Including Plural Sequential Reaction Stages Patents (Class 422/134)
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Publication number: 20010019706Abstract: The present invention is directed to a method for polymerizing olefins in a multi-stage polymerization apparatus including a gas-phase polymerization reactor in a subsequent stage. By use of the present method, the composition of gas in the gas-phase reactor is easily adjusted, and moreover, a polymer having an intended composition is produced in a consistent manner. In one aspect, the method for polymerizing olefins is performed in successive, multiple stages by use of a plurality of polymerization reactors disposed in series which include at least one gas-phase polymerization reactor after a first reactor, wherein a multi-component gas is removed from a gas-phase reactor and pressurized and/or cooled to thereby liquefy a portion of the gas; at least a portion of gas is discharged; and the remaining gas and the liquid are returned to the gas-phase reactor.Type: ApplicationFiled: March 28, 2001Publication date: September 6, 2001Applicant: Idemitsu Petrochemical Co., Ltd.Inventors: Hideki Satou, Youichi Matsuo, Itaru Matsuhiro
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Patent number: 6274091Abstract: Multiple chemical reactions are performed in a plurality of reaction vessels mounted in inlets in a manifold valve block. The manifold valve block is connected to a channel block which is utilized in conjunction with a solvent delivery system as part of the reaction cycle. The solvent fluid is drained from the reaction vessels when valves in the manifold valve block are opened while applying a vacuum thereto. Optionally, a thermal block may be utilized in conjunction with the manifold valve block and the channel block to facilitate the reaction. Upon completion of the reactant cycle, the manifold valve block is disconnected from the channel block and connected to a cleavage block assembly which contains vials for collecting reaction products. The cleavage product is drained from the reaction vessels through the manifold valve block into the vials upon opening the valves in the manifold valve block and applying a vacuum to the channel block.Type: GrantFiled: March 29, 1999Date of Patent: August 14, 2001Assignee: Berlex Laboratories, Inc.Inventors: Raju Mohan, Brad O. Buckman, Michael M. Morrissey, Andrew I. Chitty, John T. Martin
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Patent number: 6274094Abstract: The simultaneous synthesis of diverse organic compounds is performed in stackable modules which are moveable among nesting sites located on work station platforms. The reactor module includes a heat transfer block adapted to receive an array of reactor vessels, preferrably in the form of solid phase extraction cartridges without sorbent, each with an outlet port. A plurality of valves are located below the vessels. The valves consist of rows of gang-controlled stopcocks which regulate the passage of fluids from the reactor vessel outlet ports into aligned channels, each formed by a pair of threated Leur tip adapters. The reactor module may be situated over a discharge module. The inlet openings in the discharge module accept the threaded ends of the Leur tip adapters. The discharge module may consist of a multi-well collector block or a drain block. An introduction module, which includes a pressure plate having an array of openings and a septum, may be received over the reactor module.Type: GrantFiled: December 16, 1997Date of Patent: August 14, 2001Inventors: Harold Norris Weller, III, Waldemar Ruediger, R. Michael Lawrence
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Patent number: 6267930Abstract: The simultaneous synthesis of diverse organic compounds is performed in stackable modules which are moveable among nesting sites located on work station platform. The reactor module includes a block adapted to receive an array of tube-like reactor vessels. The vessels are sized to optionally accept porus polyethelyene microcannisters with radio frequency transmitter tags. Each vessel has a bottom port connected to an outlet tube. A valve block located below the reactor vessels simultaneously controls discharge through the outlet tubes. The valves block includes plates with aligned, relatively moveable sets of rib surfaces which act through Teflon encapsulated silicone O-ring cord sections to simultaneously close rows of outlet tubes.Type: GrantFiled: May 24, 1999Date of Patent: July 31, 2001Inventors: Waldemar Ruediger, Wenjeng Li, John William Allen, Jr., Harold Norris Weller, III
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Patent number: 6264891Abstract: This invention provides an apparatus for preparing chemical libraries. The apparatus includes (1) a carousel comprising a plurality of reaction mounts having at least one reaction well; (2) a rotator that rotates the carousel step-wise; (3) a fluid delivery system; (4) a drain system; and (5) a programmable computer that controls the operation of the apparatus, including the rotator, the fluid delivery system, the drain system and other systems in the apparatus. The preparation of chemical libraries involves rotating the carousel through a plurality of stations. At each station, a physical step in a reaction protocol is carried out on the reaction wells of the mount docked at the station.Type: GrantFiled: May 18, 1999Date of Patent: July 24, 2001Assignee: EOS Biotechnology, Inc.Inventors: Herbert L. Heyneker, Kim D. Ha, David K. Steinmiller, Victor Simonyi
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Publication number: 20010007014Abstract: A process for producing polycarbonate designed to improve the quality of polycarbonate as a polymerization product polymer and reduce the investment and operating costs is provided.Type: ApplicationFiled: February 23, 2001Publication date: July 5, 2001Inventors: Takatoshi Kinoshita, Kazunori Harada, Seiji Motohiro
