosis of appendicitis can lead not only to unnecessary surgery but also to delay of proper therapy for the actual underlying condition.
[0005] A dilemma for surgeons is how to minimize the negative appendectomy rate without increasing the incidence of perforation among patients referred for suspected appendicitis. What is desperately needed to more effectively treat this very common ailment is a simple, reliable diagnostic test that is capable of recognizing the earliest stages of the disease process.
[0006] The typical pathogenesis in appendicitis begins with obstruction of the lumen, although an initial inflammation of the organ can precede and even contribute to the obstruction. The secreted mucus of the appendix fills the closed lumen, causing an increase in intralumenal pressure and distension. The increased intralumenal pressure can exceed the level of capillary perfusion pressure, resulting in perturbation of normal lymphatic and circulatory drainage. Ultimately the appendix can become ischemic. The appendix mucosa is compromised, which can allow invasion of intralumenal bacteria. In advanced cases, perforation of the appendix may also occur with spillage of pus into the peritoneal cavity.
[0007] Currently, the diagnosis of appendicitis is difficult, and the difficulty persists during various stages in the progression of the condition. The following represents a hypothetical portrayal of stages and associated clinical presentations. Artisans of ordinary skill will recognize that a considerable degree of variation will occur in a given patient population.
[0008] At the earliest stages of inflammation, a patient can present with a variety of non-specific signs and symptoms. Upon obstruction, presentation can involve periumbilical pain, mild cramping, and loss of appetite. The progress toward increased lumenal pressure and distension can be associated with presentation involving the localization of pain to the right lower quadrant of the abdomen, nausea, vomiting, diarrhea, and low grade fever. If perforation occurs, a patient can present with severe pain and high fever. At this very advanced stage, sepsis can be a serious risk with a potentially fatal outcome.
[0009] Practitioners currently use several tools to aid in appendicitis diagnosis. These tools include physical examination, laboratory tests, and other procedures. Routine laboratory tests include complete blood count (CBC) with or without differential and urinalysis (UA). Other tests include a computed tomography (CT) scan of the abdomen and abdominal ultrasonography. Procedures can include, for example, laparoscopic examination and exploratory surgery.
[0010] Flum et al. attempted to determine whether the frequency of misdiagnosis preceding appendectomy has decreased with increased availability of certain techniques (Flum D R et al., 2001). These techniques included computed tomography (CT), ultrasonography, and laparoscopy, which have been suggested for patients presenting with equivocal signs of appendicitis. Flum et al. concluded as follows: “Contrary to expectation, the frequency of misdiagnosis leading to unnecessary appendectomy has not changed with the introduction of computed tomography, ultrasonography, and laparoscopy, nor has the frequency of perforation decreased. These data suggest that on a population level, diagnosis of appendicitis has not improved with the availability of advanced diagnostic testing.” The rate of misdiagnosis of appendicitis is about 9 percent in men and about 23.2 percent in women (Neary, W., 2001).
[0011] Myeloid-related Protein Complex 8/14 (MRP-8/14) is a heterodimeric complex associated with acute inflammatory conditions (for review see Striz and Trebichaysky, 2004). The complex belongs to the S100 superfamily of proteins and is also referred to S100A8/9, L1, macrophage inhibitory related protein and calprotectin. The heterodimer consists of an 8 kilodalton (MRP-8) and 14 kilodalton (MRP-14) subunit. MRP-8 and MRP-14 are alternatively named S100A8/calgranulin and S100A9/calgranulin b, respectively. MRP-8/14 is a calcium binding protein originally discovered in macrophages. Neutrophils expressing high concentrations of MRP-8/14 are found in a variety of inflammatory conditions, including rheumatoid arthritis, inflammatory bowel disease and allograft rejections (Frosch et al., 2000; Limburg et al., 2000; Burkhardt et al., 2001).
[0012] MRP-8/14 is not always diagnostic of inflammation. For example, it does not reliably indicate the presence of inflammatory diverticuli (Gasché, C. 2005). Lymphocytes do not generally contain MRP-8/14 (Hycult Biotechnology, Monoclonal Antibody to Human S100A8/A9), and therefore MRP-8/14 is not diagnostic of inflammation characterized by the presence of lymphocytes but not neutrophils. Also, this protein is not always associated with opportunistic infections (Froland, M. F., et al., 1994).
[0013] Haptoglobin is an acute phase protein that binds free hemoglobin following hemolysis. The haptoglobin-hemoglobin complex is removed by the liver. Haptoglobin is a heterotetramer composed of two alpha and two beta subunits. The alpha and beta units are derived from a single polypeptide chain precursor that is enzymatically cleaved to produce the subunits. The molecular weights of the subunits are approximately 9 kd-18 kd and 38 kd for alpha and beta, respectively.
[0014] In addition to being a hemoglobin scavenger, haptoglobin has a wide range of biological functions (Dobryszycka, 1997). Haptoglobin has been shown to be upregulated and modulate the immune response in certain infection and inflammatory conditions perhaps by regulating monocyte function (Arredouani et al., 2005). The alpha subunit has been demonstrated to be a potentially useful serum marker for ovarian cancer (Ye et al., 2003).
[0015] The ability to accurately diagnose appendicitis would be greatly augmented by the identification of molecules differentially associated with appendicitis.
SUMMARY OF THE INVENTION
[0016] This invention provides a method for diagnosing appendicitis in a patient comprising identifying at least one classical symptom of appendicitis in said patient and identifying the presence of at least one molecule differentially associated with appendicitis in a fluid or tissue sample of said patient. It is recognized in the art that the diagnosis of appendicitis is difficult, and that it is often misdiagnosed. Thus the term “diagnosing appendicitis” as used herein does not necessarily mean diagnosing appendicitis with more than usual accuracy. However, in fact, the methods of the present invention have been shown to provide improvements in correct diagnosis, with almost no false positives and few false negatives.
[0017] The term “differentially associated” with respect to a molecule “differentially associated with appendicitis” refers: (1) to a molecule present in a patient with appendicitis and not present in a patient not having appendicitis; (2) to a molecule whose relative level (amount) is distinguishing between appendicitis and non-appendicitis; (3) to a molecule present, or present at a level, in conjunction with the presence of other symptoms of appendicitis, that is diagnostic of appendicitis; and/or (4) to a molecule present, or present at a level, in conjunction with the lack of symptoms associated with conditions other than appendicitis in which the presence of the molecule occurs, that is diagnostic of appendicitis.
[0018] The diagnostic level of such a molecule is also referred to herein as the “threshold amount” or “threshold level.” The molecules differentially associated with appendicitis are preferably protein antigens.
[0019] Classical symptoms of appendicitis include: pain in the abdomen; pain that starts near the navel, then moves to the lower right quadrant of the abdomen; anorexia (loss of appetite); trouble eating accompanied by sleepiness; nausea starting after onset of pain; vomiting starting after onset of pain; vomiting accompanied by fatigue; constipation; small stools with mucus; diarrhea; inability to pass gas; low-grade fever; abdominal swelling; pain in the abdomen worsening; tenesmus (feeling of needing to move the bowels); high fever; and leukocytosis. Increased plasma viscosity is also associated with appendicitis. In one embodiment of the invention at least two or more symptoms of appendicitis are identified.
[0020] In one embodiment of this invention patients are screened to determine whether or not they have an “interfering condition,” i.e., another condition in which the molecule is present in the type of sample being tested. Patients are tested for the presence of the molecule if they do not have such an interfering condition; or are tested for the presence of appendicitis-diagnostic levels of the molecule if they do have such an interfering condition. Appendix-diagnostic levels when the patient has an interfering condition are levels higher than those present in patients who have the interfering condition but do not have appendicitis. Interfering conditions include recent allograft; septicemia; meningitis; pneumonia; tuberculosis; rheumatoid arthritis; gastrointestinal cancer; inflammatory bowel disease; skin cancer, periodontitis, preeclampsia, and AIDS.
[0021] A sample can be a fluid or tissue, and can contain whole blood, plasma, serum, milk, urine, saliva and/or cells. Fecal samples may also be used. Preferably tissue and fecal samples are liquefied before testing.
[0022] In one embodiment of this invention two or more molecules differentially associated with appendicitis are tested for. Identification of additional molecules provides greater accuracy to the method.
[0023] One molecule differentially associated with appendicitis is MRP-8/14. Another is haptoglobin. Both these molecules can be tested for in diagnosing appendicitis.
[0024] MRP-8/14 levels in the range of about 1 to about 11 μg/ml are present in patients without appendicitis. Levels higher than this provide increased accuracy in diagnosing appendicitis. Levels higher than about 10, 11, 13, 15 or 20 μg/ml of MRP-8/14 can be used to diagnose appendicitis. Haptoglobin levels in the range of about 27-139 mg/dL are found in patients without appendicitis. Levels higher than this, e.g., higher than 125, 130, 135, 139 and 150 provide increased accuracy in diagnosing appendicitis.
[0025] Other molecules that can be tested for in the methods of this invention, or that can be tested for in addition to the foregoing molecules, include unique structural proteins of the gastrointestinal tract, stress-related inflammatory mediators, immunologic factors, indicators of intestinal bacterial flora, Plasminogen Activator Inhibitor-1, fatty acid binding proteins, nuclear factor kappa beta (NFκB), specific appendix antigens (HLA-DR), inflammation associated antigens; and nucleic acids coding for any of the foregoing, including nucleic acids coding for MRP-8/14 and haptoglobin. Methods for testing for the presence of nucleic acids are known to the art.
[0026] The methods of this invention involving obtaining a first sample from a patient suspected of having appendicitis can also comprise identifying at least one molecule differentially associated with appendicitis by a process including obtaining a second fluid or tissue sample from a second patient, wherein the second patient has appendicitis; obtaining a third fluid or tissue sample from a third patient wherein the third patient has a non-appendicitis condition characterized by at least one symptom of appendicitis; and analyzing the second and third samples so as to detect a molecule differentially associated with the appendicitis in the second patient, and then identifying the presence of that molecule, or presence of an increased level of that molecule, in the first sample, thereby diagnosing appendicitis. Candidate molecules for this process of identifying molecules differentially associated with appendicitis include unique structural proteins of the gastrointestinal tract, stress-related inflammatory mediators, immunologic factors, indicators of intestinal bacterial flora, Plasminogen Activator Inhibitor-1, fatty acid binding proteins, nuclear factor kappa beta (NFκB), specific appendix antigens (HLA-DR), inflammation associated antigens, and nucleic acids coding for any of the foregoing.
[0027] This invention also provides a method for identifying a molecule differentially associated with appendicitis, the method comprising obtaining a sample from each of a plurality of patients who are undergoing surgery for suspected appendicitis; determining during surgery whether each said patient has appendicitis or not; and analyzing said samples for the presence of a molecule differentially associated with appendicitis. The samples can be blood samples or samples of appendix tissue. This method can also include determining the amount of each molecule found to be differentially associated with appendicitis in the sample. In one embodiment of the invention, following identification of the molecule in tissue, it is also identified in plasma. This requires that samples of blood be taken from patients suspected of having appendicitis. The amount of the molecule differentially associated with appendicitis in patients who have appendicitis compared with those who do not is also determined.
[0028] The methods for diagnosing appendicitis of this invention can include using test devices, e.g., cartridge test devices and dipstick test devices, and/or other means for determining the presence or absence of a molecule differentially associated with appendicitis, e.g., performing western blots, northern blots, ELISA tests, protein function tests, PCR and other assays known to the art. In testing molecules differentially associated with appendicitis that are present in patients without appendicitis, but upregulated in patients with appendicitis, assays that test for the relative amount of the molecule present in patient fluids or tissues as well as the mere presence of the molecule are required. Cartridge immunoassays can be designed to provide information on relative amounts of such molecules as described herein. Other assays known to the art including ELISAs and hospital assay devices such as the Synchron LX system of Beckman Coulter can be used to provide the amount of such molecules present in the patient, which can then be compared with amounts present in patients without appendicitis to determine whether or not the patient has appendicitis.
[0029] The methods for diagnosing appendicitis can include performing an immunological assay using a monoclonal or polyclonal antibody to the molecule differentially associated with appendicitis. Such antibodies are known to the art or can be generated by means known to the art without undue experimentation.
[0030] This invention also provides an immunoassay test device for detecting the presence of a molecule differentially associated with appendicitis in a sample. The device comprises a first monoclonal or polyclonal antibody specific to the molecule, a support for the first monoclonal or polyclonal antibody, means for contacting the first monoclonal or polyclonal antibody with the sample, and an indicator capable of detecting binding of the first monoclonal or polyclonal antibody with the molecule.
[0031] Detecting binding of the antibody with the molecule can include binding the antibody/molecule complex to a second, labeled antibody which binds to the molecule or to the antibody of the complex.
[0032] Test devices can be in the form of cartridges, dipsticks, or other conformations known to the art. The test device can also be part of a kit which can contain instructions for use, instructions for comparison of test results with results of the same test done on non-appendicitis patient, additional reagents, such as cells or fluids from non-appendicitis patients, and other reagents known to the art. These types of assay devices are known to the art and described, e.g., in U.S. Patent Publication No. 2003/0224452.
[0033] The methods for diagnosing appendicitis can include comparing the level of the molecule in the sample with a background level of the same molecule in persons not having appendicitis. This comparison can be made by any means known to the art. It can include comparing sample results with results from a second sample taken from a person known not to have appendicitis, or comparing sample results with a photograph or other representation of results from a person not having appendicitis. Test devices having means for masking non-appendicitis levels, e.g. a support having the same color or tone as indicators showing non-appendicitis levels, or a filter having the same color or tone as a non-appendicitis level, so that only higher, appendicitis-indicating levels of the molecule are detectable, e.g., by eye, can also be used. The methods of this invention can include use of control fluids having background levels of the molecule typical of non-appendicitis samples, as well as colored supports and/or light filters as discussed above.
[0034] When the sample is blood, the method can also include processing the blood by a means known to the art, such as filtration or centrifugation, for separating plasma or serum which is to be assayed.
[0035] Antibody supports are known to the art. In an embodiment of this invention, antibody supports are absorbent pads to which the antibodies are removably or fixedly attached. In the devices of this invention, any indicator means known to the art to detect antibody binding with the molecule can be used. The indicator means can include second, labeled, monoclonal or polyclonal antibodies which bind to the selected protein, which preferably bind to a substantially different epitope on the selected protein from that to which the first monoclonal or polyclonal antibodies bind, such that binding of the first monoclonal or polyclonal antibody will not block binding of the second antibody, or vice versa. The indicator means can also include a test window through which labeled antibodies can be viewed. Any label known to the art can be used for labeling the second antibody. In an embodiment of this invention, the label is colloidal gold. The second antibody can be monoclonal or polyclonal. In an embodiment of this invention, the first antibody is a polyclonal or a monoclonal antibody made using a specific polypeptide sequence of the molecule differentially associated with appendicitis, and the second antibody is a different monoclonal or polyclonal antibody which binds to a different site of the molecule or binds to the first antibody. Antibodies for MRP-8 and MRP-14 are commercially available through Cell Sciences, Canton, Mass. Monoclonal antibodies to haptoglobin useful in the methods of this invention are also known to the art, e.g., as described in U.S. Pat. No. 5,552,295.
[0036] In one embodiment of this invention, the sample to be assayed is a liquid, and the immunoassay test device is a lateral flow device comprising inlet means for flowing a liquid sample into contact with the antibodies. The test device can also include a flow control means for assuring that the test is properly operating. Such flow control means can include control antigens bound to a support that capture detection antibodies as a means of confirming proper flow of sample fluid through the test device. Alternatively, the flow control means can include capture antibodies in the control region which capture the detection antibodies, again indicating that proper flow is taking place within the device.
[0037] Methods for detecting the presence of a molecule differentially associated with appendicitis using the foregoing devices are also provided, the methods comprising: providing an immunoassay test device of this invention; contacting a first antibody with a sample; and reading an indicator which is capable of detecting binding of the first antibody. Preferably, binding indicates appendicitis in the patient being tested. Methods of using these devices can be performed in the doctor's office, emergency room, or surgery, rather than requiring sending the patient or the sample to a separate laboratory.
[0038] The devices of this invention are useful for testing the above-mentioned samples. When cells are tested, e.g., when the molecule differentially associated with appendicitis is suspected to be in blood or tissue cells rather than serum, the method and/or device can include a cell-lysing step or means using detergent, puncture or other physical or chemical process known to the art.
BRIEF DESCRIPTION OF THE FIGURE
[0039] FIG. 1 : Two-dimensional electrophoresis image of proteins from (A) normal and (B) diseased appendix tissue. Proteins were separated by isoelectric focusing on the x axis and by molecular weight on the y axis. The molecular weight in kilodaltons is shown on the left. The arrow indicates the upregulated protein, AP-93.
[0040] FIG. 2 : MRP-14 western blot analysis of normal (N) and diseased (A) tissue. The numbers are sample ID numbers. Molecular weights are shown in kilodaltons.
[0041] FIG. 3 : MRP-8 western blot analysis of normal (N) and diseased (A) tissue. The numbers are sample ID numbers. Molecular weights are shown in kilodaltons.
[0042] FIG. 4 : Relative levels of MRP-8/14 in normal and appendicitis serum as determined by ELISA. The levels are given as a fraction of the mean for the patients not having appendicitis, said fraction also being referred to herein as a “fold increase.” Dark bars represent samples from patients having appendicitis. White bars represent samples from patients not having appendicitis.
[0043] FIG. 5 : Two-dimensional electrophoresis image of proteins in depleted serum samples from (A) normal and (B) appendicitis patients. Proteins were separated by isoelectric focusing on the x-axis and by molecular weight on the y-axis. The molecular weight in kilodaltons is shown in the right. The tailed arrow indicates the upregulated protein, AP-77 (haptoglobin alpha subunit). The untailed arrow indicates a control protein that is equally abundant in diseased vs. normal.
[0044] FIG. 6 : Two-dimensional electrophoresis image of proteins from (A) normal and (B) diseased (perforated) appendix tissue. Proteins were separated by isoelectric focusing on the x axis and by molecular weight on the y axis. The molecular weight in kilodaltons is shown on the left. The arrow indicates the upregulated protein, AP-91 (haptoglobin alpha subunit).
[0045] FIG. 7 : Haptoglobin distribution. Haptoglobin western blot analysis of normal (N) and diseased (A) tissue. The numbers are sample ID numbers. Molecular weights are shown in kilodaltons. The alpha and beta subunits are >20 kd and 38 kd, respectively.
DETAILED DESCRIPTION
[0046] The vermiform appendix is recognized as a separate organ from the large and small intestines. It extends as a finger-like pouch from the base of the ascending colon, which is also called the cecum. The appendix, like the large intestine, is hollow and composed of the same three tissue layers. These three layers are a mucosa, muscularis and a serosa. The appendiceal lumen communicates with the lumen of the cecum via a round opening (os) through which the appendix adds its secretions to the fecal stream. These secretions are excess mucus produced from the appendiceal mucosa. In addition to containing mucus, the appendix also contains numerous bacteria common to the right colon. Obstruction of the appendiceal lumen is the dominant factor causing acute appendicitis. While fecaliths are the usual cause of appendiceal obstruction, hypertrophied lymphoid tissue, inspissated barium from previous x-ray studies, vegetable and fruit seeds, and intestinal worms like ascarids can also block the appendiceal lumen.
[0047] Following luminal obstruction an escalating cycle of events ensues. The proximal obstruction of the appendix produces a closed-loop obstruction that blocks the normal flow of appendiceal mucus into the cecum. The continuing normal secretion of the appendiceal mucus very rapidly fills the luminal capacity of the appendix (approximately 0.1 cc). Once the luminal capacity of the appendix is reached additional mucus production from the obstructed appendix rapidly elevates the intraluminal pressure within the organ. This elevated intraluminal pressure is exerted outward against the appendiceal wall and causes the appendix to distend. Distention stimulates nerve endings of the visceral afferent pain fibers, producing vague, dull, diffuse pain in the midabdomen or lower epigastrium. Peristalsis is also stimulated by the rather sudden distention, so that some cramping may be superimposed on the visceral pain early in the course of appendicitis.
[0048] Distention of the appendix continues, not only from continued mucosal secretion, but also from rapid multiplication of the resident bacteria of the appendix. As pressure in the organ increases, venous pressure within the appendiceal wall is exceeded. This rising intraluminal pressure then occludes capillaries and venules, but arteriolar inflow continues, resulting in engorgement and vascular congestion. Distention of this magnitude usually causes reflex nausea and vomiting, and the diffuse visceral pain becomes more severe. The inflammatory process soon involves the serosa of the appendix and in turn parietal peritoneum in the region, producing the characteristic shift in pain to the right lower quadrant (RLQ). The disease process is fairly advanced when pain is localized to the RLQ.
[0049] The mucosa of the gastrointestinal tract, including the appendix, is very susceptible to impaired blood supply. Thus mucosal integrity is compromised early in the process, allowing bacterial invasion of the deeper tissue layers. This bacterial invasion leads to appendiceal destruction and systemic liberation of various bacterial toxins. Fever, tachycardia, and leukocytosis develop as a consequence of this systemic release of dead tissue products and bacterial toxins. As progressive appendiceal distention rises, encroaching on the arteriolar pressure, ellipsoidal infarcts develop in the antimesenteric border of the appendiceal serosa. As distention, bacterial invasion, compromise of vascular supply and infarction progress, perforation occurs through one of the infarcted areas on the antimesenteric border. This perforation then releases the bacteria and its toxins into the abdominal cavity.
[0050] Appendicitis has been called the “great imitator,” as its symptoms are frequently confused with those of other conditions. This confusion stems from the nonspecific nature of the pain early in its course and the variability in how appendicitis progresses. Pain in the right lower quadrant of the abdomen is the hallmark of appendicitis but this is not typically what the patient first perceives. When the appendiceal lumen first obstructs, the patient will have few if any symptoms because the appendiceal lumen has not yet had the chance to fill with mucus. The time required to fill the appendiceal lumen is proportional to the lumen volume available behind the obstruction. This is variable and unpredictable, as that volume is dependent upon the individual's appendix size and precisely where the fecalith or other obstruction is located along that length. Should the fecalith or other obstruction be close to the tip of the appendix the available volume is relatively small and the time to symptoms or perforation short. In contrast, the opposite will be true should the fecalith or other obstruction be near the base of the appendix and provide for the largest possible appendiceal volume.
[0051] Once the appendix begins to distend, the appendicitis patient will begin to experience a nonspecific discomfort usually in the mid portion of the abdomen. This discomfort can be easily confused with common ailments such as indigestion, constipation or a viral illness. Continued appendiceal distention is also accompanied by some nausea and frequently vomiting. Rarely is the vomiting severe or unrelenting, which reinforces the confusion with common ailments.
[0052] Later in the progression of appendicitis, inflammation will have progressed to the outermost layer of the appendix. This outmost layer is called the serosa and it touches the inner lining of the abdominal cavity called the peritoneum. This contact irritates the peritoneum, producing peritonitis that is perceived by the appendicitis patient as focal pain wherever the appendix is touching the peritoneum. This too can vary between different individuals. The appendix is most usually located in the right lower quadrant under an area known as McBurney's point. McBurney's point is a position on the abdomen that is approximately two-thirds of the distance from the anterior superior iliac spine in a straight line toward the umbilicus. The appendix can, however, reside in other locations in which case the peritonitis produced by the appendix will be in an atypical location. This again is a common factor producing an erroneous diagnosis and delays surgical treatment in cases of appendicitis.
[0053] Regardless of its location, if appendicitis is allowed to progress the organ will eventually perforate. This contaminates the abdominal cavity around the perforated appendix with bacteria producing a severe infection. This infection will usually lead to a localized intra-abdominal abscess or phlegmon and can produce generalized sepsis.
[0054] To identify molecules differentially associated with appendicitis, a proteomic approach was used. A protein complex, MRP-8/14, that is present in appendix tissue in patients with acute appendicitis was identified. The highly correlative nature of this complex with appendicitis led us to examine MRP-8/14 serum levels in patients with apparent appendicitis. MRP-8/14 is significantly elevated (p<0.02) in patients with appendicitis as compared to levels in patients with apparent appendicitis yet having no appendiceal inflammation. The source of MRP-8/14 in the serum is the inflamed appendix tissue. This is consistent with the known functions of MRP-8/14.
[0055] The role of MRP-8/14 in inflammation is not fully understood but it does seem to play a vital role in retaining leukocytes in microcapillaries. Extracellular MRP-8/14 interacts with endothelial cells by binding to heparin sulfate and specifically carboxylated glycans (Robinson et al., 2002). The intracellular signal pathways and effector mechanisms induced by binding of MRP-8/14 to endothelial cells are not well defined. However, interaction of MRP-8/14 with phagocytes increases binding activity of the integrin receptor CD11b-CD18. This is one of the major adhesion pathways of leukocytes to vascular endothelium (Ryckman et al., 2003). It is believed that the MRP-8/14 utilizes the receptor for advanced glycation end products (RAGE). A relative of MRP-8/14, S100A12, is a specific ligand of RAGE expressed by endothelial cells and their interaction activates NF-kappa B binding in these cells (Hsieh et al., 2004). The NF-kappa B binding subsequently induces expression of many proinflammatory molecules, such as various cytokines or adhesion molecules. Thus, release and extracellular functions of S100 proteins represent a positive feedback mechanism by which phagocytes promote further recruitment of leukocytes to sites of inflammation. Taken together, these proteins appear to play a role in a fundamental inflammatory response in certain inflammatory conditions, and are excellent markers of appendix tissue inflammation.
[0056] Neutrophils are white blood cells that are the first to migrate from the circulation into sites of inflammation. Within neutrophils, constituting approximately 40% of total cytosolic proteins is the MRP-8/14 complex. This protein is specifically expressed only in cells of macrophage lineage, making blood monocytes and acutely activated macrophages other potential white blood cell sources of these proteins. MRP-8/14 is not usually expressed in lymphocytes nor resident macrophages or those macrophages involved in chronic inflammation. These two proteins are also known to be independently expressed by mucosal epithelium in specific states of acute inflammation.
[0057] In the case of appendicitis, the luminal obstruction and the resultant distention of the appendiceal wall triggers an inflammatory response. The circulating neutrophils are then recruited into the area, as are activated macrophages. While the expression of this protein complex is related to the activity of the macrophages in inflammation, the exact relationship between MRP-8/14 and cellular activity is not fully known. What is known is that the intracellular distribution of MRP-8/14 varies with the activation state of macrophages. Normal macrophages contain the complexes in the cytosol, but once stimulated, MRP-8/14 translocates from the cytosol to the cell membrane (specifically with the proteins of the cytoskeleton). This would imply that MRP-8/14 may be related to cell movement, phagocytosis or inflammatory signal transduction. The roles of cellular movement and signal transduction may also explain why MRP-8/14 is produced directly from vascular epithelium such as that lining the blood vessels within the appendix.
[0058] Regardless of its role in certain inflammatory conditions, MRP-8/14's abundance within cells of acute inflammation makes it an excellent detector and monitor of acute appendicitis. The first step in the inflammatory process is the recruitment of neutrophils and macrophages to a specific site. In our study, the specific site is the appendix, where those MRP-8/14-containing cells will engage the offending stimulus. This engagement will usually result in MRP-8/14 cell death and the liberation of MRP-8/14 from either the cytosol or cell membrane into the patient's circulation. At the same time, the mucosal linings of the appendix will start to produce and release MRP-8/14 to facilitate macrophage migration or inflammatory amplification. This process will then escalate as increasing amounts of MRP-8/14 cells are recruited by the appendicitis to ultimately release more MRP-8/14 into the circulation. Other examples of inflammatory states causing increases of extracellular MRP-8/14 and the tendency of these increases of MRP-8/14 to correlate with extent of inflammation are known. Specifically, chronic bronchitis, cystic fibrosis and rheumatoid arthritis are all associated with elevated serum levels of MRP-8/14 and the severity of these diseases is generally proportional to the serum levels of MRP-8/14 detected.
[0059] The physiological role of MRP-8/14 makes it an ideal clinical marker for acute appendicitis. As patients with appendicitis are generally young and healthy, they generally produce a vigorous inflammatory response. This vigorous response is believed to liberate MRP-8/14 in the earliest stages of the disease, which then escalates as appendicitis progresses. Additionally, the diseases known to be associated with elevated levels of MRP-8/14 are not common in this younger age group and usually do not produce symptomology similar to appendicitis. Finally, as MRP-8/14 is not located in nor associated with lymphocyte proliferation, this marker is not believed to be elevated in viral infections. This is an especially powerful advantage for diagnosing appendicitis, as viral infections are one of the most common imitators of appendicitis.