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Publication number: 20010005494Abstract: A process for carrying out a reaction on an organic feed (for example dimerisation, co-dimerisation, oligomerisation or metathesis of olefins) is described in which the catalyst is a catalytic metal compound dissolved in a non-aqueous ionic medium which is not or is only slightly miscible with hydrocarbons. The reaction is carried out in a system comprising at least two treatment loops each comprising at least one reaction zone and at least one zone for separating the organic and polar phases between which the polar medium containing the catalytic metal compound, and the organic phase circulate, in a counter-current, Fresh polar phase is injected into the second loop and used polar phase is eliminated from the first loop. The hydrocarbon to be transformed is injected into the first loop and the products are withdrawn from the second loop. The invention also concerns a unit for carrying out the process.Type: ApplicationFiled: February 9, 2001Publication date: June 28, 2001Applicant: Institut Francais Du PetroleInventors: Helene Olivier, Dominique Commereuc, Alain Forestiere, Francois Hugues
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Patent number: 6252016Abstract: A continuous process for preparing polymers is disclosed. The continuous process includes the steps of continuously feeding a reaction mixture containing a monomer into a non-cylindrical channel, continuously controlling the temperature of the non-cylindrical channel by exposing the surface of the non-cylindrical channel not exposed to the monomer to a temperature control medium, polymerizing the monomer in the non-cylindrical channel, and continuously removing the polymer from the non-cylindrical channel. The continuous process is suitable for the preparation of polymers containing ethylenically unsaturated monomers as polymerized units by emulsion polymerization, solution polymerization, and suspension polymerization.Type: GrantFiled: September 8, 1999Date of Patent: June 26, 2001Assignee: Rohm and Haas CompanyInventors: Richard Shu-Hua Wu, Jill Ann Wudarski, James Szkolnick Kempner
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Patent number: 6224832Abstract: Solid phase combinatorial synthesis is carried out in a multi-reactor synthesizer comprising an array of separate reactor cells (1-9) containing a solid reaction support medium (26). Subsets of the reactor cells (1-9) are interconnected with one another in a desired pattern, and, in a first reaction step, reagents (A, B, C) are circulated through the subsets. After the first reaction step is completed, the reactor cells (1-9) are rearranged into a new configuration of the subsets, and the same, or other, reagents (A, B, C) are circulated through the new subsets. The process can be repeated to produce large numbers of compounds differing from one another.Type: GrantFiled: November 20, 1998Date of Patent: May 1, 2001Assignee: SmithKline Beecham CorporationInventors: Michael Lee Moore, Dennis Shinji Yamashita
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Patent number: 6207115Abstract: The present invention concerns a process for the conversion of an olefinic C4 cut to polyisobutene and to propylene by metathesis. The process comprises three successive steps: (1) selective hydrogenation of diolefins with simultaneous isomerisation of 1-butene to 2-butenes, (2) polymerisation of the isobutene, including optional prior extraction of the isobutene, (3) metathesis of 2-butene with ethylene. Part or all of the C4 cut may originate from the metathesis of an olefinic C5 cut with ethylene after hydroisomerisation of the C5 cut. Application to C4 and C5 steam cracking cuts.Type: GrantFiled: November 30, 1998Date of Patent: March 27, 2001Assignee: Institut Francais Du PetroleInventors: Jean-Alain Chodorge, Dominique Commereuc, Jean Cosyns, Didier Duee, Bernard Torck
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Patent number: 6197264Abstract: A process for polymerization of olefin monomers by forming a fluid stream containing catalyst, continuously feeding the fluid stream into an elongated polymerization reactor having at least two successive chambers separated by dividing plates having a diameter slightly smaller than that of the polymerization rector, feeding monomers, and an optional catalyst and donor into the polymerization reactor under temperature conditions to polymerize the olefin while maintaining a mixed flow in the chambers to polymerize the monomers and optional comonomer in the fluid, and removing the resultant polymer slurry from the polymerization reactor.Type: GrantFiled: October 19, 1998Date of Patent: March 6, 2001Assignee: Borealis A/SInventors: Esa Korhonen, Pauli Leskinen, Ward Mennes, Fred Bergmann
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Patent number: 6168914Abstract: The invention provides a system and method for synthesizing chemicals onto supports in a parallel manner to produce a combinatorial collection of compounds. The system includes a plurality of middle plates, with each middle plate defining a plurality of reaction zones arranged in a two dimensional array. The reaction zones are adapted to receive a solid support, such as a sheet of membrane, and the middle plates are stackable on each other to form a three dimensional array of reaction zones. The system also includes a pair of end plates, where the middle plates are located between the end plates, and where the end plates include an array of fluid guides corresponding to the array of reaction zones, to allow for selective routing of reagents through the reaction zones.Type: GrantFiled: December 18, 1998Date of Patent: January 2, 2001Assignee: Glaxo Wellcome Inc.Inventors: David A. Campbell, Valery V. Antonenko, Harold E. Selick, Robert M. Gavin, Satoru Ida, Arthur H. Muir
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Patent number: 6162879Abstract: The present invention relates to a continuous process for polymerizing a vinyl monomer wherein a liquid reaction mixture flows through a tubular reactor equipped with a primary heat exchanger connected to a primary cooling loop where a primary coolant liquid circulates, optionally cooled by contact with a secondary heat exchanger fitted in the said primary loop and placed in a heat exchange zone of a secondary cooling device containing a secondary coolant liquid. The primary coolant liquid employed in the absence of a secondary cooling device or the secondary coolant liquid consists essentially of superheated water under pressure which produces low-pressure steam which preferably is recovered at least partly thermally or energetically.Type: GrantFiled: September 18, 1998Date of Patent: December 19, 2000Assignee: BP Chemicals LimitedInventor: Jean-Marc Galewski
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Patent number: 6140133Abstract: Provision is made, in a device and a process for the synthesis of macromolecules, for reagent solutions to be conveyed through reaction channels (15) which are connected to one another by intermediate channels (16, 17) and are preferably aligned parallel to one another, the reaction channels (15) being so displaced between individual synthesis steps relative to the carrier material acted on by the reagent solutions that, in the new position, the reaction channels (15) cover different synthesis zones from those in the previous position. In that manner provision is made for the synthesis of a large number of different sequences by relatively few synthesis steps.Type: GrantFiled: August 21, 1998Date of Patent: October 31, 2000Assignee: Novartis AGInventors: Raoul Bader, Michael Hinz, Hartmut Seliger, Robert Haener
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Patent number: 6139804Abstract: A process for producing a polyoxymethylene using a reactor having a discharging port having a weir, which process comprises introducing trioxane or a mixture of trioxane and a compound reactive therewith into the reactor from its feeding port and continuously recovering the powdery polyoxymethylene formed, from said discharging port having a weir. Owing to the presence of the weir, the residence time of reaction mixture in reactor is long, making high the conversion of the monomer.Type: GrantFiled: April 24, 1997Date of Patent: October 31, 2000Assignee: Asahi Kasei Kogyo Kabushiki KaishaInventors: Yukio Tanigawa, Hiromasa Matumoto
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Patent number: 6121054Abstract: A simple, efficient apparatus and method for separation of solid and liquid phases useful in methods of high-throughput combinatorial organic synthesis of large libraries or megaarrays of organic compounds is disclosed. The apparatus and method are useful, whether as part of an automated, robotic or manual system for combinatorial organic synthesis. In a preferred embodiment, an apparatus and method of removal of liquid phase from solid phase compatible with microtiter plate type array(s) of reaction vessels is disclosed.Type: GrantFiled: November 19, 1997Date of Patent: September 19, 2000Assignee: Trega Biosciences, Inc.Inventor: Michal Lebl
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Patent number: 6083682Abstract: The invention provides a system and method for synthesizing chemicals onto supports in a parallel manner to produce a combinatorial collection of compounds. The system includes a plurality of middle plates, with each middle plate defining a plurality of reaction zones arranged in a two dimensional array. The reaction zones are adapted to receive a solid support, such as a sheet of membrane, and the middle plates are stackable on each other to form a three dimensional array of reaction zones. The system also includes a pair of end plates, where the middle plates are located between the end plates, and where the end plates include an array of fluid guides corresponding to the array of reaction zones, to allow for selective routing of reagents through the reaction zones.Type: GrantFiled: December 19, 1997Date of Patent: July 4, 2000Assignee: Glaxo Group LimitedInventors: David A. Campbell, Valery V. Antonenko, Harold E. Selick
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Patent number: 6083697Abstract: Radiation-activated catalysts (RACs), autocatalytic reactions, and protective groups are employed to achieve a highly sensitive, high resolution, radiation directed combinatorial synthesis of pattern arrays of diverse polymers. When irradiated, RACs produce catalysts that can react with enhancers, such as those involved in autocatalytic reactions. The autocatalytic reactions produce at least one product that removes protecting groups from synthesis intermediates. This invention has a wide variety of applications and is particularly useful for the solid phase combinatorial synthesis of polymers.Type: GrantFiled: November 13, 1997Date of Patent: July 4, 2000Assignee: Affymetrix, Inc.Inventors: Jody E. Beecher, Martin J. Goldberg, Glenn H. McGall