[0060] Haptoglobin was also identified in this invention as a useful marker for appendicitis. A differential proteomic screen of depleted serum identified haptoglobin as a marker for appendicitis. A second differential screen of appendix tissue confirmed that haptoglobin is upregulated in the appendix tissue of patients with appendicitis. This finding was confirmed by western blotting of tissue protein. In particular the alpha subunit isoforms were present only in diseased tissue. Since haptoglobin is a plasma protein, it is highly valuable as a biomarker for appendicitis.
EXAMPLES
Example 1
MRP-8/14
[0061] The objective of this study was to identify a tissue-specific marker that could contribute to the decision matrix for diagnosing early acute appendicitis. A proteomic screen was used to identify a protein in the appendix specifically upregulated in acute appendicitis. MRP-8/14 was identified as present both in the diseased appendix and in serum of acute appendicitis patients.
[0062] Materials and Methods
[0063] Specimen and Serum Collection. All patients enrolled in this study were treated according to accepted standards of care as defined by their treating physicians. Prior to being approached for inclusion in our study, all patients were evaluated by a surgeon and diagnosed by that surgeon as having appendicitis. The treating surgeon's plans for these appendicitis patients included an immediate appendectomy. The specifics of all treatments such as use of antibiotics, operative technique (either open or laparoscopic) were determined by the individual surgeon.
[0064] Exclusion Criteria: Any patients with pre-existing chronic inflammatory diseases such as asthma, rheumatoid arthritis, inflammatory bowel disease, psoriasis, or neutropenia. Pregnancy was also considered an exclusion criterion.
[0065] An investigator counseled all patients about the study and informed consent was obtained. At the time of informed consent, the subject was assigned an identification number and non-personal demographic and clinical information was obtained (age, sex, race, duration of symptoms, white blood count (WBC), results of imaging studies, etc). At the time of surgery, following induction of general anesthesia, a whole blood sample (5-10 cc volume) was obtained via peripheral venopuncture. This blood specimen was then placed on ice. As soon as possible, a small sample (approximately 1 gram) of inflamed appendix was taken from the pathologic specimen and also placed on ice. The iced blood specimens were then centrifuged for 20 minutes at 3000 rpm and the separated serum isolated. This isolated serum and the piece of appendix tissue were then stored separately, frozen at −80° C.
[0066] Appendicitis Tissue Processing. Appendix tissue from appendectomy patients was harvested and stored at −80° C. until processed. Individual tissue samples were ground into powder using a sterile mortar and pestle under liquid nitrogen. Protein was extracted from tissue powder by incubating at 37° C. in Extraction Buffer (0.025M Tris-base, 200 mM Sodium Chloride, 5 mM EDTA, 0.1% Sodium Azide, pH 7.5). Samples were centrifuged for 10 minutes at 14K rpm. Supernatants were stored at −80° C. until analysis.
[0067] 2D Gel Analysis of Extracted Tissue Samples. 2D gel analysis was performed on depleted serum samples and extracted tissue samples. Isoelectric focusing (IEF) and SDS-PAGE were performed according to the Zoom (Invitrogen) protocol for 2D Gel analysis. Equal quantities of protein were analyzed on each gel.
[0068] Comparisons between negative serum gel and positive serum gel were made to determine which proteins were present in positive samples and absent in negative samples. Candidate gel spots were identified and submitted to MALDI-TOF protein identification analysis (Linden Biosciences).
[0069] Western Blot Analysis of Extracted Appendix Tissue Samples. Samples (10 μg) were subjected to standard Laemmli SDS-PAGE and proteins were transferred to nitrocellulose membrane for western blot analysis using standard techniques with chemiluminescent detection. Magic Mark Western Standard (Invitrogen) was used to determine molecular weight. MRP-8 (Calgranulin A C-19, Santa Cruz, S.C.—8112) was used in a 1:100 dilution in 0.5× Uniblock (AspenBio, Inc) for primary antibody. The secondary antibody was Peroxidase anti-goat IgG (H+L), affinity purified (Vector, PI-9500) in a 1:2000 dilution in Uniblock. MR-14 (Calgranulin B C-19, Santa Cruz, S.C.—8114) was used in a 1:100 dilution in 0.5× Uniblock for primary antibody. The secondary antibody was Peroxidase anti-goat IgG (H+L), affinity purified (Vector, PI-9500) in a 1:2000 dilution in Uniblock.
[0070] Serum MRP-8/14 Determinations. Serum levels of MRP-8/14 were determined by ELISA using a commercially available ELISA (Buhlmann 5100-Cellion S100 A8/A9) according to the manufacturer's protocol.
[0071] Results
[0072] Identification of Proteins Present in Appendix Tissue from Appendicitis Patients. A differential proteomic analysis was performed on depleted serum samples with the goal of identifying proteins elevated in patients with acute appendicitis. The analysis involved comparing samples from normal patients versus patients with perforated appendices. Blood samples were obtained immediately prior to surgery. A normal patient in this study is one that presented with abdominal pain, underwent surgery, and was found to have a normal appendix. Normal and diseased appendix tissue was collected during surgery.
[0073] The proteomic approach was to compare a pool of 4 normal samples with a pool of 4 appendicitis samples using two-dimensional electrophoresis. FIG. 1 shows the 2D profile of proteins analyzed. Comparison between the gels was performed and the most obvious difference is indicated in FIG. 1B as AP-93. Based on the gel in FIG. 1 , the molecular weight of AP-93 is approximately 14 kilodaltons. The corresponding gel slice was analyzed by MALDI-TOF and a positive identification was made. The identification was based upon spectra of two tryptic peptides, NIETIINTFHQYSVK [SEQ ID NO:1] and LGHPDTLNQGEFKELVR [SEQ ID NO:2]. The peptides correspond to the underlined residues in the following amino acid sequence of MRP-14 (GenBank Accession Number P06702):
[0000]
[SEQ ID NO: 3]
MTCKMSQLER NIETIINTFHQYSVKLGHPDTLNQGEFKELVR KDLQNFLK
KENKNEKVIEHIMEDLDTNADKQLSFEEFIMLMARLTWASHEKMHEGDEG
PGHHHKPGLGEGTP.
[0074] The MALDI-TOF identification of AP-93 as MRP-14 was confirmed by the matching molecular weights. Based on this data, MRP-14 protein was more highly abundant in the diseased sample pool than in the normal sample pool.
[0075] Presence of MRP-14 and MRP-8 in Diseased Appendix Tissue. In order to confirm the presence of MRP-14 in diseased tissue, an anti-MRP-14 antibody was used in western blotting of tissue extracts from individual normal and diseased appendices. FIG. 2 shows the western blot data from 9 normal and 11 appendicitis samples. A 14 kilodalton band is present in every appendicitis sample. There is no detectable signal in the normal samples. This data confirms the proteomic screen data and shows that the protein is an indicator of diseased appendix tissue.
[0076] Since it is known that MRP-8 exists as a dimer with MRP-14, tissue specimens were also examined for the presence of MRP-8. FIG. 3 shows the western blot data using an anti-MRP-8 antibody on the normal and diseased tissue samples. As expected, MRP-8 is present in all of the diseased appendix samples and not detectible in the normal appendix tissue. These western blot data show that the MRP-8 and MRP-14 proteins are markedly more abundant in appendicitis than in normal appendix tissue.
[0077] Elevated Serum Levels of MRP-8/14 Patients with Acute Appendicitis. The high correlation between appendicitis and the presence of MRP-8/14 in the appendix led us to examine the MRP-8/14 levels in serum of those patients and other patients subsequently added to the study. The sera were collected before surgery, banked and analyzed after the disease status was known. MRP-8/14 levels were measured using a sandwich ELISA specific for the complex.
[0078] Table 1 lists serum MRP-8/14 levels for 39 patients as determined by an ELISA manufactured by Hycult (Netherlands) and available commercially through Cell Sciences, Canton, Mass. The amounts are given as fractions compared to an average level for patients in the study without appendicitis. Note that all patients with appendicitis show a fold-increase of MRP-8/14 over average normal levels. The procedure was conducted according to instructions accompanying the ELISA product. The sample numbers do not correspond to the sample numbers shown in FIGS. 2 and 3 as the samples were renumbered.
[0000]
TABLE 1
Sample
Fraction of
Number
Clinical Diagnosis
Pathology
Grading
Normal
1
Advanced Appendicitis
Mild Acute Appendicitis
2
2.80428
2
Normal Appy
Normal
1
0.960805
3
Advanced Appendicitis
Transmural Appendicitis
3
5.554904
4
Perforated Appy
Perforated Appy-Necrosis
4
6.53913
5
Early Appy
Mild Acute Appendicitis
2
4.562059
6
Early Appy
Mild-Acute Appendicitis
1
2.881124
7
Horrible perforated
Perforated Appy-Necrosis
4
7.906886
8
Normal Appy
Mild Acute Appendicitis
2
3.971489
9
Early Appy
Transmural Appendicitis
3
3.83328
10
Advanced Appendicitis
Transmural Appendicitis
3
3.566665
11
Appendicitis
Mild Acute Appendicitis
2
3.205335
12
Appendicitis
Transmural Appendicitis
3
5.51224
13
Advanced Appendicitis
Transmural Appendicitis
3
2.92671
14
Advanced Appendicitis
Transmural Appendicitis w
4
3.866306
Necrosis
15
PERFORATED
Transmural Appendicitis
3
4.54657
16
Advanced Appendicitis
Perforated Appy
4
7.01877
17
Advanced Appendicitis
Transmural Appendicitis
3
4.25998
18
Appendicitis
Transmural Appendicitis
3
6.90312
19
Normal Appy
Normal
1
0.838679
20
Normal Appy
Normal
1
0.590095
21
Early Appy
Appendicitis with Peri appy
3
1.682291
changers
22
Normal Appy
Normal
1
1.128849
23
Advanced appendicitis
Transmural Appendicitis
4
2.338583
24
Normal Appy
Normal
1
2.478035
25
Hot appy
2.807046
26
Perforated
Perforated
4
4.954136
27
Normal
Normal
1
0.918438
28
Hot
Hot
2
4.387589
29
Early
Transmural Appendicitis
3
4.015013
30
Hot
Transmural Appendicitis
3
2.460902
31
Normal
Normal
1
0.594943
32
Hot
Transmural Appendicitis
3
4.211086
33
Perforated
Transmural Appendicitis
4
3.835219
34
Normal
Normal
1
1.968859
35
Perforated
Transmural Appendicitis
4
4.126198
36
Advanced
Transmural Appendicitis
3
2.423726
37
Hot Appy
Transmural Appendicitis
3
4.178647
38
Early
Transmural Appendicitis
3
9.584398
39
Normal
Transmural Appendicitis
2
2.835339
[0079] We have identified a protein complex that is present in the appendix and serum of appendicitis patients. Based on the western blot data, the presence of MRP-8/14 in appendix tissue is highly correlative with disease. Furthermore, levels of MRP-8/14 in serum are predictive of appendicitis. We presume that this increase is due to increased production of these proteins from systemic neutrophil infiltration of the appendix and possibly direct mucosal production of the proteins by the appendix itself. This study demonstrates that MRP-8/14 is a useful clinical marker for acute appendicitis. After our discovery that MRP-8/14 was a molecule differentially associated with appendicitis, our work was confirmed by the finding of Power, C. et al., 2004 and 2005, who reported detection of this molecule in feces of patients having acute appendicitis.
Example 2
Haptoglobin
[0080] Using a proteomic screen of serum and appendix tissue, we determined that haptoglobin is upregulated in patients with acute appendicitis. The alpha subunit of haptoglobin is an especially useful marker in screening for the disease.
[0081] Materials and Methods
[0082] Specimen and serum collection, appendicitis tissue processing, 2D gel analysis of extracted tissue samples, and western blot analysis of extracted appendix tissue samples were as described above in Example 1, except that for the western blot, affinity-purified anti-human haptoglobin (Rockland, 600-401-272) was used at a 1:5000 dilution in 0.5× uniblock for the primary antibody; and the secondary antibody was peroxidase anti-rabbit IgG (h+l), affinity purified (vector, pi-1000) in a 1:5000 dilution in uniblock.
[0083] Results
[0084] Identification of proteins present in appendix tissue from appendicitis patients. A differential proteomic analysis was performed on depleted serum samples with the goal of identifying proteins elevated in patients with acute appendicitis. The analysis involved comparing samples from normal patients versus patients with perforated appendices. Blood samples were obtained immediately prior to surgery. A normal patient in this study is one that presented with abdominal pain, underwent surgery, and was found to have a normal appendix. Normal and diseased appendix tissue was collected during surgery.
[0085] The proteomic approach was to compare a pool of 4 normal samples with a pool of 4 appendicitis samples using two-dimensional electrophoresis. FIG. 5 shows the 2D profile of proteins analyzed from serum depleted of IgG and albumin. Comparison between the gels was performed and the most obvious difference is indicated in FIG. 5B as AP-77. The protein in gel spot AP-77 was digested with trypsin and analyzed by MALDI-TOF. The resulting two peptides have the following sequences: TEGDGVYTLNNEKQWINK [SEQ ID NO:4] and AVGDKLPECEADDGCPKPPEIAHGYVEHSVR [SEQ ID NO:5]. The sequences were aligned with the alpha subunit of haptoglobin. The sequence of haptoglobin precursor (GenBank Accession Number NP005134) is shown below with the tryptic fragments underlined.
[0000]
[SEQ ID NO: 6]
MSALGAVIALLLWGQLFAVDSGNDVTDIADDGCPKPPEIAHGYVEHSVRY
QCKNYYKLR TEGDGVYTLNDKKQWINKAVGDKLPECEADDGCPKPPEIAH
GYVEHSVR YQCKNYYKLRTEGDGVYTLNNEKQWINKAVGDKLPECEAVCG
KPKNPANPVQRILGGHLDAKGSFPWQAKMVSHHNLTTGATLINEQWLLTT
AKNLFLNHSENATAKDIAPTLTLYVGKKQLVEIEKVVLHPNYSQVDIGLI
KLKQKVSVNERVMPICLPSKDYAEVGRVGYVSGWGRNANFKFTDHLKYVM
LPVADQDQCIRHYEGSTVPEKKTPKSPVGVQPILNEHTFCAGMSKYQEDT
CYGDAGSAFAVHDLEEDTWYATGILSFDKSCAVAEYGVYVKVTSIQDWVQ
KTIAEN.
[0086] FIG. 6 shows the two-dimensional electrophoresis profile comparison between diseased and normal appendix tissue proteins. Two spots, AP-91 and AP-93, were analyzed by MALDI-TOF and positive identifications were determined. AP-91 protein was determined to be identical to AP-77, haptoglobin-alpha.
[0087] Elevated haptoglobin in diseased appendix tissue. In order to confirm the presence of haptoglobin in diseased tissue, an anti-haptoglobin antibody was used in western blotting of tissue extracts from individual normal and diseased appendices. FIG. 7 shows the western blot data from 6 normal and 6 appendicitis samples. Nearly every sample contained some level of the 38 kd beta subunit, however, there appeared to be an elevated level in cases of appendicitis. A >20 kilodalton band is present in every appendicitis sample and absent from all of the normal tissue samples. This data confirms the proteomic screen data and shows that the protein is an indicator of diseased appendix tissue. The alpha subunit has higher specificity than the beta subunit.
Example 3
Method of Identifying Molecules Using Fluid Samples
[0088] In variations of this example, fluid samples can include whole blood, serum, or plasma. The samples are whole blood collected from human patients immediately prior to an appendectomy. The specimens are placed on ice and transported to the lab. The blood is then processed by centrifugation at 3000 rpm for 15 minutes. Plasma is then separated by pouring into another container
[0089] Upon performing an appendectomy, a patient is classified as having appendicitis (AP) or non-appendicitis (NAP). The classification is based on clinical evaluation, pathology, or both as known in the art. For cases of appendicitis, the clinical condition is also characterized as either perforated or non-perforated.
[0090] The samples from AP patients are optionally pooled and divided into aliquots. Optionally, a pooled aliquot is treated so as to remove selected components such as antibodies and serum albumin. Similarly, the samples from NAP patients are optionally pooled and divided into aliquots with optional treatment to remove the same selected components. Preferably the AP samples and NAP samples are processed in a similar manner.
[0091] Next, the pooled aliquots of AP and NAP samples are each subjected to two-dimensional gel electrophoresis as known in the art. The results of each sample type are compared with respect to the presence, absence, and relative expression levels of proteins. Preferably, one detects a signal corresponding to a protein derived from an AP sample that is either absent or expressed at relatively lower levels in a NAP sample. Further characterization is performed for such an AP protein.
[0092] The further characterization can include partial amino acid sequencing, mass spectrometry, and other analytical techniques as known in the art. A full length clone of the gene corresponding to the partial amino acid sequence can be isolated and expressed as a recombinant protein. The recombinant protein can be used as an antigen for detection. Alternatively, a partial or complete recombinant protein can be used to induce or otherwise generate a specific antibody reagent, polyclonal or monoclonal. The antibody reagent is used in the detection of antigen in a patient so as to aid in appendicitis diagnosis. A combination of antigenic molecules can be employed in appendicitis diagnosis.
Example 4
Method of Identifying Molecules Using Tissue Samples
[0093] Tissue samples are collected from appendicitis (AP) and non-appendicitis (NAP) patients. Preferably the tissue is the appendix. The AP or NAP tissues samples are optionally pooled so as to generate an AP tissue pool or an NAP tissue pool. The AP and NAP tissue samples are each used as a source for isolation of total RNA and/or mRNA. Upon isolation, the AP-RNA and NAP-RNA are maintained separately and used for preparation of cDNA.
[0094] A subtraction library is created using techniques available in the art. A cDNA library is optionally amplified. The cDNA library is treated so as to remove undesirable constituents such as highly redundant species and species expressed both in diseased and normal samples. Examples of the techniques include those described by Bonaldo et al. (1996) and Deichmann M et al. (2001).
[0095] Upon generation of the subtraction library, one analyzes, isolates, and sequences selected clones corresponding to sequences differentially expressed in the disease condition. Using molecular biology techniques, one selects candidates for recombinant expression of a partial or complete protein. Such a protein is then used as an antigen for detection. Alternatively, a partial or complete recombinant protein can be used to induce or otherwise generate a specific antibody reagent, polyclonal or monoclonal. The antibody reagent is used in the detection of antigen in a patient so as to aid in appendicitis diagnosis. It is envisioned that a combination of antigenic molecules can be employed in appendicitis diagnosis
Example 5
Method of Appendicitis Diagnosis by Evaluation of Plasma Sample Viscosity
[0096] Whole blood is drawn from a suspected appendicitis patient immediately prior to appendectomy. The specimens are placed on ice and transported to the clinical lab. The blood is processed by centrifugation at 3000 rpm for 15 minutes followed by separation of plasma from the sample by pouring into another container.
[0097] During the step of pouring, the samples are evaluated with respect to viscosity. Increased viscosity is indicative of appendicitis. Approximately 80% of samples corresponding to appendicitis cases demonstrate increased viscosity, whereas approximately none to less than 5% of samples corresponding to non-appendicitis cases demonstrate increased viscosity. It is noted that the degree of increased viscosity can correlate with the severity of appendicitis.
[0098] Viscosity measurements can be conducted by visual observation or by using techniques known in the art. For example, a Coulter Harkness capillary viscometer can be used (Harkness J., 1963) or other techniques (Haidekker M A, et al., 2002).
[0099] The presence of increased viscosity in plasma may be used in combination with other diagnostic techniques, for example with one or more of the following: physical examination, complete blood count (CBC) with or without differential, urinalysis (UA), computed tomography (CT), abdominal ultrasonography, and laparoscopy.
[0100] All references throughout this application, for example publications, patents, and patent documents, are incorporated by reference herein in their entireties, as though individually incorporated by reference, to the extent each reference is at not inconsistent with the disclosure in this application.
[0101] Where the terms “comprise”, “comprises”, “comprised”, or “comprising” are used herein, they are to be interpreted as specifying the presence of the stated features, integers, steps, or components referred to, but not to preclude the presence or addition of one or more other feature, integer, step, component, or group thereof.
[0102] The invention has been described with reference to various specific and preferred embodiments and techniques. However, it should be understood that many variations and modifications may be made while remaining within the spirit and scope of the invention. It will be apparent to one of ordinary skill in the art that compositions, methods, devices, device elements, materials, procedures, techniques, and embodiments, and variations respectively thereof, other than those specifically described herein can be applied to the practice of the invention as broadly disclosed herein without resort to undue experimentation. All art-known functional equivalents are intended to be encompassed by this invention. Whenever a range is disclosed, all subranges and individual values are intended to be encompassed. This invention is not to be limited by the embodiments disclosed, including any shown in the drawings or exemplified in the specification, which are given by way of example and not of limitation.
REFERENCES
[0000]
Aadland E, Fagerhol M K. Faecal calprotectin: a marker of inflammation throughout the intestinal tract. Europ J Gastroenterol Hepatol 2002; 14:1
Ahlquist D A, Gilbert J A. Stool markers for colorectal screening: future considerations. Dig Dis 1996; 14(3):132-44.
Alic M. Is fecal calprotectin the next standard in inflammatory bowel disease activity tests?. [Letter] American Journal of Gastroenterology 1999; 94(11):3370-1.
Arnott I D R, Watts D, Ghosh S. Review article: is clinical remission the optimum therapeutic goal in the treatment of Crohn's disease? Aliment Pharmacol Ther 2002; 16:857.
Arredouani M S, Kasran A, Vanoirbeek J A, Berger F G, Baumann H, Ceuppens J L. 2005. Haptoglobin dampens endotoxin-induced inflammatory effects both in vitro and in vivo. Immunology. 114(2):263-71.
Berger D, Bolke E, Seidelmann M, Beger H G. Time-scale of interleukin-6, myeloid related proteins (MRP), C reactive protein (CRP), and endotoxin plasma levels during the postoperative acute phase reaction. Shock 1997; 7(6):422-6.
Berntzen H B, Endresen G K, Fagerhol M K, Spiechowicz J, Mowinckel P. Calprotectin (the L1 protein) during surgery in patients with rheumatoid arthritis. Scand J Clin Lab Invest 1991; 51(7):643-50.
Berntzen H B, Fagerhol M K, Ostensen M, Mowinckel P, Hoyeraal H M. The L1 protein as a new indicator of inflammatory activity in patients with juvenile rheumatoid arthritis. J Rheumatol 1991; 18(1):133-8.
Berntzen H B, Munthe E, Fagerhol M K. A longitudinal study of the leukocyte protein L1 as an indicator of disease activity in patients with rheumatoid arthritis. J Rheumatol 1989; 16(11):1416-20.
Berntzen H B, Munthe E, Fagerhol M K. The major leukocyte protein L1 as an indicator of inflammatory joint disease. Scand J Rheumatol 1988; Supp 76:251-6.
Berntzen H B, Olmez U, Fagerhol M K, Munthe E. The leukocyte protein L1 in plasma and synovial fluid from patients with rheumatoid arthritis and osteoarthritis. Scand J Rheumatol 1991; 20(2):74-82.
Berstad A, Arsland G, Folvik G. Relationship between intestinal permeability and calprotectin in gut lavage fluid. Scand J Gastroenterol 2000; 35(1):64-9.
Bjarnason I, Sherwood R. Fecal calprotectin: a significant step in the noninvasive assessment of intestinal inflammation. J Pediatr Gastroent Nutr 2001; 33:11.
Bjerke K, Halstensen T S, Jahnsen F, Pulford K, Brandtzaeg P. Distribution of macrophages and granulocytes expressing L1 protein (calprotectin) in human Peyer's patches compared with normal ileal lamina propria and mesenteric lymph nodes. Gut 1993; 34(10):1357-63.
Bogumil T, Rieckmann P, Kubuschok B, Felgenhauer K, Bruck W. Serum levels of macrophage-derived protein MRP-8/14 are elevated in active multiple sclerosis. Neuroscience Letters 1998; 247(2-3):195-7
Bonaldo M F et al., 1996. Normalization and subtraction: Two approaches to facilitate Gene discovery. Genome Res. 6:791-806.
Brandtzaeg P, Dale I, Fagerhol M K. Distribution of a formalin-resistant myelomonocytic antigen (L1) in human tissues. I. Comparison with other leukocyte markers by paired immunofluorescence and immunoenzyme staining. Am J Clin Pathol 1987; 87(6):681-99.
Brandtzaeg P, Dale I, Fagerhol M K. Distribution of a formalin-resistant myelomonocytic antigen (L1) in human tissues. II. Normal and aberrant occurrence in various epithelia. Am J Clin Pathol 1987; 87(6):700-7.
Brandtzaeg P, Dale I, Gabrielsen T O. The leucocyte protein L1 (calprotectin): usefulness as an immunohistochemical marker antigen and putative biological function. Histopathol 1992; 21(2):191-6.
Brun J G, Cuida M, Jacobsen H, Kloster R, Johannesen A C, Hoyeraal H M, Jonsson R. Sjögren's syndrome in inflammatory rheumatic diseases: analysis of the leukocyte protein calprotectin in plasma and saliva. Scand J Rheumatol 1994; 23(3):114-8.
Brun J G, Haga H J, Boe E, Kallay I, Lekven C, Berntzen H B, Fagerhol M K. Calprotectin in patients with rheumatoid arthritis: relation to clinical and laboratory variables of disease activity. J Rheumatol 1992; 19(6):859-62.
Brydon W G, Campbell S S, Anderson N A, Wilson R G, Ghosh S. Faecal calprotectin levels and colorectal neoplasia. Out 2001; 48(4):579-80.
Bunn S K, Bisset W M, Main M J, Golden B E. Fecal calprotectin as a measure of disease activity in childhood inflammatory bowel disease. J Pediatr Gastroenterol Nutr 2001; 32(2):171-7
Bunn S K, Bisset W M, Main M J C, Gray E S, Olson S, Golden B E. Fecal calprotectin: Validation as a noninvasive measure of bowel inflammation in childhood inflammatory bowel disease. J Pediatr Gastroenterol Nutr 2001; 33:11.
Burkhardt K, Radespiel-Troger M, Rupprecht H D, Goppelt-Struebe M, Riess R, Renders L, Hauser I A, and U Kunzendorf 2001. An increase in myeloid-related protein serum levels precedes acute renal allograft rejection. J Am Soc Nephrol 12:1947-57.
Clark B R, Kelly S E, Fleming S. Calgranulin expression and association with the keratinocyte cytoskeleton. J Pathol 1990; 160(1):25-30
Dale I, Brandtzaeg P, Fagerhol M K, Scott H. Distribution of a new myelomonocytic antigen (L1) in human peripheral blood leukocytes. Immunofluorescence and immunoperoxidase staining features in comparison with lysozyme and lactoferrin. Am J Clin Pathol 1985; 84(1):24-34.
Dale I, Brandtzaeg P. Expression of the epithelial L1 antigen as an immunohistochemical marker of squamous cell carcinoma of the lung. Histopathol 1989; 14(5):493-502.
Dale I. Plasma levels of the calcium-binding L1 leukocyte protein: standardization of blood collection and evaluation of reference intervals in healthy controls. Scand J Clin Lab Invest 1990; 50(8):837-41.
Deichmann, M., Polychronidis, M., Wacker, J., Thome, M. & Naher, H., 2001. The protein phosphatase 2A subunit Bg gene is identified to be differentially expressed in malignant melanomas by subtractive suppression hybridization. Melanoma Research 2001(11):1-9.
Dobryszycka W. 1997. Biological functions of haptoglobin—new pieces to an old puzzle. Eur J Clin Chem Clin Biochem 35(9):647-54.
Eversole L R, Miyasaki K T, Christensen RE. Keratinocyte expression of calprotectin in oral inflammatory mucosal diseases. J Oral Pathol Med 1993; 22(7):303-7.
Eversole L R, Miyasaki K T, Christensen RE. The distribution of the antimicrobial protein, calprotectin, in normal oral keratinocytes. Arch Oral Biol 1992; 37(11):963-8.
Fagerhol M K, Andersson K B, Naess-Andresen C F, Brandtzaeg P, Dale I. Calprotectin (The L1 Leukocyte Protein) In: V L Smith & J R Dedman (Eds): Stimulus Response Coupling. The Role of Intracellular Calcium-Binding Proteins, CRC Press, Boca Raton, Fla., USA, 1990, pp. 187-210.
Fagerhol M K. Calprotectin, a faecal marker of organic gastrointestinal abnormality. Lancet 2000; 356(9244):1783-4.
Flum D R et al., 2001. Has misdiagnosis of appendicitis decreased over time? A population-based analysis. JAMA 286 (14):1748-1753.
Fosse E, Moen O, Johnson E, Semb G, Brockmeier V, Mollnes T E, Fagerhol MK, Venge P. Reduced complement and granulocyte activation with heparin-coated cardiopulmonary bypass. Annals of Thoracic Surgery 1994; 58(2):472-7.
Frosch M, Strey A, Vogl T, Wulffraat N M, Kuis W, Sunderkotter C, Harms E, Sorg C, and J Roth 2000. Myeloid-related proteins 8 and 14 are specifically secreted during interaction of phagocytes and activated endothelium and are useful markers for monitoring disease activity in pauciarticular-onset juvenile rheumatoid arthritis. Arthritis Rheum 43:628-37.
Gabrielsen T O, Brandtzaeg P, Hoel P S, Dale I. Epithelial distribution of a myelomonocytic antigen L1 in relation to cutaneous malignancies and melanocytic naevi. Br J Dermatol 1988; 118(1):59-67.
Gabrielsen T O, Dale I, Brandtzaeg P, Hoel P S, Fagerhol M K, Larsen T E, Thune P O. Epidermal and dermal distribution of a myelomonocytic antigen (L1) shared by epithelial cells in various inflammatory skin diseases. J Am Acad Dermatol 1986; 15(2 Pt 1):173-9.
Garred P, Fosse E, Fagerhol M K, Videm V, Mollnes T E. Calprotectin and complement activation during major operations with or without cardiopulmonary bypass. Annals of Thoracic Surgery 1993; 55(3):694-9.
Gasché, C., 2005. Laboratory Tests—What Do They Tell Us?, Falk Symposium Abstract, Jun. 17-18, 2005, Munich, Germany.
Gaya D R, Mackenzie J F. Faecal calprotectin: a bright future for assessing disease activity in Crohn's disease. Q J Med 2002; 95:557 (editorial).
Gilbert J A, Ahlquist D A, Mahoney D W, Zinsmeister A R, Rubin J, Ellefson R D. Fecal marker variability in colorectal cancer: calprotectin versus hemoglobin. Scand J Gastroenterol 1996; 31(10):1001-5.
Golden B E, Clohessy P A, Russell G, Fagerhol M K. Calprotectin as a marker of inflammation in cystic fibrosis. Archives of Disease in Childhood 1996; 74(2):136-9.
Haga H J, Brun J G, Berntzen H B, Cervera R, Khamashta M, Hughes G R. Calprotectin in patients with systemic lupus erythematosus: relation to clinical and laboratory parameters of disease activity. Lupus 1993; 2(1):47-50.
Haidekker M A, et al., 2002. A novel approach to blood plasma viscosity measurement using fluorescent molecular rotors. Am J Physiol Heart Circ Physio 282:H1609-H1614.
Hammer H B, Kvien T K, Glennas A, Melby K. A longitudinal study of calprotectin as an inflammatory marker in patients with reactive arthritis. Clin Exp Rheumatol 1995; 13(1):59-64.
Hanai H, Takeuchi K, lida T, Arai H, Kanaoka K, Iwasaki T, Nakamura A, Hosoda Y, Shirai N, Hirasawa K, Takahira K, Kataoka H, Sano M, Osawa M, Sugimoto S. Clinical significance of faecal calprotectin levels in patients with ulcerative colitis. Nippon Shokakibyo Gakkai Zasshi 2003; 100:21.
Harkness J., 1963. A new method for the measurement of plasma viscosity. Lancet 2:280-281.
Hetland G, Berntzen H B, Fagerhol M K. Levels of calprotectin (leukocyte L1 protein) during apheresis. Scand J Clin Lab Invest 1992; 52(6):479-82.
Homann C, Garred P, Graudal N, Hasselqvist P, Christiansen M, Fagerhol MK, Thomsen AC. Plasma calprotectin: a new prognostic marker of survival in alcohol-induced cirrhosis. Hepatol 1995; 21(4):979-85.
Hsieh H L, Schafer B W, Weigle B, and C W Heizmann 2004 S100 protein translocation in response to extracellular S100 is mediated by receptor for advanced glycation endproducts in human endothelial cells. Biochem Biophys Res Commun 316:949-59.
Hycult Biotechnology b.v., ELISA Test Kit for Human Calprotectin information sheet, Catalog No. HK325.
Hycult Biotechnology b.v., Monoclonal Antibody to Human S100A8/A9 (MRP-8/MRP-14), calprotectin Clone 27E10 information sheet, Catalog No. HM2156.
Ikemoto, M., et al. 2003. New ELISA System for Myeloid-related Protein Complex (MRP8/14) and its Clinical Significance as a Sensitive Marker for Inflammatory Responses Associated with Transplant Rejection, Clin. Chem. 49:594-600.
Johne B, Fagerhol M K, Lyberg T, Prydz H, Brandtzaeg P, Naess-Andresen CF, Dale I. Functional and clinical aspects of the myelomonocyte protein calprotectin. Molecular Pathology 1997; 50(3):113-23.
Johne B, Kronborg O, Ton H I, Kristinsson J, Fuglerud P. A new fecal calprotectin test for colorectal neoplasia. Clinical results and comparison with previous method. Scand J Gastroenterol 2001; 36(3):291-6.
Katnik et al, 1989. Monoclonal Antibodies Against Human Haptoglobin. Hybridoma 8:(5):551-560.
Kelly S E, Hunter J A, Jones D B, Clark B R, Fleming S. Morphological evidence for calcium-dependent association of calgranulin with the epidermal cytoskeleton in inflammatory dermatoses. Br J Dermatol 1991; 124(5):403-9.
Kelly S E, Jones D B, Fleming S. Calgranulin expression in inflammatory dermatoses. J Pathol 1989; 159(1):17-21.
Kerkhoff C, Klempt M, Sorg C. Novel insights into structure and function of MRP8 (S100A8) and MRP14 (S100A9). Biochimica et Biophysica Acta 1998; 1448(2):200-11.
Kjeldsen-Kragh J, Mellbye O J, Haugen M, Mollnes T E, Hammer H B, Sioud M, Forre O. Changes in laboratory variables in rheumatoid arthritis patients during a trial of fasting and one-year vegetarian diet. Scand J Rheumatol 1995; 24(2):85-93.
Koike T, Kondo K, Makita T, Kajiyama K, Yoshida T, Morikawa M. Intracellular localization of migration inhibitory factor-related protein (MRP) and detection of cell surface MRP binding sites on human leukemia cell lines. J Biochem 1998; 123(6):1079-87.
Kristinsson J, Armbruster C H, Ugstad M, Kriwanek S, Nygaard K, Ton H, Fuglerud P. Fecal excretion of calprotectin in colorectal cancer; relationship to tumor characteristics. Scand J Gastroenterol 2001; 36(2):202-7.
Kristinsson J, Roseth A, Fagerhol M K, Aadland E, Schjonsby H, Bormer O P, Raknerud N, Nygaard K. Fecal calprotectin concentration in patients with colorectal carcinoma. Diseases of the Colon & Rectum 1998; 41(3):316-21.
Kronborg O, Ugstad M, Fuglerud P, Johne B, Hardcastle J, Scholefield J H, Vellacott K, Moshakis V, Reynolds J R. Faecal calprotectin levels in a high risk population for colorectal neoplasia. Gut 2000; 46(6):795-800.
Kumar, R. K., et al. 2001. Dimeric S100A8 in human neutrophils is diminished after phagocytosis, J. Leukoc. Biol. 70(1):59-64.
Limburg P J, Ahlquist D A, Sandborn W J, Mahoney D W, Devens M E, Harrington J J and A R Zinsmeister 2000. Fecal calprotectin levels predict colorectal inflammation among patients with chronic diarrhea referred for colonoscopy. Am J Gastroenterol, 10:2831-7.
Limburg P J. Ahlquist D A. Sandborn W J. Mahoney D W. Devens M E. Harrington J J. Zinsmeister A R. Fecal calprotectin levels predict colorectal inflammation among patients with chronic diarrhea referred for colonoscopy. American Journal of Gastroenterology 2000; 95(10):2831-7.
Longbottom D, Sallenave J M, van Heyningen V. Subunit structure of calgranulins A and B obtained from sputum, plasma, granulocytes and cultured epithelial cells. Biochimica et Biophysica Acta 1992; 1120(2):215-22.
Lugering N, Stoll R, Schmid K W, Kucharzik T, Stein H, Burmeister G, Sorg C, Domschke W. The myeloic related protein MRP8/14 (27E10 antigen)-usefulness as a potential marker for disease activity in ulcerative colitis and putative biological function. Europ J Clin Invest 1995; 25(9):659-64.
Meling T R. Aabakken L. Roseth A. Osnes M. Faecal calprotectin shedding after short-term treatment with non-steroidal anti-inflammatory drugs. Scandinavian Journal of Gastroenterology 1996; 31(4):339-44.
Moen O, Fosse E, Braten J, Andersson C, Fagerhol M K, Venge P, Hogasen K, Mollnes T E. Roller and centrifugal pumps compared in vitro with regard to haemolysis, granulocyte and complement activation. Perfusion 1994; 9(2):109-17.
Muller F, Froland S S, Aukrust P, Fagerhol M K. Elevated serum calprotectin levels in HIV-infected patients: the calprotectin response during ZDV treatment is associated with clinical events. J Acq Immune Defic Syndr 1994; 7(9):931-9.
Muller, F., et al. 1994. Elevated serum calprotectin levels in HIV-infected patients: the calprotectin response during ZDV treatment is associated with clinical events, J. Acqui. Immune Defic. Syndr. 7(9):931-939.
Neary, Walter, 2001. Press Release from University of Washington, Misdiagnosis of appendicitis continues despite new tools.
Olafsdottir E, Aksnes L, Fluge G, Berstad A. Faecal calprotectin in infants with infantile colic, healthy infants, children with inflammatory bowel disease, children with recurrent abdominal pain and healthy children. Acta Paediatr 2002; 91:45.
Pekna M, Borowiec J, Fagerhol M K, Venge P, Thelin S. Biocompatibility of heparin-coated circuits used in cardiopulmonary bypass. Scand J Thorac Cardiovasc Surg 1994; 28(1):5-11.
Power, C. et al, 2005. Raised faecal calprotectin levels in patients presenting with right iliac fossa pain warrant mandatory laparoscopy: a non-invasive predictor of acute appendicitis, Thieme connect, Endoscopy 37:D01:10.1055/2-2005-868524.
Power, C., et al. 2004, Irish Society of Gastroenterology Winter Meeting Program Oral Presentation Raised Faecal Calprotectin Levels in Patients Presenting with Right Iliac Fossa Pain Warrant Mandatory Laparoscopy: A Non-invasive Predictor of Acute Appendicitis.
Robinson M J, Tessier P, Poulsom R, and N. Hogg 2002 The S100 family heterodimer, MRP-8/14, binds with high affinity to heparin and heparan sulfate glycosaminoglycans on endothelial cells. J Biol Chem. 277:3658-65.
Roseth A G, Aadland E, Grzyb K. Normalization of faecal calprotectin: a predictor of mucosal healing in patients with inflammatory bowel disease. Scand J. Gastroenterol. 2004 October; 39(10):1017-20.
Roseth A G, Fagerhol M K, Aadland E, Schjonsby H. Assessment of the neutrophil dominating protein calprotectin in feces. A methodologic study. Scand J Gastroenterol 1992; 27(9):793-8.
[0187] Roseth A G, Kristinsson J, Fagerhol M K, Schjonsby H, Aadland E, Nygaard K, Roald B. Faecal calprotectin: a novel test for the diagnosis of colorectal cancer? Scand J Gastroenterol 1993; 28(12):1073-6.
[0188] Roseth AG. Aadland E. Jahnsen J. Raknerud N. Assessment of disease activity in ulcerative colitis by faecal calprotectin, a novel granulocyte marker protein. Digestion 1997; 58(2):176-80.
[0189] Roseth AG. Fagerhol M K. Aadland E. Schjonsby H. Assessment of the neutrophil dominating protein calprotectin in feces. A methodologic study. Scandinavian Journal of Gastroenterology 1992; 27(9):793-8.
Roseth A G. Schmidt P N. Fagerhol M K. Correlation between faecal excretion of indium-11′-labelled granulocytes and calprotectin, a granulocyte marker protein, in patients with inflammatory bowel disease. Scandinavian Journal of Gastroenterology 1999; 34(1):50-4. Ryckman C, Vandal K, Rouleau P, Talbot M, and P A Tessier 2003 Proinflammatory activities of S100: proteins S100A8, S100A9, and S100A8/A9 induce neutrophil chemotaxis and adhesion. J. Immunol. 170:3233-42. Saintigny G, Schmidt R, Shroot B, Juhlin L, Reichert U, Michel S. Differential expression of calgranulin A and B in various epithelial cell lines and reconstructed epidermis. J Invest Dermatol 1992; 99(5):639-44. Sander J, Fagerhol M K, Bakken J S, Dale I. Plasma levels of the leucocyte L1 protein in febrile conditions: relation to aetiology, number of leucocytes in blood, blood sedimentation reaction and C-reactive protein. Scand J Clin Lab Invest 1984; 44(4):357-62. Semb A G, Gabrielsen T O, Halstensen T S, Fagerhol M K, Brandtzaeg P, Vaage J. Cardiac surgery and distribution of the leukocyte L1 protein-calprotectin. Europ J Cardio-Thoracic Surgery 1991; 5(7):363-7. Shanahan F. Inflammatory bowel disease: immunodiagnostics, immunotherapeutics, and ecotherapeutics. Gastroenterol 2001; 120:622. Stockley R A, Dale I, Hill S L, Fagerhol M K. Relationship of neutrophil cytoplasmic protein (L1) to acute and chronic lung disease. Scand J Clin Lab Invest 1984; 44(7):629-34. Striz, I. and I. Trebichaysky 2004. Calprotectin a Pleiotropic Molecule in Acute and Chronic Inflammation. Physiol Res. 53:245-253. Thomas P. Rihani H. Roseth A. Sigthorsson G. Price A. Nicholls R J. Bjarnason I. Assessment of ileal pouch inflammation by single-stool calprotectin assay. Diseases of the Colon & Rectum 2000; 43(2):214-20. Tibble J, Sigthorsson G, Foster R, Fagerhol M K, Bjarnason I. Faecal calprotectin and faecal occult blood tests in the diagnosis of colorectal carcinoma and adenoma. Gut 2001; 49:402. Tibble J. Teahon K. Thjodleifsson B. Roseth A. Sigthorsson G. Bridger S. Foster R. Sherwood R. Fagerhol M. Bjarnason I. A simple method for assessing intestinal inflammation in Crohn's disease. Gut 2000; 47(4):506-13. Tibble J A, Bjarnason I. Department of Medicine, Guy's, King's, St Thomas's Medical School, Bessemer Road, London SE5 9PJ, UK. Non-invasive investigation of flammatory bowel disease. Tibble J A, Bjarnason I. Department of Medicine, Guy's, King's, St. Thomas's Medical School, London, UK. Fecalcalprotectin as an index of intestinal inflammation. Tibble J A, Bjarnason I. Markers of intestinal inflammation and predictors of clinical relapse in patients with quiescent IBD. Medscape Gastroenterol 2001; 3 (2). Tibble J A. Sigthorsson G. Bridger S. Fagerhol M K. Bjarnason I. Surrogate markers of intestinal inflammation are predictive of relapse in patients with inflammatory bowel disease. [Journal Article] Gastroenterology 2000; 119(1):15-22. Tibble J A. Sigthorsson G. Foster R. Scott D. Fagerhol M K. Roseth A. Bjarnason I. High prevalence of NSAID enteropathy as shown by a simple faecal test. Gut 1999; 45(3):362-6. Ton H. Brandsnes. Dale S. Holtlund J. Skuibina E. Schjonsby H. Johne B. Improved assay for fecal calprotectin. Clinica Chimica Acta 2000; 292(1-2):41-54. Tungekar M F, Heryet A, Gatter K C. The L1 antigen and squamous metaplasia in the bladder. Histopathol 1991; 19(3):245-50. U.S. Pat. No. 5,350,687, Odink, et al., Sep. 27, 1994, Antibodies which bind to novel lymphokine related peptides. U.S. Pat. No. 5,455,160, Fagerhol, et al., Diagnostic test and kit for disease disorders in the digestive system. U.S. Pat. No. 5,552,295, Stanker, et al., Sep. 3, 1996, Monoclonal antibodies to bovine haptoglobin and methods for detecting serum haptoglobin levels. U.S. Pat. No. 6,451,550, Eckersall, Sep. 17, 2002, Haptoglobin assay. U.S. Patent Publication No. 20030224452, Colgin, et al., Pregnancy Detection. Wilkinson M M, Busuttil A, Hayward C, Brock D J, Dorin J R, Van Heyningen V. Expression pattern of two related cystic fibrosis-associated calcium-binding proteins in normal and abnormal tissues. J Cell Science 1988; 91 (Pt 2):221-30. Ye B, Cramer D W, Skates S J, Gygi S P, Pratomo V, Fu L, Horick N K, Licklider L J, Schorge J O, Berkowitz R S, Mok S C. 2003 Haptoglobin-alpha subunit as potential serum biomarker in ovarian cancer: identification and characterization using proteomic profiling and mass spectrometry. Clin Cancer Res 9(8):2904-11. Yerly S, Bouvier M, Rougemont A, Srivastava I, Perrin L H. 1990. Development of a haptoglobin ELISA. Its use as an indicator for malaria. Acta Trop. 1990 47(4):237-44. | A method is provided for diagnosing appendicitis in a patient that includes identifying at least one symptom of appendicitis in the patient and identifying the presence of at least one molecule differentially associated with appendicitis in a fluid or tissue sample of said patient. MRP-8/14 and haptoglobin are examples of molecules differentially associated with appendicitis. Devices and kits for performing the appendicitis assays of this invention are also provided. In one embodiment, the device is in a flow-through immunoassay format for testing blood samples. Further, methods for screening for molecules differentially associated with appendicitis are provided that include the use of samples from patients being operated on for suspected appendicitis. | 8 |
CROSS REFERENCE TO RELATED APPLICATION
This is a Continuation-In-Part of co-pending U.S. application Ser. No. 429,360, now abandoned filed Dec. 28, 1973.
FIELD OF THE INVENTION
This invention relates to an offset printing machine, and more particularly to a control mechanism for offset printing machines, the control mechanism being operative in a combination of an automatic mode and manual mode so as to efficiently and easily operate the printing machines.
BACKGROUND OF THE INVENTION
In conventional offset printing machine, which require several fundamental steps such as inking, dampening, paper feeding, printing, and blanket cleaning, various inventions and modifications have been made regarding mechanisms for controlling the aforementioned steps. Existing mechanisms before the present invention for controlling offset printing machines, especially in small offset printing machines suitable for business office work, are mechanically too complicated and at the same time, are cumbersome from an operator's standpoint. For example, in the mechanism shown in the U.S. Pat. No. 3,601,045, the blanket cleaning position of the control shaft is located between the original neutral position and the printing position. If there were no second neutral position, in case of any printing trouble such as paper jam, the control shaft had to be quickly shifted to the original neutral position through the blanket cleaning position, which means that the blanket surface would momentarily touch the blanket cleaning roller resulting unintentional inking on the surface of a master plate on resumption of printing. Accordingly, a second neutral position is provided before the blanket cleaning position so that in case of any printing trouble such as paper jam, the control shaft can be quickly shifted to the second neutral position without the blanket surface touching the blanket cleaning roller. Because of the existence of the second neutral position, the mechanism becomes inevitably complicated. Another example of a recent invention of control mechanism can be seen in the U.S. Pat. No. 3,731,367 and 3,731,624. In this mechanism, the blanket cleaning position of the control shaft is located beyond the original neutral position looking from the printing position of the control shaft. Because of the use of an operation lever that can not rotate 360 degree, it would be almost impossible to convert the mechanism so as to automatically clean the blanket after a pre-set number of sheets are printed.
The present invention provides a simplified control mechanism for easier operation.
OBJECTS OF THE INVENTION
A primary object of this invention is, therefore, to provide a control mechanism for an offset printing machine adapted to be easily operated and controlled by an operator.
A second object of this invention is to provide a control mechanism for an offset printing machine, by which handling of the machine in case of any printing trouble becomes easy and test printing also becomes easy through a combination of automatic mode and manual mode.
A third object of this invention is to provide a control mechanism for an offset printing machine in which the total printing process is governed by a single control shaft, the control shaft being rotatable 360 degree to finalize the total printing process via blanket cleaning process.
A fourth object of the invention is to provide a control shaft of an offset printing machine together with a knob of rotary type, which is simple in construction and accordingly maintenance-free.
A fifth object of this invention is to provide a control mechanism for an offset printing machine in which an automatic mode of operation and a manual mode of operation of the machine are well defined by stop means so that the manual mode of operation never disturbs any process progressing under the automatic mode of operation.
These and other objects and advantages of this invention will become apparent through a review of the attached drawings and a further reading of the specification and the claims.
SUMMARY OF THE INVENTION
The objects of this invention are achieved by providing a control mechanism of an offset printing machine in which continual steps (such as starting the machine, supplying dampening solution and ink to rollers, transferring of dampening solution and ink onto a master plate on a master cylinder, transferring ink onto a blanket on a blanket cylinder, feeding sheets and transferring ink onto sheets, completing of printing, blanket cleaning, and stopping the machine are easily controlled. Of the continual steps, the steps leading to actual transfer of ink onto sheets are manually performed, and the steps thereafter are automatically performed through the control shaft. A stop means installed in the printing machine precludes any erroneous manual operation.
BRIEF DESCRIPTION OF THE DRAWING
In the drawings:
FIG. 1 shows an overall cross-sectional view of the arrangement of the cylinders and rollers of the offset printing machine and associated elements;
FIG. 2 is a side view showing various members of the control mechanism for the offset printing machine when the machine is stopped;
FIG. 3 is a front view of a knob to rotate a control shaft and indications of positions of the control shaft;
FIG. 4A is a sectional side view showing a microswitch and a switch block to stop the machine;
FIG. 4B is a front view showing the relation of a stopper bracket and a stop pin;
FIG. 5 is a view of FIG. 2 showing the various members when the knob is situated at the position I of the control shaft, which is for supply dampening solution and ink onto the rollers;
FIG. 6 shows various members of FIG. 2 with the knob situated at the position II, which is for transfer of ink onto a master plate on a master cylinder;
FIG. 7 shows various members of FIG. 2 with the knob at the position III of printing;
FIG. 8 shows various members of FIG. 2 at the completion of printing;
FIG. 9 shows the position of various members of FIG. 2 when the knob is situated at the position B for blanket cleaning;
FIG. 10 is a side elevational view showing particularly the blanket cleaning apparatus and the set of cylinders;
FIG. 11 is a partial front view of FIG. 4A showing an operational relation between the switch block and the microswitch;
FIG. 12 is a side view showing an operational relationship of the control shaft with dampening and inking mechanism, and
FIG. 13 is an enlarged view showing the ratchet and the star-like cam mounted on the control shaft.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawing in detail, and initially to FIG. 1, shown is the whole construction of the offset printing machine. The reference numeral 1 shows a frame of the printing machine, in which are operatively arranged a master cylinder 2, a blanket cylinder 3, an impression cylinder 4, an ink and dampening solution applying apparatus 5, an ink fountain 6, a dampening solution fountain 7, a blanket cleaning apparatus 8 and a tank of cleaning solution 9. A sheet of paper 14 to be printed is supplied to feeding rollers 11 and is passed between the blanket cylinder 3 and the impression cylinder 4, and then is passed between eject rollers 12. Finally, the printed sheet is placed on the receiving tray 13. The master cylinder 2 and the impression cylinder 4 respectively are supported by eccentric shafts so as to make contact with the blanket cylinder 3 as they rotate.
The drawings of FIGS. 2-11 show whole construction of the control mechanism for the offset printing machine according to the present invention. As shown in FIGS. 3, 4A and 4B, a stop pin 14 on the control knob 17 extends from a bracket 16 in which a coil spring 15 is mounted and the bracket 16 is loose-fitted to the knob 17. The knob is fixed to a control shaft 18 adapted to rotate together with the stop pin 14 from the start position 0 counterclockwise as viewed in FIG. 3. The stop pin 14 is adapted to abut on the side 21 of a stop bracket 20 having a lower end 19 shaped in an arc. In this position of the stop pin 14, the knob 17 is restrained from rotating clockwise. As shown in FIG. 11, the microswitch 24 contacts a switch block 22 secured to the cam 23. The cam 23 is mounted on the control shaft 18 to rotate together with the shaft 18. The microswitch 24 operates to stop the printing machine.
The control shaft 18 has a ratchet 27 and a cam 29 at the opposite end of it, and the ratchet 27 and cam 29 are integrally secured to the opposite end so as to rotate together with the control shaft 18. As clearly shown in FIG. 13, the ratchet 27 has multiple stepped portion 25 formed around its circumference at regular distances with 45° angle to the diametral lines and also a stop pin 26 planted on its side face. The cam 29 has a multiple number of indented portions 28 formed around its circumference at distances of 45° or 60° angles to the diametral lines. The indented portions 28 engage with a roller 36 so as to correspond to the positions of the control shaft 18. The ratchet 27 and the cam 29 constitute a rotary mechanism for the control shaft 18. In relation to the rotary mechanism, a set of stoppers 30 and 31 are pivotally mounted on the machine frame 1. The stopper 30 has a bent portion 32 so that it engages with the stop pin 26 when the control shaft is set at the position III. The stopper 30 is ordinarily urged in the direction along which the engagement with the stop pin 26 is disengaged by means of a spring 33. The stopper 31 has a spring 34, so that the stopper oscillates outwardly by pressing a slanted end portion 31a of the stopper 31 by means of the stop pin 26 when the knob 17 rotates from the position III to the position B in order to move the stop pin 26 from the position of FIG. 8 to that of FIG. 9. After the stop pin 26 passes over the slanted end portion 31a, the stopper 31 returns to its original position. The microswitch 35 is functioned as shown in FIG. 9 when the stopper 31 is pressed outwardly by means of the pin 26.
An arm 37 has the roller 36 pivoted to its end and a spring 38 mounted thereon. The spring urges resiliently the arm 37 along the direction in which the roller 36 engages with the indented portions 28 of the star-shaped stop cam 29. The arm 37 holds the control shaft 18 at any suitable position.
A link 39 has slotted openings 40 within which guide pins 41 are slidingly fitted so as to allow the link 39 to move up and down. The link 39 has a stop pin 42 planted thereon at its upper end and claw 43 at its side. The claw 43 is pivoted so as to engage with the stepped portion 25 of the ratchet 27. Also, the link 39 has an engagement portion 44 extending from a side of the central portion of the link, and a roller 45 at its lower end. A L-shaped arm 46 pivoted to the frame has an end portion extended so as to engage with the roller 45 provided on the link 39. The L-shaped arm 46 and the link 39 respectively have pins 48 and 47, so that the arm 46 and the link 39 are pulled toward each other by means of a spring 49 hooked on the pins 48, 47. The arm 46 is connected to an end portion of a cam arm 50 at its another end portion through a link 51 having 59 planted thereon. The cam arm 50 has a roller 52 on another end portion thereof and constantly urged to ride on a cam 53 by means of a spring 54 expandingly mounted on the cam arm 50. The cam 53 connected to a shaft of a prime mover such as an electric motor has a high point thereon and is rotated by a prime mover or a motor of the printing machine through a gears reducer. The arm 46 oscillates when the cam 53 is rotated.
A clutch 55 has an engagement portion on its upper side and is pivoted to the frame 1. The clutch 55 has a spring 56 so that the clutch resiliently engages with the engagement portion 44 of the link 39. The clutch 55 is connected to a plunger of solenoid 57 through a link 58, so that the solenoid 57 pulls the clutch 55 through the link 58 when the solenoid is energized and disengages the clutch 55 from the engagement portion 44.