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Patent number: 6066701Abstract: The present invention provides a method for substantially continuously polymerizing olefins comprising: introducing into a first reaction zone a fresh olefin polymerization catalyst; contacting said fresh olefin polymerization catalyst in said first reaction zone with a first vent mixture at a first feed rate and under conditions sufficient to form and avoid melting a polyolefin, wherein first vent mixture comprises unreacted olefins and a diluent vented from a second reaction zone; withdrawing a vent product of unreacted olefins and diluent from said first reaction zone; withdrawing from said first reaction zone a first product mixture comprising said catalyst and said polyolefin; passing said first product mixture to said second reaction zone; contacting said first product mixture in said second reaction zone with a second vent mixture at a second feed rate and under conditions sufficient to form and avoid melting said polyolefin, wherein said second vent mixture comprises a material selected from the groupType: GrantFiled: October 29, 1997Date of Patent: May 23, 2000Assignee: Exxon Chemical Patents Inc.Inventors: Russell John Koveal, James John McAlpin, Jeffrey Lawrence Brinen
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Patent number: 6045755Abstract: In a first embodiment, this invention includes an integrated robot apparatus for performing combinatorial chemistry synthesis protocols and having interchangeable work-stations, robot arm tools, and reaction vessels and reaction vessel arrays. The work-stations and tools are specialized to perform tasks necessary for the synthesis in a plurality of the reaction vessels grouped in a plurality of the reaction vessel arrays. Preferably, these elements function interchangeably because they have standardized sizes and conformation. The work-stations and tools include those for fluid dispensing or aspirating from individual reaction vessels or from all the reaction vessels in an array simultaneously. The reaction vessels can include, alternatively, stackable, ball-sealed reaction vessels, microtitre-like reaction vessel arrays, arrays of independent reaction vessels, valve-sealed reaction vessels, septum-sealed reaction vessels, and syringe reaction vessels.Type: GrantFiled: March 10, 1997Date of Patent: April 4, 2000Assignee: Trega Biosciences,, Inc.Inventors: Michael Lebl, Vit Pokorny, Viktor Krchnak
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Patent number: 6015880Abstract: A method and apparatus are provided for preparing a substrate upon which is located microdrop-sized loci at which chemical compounds are synthesized or diagnostic tests are conducted. The loci are formed by applying microdrops from a dispenser from which a microdrop is pulse fed onto the surface of the substrate.Type: GrantFiled: March 16, 1994Date of Patent: January 18, 2000Assignee: California Institute of TechnologyInventors: John D. Baldeschwieler, Ronald C. Gamble, Thomas P. Theriault
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Patent number: 6010667Abstract: A shaft reactor for treating bulk material, including granular bulk material, in particular for the continuous post-condensation of PET, PEN or PA in the solid phase. A uniform product flow without significant decrease of the usable contents of the reactor and a decrease of the bulk pressure in the reactor is achieved by use of internals which are uncomplicated to fabricate. Internals are arranged in the reactor which comprise at least one ring and a plurality or ribs.Type: GrantFiled: February 6, 1996Date of Patent: January 4, 2000Assignee: Buehler AGInventors: Markus Meyer, Camille Borer, Bernd Kuehnemund, Martin Mueller
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Patent number: 5955029Abstract: Disclosed are devices for amplifying a preselected polynucleotide in a sample by conducting a polynucleotide polymerization reaction. The devices comprise a substrate microfabricated to define a sample inlet port and a mesoscale flow system, which extends from the inlet port. The mesoscale flow system includes a polynucleotide polymerization reaction chamber in fluid communication with the inlet port which is provided with reagents required for polymerization and amplification of a preselected polynucleotide. In one embodiment the devices may be utilized to implement a polymerase chain reaction (PCR) in the reaction chamber (PCR chamber).Type: GrantFiled: March 12, 1996Date of Patent: September 21, 1999Assignee: Trustees of the University of PennsylvaniaInventors: Peter Wilding, Larry J. Kricka
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Patent number: 5929208Abstract: A self-addressable, self-assembling microelectronic device is designed and fabricated to actively carry out and control multi-step and multiplex molecular biological reactions in microscopic formats. These reactions include nucleic acid hybridization, antibody/antigen reaction, diagnostics, and biopolymer synthesis. The device can be fabricated using both microlithographic and micro-machining techniques. The device can electronically control the transport and attachment of specific binding entities to specific micro-locations. The specific binding entities include molecular biological molecules such as nucleic acids and polypeptides. The device can subsequently control the transport and reaction of analytes or reactants at the addressed specific micro-locations. The device is able to concentrate analytes and reactants, remove non-specifically bound molecules, provide stringency control for DNA hybridization reactions, and improve the detection of analytes. The device can be electronically replicated.Type: GrantFiled: October 4, 1996Date of Patent: July 27, 1999Assignee: Nanogen, Inc.Inventors: Michael J. Heller, Eugene Tu
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Patent number: 5853567Abstract: A method for reducing the viscosity of a liquid heavy hydrocarbon feedstock comprising the steps of bringing said feedstock to a temperature capable of cracking of at least a portion of the hydrocarbons present in said feedstock and introducing said feedstock into a bottom portion of a maturation device (i.e. a "soaker"), where the feedstock is displaced from the bottom upwards, to get evacuated from a top portion of the soaker towards a fractioning unit. The invention also relates to an apparatus comprising a soaker in which are located, transversely to the direction of displacement of the feedstock to be treated, a plurality of annular discs spaced apart from one another, each disc comprising a circular central passage substantially coaxial to the soaker, the treated feedstock circulating from the bottom portion upwards in the soaker through the central passages of the various annular discs.Type: GrantFiled: December 4, 1996Date of Patent: December 29, 1998Assignee: Total Raffinage Distribution, S.A.Inventors: Luc Gouzien, Elisabeth Mouchot, Pierre Lutran, Marc Persing
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Patent number: 5851494Abstract: A solid phase synthesis reaction vessel includes a vessel with a first inlet, a second inlet, and an outlet. A first stopcock is disposed within the first inlet and a second stopcock is disposed within the outlet. Solid phase material is prevented from escaping the reaction vessel via the outlet while allowing fluid to flow through the outlet by a frit. In one embodiment, the reaction vessel includes an outer hollow shell surrounding the vessel to allow cooling or heating fluid to flow therein for controlling the temperature in the interior reaction volume. The solid phase synthesis reaction vessel provides for the independent opening and closing of each of the inlets and outlet to provide for various ways of draining the vessel, varying the conditions within the vessel, and/or adding additional materials into the vessel.Type: GrantFiled: September 4, 1997Date of Patent: December 22, 1998Assignee: Pharmacopeia, Inc.Inventors: Lawrence W. Dillard, Ian Henderson, Michael H. J. Ohlmeyer, John C. Reader
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Patent number: 5846396Abstract: The present invention provides a liquid distribution system, which is useful in a number of contexts, including in accomplishing various synthetic, diagnostic and drug screening reactions. The distribution system can comprise an alpha reservoir and a beta reservoir, a first set of parallel and adjacent first and second feeder channels and a second set of parallel and adjacent third and fourth feeder channels which are offset from the first and second feeder channels, wherein (a) the first and third feeder channels are connected to the alpha reservoir via a first connector channel that is situated above or below the second and fourth feeder channels and are independent of the beta reservoir and (b) the second and fourth feeder channels are connected to the beta reservoir via a second connector channel that is situated above or below the first and third feeder channels and are independent of the alpha reservoir. The distribution system is preferably a microscale distribution system.Type: GrantFiled: November 9, 1995Date of Patent: December 8, 1998Assignee: Sarnoff CorporationInventors: Peter John Zanzucchi, Satyam Choudary Cherukuri, Sterling Edward McBride, Robert R. Demers, Aaron W. Levine, Barry Jay Thaler, Robert Leon Quinn, Paul Leonard Braun, William Chiang, Zhonghui Hugh Fan, Steven A. Lipp, James R. Matey
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Patent number: 5833930Abstract: For the expansion of a liquid containing gas under pressure in dissolved form, it is proposed that the liquid be passed with expansion through an extended flow channel with a small cross-sectional measurement with generation of high rates of shear. The velocity of the liquid is then reduced prior to the foaming.Type: GrantFiled: February 6, 1997Date of Patent: November 10, 1998Assignees: Maschinenfabrik Hennecke GmbH, Bayer AktiengesellschaftInventors: Hans-Michael Sulzbach, Ferdinand Althausen, Herbert Steilen, Reiner Raffel, Robert Eiben, Wilfried Ebeling
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Patent number: 5820829Abstract: A hand-operated polymerizer for the polymerization of synthetic materials, such as dental plastics. The polymerizer has a housing in which a light source and a fan are disposed, and which includes a light-emitting opening for emitting the light generated by the light source. The housing contains openings for permitting cooling air to enter the housing and for allowing heated air to exit the housing. In order to prevent the operator of the polymerizer from being impaired by heated air when operating the polymerizer, at least one air-conducting member is provided, wherein the position of the air-conducting member is changeable relative to the housing.Type: GrantFiled: July 12, 1996Date of Patent: October 13, 1998Assignee: Heraeus Kulzer GmbHInventors: Dieter Schodel, Steffen Oppawsky
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Patent number: 5807525Abstract: An apparatus and process are disclosed for optimizing the repetitive steps in a solid-phase oligonucleotide synthesis by continuous optical scanning of the effluent stream from the reaction module and by computerized processing and implementation of the scanning data.Type: GrantFiled: February 29, 1996Date of Patent: September 15, 1998Assignee: Hybridon, Inc.Inventors: Stephen Allen, Hubert Koster, Edward Ashare, Donald W. Euwart, Jennifer Fernandes