A ratchet 60 pivoted to the machine frame 1 by means of a shaft 61 has a spring 67 urging the ratchet to rotate clockwise. The ratchet 60 is generally held at the position shown in FIG. 2, in which the ratchet contacts the stop pin 63. A switch plate 64 is secured to the ratchet 60 by screws screwed through an elongated opening so as to be placed at an operative relation to the ratchet 60. When the ratchet 60 rotates counterclockwise against force of a spring 67, the switch plate 64 contacts a microswitch 65 and operates the microswitch 65. An arm 68 is pivoted to the frame 1. A spring 69 is mounted to the arm 68 so as to urge its end portion to engage with the pin 59 of the link 51. A claw 72 for moving the ratchet 60 is provided at one end of the arm 68 through a pin 71. A claw 70 is pivoted to the stud 67 for preventing reverse rotation of the ratchet. The claws 70 and 72 respectively have springs 73 and 74 so that the claws engage with the toothed portion 66 of the ratchet 60.
As shown in FIG. 10, an arm 75 for cleaning the blanket is pivoted to the frame 1 and has three branches extending along three directions.
On a first branch of them, a link 77 having a pin 76 planted at its lower end is connected so that the link 77 may shift up and down according to the rocking movement of the arm 75. A short arm 78 pivoted to the frame 1 supports the middle portion of the link 77 for securing vertical movement of the link. An arm 79 has an end portion pivoted at the frame 1 and another end portion having a pin 80 planted thereon. At all positions of the control shaft 18, except for the position corresponding to the blanket cleaning, the arm 79 touches the pin 76, and is pressed downward. Accordingly, the claw 72 is pressed downward against force of the spring 74 and the claw 70 is also pressed downward through a head of claw 72. As a result, the claws 70, 72 are kept disengaged from the toothed portion 66 of the ratchet 60. A second branch of the arm 75 has a roller 81, and the roller 81 constantly contacts a cam 82 having a high point and secured to the control shaft 18. A third branch of the arm 75 is connected to the blanket cleaning apparatus 8 through a link 83.
As shown in FIG. 10, in the blanket cleaning apparatus 8, an arm 85 is secured through its end portion to an eccentric shafts 84 mounted on the frame 1, and another end portion of the arm 85 is connected to the link 83. An end portion of the arm 86 is loosely fitted to the eccentric shaft 84. The another end of the arm 86 is connected to the securing plate 87. A tank 88 of cleaning solution 9, having cleaning rollers is mounted on the securing plate 87. The securing plate 87 is pivoted on a stud 90. As the roller 81 of the arm 75 for blanket cleaning is placed on the land of cam 82, the arm 75 shifts clockwise in order to rotate the securing plate 87 around the stud 90 toward the blanket cylinder 3 through the link 83, the arm 85, the eccentric shaft 84 and the arm 86. Thus, the roller 89 is pressed to the blanket on the blanket cylinder 3.
The mechanism for contacting and detaching the master cylinder to the blanket cylinder is shown in FIG. 2. An arm 91 pivoted on the frame 1 is constantly contacted to a cam (not shown) which has a high point and secured to the control shaft 18, by means of a spring (unnumbered). Another end portion of the arm 91 is connected to an arm 94 by a link 95. When the knob 17 is placed at the position III, the arm 91 oscillates by the unshown cam and subsequently the eccentric shaft 93 is rotated by a link 95 and an arm 94 to contact the master cylinder to the blanket cylinder.
The inking and dampening apparatus, as shown in FIG. 12, has a cam 96 and a cam 97. The cams 96 and 97 are fixed on the control shaft 18. The cam 96 has a indented portion on its periphery and the cam 97 has two indented portions along its periphery. A water ductor roller 100 and ink ductor roller 106 are connected to the cam 96 through an arm 98 and a link 99. A form roller 105 is connected to the cam 97 through an arm 101, a link 102 and an arm 103. With the knob 17 at the position 0, the ink ductor roller 106 and the water ductor roller 100 stop to duct and the form roller 105 is separated from the oscillating roller 104. With the control shaft 18 at the position 1, the ink ductor roller 106 and the water ductor roller 100 begin to duct, and the form roller 105 is pressed to the oscillating roller 104, thus dampening solution and ink are supplied to the form roller 105. With the control shaft 18 at the position 11, the form roller is pressingly contacted to the master cylinder 2 in order to supply water and ink to the cylinder.
As the master cylinder 2 makes contact with the blanket cylinder 3, the sheet feeding operation is started and simultaneously a conventional sheet detecting device operates. Then, a conventional impression cylinder functioning mechanism operates to bring the impression cylinder into its printing position. A sheet counter (not shown) is provided in the printing machine, on which a desired number is to be set prior to printing. The sheet counter starts its counting operation as another first sheet is fed. The sheet counter has a microswitch (not shown) electrically connected to the solenoid 57. The solenoid 57 is also connected to the microswitches 35, 65 through an electric circuit.
The printing operation of the printing machine at various positions of the knob 17 will be explained as follows:
With the knob 17 at the position O, the master cylinder 2 and the impression cylinder 4 are respectively separated from the blanket cylinder 3, and the control mechanism for the printing machine is placed as shown in FIG. 2. In this position, the stop pin 26 is located at the bottom. Any operation of the main switch (not shown) by an operator does not start the printing machine unless the sheet counter indicates some non-zero number.
In order to start an operation of the printing machine, the knob 17 is turned from the position O to the position I, resulting in contact of the ink ductor roller 106 and the water ductor roller 100 in FIG. 12 with the oscillating roller 104, and in contact of the roller 104 with the form roller 105 by means of the cams 96, 97 of the control shaft 18. Therefore, ink and dampening solution are supplied to the form roller 105.
When the knob 17 is turned from the position I to position II, the form roller 105 is contacted with the surface of the master cylinder 2 through the arm 101 and the link 102 respectively functioned by two indented portions of the cam 97 in order to supply dampening solution and ink onto the master cylinder. Next, the knob 17 is rotated to the position III, then a locking arm (unnumbered) is rotated by the rotation by cylinder 2, and the arm 91 is oscillated from the position shown in FIG. 2 toward the right by an extended portion of the master cylinder engagement cam 92 (not shown) secured to the control shaft 18, the arm 94 oscillates through the link 95 in order to rotate the eccentric shaft 93 and to make the master cylinder 2 contact the blanket cylinder 3.
The stop pin 26 extending from the ratchet 27 is located at the positions shown in FIGS. 5, 6 and respectively as the knob 17 is rotated to the positions I, II and III. When the knob 17 is placed at the positions O, I, II, and III, the solenoid 57 is de-energized and the clutch 55 is pulled by a spring 56 so as to engage with the engagement portion 44. As a result, the link 39 is kept at its elevated position and the stopper 30 is kept at its horizontal position by a pin 42. At this time the arm 75 is kept in contacting condition with an indented portion of the cam 82 secured to the control shaft 18, so that the link 77 is located at its descended position to press down the arm 79. Then, the ratchet feeding claw 72 and the stopping claw 70 are placed at their pressed-down positions and are separated from the toothed portion 66 of the ratchet 60.
With the knob at the position III, the stop pin 26 engages with the stopper 30 as shown in FIG. 7, and accordingly the control shaft 18 is prevented (from rotating clockwise from the position III to position B). When the knob 17 is rotated to the position III, the sheet feeding apparatus II is functioned to start sheet feeding operation and the impression cylinder 4 contacts with the blanket cylinder 3 by operation of the aforementioned impression cylinder engagement mechanism. The machine starts to print and the sheet counter begins to count at the position III. During the printing process, the cam 53 is kept rotating and the arm 46 oscillates through a cam arm 50 and a link 51, and therefore the end portion of the arm 46 oscillates up and down without any influence of the roller 45 of the link 39.
Test printing of the offset printing machine is manually carried out by rotating the knob 17 from its position O to position III. In case of a printing trouble such as paper jam at the position III of printing condition of the machine, the knob 17 is manually rotated reversely from the position III to the position O through the positions II, I. At the position O, the main switch is turned off in order to rectify the printing machine.
When the printing operation is completed without any trouble, the sheet counter (not shown) shows 0. Then, a microswitch operatively connected to the sheet counter is actuated and the solenoid electrically connected to the microswitch is energized, so that the clutch 55 is pulled to the right against force of the spring 56 as shown in FIG. 8. As a result, the link 39 is disengaged from the clutch 55, and the link 39 descends slowly, guiding the pins 41 sliding through the long opening 40 by force of a spring 49 extended between a pin 48 provided at an end of the arm 46 and a pin 47 provided on the link 39. The link 39 descends together with a stop pin 42 and the claw 43 so as to disengage the stopper 30 of the pin 26 and oscillate the stopper 30 by force of a spring 33, thus the stop pin 26 is brought to a disengaged condition.
The link 39 is raised by a roller 45 when the end portion of the arm 46 oscillating through the cam 53 contacts the roller 45. The pawl 43 is raised together with the link 39 and then the claw 43 engages with the stepped portion of the ratchet 27 in order to rotate the ratchet 27 moving the pin 26 to the right. Because the ratchet 27 is rotated before the pin 42 and the stopper 30 are engaged, the stopper 30 does not engage with the pin 26.
When the ratchet 27 rotates clockwise by repeated up-and-down motion of the link 39, the pin 26 on the ratchet 27 moves a suitable angle at a time and the control shaft 18 moves from the position III to position B and finally the pin 26 abuts on a slanted surface 31a of the stopper 31. Then, the stopper 31 escapes outward when the stopper 31 is pressed by the stop pin 26, thus the pin 26 can move to the position B as shown in FIG. 9. At this time, the stopper 31 abuts on the microswitch 35 in order to operate the microswitch 35 and de-energize the solenoid 57 electrically connected to the microswitch 35. The clutch 55 is pulled by means of a spring 56 in order to lock the engagement portion 44 and to keep the link 39 at its raised position. Simultaneously, the arm 75 oscillates to the right in FIG. 10 by the extended portion of the cam 82 fixed on the control shaft 18 in order to raise the link 77. Then, the arm 79 becomes free of a pin 76 to release the claws 70, 72 from their down-pressed condition by the pin 80 of the arm 79, thus the claws 70, 72 engage with the toothed portion 66 of the ratchet 60 by force of springs 73, 74. In this engagement condition, the cam 53 is continued in its rotary motion and the claw moving arm 68 is engaged with the pin 59 of the link 51 so as to oscillate around the stud 67. The claw 72 feeds one tooth at a time of the ratchet in order to rotate the ratchet counterclockwise. Then, the claw 70 for preventing reverse rotation of ratchet follows the rotation of the ratchet 60 against the resilient force of the spring 73 and engages with one tooth at a time of the toothed portion 66 in order to prevent the ratchet from reverse rotating. Owing to the afore-described oscillating motion of the arm 75, the roller 89 of the blanket cleaning apparatus 8 connected to the eccentric shaft 84 is impressed through a link 83 to the blanket cylinder 3. While the claw 72 engages with the toothed portion 66 of the ratchet 60, the blanket is cleaned and the cleaning operation is continued. As the ratchet 60 is rotated by the claw 72, the switch plate 64 is moved together with the ratchet plate 60 and abuts against the microswitch 65 in order to close it. Accordingly, the solenoid 57 is energized to pull the clutch 55 in order to release the link 39. Thus, the link 39 starts its up and down motion in order to rotate the ratchet 27 and rotate the knob 17 to its neutral position O. At this time, the pin 26 returns to the original position shown in FIG. 2. Also the cam 92 and arm 75 return to their original position, by which the roller 89 of the blanket cleaning apparatus is separated from the blanket cylinder 3. Then, the link 77 descends to press down the arm 79, thus disengaging the claws 70, 72 from the toothed portion of the ratchet 60. The ratchet 60 rotates clockwise by force of the spring 67 and abuts against the stopper pin 63 and is stopped at the position O of the knob 17 as shown in FIG. 2. When the knob 17 is returned to the position O, the microswitch 24 shown in FIG. 4A is abutted against the switch plate 22 and the microswitch is closed, and accordingly the solenoid 57 is de-energized. Then the clutch 55 engages with the engagement portion 44 and stops the up and down motion of the link 39. At the same time, the main switch of the printing machine is turned off and all functions of the machine are stopped.
In order to adjust the time duration of the blanket cleaning operation, the location of the switch plate 64 on the ratchet 60 can be shifted through its slotted hole.
The operational relationship of the ratchet 60, the microswitches 24, 35 and 65, the microswitch incorporated in the sheet counter and the solenoid 57 will be explained as follows:
When the sheet counter shows O and the microswitch connected to the counter is operated, the solenoid 57 is energized and the clutch 55 is separated from the engagement portion 44 of the link 39 so as to move the link 39 up and down by the cam 53, resulting in the stepped portion 25 of the ratchet 27 fixed to the control shaft 18 being fed twice 45° at a time. When the ratchet 27 is fed at the third time, the pin 26 provided on the ratchet 27 releases the stopper 31 and makes contact with the microswitch 35 installed at the side of the stopper 31. As a result, the solenoid 57 is de-energized and the clutch 55 engages with the engagement portion 44 of the link 39, so that the up and down motion of the link 39 is stopped and the feeding motion of the ratchet cause by the claw 43 is stopped, the extruded portion of the cam 82 fixed on the control shaft 18 oscillates the arm 75 in order to raise the link 77.
Then, the claws 72 and 70 are released from their down pressed condition by means of a pin 80 provided on an end portion of the claw releasing arm 79, and the claws 70, 72 are engaged with the ratchet 60 by means of the springs 73, 74. The ratchet 60 is fed by the feeding claw 72 which is mounted at the end portion of the arm 68 oscillating by the pin 59 provided at the link 51 and the ratchet 60 is prevented from reverse rotation by the stop claw 70.
When the switch 64 provided on the ratchet 60 operates the microswitch 65, the solenoid 57 is energized and the link 39 is released to descend. When the link 39 raises, the ratchet 27 is rotated an angle of 45°. Thus, the knob 17 is backed to the position O and the solenoid 57 is de-energized by the microswitch 24.
The arc portion 19 of the stopper bracket 20 does not prevent the stop pin 14 of the knob 17 from relating from the position B to position O but prevent the stop pin from rotating along the reverse direction. When the bracket 16 is pressed down to descend the stop pin 14, it is disengaged from the side end 21 of the stopper bracket 20. Thus, it is possible to manually rotate the knob 17 from the position O to position B clockwise to clean the blanket. The return movement of the knob 17 from the position B to position O counterclockwise is easily carried out manually as well as automatically, because the arc portion 19 of the bracket 20 guides the stopper pin 14 and it is not necessary to push down the bracket 16.
It should be understood, of course, that the foregoing disclosure relates only to a preferred embodiment of the invention, and that it is intended to cover all changes and modifications of the example of the invention herein chosen for the purpose of the disclosure which do not constitute departures from the spirit and scope of the invention set forth in the appended claims. | A control mechanism for an offset printing machine in which total printing operation is efficiently and easily carried out through a single control shaft with a knob.
The control mechanism is operative in a combination of an automatic mode and a manual mode to utilize advantages of both modes. The control shaft is rotatively constructed in such a way that its neutral position, its position for supply of ink and dampening solution to rollers, its position for transfer of ink and dampening solution to a master cylinder, its position for paper feeding and printing, its position for blanket cleaning, and its position for stopping the machine make one complete cyclic loop. The control shaft is manually rotated stepwise from its neutral position to its position for paper feeding and printing. After a pre-set number of sheets are printed, the control shaft is automatically rotated to its position for blanket cleaning and then to its position for stopping the machine. | 1 |
BACKGROUND OF THE INVENTION
The invention relates to a bale collector comprising a frame provided with wheels, bale-carrying means, coupling means which are suitable for coupling the frame to a mobile baler in order to receive bales onto the carrying means from a bale outlet of the baler by way of a front end, viewed in the direction of travel of the carrying means, and also control means for taking the carrying means into a collecting state or into an unloading state, for collecting bales on the carrying means or unloading bales from the carrying and depositing them on the ground, the carrying means rollers with parallel horizontal axes, and the rollers being suitable for collecting a row of two or more bales thereon between the front end and a rear end of the carrying means.
A bale collector of this type is known from U.S. Pat. No. 3,010,593. The bale collector known from this document has a relatively high loading platform on which it receives bales from a baler. The bales received fall from the platform onto a conveyor at a lower level. The conveyor comprises two endless conveyor belts next to each other and at the same height, extending at right angles to the direction of travel of the collector and driven stepwise at right angles to the direction of travel, in order to form a row of bales on the belts. After a row of bales has been formed on the conveyor belts, the row is pushed by means of a bar in the opposite direction to the direction of travel onto bale-carrying means with a relatively large surface. The bale-carrying means comprise horizontal rollers, the axes of which extend at right angles to the direction of travel. The rollers are driven stepwise during loading of the bale-carrying means with rows of bales, in such a way that the rows are moved over the rollers in the opposite direction to the direction of travel. As soon as the entire receiving surface of the bale-carrying means and of the conveyor is filled with rows of bales, an unloading mechanism is put into operation, following which all collected bales are deposited on the ground.
A bale collector according to the preamble of claim 1 is also known from WO 9011007. In the case of the bale collector known from this document, the bale-carrying means consist of horizontal rollers, the axes of which run at right angles to the direction of travel. At the rear end of the bale-carrying means there is a blocking roller at a level above them. The blocking roller is provided with a conveyor screw thread. One or more rollers of the carrying means can also be provided with a conveyor screw thread. The rollers are driven in order to convey a bale received from the baler over the rollers of the bale-carrying means until it is against the blocking roller, which bale is then, or possibly simultaneously, moved by the conveyor screw thread of the rollers at right angles to the direction of travel, so that bales supplied one after another form a row of bales at right angles to the direction of travel. On completion of a row, the blocking roller is lowered, in order to convey the row of bales off the bale-carrying means. A part of the bale collector disposed further to the back can receive a number of rows of bales from the front part of the collector on a number of rollers in a horizontal plane with axes at right angles to the direction of travel and against a further blocking means, in particular a bar which can be swung away. After a suitable number of bales has been received, the blocking means of the rear part is swung away, with the result that these rows of bales are conveyed onto the ground.
There are currently balers which can produce bales of large dimensions, for example bales of straw with dimensions of 2.4 m long, 1.2 m wide and 0.7 m high, and having a weight of approximately 400 kg, or bales of silage with dimensions of 1.6 m long, 1.2 m wide and 0.7 m high, and having a weight of approximately 500 to 800 kg. On account of the large dimensions and great weights of such bales, bale collectors by means of which rows of two or more of such bales can be collected in the direction of travel and deposited on the ground essentially without spaces between the bales have not been known until now. It must be observed here that during collection, and possibly while being pushed up by following bales, such heavy bales must be prevented from exerting an unacceptably high counterpressure towards the baler, as a result of which following bales would be pressed too tightly and/or the baler would be too heavily loaded and could be damaged.
SUMMARY OF THE INVENTION
The object of the invention is therefore to provide a bale collector which is capable of collecting successively a row of two or more bales, in particular of the abovementioned large and heavy type, without the above problems occurring.
For the purpose of achieving this object, the invention provides a bale collector, comprising a frame provided with wheels, bale-carrying means, coupling means which are suitable for coupling the frame to a mobile baler in order to receive bales onto the carrying means from a bale outlet of the baler via a front end, viewed in the direction of travel of the carrying means, and also control means for taking the carrying means into a collecting state or into an unloading state, for collecting bales on the carrying means or unloading bales from the carrying means and depositing them on the ground, the carrying means comprising rollers with parallel horizontal axes, and the rollers being suitable for collecting a row of two or more bales thereon between the front end and a rear end of the carrying means, wherein the rollers form a two-part bottom which can be swung downwards, each bottom part being fixed to a corresponding sub-frame which is coupled by way of corresponding rotary means to the frame, while the axes of rotation of the rotary means extend horizontally and parallel to the direction of travel at a distance from each other which is greater than a dimension of the row of bales in a direction at right angles to the direction of travel, and for reaching the unloading state from the collecting state the control means control the rotary means for turning the bottom parts downwards in order to allow the row of bales to go through between the bottom parts and to be deposited on the ground.
The rollers can have axes which run at right angles or parallel to the direction of travel. In the latter case, the rollers have a conveyor screw thread and are driven by the drive means, and are also suitable for collecting and subsequently depositing on the ground cylindrical bales whose axes extend at right angles to the direction of travel.
The invention also provides a mobile baler having, viewed in the direction of travel, from the back a bale outlet and behind the bale outlet coupling means for coupling to coupling means of the bale collector, wherein the coupling means are rotary coupling means with an essentially vertical axis of rotation, and behind the bale outlet there is provided a supply plate, having in the centre thereof an elongated guide element which is disposed upright on the plate and running essentially parallel to the direction of travel of the baler, for the purpose of guiding over it bales coming out of the bale outlet. By this it is still easy to manoeuvre with the combination of baler and relatively long bale collector, and it is ensured that after a manoeuvre a bale partially projecting from the baler still remains essentially in line with the bale collector.
The abovementioned object of the invention is also achieved by means of a bale collector, comprising a frame provided with wheels, bale-carrying means, coupling means which are suitable for coupling the frame to a mobile baler in order to receive bales onto the carrying means from a bale outlet of the baler via a front end--viewed in the direction of travel--of the carrying means, and also control means for taking the carrying means into a collecting state or into an unloading state for collecting bales on the carrying means or unloading bales from the carrying means and depositing collected bales on the ground, the carrying means comprising rollers with parallel horizontal axes, and the rollers being suitable for collecting a row of two or more bales thereon between the front end and a rear end of the carrying means, and drive means being disposed on the frame and coupled to the rollers, which drive means in the collecting state and during the unloading drive the rollers for conveying the bales received backwards, wherein the axes of the rollers run parallel to the direction of travel, the rollers each have a conveyor screw thread, and the drive means drive the rollers in a direction of rotation which is such that a bale carried thereon is pushed backwards by the screw threads.
BRIEF DESCRIPTION OF PREFERRED EMBODIMENTS
Other features and advantages of the invention will emerge from the following description of embodiments of the bale collector and the baler according to the invention with reference to the appended drawings. In the drawings:
FIG. 1 shows in perspective a bale collector according to the invention, coupled behind a partially shown baler;
FIG. 2 shows in perspective a part of the synchronizing means of the bale collector of FIG. 1;
FIG. 3 shows in perspective a part of the locking means of the bale collector of FIG. 1;
FIG. 4 shows in perspective the bale collector of FIG. 1 in an unloading state;
FIG. 5 shows another embodiment of the bale collector according to the invention;
FIG. 6 shows in perspective a part of the locking means of the bale collector of FIG. 5;
FIG. 7 shows in perspective the bale collector of FIG. 5 in the unloading state;
FIG. 8 shows yet another embodiment of the bale collector according to the invention; and
FIG. 9 shows in perspective the bale collector of FIG. 8 with cylindrical bales collected thereon at the time of initiation of the unloading state.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows in perspective a bale collector 1 with a main frame 2, to which wheels 3 are coupled. The main frame 2 has at a front end thereof coupling means (not shown) with an essentially vertical axis of rotation, for coupling the collector 1 behind and to a mobile baler 6 with a bale outlet 7. The normal direction of travel of the baler 6 and the collector 1 during baling and collection is indicated by arrow 8.
A supporting plate or supply plate 9 is disposed on the baler 6 above the abovementioned coupling means. An upright guide element 10 is disposed on the top side of the supply plate 9, in the centre thereof and parallel to the direction of travel 8. The supply plate 9 and the guide element 10 prevent bales coming out of the bale outlet 7 from changing direction during or after manoeuvring of the combination of baler 6 and collector 1.
The bales delivered by the baler 6 are bales which can have large dimensions, for example bales of straw with dimensions of 2.4 m long, 1.2 m wide and 0.7 m high, and having a weight of approximately 400 kg, or bales of silage with dimensions of 1.6 m long, 1.2 m wide and 0.7 m high, and having a weight of approximately 500 to 800 kg.
Along the two sides of the collector 1, and symmetrically relative to bales supplied by the baler 6, two sub-frames 11 are coupled to the main frame 2 by means of rotary means 12 with axes running parallel to each other and parallel to the lengthwise direction (during use, the direction of travel 8). The distance between the axis of rotation of the rotary means 12 of one sub-frame 11 and the axis of rotation of the other sub-frame 11 is greater than the dimensions of the bales at right angles to the axes of rotation (at right angles to the direction of travel 8).
Rollers 13, whose axes of rotation run at right angles to the normal direction of travel 8, are coupled to the bottom part of each sub-frame 11.
An upwardly extending arm 15 is fixed to each sub-frame 11, a top end of which arm is rotatably fixed to an end of a further arm 16. As shown in FIG. 2, the other ends of the arms 16 are rotatable relative to each other and coupled to sliding pieces 17. The axes of rotation of the couplings between the arms 15, 16 are all parallel to the axes of rotation of the rotary means 12 of the sub-frames 11.
The sliding pieces 17 fit into recesses of straight vertical guides 18, which are fixed to the main frame 2.
The sub-frames 11 are forced into the situation shown in FIG. 1 by means of a tension spring 20 between each matching pair of arms 15, 16.
A control arm 24 is fitted at the rear side of the collector 1, which arm extends downwards, and the top end of which is coupled by means of a rotary coupling 25 to the main frame 2. The axis of rotation of the coupling 25 runs at right angles to the direction of travel 8. The bottom end of the control arm 24 is at such a low level during the collection that it is lower than the top side of bales collected on the rollers 13. The control arm 24 is forced into the position shown in FIG. 1 by means of a tension spring 26 between the main frame 2 and the control arm 24. Fixed to the control arm 24 is a pulling wire 27, which is also fixed to a locking clamp 30 which, as shown more clearly in FIG. 3, is rotatably fixed to the main frame 2 and at the other end it has a recess 31, which in the collecting position of the collector shown in FIG. 1 accommodates a strip 32, which is fixed to one of the arms 16. The clamp 30 is forced into the position shown in FIGS. 1 and 3 by means of a tension spring 33 (shown only in FIG. 3) between one end of the clamp 30 and the main frame 2.
At the front of the collector 1, an additional supporting roller 35 is disposed between the sides of the collector 1.
During operation of the baler 6, it delivers through the bale outlet 7 bales which are guided first over the supply plate 9 with the guide element 10, and then over the supporting roller 35 and the rollers 13. During movement over the rollers 13, 35 the bales push each other backwards. When a rear bale pushes against the control arm 24, the latter by way of the pulling wire 27 will cause the clamp 30 to turn, with the result that the strip 32 (FIG. 3) is released from the recess 31 of the clamp 30. The axes of rotation of the rotary means 12 are situated at such a distance on either side of the bales 38a, 38b (FIG. 4) to be collected that the weight of the bales 38a, 38b collected on the rollers 13 (FIG. 4) causes the sub-frames 11 to turn away from each other, and the bales 38a, 38b can fall between the rollers 13 onto the ground. Since the sub-frames 11 are coupled by means of the sets of arms 15, 16 and the guide means 17, 18, it is ensured that the sub-frames 11 turn simultaneously, with the result that tilting of the bales 38a, 38b about an axis running parallel to the direction of travel 8, and thus breakdown of the collector 1, are prevented. A row of bales 38a, 38b which has collected on the rollers 13 is deposited relatively quickly. Owing to the fact that the bales have pushed each other up and will be deposited simultaneously on the ground, there will be essentially no spaces between the bales 38a, 38b deposited on the ground, which makes it easier for complete rows to be picked up mechanically thereafter and processed further.
When the bale collector 1 has travelled further, the tension springs 20 ensure that the position of the collector 1 shown in FIG. 1 is resumed.
The rollers 13 can be driven by means of drive means (not shown), in order to make it easier to move backwards bales supplied by the baler 6, for the purpose of counteracting the counterpressure towards the baler 6 which occurs when the bales push each other up.
Although the embodiment of the bale collector 1 according to the invention shown in FIGS. 1 and 4 is illustrated and described for the collection of a row of two bales thereon, the collector is easily made suitable for collecting a row with more bales. This also applies to the other embodiments of the bale collector according to the invention described hereinafter.
FIGS. 5 and 7 show in perspective another embodiment of a bale collector 40 according to the invention. The bale collector 40 differs from the bale collector 1 in that the rollers 13 of the bale collector 1 are replaced by long rollers 41a, 41b, each of which is provided with a conveyor screw thread 42a, 42b, and the axes of rotation of which run parallel to the lengthwise direction (normal direction of travel 8) of the collector 40. Each roller 41a, 41b is coupled to a corresponding motor 44a, 44b. The motors 44a, 44b are in particular hydraulic motors which are coupled by way of lines 45 to a drive device (not shown) of the baler 6.
As shown, viewed in the direction of travel 8, the screw thread 42a of the right-hand roller 41a is a right-handed screw thread, and the screw thread 42b of the left-hand roller 41b is a left-handed screw thread. The motors 44a, 44b are driven in such a way that bales delivered by the baler 6 are conveyed backwards by the rollers 41a, 41b. Viewed in the direction of travel 8, the roller 41a will then turn anti-clockwise, and the roller 41b clockwise, which prevents the bales from being pressed against the sides of the collector 40.
The motors 44a, 44b are controlled in such a way that they convey bales on the rollers 41a and 41b at a speed which is preferably at most equal to the speed at which the baler 6 delivers bales.
At the rear side of the collector 40, the rear bale is retained by a retaining element 46, which is fixed to the main frame 2.
The collector 40 has similar locking means to the locking means 30-33 of the collector 1 shown in FIG. 3, but with a clamp 30' to which the wire 27 is not fastened. The collector 40 has at approximately the height of the locking means 30'-33 and further backwards a control arm 50, a top end of which is coupled rotatably to the main frame 2, and to which a wire 51 is fixed at a lower level, another end of which is fixed to a front control arm 52, which is rotatably coupled to the main frame 2, and another end of which is fixed by means of a wire 53 to the top end the clamp 30'.
When a bale passes the control arm 50, the control arm 50 will rotate (in FIG. 5 anti-clockwise), with the result that the control arm 50 by way of the wire 51 will pull the arm 52 downwards so much that when a subsequent bale passes the control arm 52 the latter will rotate further and, by way of the wire 53, will pull the clamp 30' away from the strip 32, with the result that unloading of bales collected on the rollers 41a, 41b is initiated. The sub-frames in this case will rotate to the position shown in FIG. 7, in order to allow the bales 38a, 38b through between the rollers 41a, 41b and to deposit them on the ground. The control arms 50, 52 and the clamp 30' have in the meantime returned by means of suitable springs to the initial position. When the bale collector 40 has travelled further, the tension springs 20 ensure that the position of the collector 40 shown in FIG. 5 is resumed.
If the collector 40 is of suitable dimensions, it is also suitable for the collection of cylindrical bales with axes running at right angles to the direction of travel 8.
FIG. 8 shows yet another embodiment of a bale collector 60 according to the invention. The bale collector 60 has a frame 61 to which wheels 62 are coupled. The collector 60 is coupled behind a mobile baler 63 by means of coupling means. The normal direction of travel during baling and collection is indicated by arrow 64.
The baler 63 is of a type which is suitable for producing cylindrical bales, the axes of which run at right angles to the direction of travel 64. When a bale has been produced, a rear part 65 of the baler 63 is rotated upwards, with the result that the ready bale can roll out of the baler 63.
The collector 60 has along the sides thereof two rollers 66a, 66b which are parallel to each other and to the normal direction of travel 64, and are at such a height and at such a distance from each other that they can support bales delivered by the baler 63. Viewed in the direction of travel 64, the right-hand roller 66a has a right-handed conveyor screw thread 67a, and the left-hand roller 66b has a left-handed conveyor screw thread 67b. The rollers 66a, 66b are driven by motors 68a, 68b, which are in particular hydraulic motors which are controlled from a drive unit (not shown) of the baler 63. The motors 68a, 68b drive the rollers 66a, 66b in such a way that bales received on the rollers 66a, 66b are transported backwards, and as a result of the opposite screw thread directions, the bales are prevented from being pushed against the side of the collector 60.
Disposed at the rear side of the collector 60 is a retaining element 70, a top end of which is coupled to the frame 61 by means of a horizontal rotary shaft 71 running at right angles to the direction of travel 64. The retaining element 70 is forced into the position shown in FIG. 8 by means of a spring 72, one end of which is fixed to the frame 61. An arm 73 with a crosspiece 74 is fixed to the shaft 71. A rotatable clamp 75 is coupled to the frame 61 opposite the transversepiece 74. The clamp 75 has a recess 76. In the position of the collector 60 shown in FIG. 8, the crosspiece 74 falls into the recess 76 (FIG. 9) of the clamp 75, so that the retaining element 70 is locked in the position shown.
Further forward, a control arm 80 is rotatably coupled to the frame 61. Still further forward, another control arm 81 is rotatably coupled to the frame 61. A wire 82 is connected between the arms 80 and 81. A wire 83 is connected between the arm 81 and the clamp 75. The control arms 80 and 81 are forced into the position shown in FIG. 8 by means of springs 84, 85, ends of which are fixed to the frame 61.
The design and the arrangement of the control arms 80 and 81 and the fixing of the wires 83 are such that only when a complete row of bales 90a, 90b, 90c has collected on the rollers 66a, 66b does the arm 81 by way of the wire 83 cause the clamp 75 to rotate, with the result that the lock of the retaining element 70 is released, and the bales 90a, 90b, 90c can leave the collector 60 at the rear side as a result of the rollers 66a, 66b being driven.
For the embodiment of the bale collector 60 shown in FIGS. 8 and 9, the motors 68a, 68b drive the rollers 66a, 66b, preferably at such a speed that they convey the bales 90a, 90b, 90c at a speed which is at most equal to the speed at which the baler 63 delivers the bales. During the unloading, the motors 68a, 68b can be driven in such a way that the bales 90a, 90b, 90c are unloaded at a greater conveyance speed of the rollers 66a, 66b.
The control means 80-85 and pre-tensioned blocking means and locking means 70-76 of the embodiment of the bale collector shown in FIGS. 8 and 9 can, if desired, be replaced by a single control arm at the rear end of the collector, which arm also acts as a retaining element for retaining bales until the bales, for example, exert a certain pressure on the control arm, with the result that the latter turns away in order to allow the bales to go through and be deposited on the ground. | Bale collector, includes a frame provided with wheels, bale-carrying rollers, coupling elememt suitable for coupling the frame to a mobile baler in order to receive bales onto the carrying rollers from a bale outlet of the baler via a front end--viewed in the direction of travel--of the carrying rollers, and also control mechanism for taking the carrying rollers into a collecting state or into an unloading state, for collecting bales on the carrying rollers or unloading collected bales from the carrying rollers and depositing them on the ground. The carrying rollers have parallel horizontal axes, and the rollers are suitable for collecting a row of two or more bales thereon between the front end and a rear end of the carrying rollers. In one embodiment the carrying rollers form a two-part bottom which can be swung downwards, and which, after a complete row of bales has collected thereon, in order to allow the row of bales to pass between the bottom parts and be deposited on the ground. In another embodiment, after initiation of the unloading state, the rollers are driven in order to convey the bales backwards and deposit them on the ground. | 0 |
BACKGROUND OF THE INVENTION
[0001] This application relates to the control of a refrigerant system, and in particular, to the control of indoor fan operation to prevent moisture being re-evaporated from evaporator external surfaces and then being delivered by indoor airflow into a conditioned environment, when a refrigerant compressor is shut down or during system startup.
[0002] Refrigerant systems are utilized to condition the air being delivered into an indoor environment. As an example, an air conditioning system or a heat pump is utilized to cool and dehumidify or heat air being delivered into the environment to be conditioned.
[0003] In recent years, significant attention has been paid to indoor air quality issues. In particular, precise control of the indoor relative humidity within the comfort zone has been the subject of an increased scrutiny. In part, this desired humidity control is attributed to prevention of mold, bacteria and fungus formation and growth.
[0004] As known, refrigerant systems operate at part-load conditions for most of their design life. Thus, the system operates in a start-stop mode quite frequently to satisfy the demanded sensible and latent capacity requirements, when all other means of system unloading are already exhausted. When the system is operating in a cooling mode, an evaporator that cools and dehumidifies the air being delivered into the indoor environment has cold external surfaces. Moisture forms on the cold external surfaces of the evaporator heat exchanger, while the cooled and dehumidified air flows through the heat exchanger and into the conditioned space. This moisture is removed from the air stream and continuously drained into a drain pan. When the system is shut down, there is often a significant amount of moisture accumulated on the evaporator external surfaces. As the evaporator is gradually warming up, this moisture re-evaporates and is re-introduced into the indoor airstream and consequently into the conditioned environment, since in many application cases, the indoor fan has to operate continuously to comply with legislation and regulation requirements.
[0005] Even with the indoor fan shut down simultaneously with other system components, such as a compressor, at system startup, a burst of moist air will often be supplied to the indoor environment causing undesired high humidity fluctuations and consequent occupant discomfort. Additionally, this moisture accumulated on the evaporator external surfaces will promote mold, bacteria and fungus formation and growth. It has become an industry practice to treat external evaporator surfaces with anti-microbial compounds, or employ UV lights to prevent growth of microorganisms. These measures are associated with design complexities and additional costs.
[0006] Thus, it would be desirable to provide a solution to the problems mentioned above that does not have the drawbacks of the prior art.
SUMMARY OF THE INVENTION
[0007] In a disclosed embodiment of this invention, a motor for driving the fan that blows air over the evaporator has a rotation direction reversal feature. Many of three-phase motors are already capable of phase reversal (when the phases are reversed the motor turns in the opposite direction). At a compressor shutdown, the fan is run in reverse for a short period of time, and air flows over the evaporator in an opposite direction. As the moisture is driven off the evaporator external surfaces, this moisture-loaded air is preferably disposed into the outdoor environment. In one embodiment, an airside economizer controlling the appropriate percentages of air mixture from a return duct and from an outdoor environment closes off the flow from the return duct. All of the air that removes the moisture from the gradually warming evaporator is thus delivered to the outside environment. Heat generated by the indoor fan assists in faster moisture re-evaporation and removal from external evaporator surfaces.
[0008] In a second embodiment, a supplemental exhaust fan, which in many cases is already incorporated into the system design, assists the main indoor fan in driving air over the evaporator coil in the reverse direction, while fresh air intake may be closed. It has to be noted that, in this embodiment, the return duct may be blocked by a damper and the indoor fan may be shut down completely. In the latter case, the indoor fan does not need to be equipped with the rotation direction reversal feature.
[0009] In yet another embodiment, a system equipped with a variable volume temperature (VVT) feature, and having a bypass duct, may utilize the main indoor fan and the exhaust fan to flow air over the evaporator in forward direction to remove moisture. The air would then flow through the bypass duct and then to the outdoor environment. In this embodiment, the air may be repeatedly recycled through the evaporator for a short period of time by the main indoor fan and, when a majority of moisture is removed from the evaporator and accumulated in the re-circulating air, the exhaust fan is turned on for a brief period of time to dump this moist air to the outdoor environment. In this embodiment, the main indoor fan does not have to be equipped with the rotation direction reversal feature as well.
[0010] In yet another embodiment, the refrigerant system has a reheat circuit, which is selectively run for a short period of time before the shutdown. In this case, not only indoor fan heat but also the heat from the reheat coil can be utilized to promote faster moisture re-evaporation and removal from the evaporator external surfaces. Analogously, if the refrigerant system is a heat pump, it can be run in a heating mode for a short period of time during the moisture removal process described above. Further, a hot gas by-pass circuit, as known in the industry, can be employed to bypass high pressure refrigerant from the compressor discharge region into the evaporator inlet. In this case, the hot gas bypass circuit can be utilized to assist in moisture re-evaporation and removal by providing additional preheating.
[0011] In all embodiments, the moisture removal process can be terminated by a timer or by a sensor such as a humidity sensor, a dew point sensor, a sensor measuring pressure drop across the evaporator, an evaporator surface temperature sensor, an air temperature sensor or an enthalpy sensor. In all cases, the system resumes normal operation after moisture removal is completed, either in an active cooling mode or in air circulation mode.
[0012] These and other features of the present invention can be best understood from the following specification and drawings, the following of which is a brief description.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a schematic view of the system incorporating the present invention.
[0014] FIG. 2 shows the control operation of the present invention.
[0015] FIG. 3 shows another embodiment.
[0016] FIG. 4 shows yet another embodiment.
[0017] FIG. 5 shows yet another embodiment.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0018] A refrigerant system 20 is illustrated in FIG. 1 , and serves to provide conditioned air to an environment 22 , such as a building. A thermostat 24 within the building allows a user to demand a particular temperature level as known. A control for the refrigerant system 20 thus operates the refrigerant system to achieve the demanded conditions. A closed-loop refrigerant circuit 26 includes a compressor 28 compressing refrigerant and delivering it to an outdoor heat exchanger or condenser 30 . From the condenser, the refrigerant passes through an expansion device 32 , and then to an indoor heat exchanger or evaporator 34 . An indoor fan 36 is associated with the evaporator 34 , and drives air over the evaporator 34 . As is known, a return duct 38 serves as a conduit for air delivered by the fan 36 from the indoor space 22 , and over the evaporator 34 to be conditioned. This air is then delivered to a supply duct 40 to be returned into the conditioned space 22 . An airside economizer 44 allows appropriate mixture amounts of outside air from an outdoor opening 42 and re-circulated indoor air from the return duct 38 to be delivered over the evaporator 34 . As is known, the economizer 44 is also controlled by the control for the refrigerant system 26 to comply with specified requirements.
[0019] As mentioned above, when the cooling demands within the conditioned space 22 are met and all available means of system capacity unloading are exhausted, the refrigerant system operates in a start-stop mode. During shutdown periods, moisture accumulated on the evaporator 34 external surfaces re-evaporates into the airstream and makes its way into the conditioned space, which, as mentioned above, is undesirable.
[0020] One embodiment of the present invention is illustrated in FIG. 2 . As shown in FIG. 2 , the airside economizer 44 is moved to a position where the airflow through the return duct 38 is blocked and airflow to the outdoor opening 42 is opened. The motor for the fan 36 is a reversible fan motor. For a short period of time, the motor is driven in the reverse direction to the flow of FIG. 1 , and air is pulled through the supply duct 40 and over the evaporator 34 . This air removes moisture from the evaporator 34 external surfaces and is disposed into an outdoor environment through the outdoor opening 42 . The operation in this manner removes the moisture at the refrigerant system compressor shutdowns. Heat generated by the indoor fan assists in faster moisture re-evaporation and removal from external evaporator surfaces. Preferably, such a step is taken soon after the shutdown, in case of continuous air circulation requirement, or before the next startup. This operation should continue for as long as certain criteria for the moisture removal are satisfied. Such criteria for the moisture removal process termination can be associated with a timer or a sensor such as a humidity sensor, a dew point sensor, a sensor measuring pressure drop across the evaporator, an evaporator surface temperature sensor, an air temperature sensor or an enthalpy sensor. The system resumes normal operation after moisture removal is completed, either in an active cooling mode (when a call is issued by a thermostat) or in an air circulation mode.
[0021] FIG. 3 shows another embodiment, wherein a supplemental exhaust fan 48 associated with the return duct 38 , and in many cases already incorporated into the system design, assists the main indoor fan 36 in driving air over the evaporator in the reverse direction, while the fresh air intake may be closed. Further, if desired, the return duct 38 may be blocked by a damper, and the main indoor fan 36 may be shut down completely. In the latter case, the main indoor fan 36 does not need to be equipped with the rotation direction reversal feature.
[0022] FIG. 4 shows another embodiment wherein the refrigerant system 20 is equipped with a variable volume temperature (VVT) feature and there is a bypass duct 52 between the return duct 38 and the supply duct 40 . A damper 50 associated with the supply duct 40 is closed and a damper 54 associated with the return duct 38 is closed as well. The main indoor fan 36 is operated in the conventional forward, FIG. 1 direction and does not need to be reversible. When operated, the supplemental exhaust fan 48 receives the airflow from the bypass duct 52 , and delivers that air to the outdoor environment. The main indoor fan 36 , operating in a forward direction, drives air over the evaporator 34 external surfaces to remove the accumulated moisture. In this embodiment, the air is repeatedly recycled through the evaporator for a short period of time by the main indoor fan 36 and, when a majority of moisture is removed from the evaporator 34 and accumulated in the re-circulating air, the exhaust fan is turned on, for a brief period of time, to dump this moist air to the outdoor environment. During such communication with the outdoor environment, the main indoor fan 36 may not need to be operating.
[0023] FIG. 5 shows another embodiment 60 . Embodiment 60 is similar to the FIG. 2 embodiment, however, a reheat circuit is incorporated in the refrigerant system design. As known, for example, a three-way valve 62 would selectively bypass refrigerant to a reheat coil 61 , and return the refrigerant to a point 64 in the main refrigerant circuit. Reheat circuits can tap and return at least a portion of refrigerant to any number of locations within a main refrigerant circuit, and the disclosed locations are merely shown as one example. As known, reheat circuits typically serve to reheat the indoor air downstream of the evaporator (where the air was cooled and dehumidified), in case there is a dehumidification demand (humidistat call) and no significant cooling demand (no thermostat call) in the conditioned space. However, in this invention, the reheat coil 61 serves to further facilitate moisture removal process from external surfaces of the evaporator 34 . In the embodiment 60 , before the refrigerant compressor is shutdown, the refrigerant system is operated in the reheat mode, for a short period of time, to allow the reheat coil to warm up to its conventional operating temperature. When the refrigerant compressor 28 is shutdown and the indoor fan 36 is operated in reverse, not only the indoor fan heat but also the heat from the reheat coil 61 is utilized to warm up air flowing over the evaporator 34 to promote faster moisture re-evaporation and removal.
[0024] Analogously, if the refrigerant system is a heat pump, it can be run in a heating mode, for a short period of time, during moisture removal process to allow the indoor heat exchanger (serving as a condenser in the heating mode of operation) to warm up and facilitate the moisture removal process during indoor airflow reversal, as described above. It has to be noted that the refrigerant system can be operated in a heating mode, for a short period of time, prior to the refrigerant compressor shutdown with the indoor fan 36 turned off. This allows the indoor heat exchanger to warm up faster. When the desired temperature is reached, the indoor fan is operated in reverse, as described above, during the moisture removal process. In the same manner, hot gas bypass to the evaporator inlet can be utilized to assist in moisture re-evaporation and removal.
[0025] It is understood that although single-circuit configurations have been disclosed, the benefits of the invention are applicable to multi-circuit system arrangements.
[0026] Although preferred embodiments of this invention have been disclosed, a worker of ordinary skill in this art would recognize that certain modifications would come within the scope of this invention. For that reason, the following claims should be studied to determine the true scope and content of this invention. | Various control methods are disclosed for removing moisture from the external surfaces of an evaporator in a refrigerant system to avoid moisture entering a conditioned space. In one embodiment, the evaporator fan is driven in a reverse direction, and the air is guided to the outdoor environment. In other embodiments, a supplemental exhaust fan is utilized in conjunction with the evaporator fan. Also, a reheat circuit, hot gas bypass circuit, or specific features of a heat pump unit may be utilized to more efficiently perform the moisture removal. | 5 |
RELATED APPLICATION
This application is a continuation-in-part application of U.S. application Ser. No. 10/273,249, now U.S. Pat. No. 6,844,829 entitled A Hemocompatible Coated Polymer & Related One-Step Methods which was filed on Oct. 18, 2002.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a hemocompatible surface coated polymer system comprising an organic phase and an aqueous phase. More specifically, the present invention relates to polymer having organic and aqueous phases, where the organic phase comprises polymerizable monomers and at least one initiator and the aqueous phase comprises at least one dispersing agent, at least one free radical inhibitor and at least one buffering agent, and the organic phase is immiscible in the aqueous phase, and the dispersing agent forms a hemocompatible surface on the polymer.
2. Description of Related Art
It has been known and practiced in the art of suspension polymerization to manufacture polymers with a hemocompatible coating using a two-step process. In the first step of the two-step process, polymeric beads are manufactured by polymerizing monomer droplets using suspension polymerization. In the second step of the process, a hemocompatibilizing film is applied onto the exterior surface of the polymer to provide the hemocompatible coating. Unlike the prior art, the polymers of the present invention have aqueous and organic phases where the organic phase is immiscible in the aqueous phase, and the dispersing agent used in the aqueous phase forms a hemocompatible surface on the polymer.
SUMMARY OF THE INVENTION
The present invention provides for hemocompatible coated polymer system comprising an organic phase and an aqueous phase. In one embodiment, the organic phase comprises polymerizable monomers and at least one initiator and the aqueous phase comprises at least one dispersing agent, at least one free radical inhibitor and at least one buffering agent. In another embodiment, the organic phase of the system of the present invention is immiscible in the aqueous phase, and the dispersing agent forms a hemocompatible surface on the polymer.
In still another embodiment, the monomer is a monofunctional monomer, and the monofunctional monomer is selected from a group consisting of styrene, ethylstyrene, acrylonitrile, butyl methacrylate, octyl methacrylate, butyl acrylate, octyl acrylate, cetyl methacrylate, cetyl acrylate, ethyl methacrylate, ethyl acrylate, vinyltoluene, vinylnaphthalene, vinylbenzyl alcohol, vinylformamide, methyl methacrylate, methyl acrylate and mixtures thereof.
In yet another embodiment, the monomer is a polyfunctional monomer, and the polyfunctional monomer is selected from a group consisting of divinylbenzene, trivinylbenzene, divinylnaphthalene, trivinylcyclohexane, divinylsulfone, trimethylolpropane trimethacrylate, trimethylolpropane dimethacrylate, trimethylolpropane triacrylate, trimethylolpropane diacrylate, pentaerythritol dimethacrylate, pentaerythritol trimethacrylate, pentaerythritol tetramethacrylate, pentaerythritol diacrylate, pentaerythritol triiacrylate, pentaerythritol tetraacrylate, dipentaerythritol dimethacrylate, dipentaerythritol trimethacrylate, dipentaerythritol tetramethacrylate, dipentaerythritol diacrylate, dipentaerythritol triacrylate, dipentaerythritol tetraacrylate, divinylformamide and mixtures thereof.
In still yet another embodiment, the initiator of the system of the present invention is selected from a group consisting of diacyl peroxides, ketone peroxides, peroxyesters, dialkyl peroxides, peroxyketals, azoalkylnitriles, peroxydicarbonates and mixtures thereof. In a further embodiment, the dispersing agent is selected from a group consisting of poly(N-vinylpyrrolidinone), hydroxyethyl cellulose, hydroxypopyl cellulose, poly(hydroxyethyl methacrylate), poly(hydroxyethyl acrylate), poly(hydroxypropyl methacrylate), poly(hydroxypropyl acrylate), poly(dimethylaminoethyl methacrylate), poly-(dimethylaminoethyl acrylate), poly(diethylamimoethyl methacrylate), poly-(diethylaminoethyl acrylate), poly(vinyl alcohol), salts of poly(methacrylic acid), and salts of poly(acrylic acid) and mixtures thereof.
In still a further embodiment, the free radical inhibitor is selected from a group consisting of p-nitrosophenoxide salts, sodium nitrate, N-hydroxy-N-methylglucamine, N-nitroso-N-methylglucamine and mixtures thereof. In yet a further embodiment, the buffering agent is selected from a group consisting of carbonate salts, bicarbonate salts, boric acid salts, salts of phosphoric acid and mixtures thereof. In still yet a further embodiment, the organic phase further comprises at least one porogen, and the porogen is selected from a group consisting of aliphatic hydrocarbons, dialkyl ketones, aliphatic carbinols and mixtures thereof. In another further embodiment, the polymer is a porous polymer.
In still another further embodiment, the present invention relates to a hemocompatible surface coated polymer system comprising an organic phase and an aqueous phase, the system being manufactured by a method comprising: forming the organic phase comprising polymerizable monomers and at least one initiator; forming the aqueous phase comprising at least one dispersant agent, at least one free radical inhibitor, and at least one buffering agent; dispersing the organic phase into the aqueous phase to thereby form organic phase droplets; and polymerizing the organic phase droplets coated with the dispersing agent to thereby form the hemocompatible surface coating on the polymer. In yet another further embodiment, the polymerization of the organic phase is formed by heating a mixture of the organic and aqueous phases.
In still yet another further embodiment, the present invention relates to a method of manufacturing a hemocompatible surface coated polymer system comprising an organic phase and an aqueous phase, the method comprising: forming the organic phase comprising polymerizable monomers and at least one initiator; forming the aqueous phase comprising at least one dispersant agent, at least one free radical inhibitor, and at least one buffering agent; dispersing the organic phase into the aqueous phase by agitation to form a suspension of organic droplets; and polymerizing the organic phase by heating the suspension of the organic phase droplets coated with the dispersing agent to thereby form the hemocompatible surface coating on the polymer.
In another embodiment, the present invention relates to a polymer with a hemocompatible coating comprising at least one crosslinking agent for making the polymer and at least one dispersing agent whereby the dispersing agent forms a hemocompatible surface on the polymer.
In another embodiment, the biocompatibilizing polymer comprises poly(N-vinylpyrrolidinone). In still another embodiment, the biocompatibilizing polymer is selected from a group consisting of poly(hydroxyethyl methacrylate), poly(hydroxyethyl acrylate), poly(dimethylaminoethyl methacrylate), salts of poly(acrylic acid), salts of poly(methacrylic acid), poly(diethylaminoethyl methacrylate), poly(hydroxypropyl methacrylate), poly(hydroxypropyl acrylate), poly(N-vinylpyrrolidinone), poly(vinyl alcohol) and mixtures thereof. In another embodiment, the salts may be sodium and potassium salts and in still another embodiment, the salts are water-soluble salts.
In yet another embodiment, the dispersing agent is selected from a group consisting of hydroxyethyl cellulose, hydroxypopyl cellulose, poly(hydroxyethyl methacrylate), poly(hydroxyethyl acrylate), poly(hydroxypropyl methacrylate), poly(hydroxypropyl acrylate), poly(dimethylaminoethyl methacrylate), poly(dimethylaminoethyl acrylate), poly(diethylamimoethyl methacrylate), poly(diethylaminoethyl acrylate), poly(vinyl alcohol), salts of poly(methacrylic acid), and salts of poly(acrylic acid) and mixtures thereof.
In still another embodiment, the crosslinking agent is selected from a group consisting of divinylbenzene, trivinylbenzene, divinylnaphthalene, trivinylcyclohexane, divinylsulfone, trimethylolpropane trimethacrylate, trimethylolpropane dimethacrylate, trimethylolpropane triacrylate, trimethylolpropane diacrylate, pentaerythrital tetra-, tri-, and dimethacrylates, pentaerythritol tetra-, tri- and diacrylates, dipentaerythritol tetra, tri-, and dimethacrylates, dipentaerythritol tetra-, tri-, and diacrylates, divinylformamide, and mixtures thereof.
In still yet another embodiment, the crosslinking agent comprises divinylbenzene. In a further embodiment, the crosslinking agent comprises trivinylcylohexane. In yet a further embodiment, the crosslinking agent comprises trivinylbenzene.
In still a further embodiment, the crosslinking agent comprises copolymers of divinylbenzene with comonomers being selected from a group consisting of styrene, ethylstyrene, acrylonitrile, butyl methacrylate, octyl methacrylate, butyl acrylate, octyl acrylate, cetyl methacrylate, cetyl acrylate, ethyl methacrylate, ethyl acrylate, vinyltoluene, vinylnaphthalene, vinylbenzyl alcohol, vinylformamide, methyl methacrylate, methyl acrylate and mixtures thereof.
In still yet a further embodiment, the polymer with the hemocompatible surface is a porous polymer. In another further embodiment, the polymer with the hemocompatible surface is an ion exchange polymer. In a further embodiment, the polymer is an affinity polymer. In yet another further embodiment, the biocompatibilizing polymer becomes grafted to the surface of the polymer to provide a polymer with the hemocompatible surface. For purposes of this invention, the term grafting is defined as chemically bonded with potential entanglement such that the dispersing agent is physically restricted from leaving the surface of the polymer.
In another embodiment, the present invention relates to a polymer manufactured by a process comprising: simultaneously polymerizing and coating with at least one crosslinking agent for making the polymer and using at least one dispersing agent to form a hemocompatible coated polymer.
For purposes of this invention, the term hemocompatibility is defined as a condition whereby a material, when placed in contact with whole blood and blood components or physiological fluids, results in clinically acceptable physiological changes. In another embodiment, the dispersing agent is a biocompatibilizing polymer. A biocompatibilizing polymer is defined as a polymer, which forms a surface over a nonbiocompatible material, making the polymeric system compatible with physiological fluids and tissues. The term crosslinking agent is defined as a linking agent such as a polyfunctional monomer that links two or more polymer chains or segments of the same polymer chain together. The term dispersing agent is defined as a substance that imparts a stabilizing effect upon a finely divided array of immiscible particles suspended in a fluidizing medium. The immiscible particles can be a solid, liquid or gas and the fluidizing medium can be a liquid or a gas.