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Patent number: 5792430Abstract: A solid phase organic synthesis device comprising a manifold and an optional heating block mounted to an upper surface of the manifold. The manifold includes an internal cavity and a first array of holes coupled to the internal cavity. The heating block includes a second array of holes vertically aligned with the corresponding holes of the first array. The first and second arrays of holes are adapted to accommodate flow-through reaction vessels. Each reaction vessel is secured in one of the holes of the first array and a vertically-aligned one of the holes of the second array. The interiors of the reaction vessels are in communication with the internal cavity of the manifold. The flow-through reaction vessels, which contain solid phase resins for solid phase organic synthesis, are controlled by regulating the pressure within the manifold.Type: GrantFiled: July 25, 1997Date of Patent: August 11, 1998Assignee: Monsanto CompanyInventor: Bruce C. Hamper
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Patent number: 5792431Abstract: Solid phase combinatorial synthesis is carried out in a multi-reactor synthesizer comprising an array of separate reactor cells containing a solid reaction support medium. Subsets of reactor cells are interconnected with one another in a desired pattern, and, in a first reaction step, reagents are circulated through the subsets. After the first reaction step is completed, the reactor cells are rearranged into a new configuration of subsets, and the same, or other, reagents are circulated through the new subsets. The process can be repeated to produce large numbers of compounds differing from one another.Type: GrantFiled: May 30, 1996Date of Patent: August 11, 1998Assignee: SmithKline Beecham CorporationInventors: Michael L. Moore, Dennis Yamashita
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Patent number: 5779977Abstract: Apparatus and method for performing a nucleic acid amplification reaction and preferably a polymerase chain reaction (PCR) in a reaction mixture in at least one capillary tube. Several different embodiments are disclosed. One embodiment cycles a sample through a capillary tube loop passing through two thermostatted fluid baths. Another embodiment has the capillary tube routed alternatingly between two heat exchangers to that the sample makes only one pass through the tube. Other embodiments maintain the heat exchangers stationary and translate the samples between them. Still further embodiments maintain the samples stationary and either automatically translate or rotate the heat exchangers past the samples contained within the capillary tubes to perform the thermal cycles necessary for the amplification reaction.Type: GrantFiled: March 26, 1997Date of Patent: July 14, 1998Assignee: The Perkin-Elmer CorporationInventors: Lawrence A. Haff, Enrico Picozza, Will Bloch, Timothy M. Woudenberg
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Patent number: 5762881Abstract: An apparatus for multiple, simultaneous synthesis of compounds. The apparatus includes a reaction block having a heating layer, a cooling layer, each of which may perform both functions, and a collection sump. A plurality of reaction tubes are supported in the reaction block in a matrix. Each reaction tube has a top outlet, a bottom outlet and a filter above the bottom outlet. Spool valves are located to control the bottom outlets of the reaction tubes. Obturators are provided to close the top outlets of the reaction tubes and to provide venting for the reaction tubes. The collection sump alternately may be equipped with individual collection tubes for each reaction tube. Each reaction tube is formed with a restrictive waist and protrusions arranged in a pattern between the waist and its bottom outlet to improve the mixing of the resinous solid supports by creating turbulence. The restrictive waist limits the height of the vortex of solution during mixing and reaction to facilitate heating and refluxing.Type: GrantFiled: October 29, 1996Date of Patent: June 9, 1998Assignee: Bohdan Automation, Inc.Inventors: James R. Harness, Larry W. Markus, Tadeusz J. Wozny, Albert T. Grzybowski, Andrew J. Grzybowski, Richard D. Kanowske, Thomas Drehobl, Rudy H. Haidle, Kenneth R. Kaufhold
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Patent number: 5753190Abstract: The present invention discloses a polymerization system having at least two reaction chambers wherein vacuum is used to remove vapors therefrom comprising a single vacuum system for supplying vacuum in increasing amounts to successive reaction chambers. Also disclosed is a polymerization process having at least first and second reaction chambers in which the pressure is decreased successively from said first chamber to a final chamber.Type: GrantFiled: July 21, 1995Date of Patent: May 19, 1998Assignee: Eastman Chemical CompanyInventors: Douglas M. Haseltine, Thomas L. Yount, Jimmy L. Ryans
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Patent number: 5746982Abstract: Apparatus for the synthesis of chemical compounds consists of a housing having a top, front, side and rear walls surrounding and enclosing a reaction table. A track on the rear wall of the housing carries a pair of extending arms on each of which is movably mounted a vertically extendible probe for positioning at various locations over the reaction table. At least on control syringe communicates between the probe and containers for system fluids. A programmable controller is provided for control of the syringe and probes. A reaction block on the reaction table consists of a body having an upper portion and a lower portion and an upper and lower surface and a multiplicity of reaction wells for carrying out the synthesis. Each reaction well is closed at its lower end and open to the upper surface. A flushing conduit is located adjacent each of the well and is in fluid communication with the closed lower end of the reaction well.Type: GrantFiled: February 29, 1996Date of Patent: May 5, 1998Assignee: Advanced ChemTech, Inc.Inventors: Hossain Saneii, Mohammad R. Boroomand, Michael R. Ferriell