In another embodiment, the crosslinking agent is polymerized with at least one vinyl monomer. In a further embodiment, the dispersing agent forms a hemocompatible coating on a surface of the polymer. In yet a further embodiment, the coating of the polymer is equivalent to the surface of the polymer.
In still a further embodiment, the polymer is processed in non-pyrogenic water. For purposes of this invention, non-pyrogenic shall be defined by U.S.P. 25, Monograph (151) Pyrogenic Test, U.S. Pharmacopeia National Formulary.
In still yet another embodiment, the polymer of the present invention is prepared by suspension polymerization. For purposes of the invention, suspension polymerization is defined as the polymerization of monomer droplets dispersed in an immiscible liquid. Based upon an Elemental Analysis of the Polymer s Surface by X-Ray Photoelectron Spectroscopy (XPS), the dispersing agent becomes chemically grafting onto the surface of the polymer as the monomer droplets are transformed into polymeric beads. Polymers coated with poly(N-vinylpyrrolidinone) have been found to be biocompatible and hemocompatible. The hemocompatible polymers of the present invention pass the Lee White clotting tests and the tests for the hemolysis of red blood cells.
In another embodiment, the polymer of the present invention is a porous polymer. The term porous polymer is defined as a polymer particle having an internal pore structure with a porosity resulting from voids or holes throughout the polymer matrix. In still another embodiment, the polymer is an ion exchange resin or polymer. An ion exchange resin or polymer is a resin or polymer carrying ionogenic groups that are capable of exchanging ions or of sequestering ions. The ion exchange polymers of the present invention are beneficial when used with blood for removing and isolating varying ions and ionogenic molecules.
In still yet another embodiment, the present invention relates to a polymer with a hemocompatibilizing surface coating. In a further embodiment, the coated polymer is manufactured by a one step process comprising: simultaneously coating and polymerizing monomer droplets in a suspension polymerization procedure with at least one dispersing agent having encapsulated the droplets with a hemocompatible coating to thereby form a polymer with a hemocompatible surface-coating grafted onto the surface of the polymer beads.
In another embodiment, the present invention relates to a method of manufacturing a biocompatible and hemocompatible surface coated polymer. In still another embodiment, the method comprises: polymerizing monomer droplets comprising at least one crosslinking agent and simultaneously coating the resulting polymer beads using at least one dispersing agent to form a biocompatible surface coated polymer. In still another embodiment, the coated polymers are hemocompatible. In yet another embodiment, the polymer is formed using a suspension polymerization procedure. In another embodiment, the polymer is formed using an emulsion polymerization procedure followed by growing the particles with additional monomer feed.
In still another embodiment, the present invention relates to an application of use whereby the hemocompatible surface coated polymers of the present invention are utilized for medical applications. In another embodiment, the hemocompatible polymers of the present invention may be used to isolate and/or remove target substances from blood and physiological fluids and for specific treatments. In a further embodiment, the hemocompatible polymers of the present invention may be used in preserving organs. In yet another embodiment, the present invention relates to an apparatus for isolating blood components and for purifying blood using the hemocompatible surface coated polymers of the present invention. In one embodiment, the apparatus comprises a cartridge containing the hemocompatible polymers of the present invention.
In yet a further embodiment, the present invention relates to a polymer with a hemocompatible surface coating, the polymer being manufactured by a method comprising: polymerizing monomer droplets comprising at least one crosslinking agent to form a polymer and developing a surface coating on the polymer by using at least one dispersing agent carrying hydroxyl groups followed by a reaction of hydroxyl groups with a vinyl monomer or polymer to thereby form the hemocompatible surface coating on the polymer.
In still yet a further embodiment, the present invention also relates to a method of manufacturing a hemocompatible surface coated polymer using a one step process, the method comprising: polymerizing monomer droplets comprising at least one crosslinking agent to form a polymer and developing a surface coating on the polymer by using at least one dispersing agent carrying hydroxyl groups followed by a reaction of hydroxyl groups with a vinyl monomer or polymer to thereby form the hemocompatible surface coating on the polymer.
In another embodiment, the present invention relates to a polymer having a hemocompatible-coated surface, the polymer being manufactured by a two-step process comprising: polymerizing monomer droplets comprising at least one crosslinking agent and at least one dispersing agent to form a polymer; and coating the surface of the polymer by crosslinking a monovinyl monomer and a polyfunctional monomer mixture over the surface of the polymer bead to thereby form the hemocompatible coating on the surface of the polymer.
In a further embodiment, the present invention relates to a method comprising: polymerizing monomer droplets comprising at least one crosslinking agent and at least one dispersing agent to form a polymer; and coating the surface of the polymer by crosslinking a monovinyl monomer and a polyfunctional monomer mixture over the surface of the polymer bead to thereby form the hemocompatible coating on the surface of the polymer.
In another embodiment, the present invention relates to a hemocompatible system comprising an organic phase and an aqueous phase, wherein the organic phase composed of the polymerizable monomers and the porogen are dispersed into a slurry of droplets by agitation throughout the aqueous phase which is formulated to effect the stability of the droplets by the water-miscible dispersant and to quench polymer growth in the aqueous phase by carrying a water-soluble free radical inhibitor.
DETAILED DESCRIPTION OF THE INVENTION
As required, detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention that may be embodied in various forms. The figures are not necessary to scale, some features may be exaggerated to show details of particular components. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention.
The specific example below will enable the invention to be better understood. However, they are given merely by way of guidance and do not imply any limitation.
EXAMPLE 1
The first polymer synthesis was targeted at an aqueous to organic volume ratio of 1.0. Table 1 below illustrates the targeted dispersion mixture designed for Example 1 using a fifty (50) liter reaction.
TABLE 1
Dispersion Mixture Desires for 50 Liters
Aqueous/Organic Volume Ratio
1.0
Volume of Organic Phase, ml
25,000.0
Volume of Aqueous Phase, ml
25,000.0
Density of Organic Phase, g/ml
0.83490
Weight of Organic Phase, g
20,872.5
Density of Aqueous Phase, g/ml
1.005
Weight of Aqueous Phase, g
25,125.0
Polymerizable Monomers, DVB plus EVB, g
8766.45
Total Volume of Organic & Aqueous Phases, ml
50,000.0
Total Weight of Organic & Aqueous Phases, g
45,997.5
The procedure for the polymerization in Example 1 is initiated by the preparation of an aqueous phase and an organic phase. Table 2 and 3 below illustrate the components of the aqueous phase composition for the polymer synthesis by weight percent (%) and by quantity of the components in grams (g), respectively.
TABLE 2
Aqueous Phase Composition
Ultrapure Water, wt. %
98.089
Water from Aqueous 45% Solution of
0.611
Poly (N-vinylpyrrolidinone), wt. %
Poly(N-vinylpyrrolidinone) Pure, wt. %
0.500
Sodium Carbonate, wt. %
0.500
Sodium Nitrite, wt. %
0.300
Other dispersants, such as poly(vinyl alcohol) have been used as a substitute for the poly(N-vinylpyrrolidinone).
TABLE 3
Aqueous Phase Charges
Ultrapure Water, g
24,644.83
Water from Aqueous 45% Solution of
(153.542)
Poly(N-vinylpyrrolidinone), g
Poly(N-vinylpyrrolidinone) Pure, g
(125.625)
Aqueous Poly(N-vinylpyrrolidinone) Solution,
279.167
45 wt. %, g
Sodium Carbonate, g
125.625
Sodium Nitrite, g
75.375
Weights in parenthesis are part of other charged materials
Total Weight of Aqueous Phase, g
25,124.997
Table 4 and 5 illustrate the components of the organic phase composition for the polymer synthesis by weight percent (5) and by quantity of the components in grams (g), respectively.
TABLE 4
Organic Phase Composition
Divinylbenzene (DVB), wt. %
26.998
Ethylvinylbenzene (EVB), wt. %
15.0024
Inerts, wt. %
0.41567
Toluene, wt. %
27.134
Isooctane, wt. %
30.450
Benzoyl Peroxide, wt. % of polymerizable monomers
1.03
Other immiscible porogens such as isooctane, cyclohexane and nonane have been substituted, both singularly and in combination with one another, for the mixture of toluene and isooctane.
TABLE 5
Organic Phase Charges
Divinylbenzene, Pure, g
(5635.069)
Ethylvinylbenzene, Pure, g
(3131.381)
Commercial DVB, Dow 63.5%, g
8853.211
Inerts, g
(86.761)
Toluene, g
5663.613
Isooctane, g
6355.676
Weights in parenthesis are part of commercial DVB
Total Weight of Organic Phase, g (excluding BPO)
20,872.50
Benzoyl Peroxide, BPO, Pure, g
90.294
75 weight percent BPO, g
120.393
97 weight oercent BPO, g
93.087
Upon preparation of the aqueous and organic phases, the aqueous phase is introduced into the reactor. The reactor is set at an agitation rate sufficient to produce droplet slurry throughout the reaction volume. The aqueous phase is then heated to 65 degrees Celsius with agitation and a nitrogen sweep through the headspace in order to displace oxygen from the reactor space. The organic phase is then introduced into the reactor by pouring or pumping the organic phase onto the aqueous phase under agitation at a stirring rate of at least 86 revolutions per minute. The droplet dispersion is then stirred at 86 revolutions per minute for at least fifteen (15) minutes to set the droplet size and allow the droplet slurry to equilibrate as the temperature is raised from about 65 degrees to about 70 degrees Celsius. Once the droplet dispersion is homogenous throughout the reaction volume, the slurry is then heated to about 75 plus or minus 2.0 degrees Celsius and held at that temperature for ten (10) hours.
The slurry is cooled to about 70 degrees Celsius and the stirrer is turned off, and the polymer beads are allowed to collect at the top of the fluid bed. The mother liquor is then removed from the bottom of the reactor via a pump until the bead bed approaches within about one (1) inch from the bottom of the reactor. The mother liquor is discarded.
A sufficient amount of ultrapure water at ambient temperature is added to fluidize the bead bed and the slurry is heated to 60%. The quantity of water needed to wash the beads will be approximately one (1) bed volume or about 25 liters of water. Upon adding the water, the stirrer is then restarted and agitated at a stir rate of 106 revolutions per minute for about thirty (30) minutes while being heated to 60%. The stirring is stopped and the beads are allowed to collect at the top of the fluid bed.
The liquor is then drained from the bottom of the reactor via a pump until the bead bed approaches within about one (1) inch from the bottom of the reactor. The wash liquor is discarded. The beads are then washed with the 60 degree Celsius ultrapure water for at least five (5) washes or until the bulk fluid is transparent and free of junk polymer (a clear liquor is achieved). The water-wet bead slurry is transferred to a column that is fitted with a solid-liquid separator at the bottom of the column. The separator may be a mesh or screen made from Teflon, nylon, polypropylene, stainless steel, or glass with pore openings in the size from about 100 to about 300 microns.
The porogen mixture is displaced from the beads by a downflow treatment with ten (10) bed volumes of isopropyl alcohol at a flow rate of one (1) bed volume per hour. The isopropyl alcohol is displaced from the beads with water at a downflow treatment with ten (10) bed volumes of ultrapure water (pyrogen and endotoxin free) at a flow rate of one (1) bed volume per hour. The polymer beads are then transferred from the column into plastic containers for transport to the thermal steam-flux cleaner.
Alternatively, the porogen is displaced from the beads by a thermal-gas-flux treatment in which the porogen filled beads are heated from about 150 degrees to about 180 degrees Celsius under an upflow gas flux for approximately six (6) hours. The hot gas flux can be either super heated stream or hot nitrogen gas. The dried, cleaned, porogen free beads are wetted out with an aqueous solution of isopropyl alcohol in water for further handling prior to being packed into containers.
EXAMPLE 2
Other experimental procedures were conducted to make the polymeric beads manufactured by similar polymerization procedures described in Example 1 and under the variations identified in the Table of Inputs (Table 6) with the resulting responses tabulated in the Tables of responses (Table 7). Tables 6 & 7 are set forth below:
TABLE 6
Experimental Program: Input
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample ID
Sample ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
LDM
02-001
02-004
02-006
02-008
02-010
02-012
02-015
02-016
02-017
02-022
02-025
Organic Phase Composition
Monomer (DVB & EVB) Wt. %
42.0
42.0
42.0
42.0
40.7
50.0
40.0
40.0
45.0
45.0
45.0
Porogen Wt. %
58.0
58.0
58.0
58.0
59.3
50.0
60.0
60.0
55.0
55.0
55.0
Porogen/Monomer Ratio
1.3810
1.3810
1.3810
1.3810
1.457
1.000
1.500
1.500
1.222
1.222
1.222
Benzoyl Peroxide (BPO) Wt. %
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
Porogen Composition
Isooctane, Wt. %
52.5
52.5
52.5
52.5
53.5
60.0
99.327
99.327
99.174
99.174
99.274
Toluene, Wt. %
46.769
46.769
46.769
46.769
45.81
38.99
0
0
0
0
0
Inerts, Wt %
0.731
0.731
0.731
0.731
0.693
1.010
0.6734
0.6734
0.826
0.826
0.726
Toluene, plus Inerts, Wt. %
47.5
47.5
47.5
47.5
46.5
40.0
...
...
...
...
...
Isooctane/Toluene plus Inerts Ratio
1.105
1.105
1.105
1.105
1.1505
1.500
...
...
...
...
...
Aqueous Phase Composition
Sodium Carbonte, Wt. %
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
Sodium Nitrite, Wt. %
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
Poly (N-Vinylpyrrolidione),
0.500
0.500
0.450
0.400
0.400
0.400
0.100
0.400
0.500
0.500
1.000
Wt. %
PVP K 30, 45–55 Kdaltons,
0
0
0
0
0
0
0
0
0
0.250
1.000
Wt. %
PVP K 60, 400–500 Kdaltons,
0.500
0.500
0.450
0.400
0.400
0.400
0.100
0.400
0.500
0.250
0
Wt. %
Poly (Vinyl alcohol), Wt. %
0.01
0.01
0.05
0.100
0.100
0.100
0.400
0.100
0
0
0
Molecular Size, Kdaltons
88.0
88.0
95.0
95.0
95.0
95.0
95.0
95.0
...
...
...
Amount Hydrolized, %
85
85
95
95
95
95
95
95
...
...
...
Aqueous/Organic Phase Volume Ratio
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
1.1
1.1
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
LDM
02-028
02-029
02-030
02-031
02-032
02-033
02-034
02-036
02-038
02-040
02-042
02-044
Organic Phase Composition
Monomer (DVB & EVB) Wt. %
45.0
45.0
45.0
45.0
45.0
50.0
55.0
55.0
55.0
55.0
55.0
55.0
Porogen Wt. %
55.0
55.0
55.0
55.0
55.0
50.0
45.0
45.0
45.0
45.0
45.0
45.0
Porogen/Monomer Ratio
1.222
1.222
1.222
1.222
1.222
1.000
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
Benzoyl Peroxide (BPO) Wt. %
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
Porogen Composition
Isooctane, Wt. %
99.274
99.274
99.274
99.274
99.274
99.112
98.915
98.915
98.915
98.915
98.915
98.915
Toluene, Wt. %
0
0
0
0
0
0
0
0
0
0
0
0
Inerts, Wt %
0.726
0.726
0.726
0.726
0.726
0.8878
1.085
1.085
1.085
1.085
1.085
1.085
Toluene, plus Inerts, Wt. %
...
...
...
...
...
...
...
...
...
...
...
...
Isooctane/Toluene plus Inerts Ratio
...
...
...
...
...
...
...
...
...
...
...
...
Aqueous Phase Composition
Sodium Carbonte, Wt. %
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
Sodium Nitrite, Wt. %
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
Poly (N-Vinylpyrrolidione),
0.700
0.900
1.000
1.000
1.500
1.000
0.500
1.300
1.100
1.000
0.200
0.300
Wt. %
PVP K 30, 45–55 Kdaltons,
0.700
0.900
1.000
1.000
1.500
0.9
0
1.000
1.000
0.800
0
0
Wt. %
PVP K 60, 400–500 Kdaltons,
0
0
0
0
0
0.100
0.500
0.300
0.100
0.200
0.200
0.300
Wt. %
Poly (Vinyl alcohol), Wt. %
0
0
0
0
0
0
0
0
0
0
0
0
Molecular Size, Kdaltons
...
...
...
...
...
...
...
...
...
...
...
...
Amount Hydrolized, %
...
...
...
...
...
...
...
...
...
...
...
...
Aqueous/Organic Phase
1.2
1.2
1.145
1.2
1.2
1.1
1.1
1.0
1.0
1.0
1.0
1.0
Volume Ratio
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
LDM
02-047
02-049
02-050
02-052
02-054
02-055
02-059
02-061
02-073
02-074
02-075
02-079
Organic Phase Composition
Monomer (DVB & EVB) Wt. %
55.0
55.0
55.0
55.0
55.0
55.0
55.0
55.0
55.0
55.0
55.0
55.0
Porogen Wt. %
45.0
45.0
45.0
45.0
45.0
45.0
45.0
45.0
45.0
45.0
45.0
45.0
Porogen/Monomer Ratio
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
0.8182
Benzoyl Peroxide (BPO) Wt. %
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
1.03
Porogen Composition
Isooctane, Wt. %
98.915
98.915
98.915
98.915
98.915
98.915
98.915
98.915
98.915
98.915
98.915
98.915
Toluene, Wt. %
0
0
0
0
0
0
0
0
0
0
0
0
Inerts, Wt %
1.085
1.085
1.085
1.085
1.085
1.085
1.085
1.085
1.085
1.085
1.085
1.085
Toluene, plus Inerts, Wt. %
...
...
...
...
...
...
...
...
...
...
...
...
Isooctane/Toluene plus Inerts Ratio
...
...
...
...
...
...
...
...
...
...
...
...
Aqueous Phase Composition
Sodium Carbonte, Wt. %
0.300
0.100
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
0.500
Sodium Nitrite, Wt. %
0.300
0.100
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
0.300
Poly (N-Vinylpyrrolidione),
0.010
0.010
0
0.05
0
0
0
0
0
0
0
0
Wt. %
PVP K 30, 45–55 Kdaltons,
0.010
0.010
0
0.05
0
0
0
0
0
0
0
0
Wt. %
PVP K 60, 400–500 Kdaltons,
0
0
0
0
0
0
0
0
0
0
0
0
Wt. %
Poly (Vinyl alcohol), Wt. %
0.250
0.400
0
0
0
0
0
0.300
0.300
0.300
0.300
0.300
Molecular Size, Kdaltons
95
95
...
...
...
...
170
170
170
170
170
170
Amount Hydrolized, %
95
95
...
...
...
...
88
88
88
88
88
88
Natrosol Plus, Wt. %
0
0
0.500
0.300
0.300
0.300
0
0
0
0
0.05
0
Aqueous/Organic Phase
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
Volume Ratio
Sample
Sample
Sample
ID
ID
ID
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
LDM
02-082
02-083
02-086
ID
ID
ID
ID
ID
ID
ID
ID
ID
Organic Phase Composition
Monomer (DVB & EVB) Wt. %
55.0
55.0
55.0
Porogen Wt. %
45.0
45.0
45.0
Porogen/Monomer Ratio
0.8182
0.8182
0.8182
Benzoyl Peroxide (BPO) Wt. %
1.03
1.03
1.03
Porogen Composition
Isooctane, Wt. %
98.915
98.915
98.915
Toluene, Wt. %
0
0
0
Inerts, Wt %
1.085
1.085
1.085
Toluene, plus Inerts, Wt. %
...
...
...
Isooctane/Toluene plus Inerts Ratio
...
...
...
Aqueous Phase Composition
Sodium Carbonte, Wt. %
0.500
0.500
0.500
Sodium Nitrite, Wt. %
0.300
0.300
0.300
Poly (N-Vinylpyrrolidione),
0
0
0
Wt. %
PVP K 30, 45–55 Kdaltons,
0
0
0
Wt. %
PVP K 60, 400–500 Kdaltons,
0
0
0
Wt. %
Poly (Vinyl alcohol), Wt. %
0.300
0.300
0.3
Molecular Size, Kdaltons
170
88
170
Amount Hydrolized, %
88
85
88
Natrosol Plus, Wt. %
0
0
0
Aqueous/Organic Phase
1.0
1.0
1.0
Volume Ratio
TABLE 7
Experimental Programs: Response
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
Sample
ID
ID
ID
ID
ID
ID
ID
ID
ID
ID
LDM
02-001
02-004
02-006
02-008
02-010
02-017
02-025
02-034
02-036
02-038
Surface Characteristics
SEM; description (smooth,
nodes,
nodes,
nodes,
nodes,
nodes,
no nodes,
no nodes,
no nodes,
no nodes,
nodes,
nodes present, open or
closed
closed
closed
closed
closed
open
open
open
open
closed
closed pore structure)
Internal Pore Stucture
(Dry Beads)
BET Surfrace Area, {overscore (S)}, m 2 g −1
563.5
652.8
615.7
614.4
661.4
520.9
540.0
537.2
556.6
556.6
Porosity, Pwt in ml · g −1
0.9210
1.5370
1.53085
1.7245
1.7722
1.1241
1.3899
1.9069
1.9588
1.8754
Pore modes greater than
150
250,
250
430
490
250, 390,
320, 440
380, 490
210, 280
210, 280,
100 Å diameter from
400
500
550
495 640,
550, 750
620, 930
380, 500,
380 500,
Desorption Isotherm.
920 1400,
1200,
650
650, 930
List each
1900
2900
Pore modes range in Å greater
100–250
100–500
100–600
100–700
100–600
100–2300
100–2900
100–1600
100–1600
100–1600
than 100 Å diameter,
Desorption Isotherm.
Cytochrome C Sorption
Static Assesment 500 mg/
Liter Conc.
Mg Cyto C sorbed/g dry
15.2
43.35
42.95
63.05
79.7
135.0
155.8
86.6
82.0
54.8
polymer at 3 hr contact
% of Cyto C removed from
19.42
53.80
51.46
66.22
73.78
82.64
82.49
85.12
85.26
57.82
solution at 3 hr contact
Serum Albumin Sorption
% removed from solution with
6.1
4.15
4.38
4.9
a concentration of
35,000 mg/l of serum albumin
Mg BSA (or HSA) sorbed/g
681.6
488.22
301.46
311.96
dry polymer at 3 hr contact
Coating Assesment
ESCA Measurements for
Surface Components, Atom
Fraction on surface
C
0.8702
0.8722
0.8917
0.8881
0.8855
0.8613
0.8520
0.8981
0.8682
0.8901
O
0.0784
0.0758
0.0682
0.0729
0.0860
0.1106
0.1480
0.0778
0.0935
0.0771
N
0.0514
0.0520
0.0401
0.0390
0.0284
0.0281
none
0.0241
0.0383
0.0328
detected
Sample ID
Sample ID
Sample ID
Sample ID
Sample ID
Sample ID
Sample ID
Sample ID
Sample ID
LDM
02-040
02-044
02-054
02-055A
02-075
02-079
02-082
02-083
02-086
Surface Characteristics
SEM; description (smooth,
nodes,
nodes,
nodes,
nodes,
nodes,
nodes,
nodes present, open or
closed
closed
closed
closed
closed
closed
closed pore structure)
Internal Pore Stucture
(Dry Beads)
BET Surface Area, {overscore (S)}, m 2 g −1
549.6
545.4
536.8
525.2
531.5
528.9
Porosity, Pwt in ml · g −1
1.8356
1.6420
1.6567
1.6957
1.5232
1.3708
Pore modes greater than 100 Å
300; 390;
250; 310;
280; 350;
290; 390;
200; 310;
210; 280;
diameter from Desorption
500; 650;
450; 550;
460; 600;
500; 640;
410; 530;
380; 490; 620;
Isotherm. List each
950
790; 1200
810; 1900
990
740; 900; 1200
900; 1300
Pore modes range in Å greater
100–1600
100–2000
100–2900
100–1700
100–2400
100–2400
than 100 Å diameter, Desorption
Isotherm.
Cytochrome C Sorption
Static Assesment 500 mg/
Liter Conc.
Mg Cyto C sorbed/g dry
57.7
61.7
73.9
57.8
32.8
61.1
polymer at 3 hr contact
% of Cyto C removed from
61.43
65.55
79.83
63.63
39.00
74.89
solution at 3 hr contact
Serum Albumin Sorption
% removed from solution with
3.07
4.12
a concentration of 35,000 mg/l
of serum albumin
Mg BSA (or HSA) sorbed/g dry
192.10
257.96
polymer at 3 hr contact
Coating Assesment
ESCA Measurements for
Surface Components, Atom
Fraction on surface
C
0.8586
0.8748
0.8238
0.7924
0.8441
0.8830
O
0.0982
0.0897
0.1745
0.2076
0.1559
0.1170
N
0.0432
0.355
none
none
none
none
detected
detected
detected
detected
Numerous modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that within the scope of the attendant claims attached hereto, this invention may be practiced otherwise than as specifically disclosed herein. | A polymer system with a hemocompatible film or coating is provided, the system comprises an organic phase and an aqueous phase, the organic phase comprises polymerizable monomers and at least one initiator and the aqueous phase comprises at least one dispersing agent, at least one free radical inhibitor and at least one buffering agent, the organic phase is immiscible in the aqueous phase, and the dispersing agent forms a hemocompatible surface on the polymer. | 2 |
TECHNICAL FIELD
The present invention relates to vane-type camshaft phasers for varying the phase relationship between crankshafts and camshafts in internal combustion engines; more particularly, to such phasers wherein a locking pin assembly is utilized to lock the phaser rotor with respect to the stator at certain times in the operating cycle; and most particularly, to a phaser having a bias spring system to assist in locking a phaser rotor at a rotational position intermediate between full phaser advance and full phaser retard positions.
BACKGROUND OF THE INVENTION
Camshaft phasers for varying the phase relationship between the crankshaft and a camshaft of an internal combustion engine are well known. A prior art vane-type phaser generally comprises a plurality of outwardly-extending vanes on a rotor interspersed with a plurality of inwardly-extending lobes on a stator, forming alternating advance and retard chambers between the vanes and lobes. Engine oil is supplied via a multiport oil control valve (OCV), in accordance with an engine control module, to either the advance or retard chambers as required to meet current or anticipated engine operating conditions.
In a typical prior art vane-type cam phaser, a locking pin, disengage-able by oil pressure, is slidingly disposed in a bore in a rotor vane to permit rotational locking of the rotor to the stator (or sprocket wheel or pulley) under certain conditions of operation of the phaser and engine. In older prior art phasers, it is desired that the rotor be locked at its parked position at an extreme of the rotor authority, either at the full retard position as in the case of an intake camshaft phaser or at the full advance position as in the case of an exhaust camshaft phaser. To assist in positioning the rotor for lock pin engagement, it is known to incorporate a mechanical stop for the rotor and a torsional bias spring acting between the rotor and the stator to urge the rotor against the stop for locking.
In newer prior art phasers as disclosed in co-pending application having Ser. No. 11/225,772, it is desirable that the rotor be lockable to the stator at an intermediate position, preferably within an increased rotor range of rotational authority. A known problem in such phasers is that there is no mechanical means such as a stop to assist in positioning the rotor for locking in an intermediate position; thus, locking is not reliable, and an unacceptably high rate of locking failures may occur.
Further, in prior art phasers, the torsion spring may generate an unwanted torque on the rotor about an axis orthogonal to the rotor axis, causing the rotor to become slightly cocked within the stator chamber before the phaser is installed onto the end of a camshaft during engine assembly. This cocking is permitted by necessary clearances between the rotor and the stator. Although relatively slight, such cocking can be large enough to prohibit entry of the camshaft into the rotor during engine assembly.
What is needed in the art is an improved vane-type camshaft phaser having additional range of rotational authority wherein the rotor may be reliably locked to the stator at an intermediate position within the range of authority.
What is further needed in the art is an improved vane-type camshaft phaser wherein the rotor of an assembled phaser may be reliably entered onto the end of a camshaft during engine assembly.
It is a principal object of the present invention to cause a rotor lock pin to be properly positioned for engagement with a stator.
It is a further object of the present invention to increase the reliability of entry of the rotor of an assembled phaser onto an engine camshaft during engine assembly.
SUMMARY OF THE INVENTION
Briefly described, a vane-type camshaft phaser in accordance with the invention for varying the timing of combustion valves in an internal combustion engine includes a rotor having a plurality of vanes disposed in a stator having a plurality of lobes, the interspersion of vanes and lobes defining a plurality of alternating valve timing advance and valve timing retard chambers with respect to the engine crankshaft. The rotational authority of the rotor within the stator with respect to top-dead-center of the crankshaft is preferably between about 40 crank degrees before TDC (valve timing advanced) and about 20 crank degrees after TDC (valve timing retarded). It is generally desirable that an engine be started at a camshaft position of about 10 crank degrees valve retard. Thus, an improved phaser in accordance with the present invention includes a lock pin seat formed in the stator at the appropriate position of intermediate rotation and a locking pin slidably disposed in a vane of the rotor for engaging the seat to lock the rotor at the intermediate position for engine starting.
A pre-loaded bias spring system disposed on the phaser cover plate urges the rotor toward the locking position from any rotational position retarded of the locking position. When the rotor is moving in a phase-advance direction, at or near the rotor locking position the bias spring system becomes disengaged from the rotor. When the rotor is moving in a phase-retard direction, at or near the rotor locking position the bias spring system is engaged, causing the rotor to decelerate and thereby increasing the reliability of locking.
Two embodiments of such a bias spring system are presented, one comprising a torsion spring and the other comprising a pair of compression springs. In each embodiment, the phaser may be assembled without having the spring system coupled to the rotor, thereby overcoming the rotor cocking problem inherent in prior art phasers and assuring reliable mounting of an assembled phaser onto a camshaft during engine assembly.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is an elevational cross-sectional view of a prior art vane-type camshaft phaser, showing direct entry of an engine camshaft into a rotor, and also showing an internal torsion bias spring for biasing the rotor to a fully retarded position within the stator;
FIG. 1 a is an exploded isometric view of a partial cam phaser including the pulley/sprocket, the stator, the rotor and the locking pin mechanism.
FIG. 2 is a plan view of an improved camshaft phaser showing a first embodiment of a bias spring system in accordance with the invention;
FIG. 3 is an isometric view of the phaser and bias spring system shown in FIG. 2 ;
FIG. 4 is an exploded isometric view of an improved camshaft phaser showing a second embodiment of a bias spring system in accordance with the invention;
FIG. 5 is an assembled view of the phaser shown in FIG. 4 ; and
FIG. 6 is a cutaway isometric view from below of a portion of the second embodiment shown in FIGS. 4 and 5 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 , a typical prior art vane-type camshaft phaser 10 includes a pulley or sprocket 12 for engaging a timing chain or belt (not shown) operated by an engine crankshaft (not shown). A stator 14 is disposed against pulley/sprocket 12 and is rotationally immobilized with respect to pulley/sprocket 12 . Stator 14 is provided with a central chamber 16 for receiving a rotor 18 having a hub 20 . Hub 20 is provided with a recess 22 that is coaxial with a central bore 24 in pulley/sprocket 12 , allowing access of an end of engine camshaft 26 into rotor hub 20 during mounting of phaser 10 onto an internal combustion engine 27 during assembly thereof. Central chamber 16 is closed by a cover plate 28 , forming advance and retard chambers between the rotor and the stator in chamber 16 . A rotor hub extension 30 is pressed into a recess in rotor hub 20 and extends rotatably through a central opening in cover plate 28 . A target wheel 32 is mounted onto rotor hub extension 30 by an axial mounting bolt (not shown) that attaches phaser 10 to camshaft 26 during assembly of engine 27 . Thus target wheel 32 turns with and is indicative of the rotational position of rotor 18 and camshaft 26 . Cover plate 28 and stator 14 are secured to pulley/sprocket 12 via a plurality of binder screws 34 extending through stator 14 outside of chamber 16 . A torsional bias spring 36 is disposed coaxially of rotor hub extension 30 , having a first tang 38 anchored to sprocket/pulley 12 , as for example, by engagement with the protruding head of a binder screw 34 , and having a second tang 40 anchored to rotor 18 , as for example, by engagement with a stop 42 on target wheel 32 . Bias spring 36 is pre-loaded between the rotor and stator during assembly of phaser 10 to urge rotor 18 toward the full operational retard position within chamber 16 , thereby causing the rotor cocking problem described above.
Referring now to FIG. 1 a , locking pin mechanism 44 comprises locking pin 46 having annular shoulder 47 , return spring 48 , and bushing 49 . Spring 48 is disposed inside pin 46 , and bushing, pin, and spring are received in a longitudinal bore 50 formed in oversized vane 52 of rotor 18 , an end of pin 46 being extendable by spring 48 from the underside of the vane. A pin seat 54 is formed in the inside surface of pulley/sprocket 12 for receiving an end portion of pin 46 when extended from bore 50 to rotationally lock rotor 18 to pulley/sprocket 12 and, hence, stator 14 . The operation of locking mechanism 44 is described in co-pending application Ser. No. 11/225,772. Note that, by angularly positioning bore 54 on the inside surface of pulley/sprocket 12 , within the range of rotational authority 56 of rotor 18 , engagement of the locking mechanism can cause the rotor to be locked in its full retard position ( 54 a ), its full advance position ( 54 c ), or any intermediate position ( 54 b ) therebetween.
Referring now to FIGS. 2 and 3 , a first embodiment 110 of an improved camshaft phaser in accordance with the invention includes an improved bias spring system 136 that replaces prior art torsional bias spring 36 . System 136 comprises at least one compression spring assembly 160 disposed on cover plate 128 and a torque arm 162 mounted for rotation with a phaser rotor (not visible in FIGS. 2 and 3 ) as by being secured thereto by a nut 164 screwed onto a threaded stud 165 extending from a phaser mounting bolt. (A conventional target wheel, not shown, also may be mounted by obvious means onto stud 165 .) Compression spring assembly 160 comprises a coil spring 166 mounted in a bore formed in a housing 168 on cover plate 128 and having a plunger 170 extending therefrom for engagement with torque arm 162 . Housing 168 is rotationally formed on cover plate 128 , and torque arm 162 is rotationally positioned on the rotor after the phaser is installed onto a camshaft, such that in all positions of rotor advance phase angle (advance direction 172 ) from the position shown in FIGS. 2 and 3 , rotor motion is not influenced by bias spring system 136 because torque arm 162 is moving away from plunger 170 . However, in all positions of rotor retard phase angle (retard direction 174 ) from the position shown in FIGS. 2 and 3 , rotor motion is influenced by bias spring system 136 because torque arm 162 is engaged by spring-loaded plunger 170 . In a currently preferred embodiment, the position of the rotor and torque arm shown in FIGS. 2 and 3 , wherein retard motion of the torque arm is braked by bias spring system 136 , corresponds to the intermediate locking position ( 54 b in FIG. 1 a ) of an internal lock pin system (not visible in FIGS. 2 or 3 ). Further in a currently preferred embodiment, the intermediate locking position separates the rotor range of authority into a phase-advance range ( 58 b in FIG. 1 a ) and a phase-retard range ( 58 a in FIG. 1 a ), and a bias spring system in accordance with the invention is engageable with the rotor only within the phase-retard range.
Thus, in operation bias spring system 136 creates a time window wherein the lock pin and seat are roughly aligned for locking. Bias spring system 136 is active only in retard modes of phaser operation, wherein system 136 will always tend to return the rotor to its locking position when the retard mode is deactivated. Further, bias spring system 136 cannot cause the undesirable rotor cocking described above in prior art phasers. Preferably, improved phaser 110 is assembled and installed with the rotor in a locked position within the stator, and then torque arm 162 is secured in position against plungers 170 by nut 164 .
In a presently preferred embodiment, improved bias spring system 136 comprises two torque arms 162 disposed 180° apart and two compression spring assemblies 160 disposed 180° apart, as shown in FIGS. 2 and 3 , which arrangement imposes a balanced torque on the rotor in operation.
Referring now to FIGS. 4 through 6 , a second embodiment 210 of an improved camshaft phaser in accordance with the invention includes an improved bias spring system 236 that replaces prior art torsional bias spring 36 . In spring system 236 , the torsion bias spring is mounted substantially as shown for prior art spring 36 in FIG. 1 . Spring 236 is mounted on rotor hub extension 230 , and first tang 238 engages a bolt head 34 to ground the spring to sprocket 12 . However, in an improvement over prior art spring system 36 , a spring stop 280 extends from cover plate 228 toward modified target wheel 232 for engaging second spring tang 240 . Stop 280 is located radially inboard of target wheel modified stop 242 . Further, stop 280 is located substantially coaxially with the locking position of an internal lock pin system (not visible). Thus the torsion spring as installed, and shown in FIG. 4 , is grounded at both tangs 238 , 240 to the cover plate and exerts no torque or cocking moment on the rotor hub extension 230 or the rotor, permitting reliable installation of the improved phaser 210 onto a camshaft end 26 during assembly of engine 27 ( FIG. 1 ). During such installation, after the phaser is positioned on the camshaft end, target wheel 232 is installed over spring 236 and rotated counterclockwise (retard direction 274 ) until stop 242 engages second spring tang 240 outboard of spring stop 280 . The camshaft mounting bolt (not shown) is then tightened, fixing the rotational relationship between stop 280 , second tang 240 , and target wheel stop 242 .
The operational characteristics of improved phaser 210 are identical with those of improved phaser 110 as previously described. In operation, during all phase-advance modes ( 58 a in FIG. 1 a ), target wheel stop 242 is not engaged with second tang 240 , and thus spring 236 has no influence on motion of the rotor. As in first embodiment 110 , in all positions of rotor retard phase angle (retard direction 274 ) from the position shown in FIGS. 4 and 6 rotor motion is influenced by bias spring system 236 because second tang 240 is engaged by target wheel stop 242 . As noted above, the position of the target wheel and second tang shown in FIGS. 4 and 6 , wherein retard motion of the rotor is braked by bias spring system 236 , corresponds to the locking position of an internal lock pin system (not visible) into the stator. Thus, bias spring system 236 creates a time window where the lock pin and seat are roughly aligned for locking. Bias spring system 236 is active only in retard modes of phaser operation, wherein the spring system will always tend to return the rotor to its locking position when the retard mode is deactivated.
While the invention has been described by reference to various specific embodiments, it should be understood that numerous changes may be made within the spirit and scope of the inventive concepts described. Accordingly, it is intended that the invention not be limited to the described embodiments, but will have full scope defined by the language of the following claims. | A vane-type camshaft phaser for varying the timing of combustion valves in an internal combustion engine includes a seat formed in the sprocket at the appropriate position of intermediate rotation and a locking pin slidably disposed in a vane of the rotor for engaging the seat to lock the rotor at the intermediate position. A bias spring system disposed on a cover plate urges the rotor toward the locking position from any position retarded of the locking position. A first spring system embodiment comprises a pair of compression spring assemblies. A second spring system embodiment comprises an internal torsion spring. In each embodiment, the phaser may be assembled without having the spring system coupled to the rotor, thereby overcoming a rotor cocking problem inherent in prior art phasers, assuring reliable mounting of an assembled phaser onto an engine camshaft. | 5 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a non-provisional of U.S. Provisional Patent Application Ser. No. 61/552,362, filed Oct. 27, 2011, which is incorporated by reference and to which priority is claimed.
[0002] The present application is related to U.S. Pat. No. 8,155,752 (the '752 patent).
FIELD OF THE INVENTION
[0003] This application relates to improved circuitry for an implantable medical device having a single coil for both telemetry and power reception.
BACKGROUND
[0004] Implantable stimulation devices generate and deliver electrical stimuli to nerves and tissues for the therapy of various biological disorders, such as pacemakers to treat cardiac arrhythmia, defibrillators to treat cardiac fibrillation, cochlear stimulators to treat deafness, retinal stimulators to treat blindness, muscle stimulators to produce coordinated limb movement, spinal cord stimulators to treat chronic pain, cortical and deep brain stimulators to treat motor and psychological disorders, occipital nerve stimulators to treat migraine headaches, and other neural stimulators to treat urinary incontinence, sleep apnea, shoulder subluxation, etc. The present invention may find applicability in all such applications and in other implantable medical device systems, although the description that follows will generally focus on the use of the invention in a Bion® microstimulator device system of the type disclosed in U.S. Patent Publ. No. 2010/0268309. However, the invention can also be used in a Spinal Cord Stimulator (SCS), such as is disclosed in U.S. Pat. No. 7,444,181, for example.
[0005] Microstimulator devices typically comprise a small, generally-cylindrical housing which carries electrodes for producing a desired stimulation current. Devices of this type are implanted proximate to the target tissue to allow the stimulation current to stimulate the target tissue to provide therapy for a wide variety of conditions and disorders. A microstimulator usually includes or carries stimulating electrodes intended to contact the patient's tissue, but may also have electrodes coupled to the body of the device via a lead or leads. A microstimulator may have two or more electrodes. Microstimulators benefit from simplicity. Because of their small size, the microstimulator can be directly implanted at a site requiring patient therapy.
[0006] FIG. 1 illustrates an exemplary implantable microstimulator 100 . As shown, the microstimulator 100 includes a power source 145 such as a battery, a programmable memory 146 , electrical circuitry 144 , and a coil 147 . These components are housed within a capsule 202 , which is usually a thin, elongated cylinder, but may also be any other shape as determined by the structure of the desired target tissue, the method of implantation, the size and location of the power source 145 , and/or the number and arrangement of external electrodes 142 . In some embodiments, the volume of the capsule 202 is substantially equal to or less than three cubic centimeters.
[0007] The battery 145 supplies power to the various components within the microstimulator 100 , such the electrical circuitry 144 and the coil 147 . The battery 145 also provides power for therapeutic stimulation current sourced or sunk from the electrodes 142 . The power source 145 may be a primary battery, a rechargeable battery, a capacitor, or any other suitable power source. Systems and methods for charging a rechargeable battery 145 will be described further below.
[0008] The coil 147 is configured to receive and/or emit a magnetic field that is used to communicate with, or receive power from, one or more external devices that support the implanted microstimulator 100 , examples of which will be described below. Such communication and/or power transfer may be transcutaneous as is well known.
[0009] The programmable memory 146 is used at least in part for storing one or more sets of data, including electrical stimulation parameters that are safe and efficacious for a particular medical condition and/or for a particular patient. Electrical stimulation parameters control various parameters of the stimulation current applied to a target tissue including the frequency, pulse width, amplitude, burst pattern (e.g., burst on time and burst off time), duty cycle or burst repeat interval, ramp on time and ramp off time of the stimulation current, etc.
[0010] The illustrated microstimulator 100 includes electrodes 142 - 1 and 142 - 2 on the exterior of the capsule 202 . The electrodes 142 may be disposed at either end of the capsule 202 as illustrated, or placed along the length of the capsule. There may also be more than two electrodes arranged in an array along the length of the capsule. One of the electrodes 142 may be designated as a stimulating electrode, with the other acting as an indifferent electrode (reference node) used to complete a stimulation circuit, producing monopolar stimulation. Or, one electrode may act as a cathode while the other acts as an anode, producing bipolar stimulation. Electrodes 142 may alternatively be located at the ends of short, flexible leads. The use of such leads permits, among other things, electrical stimulation to be directed to targeted tissue(s) a short distance from the surgical fixation of the bulk of the device 100 .
[0011] The electrical circuitry 144 produces the electrical stimulation pulses that are delivered to the target nerve via the electrodes 142 . The electrical circuitry 144 may include one or more microprocessors or microcontrollers configured to decode stimulation parameters from memory 146 and generate the corresponding stimulation pulses. The electrical circuitry 144 will generally also include other circuitry such as the current source circuitry, the transmission and receiver circuitry coupled to coil 147 , electrode output capacitors, etc.
[0012] The external surfaces of the microstimulator 100 are preferably composed of biocompatible materials. For example, the capsule 202 may be made of glass, ceramic, metal, or any other material that provides a hermetic package that excludes water but permits passage of the magnetic fields used to transmit data and/or power. The electrodes 142 may be made of a noble or refractory metal or compound, such as platinum, iridium, tantalum, titanium, titanium nitride, niobium or alloys of any of these, to avoid corrosion or electrolysis which could damage the surrounding tissues and the device.
[0013] The microstimulator 100 may also include one or more infusion outlets 201 , which facilitate the infusion of one or more drugs into the target tissue. Alternatively, catheters may be coupled to the infusion outlets 201 to deliver the drug therapy to target tissue some distance from the body of the microstimulator 100 . If the microstimulator 100 is configured to provide a drug stimulation using infusion outlets 201 , the microstimulator 100 may also include a pump 149 that is configured to store and dispense the one or more drugs.
[0014] Turning to FIG. 2 , the microstimulator 100 is illustrated as implanted in a patient 150 , and further shown are various external components that may be used to support the implanted microstimulator 100 . An external controller 155 may be used to program and test the microstimulator 100 via communication link 156 . Such link 156 is generally a two-way link, such that the microstimulator 100 can report its status or various other parameters to the external controller 155 . Communication on link 156 occurs via magnetic inductive coupling. Thus, when data is to be sent from the external controller 155 to the microstimulator 100 , a coil 158 in the external controller 155 is excited to produce a magnetic field that comprises the link 156 , which magnetic field is detected at the coil 147 in the microstimulator. Likewise, when data is to be sent from the microstimulator 100 to the external controller 155 , the coil 147 is excited to produce a magnetic field that comprises the link 156 , which magnetic field is detected at the coil 158 in the external controller. Typically, the magnetic field is modulated, for example with Frequency Shift Keying (FSK) modulation or the like, to encode the data. For example, data telemetry via FSK can occur around a center frequency of 125 kHz, with a 129 kHz signal representing transmission of a logic ‘1’ and 121 kHz representing a logic ‘0’.
[0015] An external charger 151 provides power used to recharge the battery 145 ( FIG. 1 ). Such power transfer occurs by energizing the coil 157 in the external charger 151 , which produces a magnetic field comprising link 152 . This magnetic field 152 energizes the coil 147 through the patient 150 's tissue, and which is rectified, filtered, and used to recharge the battery 145 . Link 152 , like link 156 , can be bidirectional to allow the microstimulator 100 to report status information back to the external charger 151 . For example, once the circuitry 144 in the microstimulator 100 detects that the power source 145 is fully charged, the coil 147 can signal that fact back to the external charger 151 so that charging can cease. Charging can occur at convenient intervals for the patient 150 , such as every night.
[0016] FIG. 3A shows the circuitry within microstimulator 100 that is coupled to coil 147 . Such circuitry is explained in detail in the '752 patent that was incorporated by reference above. Therefore, the circuitry is only briefly explained here.
[0017] As explained in the '752 patent, the circuitry of FIG. 3A is beneficial because it uses a single coil L 1 ( 147 ) receiving a magnetic charging field 152 from the external charger 151 , and for transmitting and receiving data telemetry 156 to and from the external controller 155 . (The external charger 151 and external controller 155 are shown in FIG. 3A as one integrated unit for simplicity).
[0018] Coil 147 is connected at one end through transistor switch M 1 to a voltage, Vbat, provided by the battery 145 in the microstimulator 100 , which may ranges from 2.5V to 4.2 Volts. Coil 147 is connected at its other end through transistor switch M 2 to ground. Capacitor C 1 is connected in parallel with coil 147 , thus forming a resonant tank circuit, and tunes the tank circuit to a particular frequency for transmitting or receiving data telemetry to and from the external controller 155 (e.g., approximately 125 kHz). A series combination of a capacitor C 2 and transistor switch M 3 are also connected in parallel to coil 147 . Transistor M 3 is turned on during receipt of a magnetic charging field along link 152 from the external charger 151 to tune the tank circuit to the frequency of the magnetic charging field (e.g., approximately 80 kHz). Also connected in parallel with coil 147 is a full bridge rectifier represented by diodes D 1 -D 4 for producing DC voltage Vout. A half bridge rectifier could also be used. Diodes D 1 -D 4 may comprise, for example, Schottky diodes having forward voltage drops of approximately 0.4V. A transistor switch M 4 is also connected between the rectifier circuitry and ground.
[0019] DC voltage Vout is received at storage capacitor C 3 , which smooths the voltage before being passed to charging circuitry 92 . Charging circuitry 92 is used to charge battery source 145 in a controlled fashion. If needed, a Zener diode D 5 or other suitable voltage clamp circuit may be connected across capacitor C 3 to prevent Vout from exceeding some predetermined value, e.g., 6.2V.
[0020] FIG. 3B shows the status of transistor switches M 1 -M 4 for the energy receive, data receive, and data transmit modes. As shown, to operate in an energy receive mode, the circuit will turn switches M 1 , M 2 and M 4 OFF, and will turn switch M 3 ON. Turning M 3 ON includes capacitor C 2 in parallel with capacitor C 1 , which, in conjunction with the inductance formed by the coil 147 , forms a resonant circuit which is tuned to the frequency of the magnetic charging field. The circuit of FIG. 3A may also operate in a data transmit mode during charging by employing back telemetry known as Load Shift Keying (LSK), in which case transistor M 4 is modulated with the data to be transmitted back to the external charger 151 . Switches M 1 -M 4 is typically standard semiconductor switches, such as MOSFET switches.
[0021] For the circuit of FIG. 3A to operate in a data receive mode, the circuit will turn switches M 1 , M 3 and M 4 OFF, and will turn switch M 2 ON. Turning M 3 off excludes capacitor C 2 from the resonant circuit, whose tuning is thus governed by coil 147 and capacitor C 1 . With capacitor C 2 excluded, the resonant circuit is tuned to a higher frequency matching the operation of the external controller 155 . Turning M 2 ON grounds the resonant circuit, which provides an input to the receiver, which demodulates the received data (DATA RCV). The receiver can either comprise a differential input as illustrated in solid lines in FIG. 3A , or can comprise a single-ended non-differential input in which one of the inputs is grounded, as shown by the dashed line in FIG. 3A .
[0022] As further shown in FIG. 3B , the circuit of FIG. 3A may also operate in a data transmit mode by turning switches M 3 and M 4 OFF, by modulating switch M 2 with a data signal (DATA XMIT), and by turning switch M 1 ON. Under these conditions, the resonant circuit is once again, by virtue of transistor M 3 being OFF, tuned to the higher frequency, and will broadcast a signal to the external control unit 151 / 155 along link 156 accordingly, with the energy for the radiation being supplied from the battery voltage, Vbat, via transistor M 1 . The transmitter receiving the data to be transmitted (DATA XMIT), is shown coupled to transistor M 2 , but could also couple to transistor M 1 .
[0023] Thus, it is seen that by selectively controlling the state of the switches M 1 -M 4 , the circuit of FIG. 3A may operate in different modes, using only a single coil 147 . Such modes may be invoked in a time-multiplexed manner, e.g., with a first mode being followed by a second mode, depending upon the particular application at hand. Control signals M 1 -M 4 , as well as DATA XMIT, are ultimately issued by a microcontroller 160 in the microstimulator 100 , and DATA RCV is received by that microcontroller.
[0024] The inventors have noticed that integrating such functionality into a circuit with only one coil 147 presents technical challenges. For one, it is difficult to operate a MOSEFT switch M 1 during the energy receive mode because of the large swing in AC voltage produced at the drain of transistor M 1 (node X in FIG. 3A ). During the energy receive mode, transistors M 1 and M 2 are off, thus decoupling the coil 147 from Vbat and ground. As a result, the AC voltage across the coil 147 is somewhat indeterminate, but will still be bounded by the various diodes in the circuit. For example, the maximum voltage at node X will be determined by the threshold voltage of diode D 3 and the breakdown voltage of Zener diode D 5 . Assuming low-threshold-voltage Schottky diodes in the rectifier (Vts=0.4V) and a breakdown voltage in the Zener diode D 5 of 6.2V, node X will not exceed 6.6 Volts or so. At node Y, i.e., the drain of switch M 2 , the voltage is clamped by diode D 2 , such that node Y cannot drop below its threshold, i.e., −0.4V. Therefore, in accordance with the nature of the AC circuitry, the voltages at nodes X and Y will vary from −0.4V to 6.6V during the energy receive mode.
[0025] FIG. 3C shows switches M 1 and M 2 in cross section to better appreciate the problems of the prior art circuitry of FIG. 3A . Assuming switch M 2 is an N-channel silicon MOSFET device as indicated by the p/n doped regions, there is no concern of leakage through that switch in the energy receive mode. The body diode B 2 in switch M 2 will have threshold voltage of about Vt=0.6V or so. Therefore, even at lower voltages present at node Y (i.e., −0.4 V), body diode B 2 will not become forward biased and conduct; again, it is clamped and prevented from going below this voltage by Schottky diode D 2 . (It is assumed that the substrate of switch M 2 is tied to its source and is thus held at ground, i.e., Vsub 2 =0V). Thus, there is no risk of inadvertent leakage from a traditional silicon MOSFET switch M 2 , and that transistor can be turned off as is desired in the energy receive mode.
[0026] By contrast, these same voltages at node X do present a leakage problem in switch M 1 . There is no means for clamping the voltage at node X akin to diode D 2 . Moreover, the substrate of switch M 1 is typically connected to its source, Vbat (i.e., Vsub 1 =Vbat). As such, the body diode B 1 in switch M 1 will leak when the voltage at node X is less than Vbat−Vt. Given typical voltage ranges of 2.5V<Vbat<4.2V, body diode B 1 will become forward biased when node X is at lower voltages, for example from −0.4V to perhaps 3V or so. This at least partially defeats the operation of switch M 1 , which is supposed to be off at all times during the energy receive mode. Worse, because the substrate of switch M 1 is tied to Vbat, such leakage will occur directly from the battery 145 . This is contrary to the desired purpose of the energy receive mode—which is to charge the battery−and also defeats the charging circuitry 92 ( FIG. 3A ), which is meant to isolate the battery during the energy receive mode and control its charging.
[0027] Better means of switching are possible in lieu of a traditional MOSFET switch M 1 , but would involve the use of multiple transistors, and more complicated means of control, such as the use of non-standard signals levels to control such transistors. Thus, a better solution is needed to support the sort of single-coil multi-function communication circuitry of FIG. 3A , and a solution is provided in this disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 shows a microstimulator of the prior art.
[0029] FIG. 2 shows a microstimulator of the prior art as implanted in a patient, as well as an external controller and an external charger.
[0030] FIGS. 3A-3C show the communication and charging circuitry in the microstimulator of the prior art, and the various modes in which such circuitry can be operated.
[0031] FIGS. 4A and 4B show the communication and charging circuitry in a microstimulator in accordance with an embodiment of the invention using an opto-switch, as well as the various modes in which such circuitry can be operated.
[0032] FIG. 5 shows further details of one example of an opto-switch useable in an embodiment of the invention.
DETAILED DESCRIPTION
[0033] Improved circuitry for an implantable medical device is disclosed that utilizes an “opto-switch” (i.e., an optically-isolated switch, such as a photocoupler) that allows for a single coil to be used safely and reliably for both charging and communication.
[0034] Opto-switches use light waves to provide switching control with electrical isolation between the photocoupler's input (its gating signal) and its output (the two terminal of the switch). An exemplary opto-switch contains a source of light (e.g., a near infrared light-emitting diode (LED)) controlled by an electrical gating control signal; an optical channel for transmitting that light; and a photosensor for receiving that light and shorting the two terminals of the switch. In other words, the gating control signal is optically coupled to the photosensor, thus controlling the opto-switch. The photosensor can be, for example, a photoresistor, a photodiode, a phototransistor, a silicon-controlled rectifier (SCR), or a triac. An opto-switch allows use of a low voltage gating control signal irrespective of the voltages at its output because the control signal is electrically decoupled from those output voltages.
[0035] The inventors have realized that such a non-semiconductor-based switch is beneficial when gating AC signals in a resonant tank circuit, such as in the single-coil multi-function telemetry and energy receive circuitry of FIG. 3A , and such an improvement is shown in the improved microstimulator 200 of FIG. 4A . Similar to the single-coil circuitry of FIG. 3A , the single-coil circuitry of FIG. 4A can receive and transmit data, and can receive power for charging the implantable medical device. New to the circuitry of FIG. 4A is the use of an opto-switch M 1 ′, which is controlled by gating control signal, Ictrl, which is electrically decoupled from the voltages on the output side of M 1 ′, i.e., from Vbat and node X. As noted earlier, node X is subject to large voltage swings, particularly in the energy receive mode when M 1 ′ is off. By electrically isolating node X from its gating control signal Icntl in the opto-switch M 1 ′, this switch is easier to control. Moreover, the opto-switch M 1 ′ is not subject to leakage regardless of the voltage level at node X.