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Patent number: 5744102Abstract: Solid phase synthesizer and method of use for synthesis of a polymer. The synthesizer has a generally horizontal elongated vessel for holding a solid support and liquid having two ends, each end having a porous blocker to prevent the solid support from leaving the vessel but allowing passage of the liquid from the vessel. A particulate solid support is held within the vessel and has a size sufficient to prevent passage through the blocker.Type: GrantFiled: January 30, 1996Date of Patent: April 28, 1998Assignee: Chugai Biopharmaceuticals, Inc.Inventor: James Scott Eadie
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Patent number: 5744101Abstract: A synthetic strategy for the creation of large scale chemical diversity. Solid-phase chemistry, photolabile protecting groups, and photolithography are used to achieve light-directed spatially-addressable parallel chemical synthesis. Binary masking techniques are utilized in one embodiment. A reactor system, photoremovable protective groups, and improved data collection and handling techniques are also disclosed. A technique for screening linker molecules is also provided.Type: GrantFiled: February 14, 1995Date of Patent: April 28, 1998Assignee: Affymax Technologies N.V.Inventors: Stephen P. A. Fodor, Lubert Stryer, James L. Winkler, Christopher P. Holmes, Dennis W. Solas
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Patent number: 5738829Abstract: A process and apparatus for the cleavage and deprotection of newly synthesized oligonucleotides from solid supports, which involves incubating the solid support in an environment comprising gaseous cleavage/deprotection reagent such as gaseous ammonia or ammonium hydroxide vapors. The method lends itself well to the use of supports such as microtiter plates, that can be used to simultaneously perform up to 96 individual synthetic processes.Type: GrantFiled: February 15, 1996Date of Patent: April 14, 1998Assignee: Barrskogen, Inc.Inventor: Tomas Kempe
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Patent number: 5733509Abstract: A plurality of oligonucleotides are synthesized at a plurality of locations on a substrate using a plurality of dispensing bars. Each of the plurality of dispensing bars has a respective plurality of dispensing heads arranged along a respective axis. Each of the plurality of dispensing bars is operative to selectively deposit a volume of a respective one of a plurality of nucleotide bases in any of a row of locations. A positioning mechanism positions the substrate with respect to the plurality of dispensing bars. A controller controls the plurality of dispensing bars and the positioning mechanism so that, at each of the plurality of locations, a respective sequence of nucleotide bases is deposited to form a respective oligonucleotide.Type: GrantFiled: April 17, 1996Date of Patent: March 31, 1998Assignee: Motorola, Inc.Inventors: Donald E. Ackley, Chan-Long Shieh, Thomas B. Harvey, III
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Patent number: 5720923Abstract: Apparatus and method for performing a nucleic acid amplification reaction and preferably a polymerase chain reaction (PCR) in a reaction mixture in at least one capillary tube. Several different embodiments are disclosed. One embodiment cycles a sample through a capillary tube loop passing through two thermostatted fluid baths. Another embodiment has the capillary tube routed alternatingly between two heat exchangers to that the sample makes only one pass through the tube. Other embodiments maintain the heat exchangers stationary and translate the samples between them. Still further embodiments maintain the samples stationary and either automatically translate or rotate the heat exchangers past the samples contained within the capillary tubes to perform the thermal cycles necessary for the amplification reaction.Type: GrantFiled: August 31, 1994Date of Patent: February 24, 1998Assignee: The Perkin-Elmer CorporationInventors: Lawrence A. Haff, Enrico Picozza, Will Bloch, Robert Ragusa, Joseph DiCesare, David Tracy, Paul Saviano, Timothy M. Woudenberg
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Patent number: 5677195Abstract: A method and device for forming large arrays of polymers on a substrate (401). According to a preferred aspect of the invention, the substrate is contacted by a channel block (407) having channels (409) therein. Selected reagents are delivered through the channels, the substrate is rotated by a rotating stage (403), and the process is repeated to form arrays of polymers on the substrate. The method may be combined with light-directed methodolgies.Type: GrantFiled: November 20, 1992Date of Patent: October 14, 1997Assignee: Affymax Technologies N.V.Inventors: James L. Winkler, Stephen P. A. Fodor, Christopher J. Buchko, Debra A. Ross, Lois Aldwin, Douglas N. Modlin
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Patent number: 5651943Abstract: An apparatus and method are provided for the synthesis of compounds, e.g., oligomers or polymers, by the repeated steps of coupling various subunits onto solid supports. The apparatus has for a first member a vessel having chambers opening to a surface of the member, and has for a second member a vessel having a single chamber opening to a surface of the second member. The chambers preferably have filtered apertures to permit passage of gas or liquid while retaining the solid supports in the chambers. The first member is joined with the second member, forming a pair, such that the openings of the first member open into the second member. The first member is used for synthesis reactions and for holding unmixed compounds coupled to solid supports. The second member is used for mixing the solid supports. The solid supports are transferred from one member to another, e.g., by inverting the pair.Type: GrantFiled: July 11, 1994Date of Patent: July 29, 1997Assignee: Arizona Board of Regents, on behalf of the University of ArizonaInventors: Kit Sang Lam, Sydney E. Salmon
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Patent number: 5643970Abstract: For the expansion of a liquid containing gas under pressure in dissolved form, it is proposed that the liquid be passed with expansion through an extended flow channel with a small cross-sectional measurement with generation of high rates of shear. The velocity of the liquid is then reduced prior to the foaming.Type: GrantFiled: December 14, 1995Date of Patent: July 1, 1997Assignees: Maschinenfabrik Hennecke GmbH, Bayer AktiengesellschaftInventors: Hans-Michael Sulzbach, Ferdinand Althausen, Herbert Steilen, Reiner Raffel, Robert Eiben, Wilfried Ebeling
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Patent number: 5643738Abstract: Methods are provided for synthesizing a plurality of compounds in parallel. The methods use cross-over channels for moving samples from a reservoir of starting materials into a plurality of wells. The movement is achieved, for example, using an electrokinetic pump.Type: GrantFiled: May 31, 1995Date of Patent: July 1, 1997Assignee: David Sarnoff Research Center, Inc.Inventors: Peter John Zanzucchi, Satyam Choudary Cherukuri, Sterling Edward McBride, Amrit Kaur Judd
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Patent number: 5641459Abstract: A machine for synthesizing oligonucleotides has individual pumping modules for connection to each of a number of different monomers and to other fluids used in the synthesizing process. Each pumping module includes a pump and a three-port/three-way valve with the first inlet port connected to receive the fluid, and the second port connected to receiving a flushing agent, such as acetonitrile. A valving arrangement downstream from the pumping modules selects a monomer. The selected monomer and other fluids pass through flow sensors which provides signals to a controller, which uses these signals to regulate the pumping of the pumps. At least some of the valves allow multiple inlet ports to be kept open at the same time, thus allowing certain of the liquids to be mixed within the valves. The various pumps, valves and sensors are mounted to the exterior of a cabinet and arranged such that the liquid handling portions are exterior to the cabinet, while electrical portions are within the cabinet.Type: GrantFiled: August 17, 1995Date of Patent: June 24, 1997Assignee: Pharmacia Biotech ABInventor: Lars Holmberg
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Patent number: 5624711Abstract: Methods and derivatized supports which are useful in solid-phase synthesis of peptides, oligonucleotides or other small organic molecules as well as arrays of ligands. The methods provide means to control the functional site density on a solid support. Some of the derivatized supports are polymer-coated or glycan-coated. Other methods for regenerating the surface of a used ligand array are also provided.Type: GrantFiled: April 27, 1995Date of Patent: April 29, 1997Assignee: Affymax Technologies, N.V.Inventors: Steven A. Sundberg, David Fujimoto
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Patent number: 5599507Abstract: A polycondensation reactor for processing low viscosity polyester or another polymer into relatively highly viscosity polymer comprises a substantially cylindrical horizontal reactor vessel with a polymer inlet and a polymer outlet adjacent its opposite ends and a vapor exhaust opening in the upper side of the vessel at its outlet end. A polymer agitator is rotated axially within the chamber and includes plural alternating annular overflow and underflow baffles and multiple perforated film-forming screens disposed therebetween in parallel spaced relation to one another. The overflow baffles are in peripheral polymer-sealing relation to the vessel while the underflow baffles have multiple underflow recesses in their outer peripheries, whereby the baffles define a tortuous polymer flow path alternately through their respective polymer overflow and underflow openings to control residence time, distribution and viscosity growth as the polymer flows between the baffles.Type: GrantFiled: November 9, 1994Date of Patent: February 4, 1997Inventors: Gordon Shaw, Rainer A. Schaller, W. Jeffrey Stikeleather, Michael D. Melton, Harmut Hey, Roland Schmidt, Rolf Hartmann, Hans Lohe
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Patent number: 5580523Abstract: A modular reactor system and method for synthesizing chemical compounds characterized by a uniform temperature throughout the reaction mixture by use of a continuous flow reactor under high pressure. The apparatus includes a number of generic components such as pumps, flow channels, manifolds, flow restrictors, and valves. Modular reactors, separator and analyzers on an assembly board provide a system where a modular reactor unit has an I.D. of up 100 .mu.m to optimize control of residence time within a reaction zone.Type: GrantFiled: April 1, 1994Date of Patent: December 3, 1996Inventor: Allen J. Bard
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Patent number: 5565175Abstract: An apparatus and method for producing ethylene polymer are provided which employ a conduit in the form of a closed loop (i.e. loop reactor) for receiving a flow of a monomer which includes ethylene, a polymerization catalyst and a diluent therethrough for the polymerization of the monomer to ethylene polymer. The conduit comprises at least one pipe constructed of rolled plate around which coolant fluid passes in heat exchange relationship.Type: GrantFiled: October 1, 1990Date of Patent: October 15, 1996Assignee: Phillips Petroleum CompanyInventors: John D. Hottovy, Frederick C. Lawrence, Barry W. Lowe, James S. Fangmeier