[0036] FIG. 4B shows the status of switches M 1 ′, M 2 , M 3 and M 4 when placing the improved microstimulator 200 in data transmit, data receive, and energy receive modes, and to tune the resonance of the tank circuit. These switches operate as before, including the opto-switch M 1 ′, which is OFF during the energy receive mode, OFF during the data receive mode, and ON during the data transmit mode. Because the opto-switch M 1 ′ is different from the MOSFET switches M 2 , M 3 , and M 4 , its gating control signal Ictrl may also differ, but is simple to generate. For example, it may only be necessary to provide a small voltage, Vctrl, at the input of the opto-switch M 1 ′, which voltage is sufficient to forward bias the LED in the opto-switch and turn it on. A simple regulator circuit can be used to derive Vctrl if necessary. As before, the control signals for the switches can come from microcontroller 160 . As the basic operation of the circuitry has not changed from its description in the Background, such operation is not repeated here.
[0037] FIG. 5 shows the internal circuitry of an exemplary opto-switch that can be used for switch M 1 ′, which can comprise for example TOSHIBA® Photocoupler Photo Relay, Toshiba Part No. TLP3231. This opto-switch is relatively small, measuring about 4.2×2.0×1.8 mm in volume, which is suitably small for inclusion inside an implantable medical device. Terminals 1 and 2 of opto-switch M 1 ′ receive the gating control signal, Ictrl, which causes LED 94 to emit light 95 through the optical channel inside the switch.
[0038] This light is received by two serially-connected photo-sensitive MOSFET transistors 97 a and 97 b which act as the photosensor. When illuminated, these normally “off” transistors 97 a and 97 b are turned “on.” In other words, transistors 97 a and 97 b are normally open between Terminals 3 and 4 , but become a short circuit when illuminated by the LED 94 . These transistors 97 a and 97 b are thus completely electrically isolated from the gating control signal, Ictrl, making M 1 switch easier to control even though subject to varying AC voltages at its output terminals.
[0039] Moreover, the two transistors in the opto-switch M 1 are coupled “back to back,” resulting in two body diodes B 3 and B 4 which are back to back. Thus, and unlike the traditional MOSEFT switch M 1 of the prior art ( FIG. 3A ), opto-switch M 1 ′ cannot leak to the substrate: regardless of the voltage at node X, at least one of the body diodes B 3 or B 4 will be reversed biased, thus preventing leakage.
[0040] Modifications to the circuitry of FIG. 4A , and the opto-switch M 1 ′, are possible. For example, it is not strictly necessary that the opto-switch M 1 ′ occur on the high side of the coil 147 proximate to Vbat. With modification to the polarity of the circuit, the opto-switch could also occur on the low side of the circuit proximate to ground. Opto-switches could also be used in lieu of both of traditional MOSFET switches M 1 and M 2 , although as explained earlier using an opto-switch for switch M 2 is not necessary, at least in the context of the particular circuit of FIG. 4A . It is not strictly necessary that the transmitter be coupled to switch M 2 ; it could also be coupled to the opto-switch M 1 ′ at the high end of the circuit. Finally, while an opto-switch is particularly preferred to provide isolation between the switch's input and output, the mere use of back-to-back transistors could be used without optical coupling to its gating control input. That is, traditional electrical signals could be provided to the gates of the back-to-back transistors, although this may require the use of more complicated control signals. Still other modifications are possible.
[0041] Although illustrated as useful in the single-coil, multi-function communication circuitry of FIG. 4A , it should be noted that opto-switches can be used in connection with other types of communication circuitry present in an implantable medical device. In short, an opto-switch may be used in any such communication circuitry in which it is desirable to isolate AC voltages in the tank circuitry from the control for that circuit. One or more opto-switches may for example be used with a resonant tank circuit in which the coil and capacitor are serially connected.
[0042] While the invention herein disclosed has been described by means of specific embodiments and applications, numerous modifications and variations could be made thereto by those skilled in the art without departing from the literal or equivalent scope of the inventions set forth in the claims. | Combination charging and telemetry circuit for use within an implantable medical device uses a single coil for both charging and telemetry that is controlled via the use of an opto-switch. One or more capacitors are used to tune the coil to different frequencies for receiving power from an external device and for the telemetry of information to and from an external device. The opto-switch is coupled to the resonant circuit, but because its input is electrically decoupled from its output, it easy to control. | 0 |
STATEMENT OF GOVERNMENT INTEREST
The invention described herein may be manufactured and used by or for the Government for governmental purposes without the payment of any royalty thereon.
BACKGROUND OF THE INVENTION
This invention relates generally to weapon simulators, and, more particularly to a gun simulator system which contains a laser and is readily adaptable for use in an aircraft. Additionally, the system is capable of incorporating trajectory as well as range information in order to provide a more accurate simulation.
In today's military environment it is necessary for combat air crew to maintain a high degree of combat effectiveness. To keep this fine edge of combat readiness, it is desirable to establish and maintain realistic training programs. Such training programs, in order to be effective, must promote participation by the combatants. For example, todays fighter pilot must develop skills that will not only allow him to successfully maneuver his weapon platform in an air-to-air engagement, but also to effectively identify and destroy assigned ground targets.
An effective means of training todays figher pilot outside of the classroom is the air-to-air and air-to-ground engagement simulation. Such simulation takes place at electronic warfare ranges which provide the pilot with as near perfect electronic simulation of surface-to-air and air-to-air combat engagements as it is possible, short of actual missile launch and active anti-aircraft gun fire. By providing the most realistic ground based threat signals available, it is possible to simulate those violent interreactions of weapon systems in combat.
One type of training involves gunnery ranges which utilize cloth targets with acoustic detection devices that can detect the supersonic airblast created as fired projectiles pass through the cone of detection. Since this cone of detection is approximately the same dimensions as the targets, an accurate count of each bit can be recorded. This reading is transmitted via radio to each pilot as a score after each target pass. Unfortunately, this type of training may involve some danger and in addition is extremely expensive.
As an alternative, laser gun simulator systems have been utilized in the training of combat troops. For example, the U.S. Army's "Multiple Integrated Laser Engagement System" (MILES) is made up of a series of lasers mounted on various infantry and motorized armor. Each type of weapon associated with a particular laser is pulse coded. Each person and weapon system is equipped with a series of laser detectors mounted, for example, on a lightweight belt. The belt or harness is worn by the man and attached by convenient securing means to the vehicles. Each type of system (man, tank, truck, etc.) has a code in its receiving system that will respond to a hit by a weapon of sufficient size to cause damage or destruction. If a weapon of smaller size is fired against such a target (such as M-16 rifle against a M-60 tank), no damage or kill response is generated by the receiver. Unfortunately, this type of system fails to provide complete safety of operation and in addition does not take into account various parameters of actual battlefield conditions, such as, for example, the trajectory of ammunition fired during simulation. Consequently, although effective to some degree, laser gun simulator systems of the past left much to be desired in providing the required accuracy and safety for adequate training.
SUMMARY OF THE INVENTION
The instant invention overcomes the problems encountered in the past by providing a laser gun simulator system which, although utilizing a laser, is completely eye safe as well as capable of incorporating therein trajectory, range, and approach angle information.
The gun simulator system of this invention is readily adaptable for use within conventional aircraft. The gun simulator system is easily mounted in a pod that would attach to an aircraft missile rail or other external mount. The laser gun utilized with the system of this invention is self-contained requiring only normal aircraft voltages for operation and a "fire" command input. When commanded by the pilot, the laser gun would "fire" for as long as a manual preset rounds available counter permitted, and at a rate consistent with real gun specifications. The entire system would be capable of being reset for further passes. Thus, gunnery practice could continue for as long as aircraft fuel and range time permitted.
The gun simulator system of this invention is made up of a laser as well as its associated electronics. The pulses emitted by the laser (or laser gun) are reflected from a target. In operation, the laser gun fires a first laser "round" made up of a plurality of pulses for determining range. That is, the plurality of laser "range" pulses are sent out in a "fanned" fashion at a preset angular displacement to the target. If a "range" pulse hits the target, the laser pulse is reflected and received by the airborne laser receiver. Actual range is calculated by a microprocessor within the system as a function of the round trip time it took that pulse to travel to the target and back to the receiver.
If the fired pulse is not received within a preselected period of time, the system registers "no hit". The firing continues until a "yes" answer is received, that is, a fired pulse has been returned to the receiver within the preselected period of time. This time period is analyzed by the conventional microprocessor within the simulator system in order to determine whether, in fact, the range was greater than 3,500 feet, less than 2,000 feet or between 3,500 feet and 2,000 feet.
If the range is between the latter (between 3,500 feet and 2,000 feet), appropriate ballistic information, which is also fed into the microprocessor, provides information which calculates the appropriate trajectory of a "bullet" for the particular range involved. This trajectory information is utilized in sending a signal to a beam deflector which allows for a subsequently fired "bullet" pulse to be emitted at the proper trajectory. The "bullet" pulse is also coded in such a manner so as to be recorded at the target as well as return a signal to the aircraft. If the returned "bullet" pulse is received by the receiver during the appropriate time interval, the simulator system of this invention records a "hit". If there is no reception, a "no" hit is recorded. The range information can be stored in the microprocessor each time the gun trigger is pressed. If required, the range can be stored for every bullet fired or every fifth bullet. The resolution of this type of storage will depend on the aircraft speed. For example, at 600 MPH if range is stored for every bullet fired, the range resolution will be approximately 10 feet and every fifth bullet will provide 50 feet resolution.
The gun simulator system of this invention can be utilized to realistically simulate air-to-ground strikes and air-to-air strikes. The targets are easily equipped with photodiode arrays and reflective material. By adding a non-pyrotechnique smoke charge to the target, an additional aircrew simulation is provided by actually seeing the target exhibit a type of visual cue associated with target damage when in fact struck by an appropriately coded "bullet" pulse.
In addition, the system of this invention can be easily made compatible with the Army's "Multiple Integrated Laser Engagement System." For each type of weapon, the associated laser is pulse coded and each person and target is equipped with a series of laser detectors mounted on a lightweight belt in the MILES concept. A code in the receiving system will respond to a hit by a weapon of sufficient size to cause damage or destruction.
It is therefore an object of this invention to provide a gun simulator system which is capable of producing accurate simulation based not only on range but also on ballistic trajectory.
It is a further object of this invention to provide a gun simulator system which is completely eyesafe.
It is another object of this invention to provide a gun simulator system which is readily adaptable for incorporation within an aircraft.
It is still a further object of this invention to provide a gun simulator system which is compatible with already existing gun simulator systems.
It is still another object of this invention to provide a gun simulator system which is economical to produce and which utilizes currently available components that lend themselves to standard mass producing manufacturing techniques.
For a better understanding of the present invention, together with other and further objects thereof, reference is made to the following description taken in conjunction with the accompanying drawing and its scope will be pointed out in the appended claims.
DETAILED DESCRIPTION OF THE DRAWING
FIG. 1 is a pictorial representation of an aircraft utilizing the gun simulator system of this invention and approaching and firing at a ground target;
FIG. 2 is a schematic representation of the gun simulator system of this invention; and
FIG. 3 is a schematic representation of the laser of the gun simulator system of this invention firing at a target.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A pictorial representation of the operaton of the gun simulator system 10 is shown in FIG. 1 of the drawing where an aircraft 12 is depicted firing at a ground target 14.
Reference is now made to FIG. 2 of the drawing, which represents in schematic fashion a block diagram of the gun simulator system 10 of this invention. The gun simulator system 10 is made up of six main components, (1) a transmitter 16, (2) a beam modulator 18, (3) a beam splitter 20, (4) a receiver 22, (5) a range counter 24, and (6) a microprocessor 26. In addition, a target 14 (shown in FIGS. 1 and 2 of the drawing) is utilized in conjunction with the gun simulator system 10 of this invention.
The gun simulator system 10 is readily adaptable for use within any conventional aircraft 12 or the like by being mounted in a pod (not shown) that would ordinarilly attach to the aircraft missile rail. If desired, simulator system 10 can be mounted on an external mount in which trigger inputs can be made available to fire transmitter 16. The transmitter 16 is self-contained and requires only normal aircraft voltages for operation and a "fire" command input. If desirable, a telescope could be mounted on transmitter 16 so that it can be easily boresighted.
For a clear and concise understanding of this invention the description set forth hereinbelow will set out with specificity the elements making up laser gun simulator system 10 of this invention.
Transmitter 16 is the form of a conventional laser with details thereof set forth hereinbelow. An essential consideration of the gun simulator system 10 of this invention is that the laser utilized within the invention be completely eye-safe. The Health, Education and Welfare (HEW) class criteria is defined by the Radiation Control Act of 1968, which sets the performance standards for the laser products. This standard is based around the amount of laser energy that the eye can withstand without damage. The Class I criteria is considered to be totally eyesafe even when the eye is continuously exposed for long periods.
According to the HEW standards, Class I acceptable emission limits for laser radiation is given hereinbelow.
For wavelength>400 nm but≦1400 nm and emission duration 1.0×10 -9 sec to 2×10 5 sec, the Class I accessible radiation limit is given by:
R=10K.sub.1 K.sub.2 t.sup.1/3 Joules/CM.sup.2 /Sr
where k 1 =10(λ-700)/515) for 800 nm to 1060 nm
where k 2 =1 for sampling internal t≦100 sec.
Thus, the selection of an eye-safe laser (transmitter 16) will be based on the following five (5) factors:
1. The power level
2. The pulse duration
3. The repetition rate
4. The wavelength
5. The beam width
Several different types of lasers will meet the above requirement. However, the GaAlAs laser is preferable with this invention due to its size, weight, simplicity of modulation, fast rise time, and cost. Secondly, the wavelength of the laser selected must be at a high quantum efficiency for the receiver selected.
GaAlAs lasers suitable for application with the gun simulator system 10 of this invention are available commercially from RCA, Laser Diode Lab etc. The fast rise time pulses are obtained by using an avalanche diode pulser for the laser. The pulser and laser integration unit is conventional and can be purchased commercially from American Laser Systems Inc., Meret, Power Technology, Inc., etc.
TYPICAL SPECIFICATIONS FOR TRANSMITTER 16
______________________________________Type of Laser GaAlAs______________________________________OpticalPeak Power 5 wattsWavelength 840 nm ± 20 nmPulse width 30 NS for range pulse 100 nm for "Bullet" PulseBeam Divergence 10 MR with 25 mm EFL Optics 2.5 MR with 100 mm EFL Optics 1.3 MR with 200 mm EFL OpticsBoresight Telescope 20X, Accuracy ± 0.5 Min.ElectricalRepetition Rate 10 KHzRisetime 10 nsec or lessDigital Input 10 KHz, 100 KΩ5vPower Consumption 2.5 watts______________________________________
Optically aligned with transmitter 16 is a beam deflecting means such as a conventional beam modulator 18 which is capable of establishing the initial beam direction and angle through which the laser pulses scan. In addition, modulator 18 establishes the "bullet" pulse direction in a manner to be described in detail hereinbelow.
Since mechanical modulators such as high speed gear drives are unacceptable with the instant invention, the appropriate modulator would be of the acousto-optical type. Such a modulator 18 scans pulses emanating from transmitter 16 by bending each beam of pulses over a preselected range of angles. The acousto-optical modulator 18 is made of an R.F. driver, a piezo-electric crystal and a beam deflector. The R.F. drive frequency is changed (50-150 MHz), which produces a variable space grating because of the change in the acoustic wavelength. The light is then defracted at a variable angle, which is a linear function of drive frequency. An instantaneous frequency change will cause a step in the beam position.
The resolution of an acousto-optic deflector is expressed in resolvable spots given by the equation: ##EQU1## where γ=Transmit time or flyback time. Δf=Sweep range of R.F. drive signal.
α=Constant determined by laser beam profile and the MTF required.
d=Laser beam dimension in the Bragg diffraction plane.
v=Acoustic velocity.
A typical acoustic-optic deflector fabricated from single crystal Tellurium dioxide (TeO 2 ) provides acoustic velocity 617 m/sec and for beam of 16.5×6 mm with Δf of 50 MHz at center frequency 100 MHz gives 1000 spot resolution. A typical R.F. driver contains a varactor-tuned oscillator, a fast-acting digitally controlled R.F. switch, and a Class-A power amplifier. The oscillator features good tuning linearity and fast show rate. The R.F. switch is TTL compatible and its switching time (rise time) is usually 5 nsec. The acousto-optic beam deflectors of this type can be obtained from Isomate Inc. and Harris Corporation, etc., as a standard off-the-shelf device.
Acousto-optical modulator 18 is capable of operation with both the initial "range" pulses as well as the "bullet" pulse. When the gun trigger initiating the operation of the gun simulator system 10 of this invention is pushed, the laser may not be pointed to target 14. Hence, modulator 18 will scan vertically to locate the target. At 3500 ft., if aircraft 12 is positioned correctly, the laser pulse will miss the target approximately 21 ft. Thus, the angle the modulator has to scan is only 6 mR. However, a typical modulator will scan 50 mR. Thus, the ranging information can be obtained, even if the aircraft approach elevation is not correct for the bullet hit on the target.
Once the ranging information is obtained, microprocessor 26 will provide ballistic information in order to deflect the laser beam correctly for the bullet drop trajectory over a particular range.
TYPICAL SPECIFICATIONS FOR MODULATOR 18
______________________________________OpticalAcoustic Medium TeO.sub.2Operation Wavelength 400-1100 nmOpticalTransmission 70% MinLaser Polarization RandomActive Aperture 4 mm × 50 mmScan Angle ± 1.5 degrees (50 mR)Scan Resolution ± 1 min.ElectricalTuning Characteristic Linear freq. vs. Tuning Voltage ± 1% linearityTuning Voltage + 4V to + 17VBandwidth f 50 MHzAccess Time 25 M SecR.F. Drive Power 2.5 Watts______________________________________
A conventional beam divider such as beam splitter 20 is optically aligned with modulator 18 so as to allow substantially all of the energy from the pulses emitted from laser transmitter 16 to pass therethrough as output 28 in the form of "range" pulses and "bullet" pulses. A small portion 30 (approximately 3%) of the energy of the pulses are redirected and utilized for initiating the operation of counter 24 in a manner to be set forth in detail hereinbelow.
Receiver 22 which is utilized within gun simulator system 10 of this invention, detects the incoming pulses 32 which reflect off target 14. This receiver 22 can be of a variety of types of detectors, such as, for example, (1) a PIN silicon diode, (2) an avalanche silicon diode and (3) a photomultiplier.
The selection of the detector or receiver 22 utilized in the gun simulator system 10 of this invention depends upon the speed, sensitivity, quantum efficiency, size-weight restrictions, as well as cost. However, the important parameter that describes the performance of receiver 22 is the signal to noise ratio.
The signal power incident on receiver 22 can be given by equation: ##EQU2## where P t =peak power of the source, watts.
T t =transmission through the transmitter (collimating) optics.
A r =receiver aperture area, m 2
T r =transmission through the receiver (collecting) optics.
R=transmitter to receiver range, m
θ T =transmitter beam width, radians
R t =reflectance from the target
ρ=atmospheric extinction coefficient, km -1
It may be noted that using a reflective coating and target 14 at 30 degrees, a small percentage of power will be reflected back to receiver 22.
The noise consists of the receiver noise (N) caused by the detector dark current and post-detector thermal noise depends on the characteristic of the detector. The background (B), is also very important. ##EQU3## where H.sub.λ =background spectral irradiance
F o =passband of the receiver filter
Ω r =receiver field of view
A r =receiver aperture area
T r =transmission through the receiver optics
R=transmitter to receiver range.
For error free operation of receiver 22, S>>B+N is required.
TYPICAL SPECIFICATION FOR RECEIVER 22
______________________________________Detective Type APD/Photomultiplier______________________________________OpticalClear Aperture: >4"Dia (8.1 × 10.sup.-3 m.sup.2)Field of View: 5-10 mRTransmission throughOptical System: >50%Optical band pass filter 10 nmWavelength sensitivity 800-900 nMElectricalRise time <10 nsecBandwidth >10 MhzDetector thermal noise <10 × 10.sup.-24 A/Hz______________________________________
A range counter 24 is interposed between beam splitter 20 and receiver 22. During operation, beam splitter 20 directs a portion of each pulse 28 as pulse 30 to counter 24 in order to indicate the emission of output "range" pulses 28 of gun simulator system 10 of this invention. Pulse 30 is fed through a conventional PIN silicon diode 34 to range counter 24. The reflected signal 32 from receiver 22 is also fed into range counter 24, the operation of which is described hereinbelow.
Range counter 24 performs the time-range measurements using standard components and provides wide dynamic range (500-5000 feet distance) and high resolution and accuracy (±2 feet). Range counter 24 receives a start signal from PIN silicon diode 34 (or, if desired, microprocessor 26) when gun simulator system operation begins, at, for example, the activation of a trigger. During operation of simulator 10, receiver 22 will not receive return pulse 32 from target 14 if output "range" pulse 28 misses target 14 or if target 14 is out of the range of transmitter 16 (laser). This range is established by microprocessor 26 at a preselected distance of, for example, 5000 feet. For example, if the "range" pulse is fired every 100 micro seconds and receiver 22 fails to receive a return pulse within 10 micro seconds (100 laser pulses at 10 KHz rate), the time between a start and stop signal at counter 24, microprocessor 26 will store a "no hit." Any returned pulses 32 received by receiver 22 will provide time information by way of counter 24 to microprocessor 26. Microprocessor 26 will analyze the time information in terms of distance, that is, the time required to start and stop counter 24 will determine distances greater than 3,500 feet, 3,500 to 2,000 feet, and less than 2,000 feet.
In addition, microprocessor 26 can analyze a conventional ballistic trajectory information program in order to establish if, in fact, a "range" pulse would be a hit if the trajectory of the bullet were taken into account. However, under normal operating conditions, microprocessor 26 sends a signal to modulator 18 with the appropriate trajectory information and thereby directs a "bullet" pulse from the system at the appropriate trajectory in a manner more fully described hereinbelow.
Microprocessor 26 which performs the above procedures is conventional and can be easily obtained by the ordering of, for example, a 8080A microprocessor. Such a microprocessor 26 is capable of analyzing data in terms of range information and trajectory information with the number of "no hits" and "hits" stored and displayed in a conventional display 36, if desired. This display may be mounted in the cockpit of aircraft 12.
A conventional CPU, a self-contained, single board microprocessor 26 which includes the central processor, system clock, RAM and ROM memories with I/O lines can be used in this application. These types of units provide six general purpose 8-bit registers, an accumulator, a 16-bit program counter and a 16-bit stack pointer register. The 16-bit program counter allows direct addressing of up to 64 K bytes of memory. The stack pointer controls addressing of an external stack located anywhere within the read/right memory. This type of Board Level Computers (BLC) can be provided with up to 4 K bytes read only memory in increments of 1 k.
Target 14 is of any conventional design but must be compatible with transmitter 16 (laser) of gun simulator system 10 of this invention. Hence, the reflectors 38 (shown in FIG. 1 of the drawing) of target 14 in order to be receptive to the laser pulses 28 of a laser meeting the Class I criteria are preferred to have one inch to three inch diameter plastic reflectors as well as glass corner reflectors. Photodetectors (not shown) mounted on target 14 will react to only "bullet" pulses and trigger a small non-pyrotechnique light strobe unit. Therefore, as the aircrew fires at target 14 they will receive visual cueing from the target and/or target area indicating their simulator projectile impacts. These strobe units can be set at a cycle rate that would provide the most suitable pilot visually related mental response; that is necessary because if the light response is as rapid as the actual voltage rate (100/seconds) it will appear as a continuous light.
MODE OF OPERATION
In operation, a gun trigger operably attached to microprocessor 26 is pushed or otherwise activated in order to initiate the action of gun simulator system 10. This is the only input required for the system operation. A variety of conventional programs are introduced into a microprocessor 26. These programs provide microprocessor 26 with range information (a correlation between output and return pulse time and range), ballistic trajectory information, (a relationship between bullet trajectory and range), and the desired approach angle of aircraft 12 (10° or 30°).
Initially, microprocessor 26 provides an R.F. generator 40 a correct frequency based upon this approach angle. The output signal 42 of R.F. generator 40 activates modulator 18 accordingly and thereby sets the initial output angle for output pulses 28. The initial activation of microprocessor 26 also sends a signal to commence the firing of "range" pulses 28 from transmitter 16.
As shown in FIG. 3 of the drawing the "range" pulses 28 are fired over a period of, for example, 10 msec (100 pulses) in a fan-like fashion. This scanning of pulses 28 is performed by modulator 18. In addition, each "range" pulse is utilized to start or reset range counter 24.
Beam splitter 20 placed in the optical path of the "range" pulses emanating from transmitter 16 provides a portion of the output pulse 28 as an input pulse 30 for each "range" pulse to PIN silicon photodiode 34 which starts counter 24. The range pulses 28 constitute the initial output of the gun simulator system 10 of this invention.
If a "range" pulse 28 is not returned or received by receiver 22 due to wrong approach (pulse did not hit target 14) or wrong range (greater than 5,000 feet), a "No" answer is recorded by microprocessor 26. Since 20 mm bullets are fired at a rate of 100 rounds per second through a Gatling gun there is a 10 msec time interval between two consecutive shots. In this time interval of the 10 ms, 100 laser "range" pulses 28 can be fired at a rate of 10 KHz. Thus, the laser "range" pulses will be fired at intervals of 100 msec., however, microprocessor 26 can be preset for any range distance. For the Class I laser, 5,000 feet preset distance appears appropriate.
If the returned "range" pulse 28 is not received by receiver 22 and there is no stop signal received by range counter 24 within 10 msec, the time required for a range pulse 28 to go 5,000 feet and back, range counter 24 will be waiting for another start pulse from PIN silicon diode 24. Hence, after 100 "No" answers from microprocessor 26 a "no hit" bullet has been fired.
If receiver 22 receives a "Yes" answer, that is, a returned "range" pulse 28 did in fact strike target 14 and returned to receiver 22, microprocessor 26 sorts out the range. If the range is greater than 3,500 feet or less than 2,000 feet once again a "no hit" is scored. However, if the range is between 3,500 feet and 2,000 feet, microprocessor 26 goes to the ballistic trajectory information program in order to obtain a correct bullet drop based on the range and approach angle. The appropriate R.F. frequency is sent to modulator 18 in order to set modulator 18 at the appropriate angle. At the same time, microprocessor 26 provides a "bullet" pulse signal 44 and transmitter 16 fires a "bullet" pulse at the appropriate angle. The "bullet" pulse resets counter 24 for a "bullet" pulse. If the "bullet" pulse hits target 14 and is received by receiver 22 within the appropriate time interval, microprocessor 26 scores a "hit". If the "bullet" pulse does not return a "no hit" is recorded by microprocessor 26. This information can be stored in microprocessor 26 for future display. The range information can be also stored in microprocessor 26 each time the gun trigger is pressed. If required, the range can be stored for every bullet fired or, for example, every fifth bullet. The resolution of this type of storage will depend on the aircraft speed. For example, at 600 MPH, if range is stored for every bullet fired the range resolution would be approximately 10 feet and every fifth bullet would provide 50 feet resolution.
As an alternative, microprocessor can in actuality make a comparison between range and trajectory of a "range" pulse and at that time determine whether or not a hit on target 14 has, in fact, been made. This can be accomplished without actually firing a "bullet" pulse. However, with such a determination the pilot would not be able to visually see on the ground a "hit" and would have to rely solely on microprocessor feedback.
By utilizing "bullet" pulses the system can be used to realistically simulate air-to-ground strike missions against live targets such as trucks, tanks, SAM AAA simulators, search radars, etc. Any ground target can be easily equipped with the photodiode array and reflective material. By adding a non-pyrotechnique smoke charge to the target, an additional aircrew stimulation is provided by actually seeing the target exhibit a type of visual tube associated with target damage.
In addition, the laser gun simulator system 10 of this invention can be easily made compatible with, for example, the Army's "Multiple Integrated Laser Engagement System." With such an arrangement, for each type of weapon, the associated laser is pulse coded and each person and weapon system is equipped with a series of laser detectors mounted on a lightweight belt within the concept. Each type of system has a code in its receiving system that would respond to a hit by a weapon of sufficient size to cause damage or destruction. For example, if a weapon of smaller size is fired against it, no damage or kill response is generated by receiver 22.
Although this invention has been described with reference to a particular embodiment, it will be understood to those skilled in the art that this invention is also capable of a variety of alternate embodiments within the spirit and scope of the appended claims. | A gun simulator system which is capable of safely simulating any airborne gun. The simulation takes into account not only aircraft approach angle but also preselected range and bullet trajectory. In so doing, the gun simulator system records hits both on the ground and in the aircraft for each pass. In addition, the simulator system is readily adaptable for use with already existing simulator programs. | 5 |
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